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Delta V Series

Isotope Ratio Mass Spectrometers

Operating Manual

1174000 Revision E November 2018


Delta V Series
Isotope Ratio Mass Spectrometers

Operating Manual

1174000 Revision E November 2018


Legal Notices
© 2018 Thermo Fisher Scientific Inc. All rights reserved.

Original Operating Instructions


Excel, Microsoft and Windows are registered trademarks of Microsoft Corporation in the United
States and other countries.

The following are registered trademarks in the United States and possibly other countries: HiPace is a
registered trademark of Pfeiffer Vacuum Technology AG. Pertinax is a registered trademark of Dr.
Dietrich Müller GmbH. Swagelok is a registered trademark of the Swagelok Company. Teflon and
Viton are registered trademarks of E. I. du Pont de Nemours & Co.

All other trademarks are the property of Thermo Fisher Scientific Inc. and its subsidiaries.

Thermo Fisher Scientific Inc. does not endorse any manufacturer or products other than its own.
Unless otherwise stated, companies and products listed in this document are given as examples only.

Thermo Fisher Scientific Inc. provides this document to its customers with a product purchase to use
in the product operation. This document is copyright protected and any reproduction of the whole or
any part of this document is strictly prohibited, except with the written authorization of Thermo
Fisher Scientific Inc.

Release History: Revision A released in August 2005.


Revision B released in May 2011.
Revision C released in March 2016.
Revision D released in August 2017.
Revision E released in November 2018.
C
Contents
Chapter 1 Using this Manual .................................................................1-1
About this Manual ......................................................... 1-1
Typographical Conventions ........................................... 1-2
Signal Words............................................................... 1-2
Viewpoint Orientation................................................ 1-2
Data Input .................................................................. 1-2
Topic Headings........................................................... 1-3
Reference Documentation.............................................. 1-4
Contacting Us................................................................ 1-6

Chapter 2 Scope of Delivery ..................................................................2-1


Standard System Components ....................................... 2-2
Optional System Components ....................................... 2-2

Chapter 3 System Description ...............................................................3-1


Basic Instrument ............................................................ 3-2
Differences between Delta V Advantage MS and
Delta V Plus MS ............................................................ 3-3
Front View..................................................................... 3-4
Mounting and Removing the Side Panels.................... 3-5
Control Panel................................................................. 3-6
The LEDs at the Control Panel................................... 3-7
Plug and Measure Concept ............................................ 3-9
Grounding Cable for Peripherals............................... 3-11
Configurating Plug and Measure Devices.................. 3-11
Connections at the Rear Panel ..................................... 3-12
Power Supply Panel .................................................. 3-13
Right Side and Dual Inlet System Cabinet ................... 3-19
Turbomolecular Pump of the Dual Inlet System....... 3-21
Pressure Reducer for Compressed Air........................ 3-22
Fore Vacuum Pumps................................................. 3-23
Heat and Exhaust Gas Removal ................................ 3-25
Additional Valve ....................................................... 3-26
Dual Inlet Board ....................................................... 3-28
Microvolume Cabinet .................................................. 3-29
Power Sockets and Plugs ........................................... 3-30
Position of Microvolume and Autocool Unit ............ 3-31
Ion Source Cabinet ...................................................... 3-32
Arrangement of Amplifiers ........................................ 3-33
Assignment of Amplifiers to Cups............................. 3-34
Analyzer Cabinet.......................................................... 3-35

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) i


Contents

Three-Way Valve and Check Valve........................... 3-36


Turbomolecular Pumps of the Analyzer .................... 3-37
Working Principle of the Turbomolecular Pumps..... 3-38
Analyzer .................................................................... 3-39
Analyzer Heater......................................................... 3-42
Ion Source................................................................. 3-43
Ion Generation.......................................................... 3-45
Trap Current and Box Current ................................. 3-46
Lenses ....................................................................... 3-47
Collector Systems...................................................... 3-48
Amplifiers and VFCs................................................. 3-55
Arrangement of Several Amplifiers ............................ 3-57
Electromagnet ........................................................... 3-59
Electronics Cabinet ...................................................... 3-60
Focus Quad Power Supply Board.............................. 3-60
Power Supply for Amplifiers and VFC ...................... 3-61
Power Distribution Board ......................................... 3-61
Electronic Components for Data Acquisition............ 3-63
Grounding of the Delta V Series Instrument............. 3-63

Chapter 4 Dual Inlet System (Optional) ............................................... 4-1


Layout of the Dual Inlet System..................................... 4-2
Working Principle of the Dual Inlet System................... 4-4
Valves of the Dual Inlet System...................................... 4-5
Parts of a Valve ........................................................... 4-5
Arrangement in Valve Blocks ...................................... 4-6
Manifold Block with Solenoid Valves.......................... 4-7
Compressed Air Distributor ........................................... 4-8
Changeover Valve .......................................................... 4-8
Layout of the Changeover Valve.................................. 4-8
Operating Pneumatic Valves ..................................... 4-10
Connecting Dual Inlet Peripherals Using Stainless
Steel Capillaries......................................................... 4-10
Connecting Dual Inlet Peripherals Using Nickel
Capillaries ................................................................. 4-11
Changeover Extension.................................................. 4-12
Multiport ..................................................................... 4-12
Dismantling the Multiport........................................ 4-13
TubeCracker ............................................................. 4-14
Reference Gas Refill .................................................. 4-14
Microvolume ............................................................... 4-15
Autocool Unit ........................................................... 4-17
Autocool Refill Device ................................................. 4-19
Working Principle..................................................... 4-20
Refill Tube for Liquid Nitrogen ................................ 4-20
Protective Tube for Fill Level Controller................... 4-20

ii Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific


Contents

Chapter 5 Safety .......................................................................................5-1


Safety Symbols and Signal Words in This Manual ......... 5-2
Observing This Manual .............................................. 5-2
Safety Symbols on the Instrument.................................. 5-3
Rating Plate.................................................................... 5-6
Intended Use.................................................................. 5-7
Qualification of the Personnel..................................... 5-8
Permitted Materials..................................................... 5-8
Electric Safety Precautions ............................................. 5-9
Safety Instructions for Wearers of Medical Implants .... 5-10
In Case of Emergency .................................................. 5-11
Residual Hazards.......................................................... 5-12
Safety Instructions for the Autocool Unit.................. 5-13
Personal Protective Equipment ................................. 5-13

Chapter 6 System Setup..........................................................................6-1


Laboratory Conditions ................................................... 6-2
Power Supply .............................................................. 6-2
Gas Supply.................................................................. 6-3
Temperature ............................................................... 6-5
Air Conditioning System............................................. 6-5
Humidity .................................................................... 6-6
Exhaust System ........................................................... 6-6
Floor and Vibration .................................................... 6-6
Radio Frequencies ....................................................... 6-7
Magnetic Fields........................................................... 6-7
System Preparation ........................................................ 6-7
Placing the Instrument................................................ 6-7
Preparing the Pumping System ................................. 6-12
Connecting the Computer to the IRMS.................... 6-13
Connecting Peripherals to the IRMS......................... 6-13
Creating an Isodat Backup ........................................... 6-14
Starting Isodat the Very First Time .............................. 6-17
Creating a Gas Configuration ...................................... 6-20
Creating a Configuration ............................................. 6-25
Source Heater .............................................................. 6-28
Calibrating and Adjusting the System .......................... 6-29
Checking the Vacuum............................................... 6-30
Introducing Gas into the Continuous Flow System... 6-32
Introducing Gas into the Dual Inlet System.............. 6-33
High Voltage Supply - Adjusting Potentials .............. 6-37
Magnet Steps and Mass Selection.............................. 6-39
Magnet Calibration................................................... 6-39
Mass Calibration ....................................................... 6-41
Jump Calibration for Elemental Analyzer
Applications .............................................................. 6-48
Peak Shapes............................................................... 6-50
Peak Center Scan ...................................................... 6-52

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) iii
Contents

Peak Center Offset .................................................... 6-57


Electronic Offset ....................................................... 6-59
Crimp Adjustment .................................................... 6-60
Calibrating the Bellows ............................................. 6-61
Focus Settings of the IRMS....................................... 6-66
Auto Focusing........................................................... 6-70
Manual Focusing - Tune Scan................................... 6-71
Resetting the Mass Spectrometer.................................. 6-73

Chapter 7 Operation ................................................................................ 7-1


Safety Guidelines for Operation ..................................... 7-2
Isodat Software Suite...................................................... 7-2
Starting Up the Instrument ............................................ 7-4
Shutting Down the Instrument ...................................... 7-5
Creating a New Method................................................. 7-6
Creating a New Sequence and Starting Acquisition........ 7-9
²H/¹H Measurements .................................................. 7-13
Determining the H3 Factor ....................................... 7-13
Creating a Method for H3 Factor Determination ...... 7-14
Creating a Sequence for H3 Factor Determination
and Starting Acquisition............................................ 7-16
Dual Inlet System ........................................................ 7-18
Switching Positions of the Changeover Valve............ 7-19
Changeover Valve in Dual Inlet Measurement .......... 7-20
Shot Noise Limits of Precision in Dual Inlet
Measurements ........................................................... 7-21
Switching Positions of the Changeover Extension ..... 7-22
Combined Multiport-Microvolume Measurement .... 7-24
Reference Refill ......................................................... 7-26
Editing a Configuration in Advanced Mode................. 7-27
Device Editor ............................................................ 7-29
Events Tab ................................................................ 7-32
Sequence Tab............................................................ 7-34
Monitor Parameter Tab ............................................ 7-36
System Start Values Tab............................................ 7-36
Viewing Results............................................................ 7-40
Representation of Data.............................................. 7-41
Graphical Representation .......................................... 7-43
Recalculation............................................................. 7-45
Exporting Results ......................................................... 7-46
Creating an Export Template.................................... 7-47
Applying an Export Template ................................... 7-51

Chapter 8 Troubleshooting .................................................................... 8-1


Checking Performance Data .......................................... 8-2
Absolute Sensitivity ........................................................ 8-3
Principle of Testing Absolute Sensitivity ..................... 8-5
Abundance..................................................................... 8-5

iv Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific


Contents

Principle of Testing Abundance .................................. 8-6


Sources of Error .......................................................... 8-6
Amplifier Test ................................................................ 8-6
Compression Factor ....................................................... 8-7
Linearity......................................................................... 8-7
Source of Error............................................................ 8-7
Peak Flatness.................................................................. 8-8
Relative Sensitivity ......................................................... 8-8
Sources of Error .......................................................... 8-9
Resolution...................................................................... 8-9
Example .................................................................... 8-10
Signal Stability ............................................................. 8-11
Sources of Error ........................................................ 8-11
System Stability............................................................ 8-11

Chapter 9 Maintenance ..........................................................................9-1


Safety Guidelines for Maintenance................................. 9-2
General Advice for Maintenance .................................... 9-3
Inspection- and Servicing Plan ....................................... 9-4
Basic Rules for Cleaning................................................. 9-6
Baking the System.......................................................... 9-7
Ion Source...................................................................... 9-8
Accessing the Ion Source ............................................. 9-9
Dismounting the Ion Source ....................................... 9-9
Reinserting the Ion Source ........................................ 9-12
Replacing the Cathode Unit...................................... 9-14
Cleaning the Parts of the Ion Source ......................... 9-16
Replacing the Ion Source Heaters.............................. 9-17
Checking the Ion Source........................................... 9-18
Vacuum Pumps............................................................ 9-19
Checking Oil Levels .................................................. 9-19
Replacing Oil ............................................................ 9-20
Vacuum System ........................................................... 9-20
Detecting Leaks......................................................... 9-20
Contaminations ........................................................ 9-21
Viton Gaskets............................................................ 9-22
Cleaning Vacuum Components ................................ 9-22
Pressure Reducer for Compressed Air........................... 9-23
Dual Inlet System ........................................................ 9-24
Crimp Adjustment .................................................... 9-24
Replacing a Pneumatic Valve ....................................... 9-25
Disassembling a Pneumatic Valve ............................. 9-26
Reassembling a Pneumatic Valve............................... 9-28
Reinserting a Pneumatic Valve into its Valve Block... 9-31
Autocool Refill Device ................................................. 9-33
Checking the Liquid Nitrogen Evaporation Rate ...... 9-33
Maintaining the Dewar Vessel................................... 9-34
Working With Liquid Nitrogen................................ 9-34
Needle Valves............................................................... 9-35

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) v


Contents

Removing the Needle Valve Heater........................... 9-36


Leaks at the Needle Valves ........................................ 9-37
Connecting a New Peripheral ................................... 9-38
Baking a Needle Valve .............................................. 9-39
Stainless Steel Capillaries and Fused Silica Capillaries .. 9-39
Removing the Blind to Access the Capillaries ............ 9-40
Putting Capillaries through ....................................... 9-41
Baking Stainless Steel Capillaries............................... 9-42
Replacing Capillaries................................................. 9-45
Adjusting Capillaries ................................................. 9-46
Nickel Capillaries ......................................................... 9-47
Handling Nickel Capillaries ...................................... 9-47
Installing Nickel Capillaries ...................................... 9-48
Cutting Nickel Capillaries......................................... 9-48
Baking Nickel Capillaries .......................................... 9-48
Crimping Nickel Capillaries...................................... 9-49
Penning Gauge............................................................. 9-50
Putting the Penning Gauge Into Operation Again .... 9-50
Disconnecting and Cleaning the Penning Gauge ...... 9-51
Measurement Points for the Penning Gauge ............. 9-52
Adjusting the Set Point of the Penning Gauge .......... 9-53
Amplifier Area and Three-Way Valve........................... 9-55
Venting the Amplifier Housing................................. 9-57
Evacuating the Amplifier Housing with an
Evacuated Analyzer ................................................... 9-57
Evacuating the Amplifier Housing with Vented
Analyzer .................................................................... 9-57
Thermo Fisher Scientific Service .................................. 9-58
Health and Safety Form ............................................ 9-58
Services to be Performed by Thermo Fisher
Scientific Service Only .............................................. 9-58

Appendix A Legal Documents.................................................................. A-1

Glossary ................................................................................. G-1

Index......................................................................................... I-1

vi Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific


T
Technical Data of the Delta V Series Instruments

The table summarizes the most important technical data of the Delta V
Series instruments. See the respective chapters of the manual for details
and additional instrument properties.

Parameter Specification Value


Instrument Properties
Mass spectrometer Depth × width × height 78 cm × 81 cm × 92 cm
(30.7 in × 31.9 in × 36.2 in)
Weight 300 kg (660 lb)
Complete system Noise level below 50 dB(A)
(incl. data system) Heat generation 1.5 kW during normal operation
2.0 kW during bakeout (basic system)
Power Requirements
Mass spectrometer Input Nominal voltage 230/400 V; 50/60 Hz AC
Dedicated line voltage, must be free of spikes
Supply system Three-phase, 5-wire system in ‘Y’ configuration
(neutral wire must be connected to earth)
Voltage fluctuation ±10%
Internal fuses Phases fused with 15 A (L1), 10 A (L2), 6 A (L3)a
Output 1× 230 V AC, 50/60 Hz, max. 15 A
4× 230 V AC, 50/60 Hz, max. 10 Ab
Gas Requirements
Compressed air Pressure Compressed air with a pressure of ≥ 6 bar (≥ 600 kPa;
≥ 87 psi) is recommended for the laboratory.

To work properly, instrument and peripherals need a


stable working pressure of 5 bar (500 kPa; 73 psi)
provided by the internal pressure regulator inside the
MS.

A maximum pressure of 10 bar (1 MPa; 145 psi) is


allowed.
Operating Environment
Laboratory temperature 18 to 24 °C (64 to 75 °F)
Max. temperature fluctuation ±1 °C/h
Humidity 40 to 60%, non-condensing and non-corrosive
atmosphere
a
One 15 A fuse for one bigger socket (J7); one 10 A fuse for all four sockets; one 6 A fuse for the IRMS
b
The four outputs (J8) are secured with one 10 A fuse, that is, the sum of the output currents must not exceed 10 A.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) vii
Technical Data of the Delta V Series Instruments

viii Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
1
Using this Manual

Welcome to your Thermo Scientific™ Delta V™ Series system! Delta V


Series systems are Isotope Ratio Mass Spectrometers and comprise the
instruments Delta V Plus and Delta V Advantage.

Contents

• About this Manual on page 1-1

• Typographical Conventions on page 1-2

• Reference Documentation on page 1-4

• Contacting Us on page 1-6

About this Manual


This Delta V Series Operating Manual contains precautionary statements
that can prevent personal injury, instrument damage, and loss of data if
they are properly followed. It also describes the modes of operation and
principle hardware components of your Delta V instrument. In
addition, this manual provides step-by-step instructions for cleaning and
maintaining your instrument.

This Delta V Series Operating Manual is intended for all personnel that
need a thorough understanding of the instrument (to perform
maintenance or troubleshooting, for example).

Designed, manufactured and tested in an ISO9001 certified facility, this


instrument has been shipped to you from our manufacturing facility in a
safe condition. This instrument must be used as described in this
manual. Any use of this instrument in a manner other than described
here may result in instrument damage and/or operator injury.

Read this manual carefully before using the instrument and keep it for
future reference.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 1-1
Using this Manual
Typographical Conventions

Typographical Conventions
This section describes typographical conventions that have been
established for Thermo Fisher Scientific manuals.

Signal Words
Make sure that you follow the precautionary statements presented in
this manual. The special notices appear different from the main flow of
text:

NOTICE Points out possible material damage, data loss, impaired data quality
and other important information in connection with the instrument.

Tip Highlights helpful information that can make a task easier.

Viewpoint Orientation
The expressions left and right used in this manual always refer to the
viewpoint of a person that is facing the front side of the instrument.

Data Input
Throughout this manual, the following conventions indicate data input
and output via the computer:

• Messages displayed on the screen are represented by capitalizing the


initial letter of each word and by italicizing each word.

• Input that you enter by keyboard is identified by quotation marks:


single quotes for single characters, double quotes for strings.

• For brevity, expressions such as “choose File > Directories” are used
rather than “pull down the File menu and choose Directories.”

• Any command enclosed in angle brackets < > represents a single


keystroke. For example, “press <F1>” means press the key labeled
F1.

• Any command that requires pressing two or more keys


simultaneously is shown with a plus sign connecting the keys. For
example, “press <Shift> + <F1>” means press and hold the <Shift>
key and then press the <F1> key.

• Any button that you click on the screen is represented in bold face
letters. For example, “click Close.”

1-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Using this Manual
Typographical Conventions

Topic Headings
These headings are used to show the organization of topics in a chapter:

Chapter Name

Second Level Topics

Third Level Topics

Fourth Level Topics

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 1-3
Using this Manual
Reference Documentation

Reference Documentation
This Delta V Series Operating Manual represents the Original Operating
Instructions. In addition to this manual, Thermo Fisher Scientific
provides other documents for the Delta V Series mass spectrometers that
are not part of the Original Operating Instructions. Reference
documentation for the Delta V Series mass spectrometers includes the
following:

• Gas Isotope Ratio MS Pre-Installation Requirements Guide

This guide contains information on the required environmental


conditions in the intended location for the instrument.

• Delta V Series Consumables and Parts Catalog

This manual lists part numbers of key consumables and spare part
items for the instrument.

Reference documentation for peripherals used with the Delta V Series


mass spectrometers includes the following:

• ConFlo IV Operating Manual

• EA IsoLink CN Operating Manual

• EA IsoLink CN/OH Operating Manual

• EA IsoLink CNSOH Operating Manual

• FLASH HT 2000 Operating Manual

• FlashSmart Operating Manual

• GasBench II Operating Manual

• GC IsoLink II Operating Manual

• Kiel IV Carbonate Device Operating Manual

• LC IsoLink Operating Manual

• PreCon Operating Manual

• Ramped GC Oven Operating Manual

• TC/EA Operating Manual

You can access PDF files of the documents listed above and of this
manual from the data system computer or other electronic storage
devices.

A printed version of this Delta V Series Operating Manual is shipped


with the instrument.

1-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Using this Manual
Reference Documentation

Refer also to the user documentation provided by the manufacturers of


third party components:

• Forepump

• Turbomolecular pumps

• Data system computer and monitor

• Material Safety Data Sheets (MSDSs)

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 1-5
Using this Manual
Contacting Us

Contacting Us
There are several ways to contact Thermo Fisher Scientific. You can use
your smartphone to scan a QR Code, which opens your email
application or browser.

Contact Link / Remarks QR Code


Brochures and Ordering www.thermofisher.com/deltav
Information

Service Contact www.unitylabservices.com

Technical Documentation ❖ To get user manuals for your product


SharePoint
1. With the serial number (S/N) of your instrument, request
access on our customer SharePoint as a customer at
www.thermoscientific.com/Technicaldocumentation

2. For the first login, you have to create an account. Follow the
instructions given on screen. Accept the invitation within six
days and log in with your created Microsoft™ password.
3. Download new revisions of user manuals and other
customer-oriented documents for your product. Translations
into other languages may be available there as well.
Customer Feedback ❖ To suggest changes to this manual

You are encouraged to report errors or omissions in the text or


index. Send an email message to the Technical Editor at
documentation.bremen@thermofisher.com.

1-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
2
Scope of Delivery

This chapter lists the standard components of your Delta V Series IRMS
system and optional components.

Contents

• Standard System Components on page 2-2

• Optional System Components on page 2-2

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 2-1
Scope of Delivery
Standard System Components

Standard System Components


The Delta V Series standard system comprises the following
components:

• Delta V Series mass spectrometer

• Data system computer with monitor

• Fore vacuum pump

• Turbomolecular pump

• Installation Kit including:


- Equipment for connecting the above components (tubings,
cables)
- Computer equipment
- Tools for installation and maintenance
- Spare parts

• Printed manuals
- Delta V Series Operating Manual

In addition to this printed manuals, other documents for the


Delta V Series mass spectrometers are available as PDF files on the
data system computer. See “Reference Documentation” on page 1-4
for a list.

Optional System Components


For reference, the following list contains optional components that are
frequently shipped with the Delta V Series IRMS system. They are not
part of the standard system and may therefore not be present in your
laboratory:

• Dual Inlet system

• Multiport

• Microvolume

• Differential pump module with Pfeiffer HiPace™ 80

• Collector systems with more that five cups

2-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
3
System Description

This chapter describes the parts and functions of the Delta V Series mass
spectrometers (that is, Delta V Plus and Delta V Advantage
instruments).

Contents

• Basic Instrument on page 3-2

• Differences between Delta V Advantage MS and Delta V Plus MS on


page 3-3

• Front View on page 3-4

• Control Panel on page 3-6

• Plug and Measure Concept on page 3-9

• Connections at the Rear Panel on page 3-12

• Right Side and Dual Inlet System Cabinet on page 3-19

• Microvolume Cabinet on page 3-29

• Ion Source Cabinet on page 3-32

• Analyzer Cabinet on page 3-35

• Electronics Cabinet on page 3-60

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-1
System Description
Basic Instrument

Basic Instrument
The Delta V Series mass spectrometers are primarily designated to
measure the isotope ratios of H/D, 13C/12C, 15N/14N, 18O/16O, 34S/32S,
37
Cl/35Cl and other elements that can be transformed into gaseous
substances. The gases used with this type of IRMS are, for example,
CO2, H2, N2, NO, N2O, O2, SO2, and CH3Cl.

Tip To reach a high performance level with the Delta V Series mass
spectrometers, make use of the operator courses at our facilities in
Bremen and/or onsite.

The Delta V Series mass spectrometers provide a flexible and open


platform for the connection of inlet systems and preparation devices.
Thermo Scientific-supplied inlet systems are automatically recognized
by the Plug and Measure (PnM) concept. In addition, the system is
open for easy connection and control of custom inlet/preparation
systems.

For classical applications, the basic instrument can be equipped with a


Dual Inlet system. It is of modular design for the adaptation of different
inlet modules. This enables a configuration of the instrument tailored to
the requirements of the operator.

The following devices can be connected on the sample side:

• a secondary inlet system for up to 20 samples, for example, a


Multiport with or without automatic TubeCrackers

• a Microvolume for very small samples

• external multisample inlets for separating and purifying samples

• installations for “on-line” coupling to a gas chromatograph,


Elemental Analyzer, or other peripherals

3-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Differences between Delta V Advantage MS and Delta V Plus MS

Differences between Delta V Advantage MS and Delta V Plus MS


Table 3-1 lists differences between the Delta V Advantage and the
Delta V Plus instrument.

Table 3-1. Differences between Delta V Advantage and Delta V Plus instrument
Feature Delta V Advantage MS Delta V Plus MS
Focus Quad — Equipped with Focus Quad
Focus Quad Power Supply — Focus Quad power supply board is
Board needed to control it.
Aperture Aperture is equipped with an Aperture is shorter as the bracket is
additional bracket. missing.
Ion beam dimension Ion beam is narrower. Focal depth is Ion beam is wider.
satisfactory to hit the cups.
— A focus quad is necessary to later on
focus the ion beam on the cups again.
Sensitivity Sensitivity is lower than with Delta V Sensitivity is higher than with
Plus instrument (about Delta V Advantage instrument
1500 molecules per ion). (about 900 molecules per ion).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-3
System Description
Front View

Front View
Figure 3-1 shows a Delta V Series instrument in front view.

5 2

Labeled Components: 1=top showing Multiport with pre-fit Swagelok™ pipe


connection, 2=removable door for Dual Inlet system, 3=space for
Microvolume and Dewar vessel or storage behind door, 4=door to ion source
and amplifiers, 5=control panel
Figure 3-1. Delta V Series instrument in front view

The top 1 in Figure 3-1 shows the Multiport fitted with Swagelok™ pipe
connections.

The door 2 gives access to the optional Dual Inlet system. For details, see
“Right Side and Dual Inlet System Cabinet” on page 3-19. If no Dual
Inlet system is available, the cabinet may be used as storage space.

With a Dual Inlet system, the sample vials together with their
supportive brackets are arranged in front the door 2. The door cannot be
opened, but only be removed: remove the door by holding it at its top
and bottom and then drawing it upwards. Removing the door is easier
when the door 3 below is opened as well.

3-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Front View

The door 3 gives access to an inspection glass to control the oil level of
the fore vacuum pumps, an optional Microvolume with the related
liquid nitrogen container, and the socket shelves at the left wall
providing various heating elements. For details, see “Microvolume
Cabinet” on page 3-29.

If no Microvolume is available, the place behind the door 3 is empty and


can be used as storage space to hold spare parts or expendables in
readiness (for example, a reactor or reactor packing materials, if an
Elemental Analyzer is available).

The door 4 is screwed close and must only be opened by skilled service
personnel. It gives access to the ion source (for example, to clean it
during maintenance or to exchange the filament) and to the amplifiers
in case of an electronic defect. For details, see “Ion Source Cabinet” on
page 3-32.

The pump switch and pump-related LEDs are located at the control
panel 5. For details, see “Control Panel” on page 3-6.

Mounting and Removing the Side Panels


To easily mount the panels, metallic bolts have been installed on the top
and bottom of the frame. See Figure 3-2.

Figure 3-2. Bolts at frame

To remove a side panel, hold the panel at its top and bottom (not at the
side) and pull it upwards.

Take care of the green-yellow ground wire which has been fastened
onto the side door according to Figure 3-63. Temporarily remove it.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-5
System Description
Control Panel

Control Panel
Figure 3-3 shows the control panel which is located top left at the front
of your Delta V Series instrument. See also 5 in Figure 3-1.

1 2 3
11 4

6
10 9 8 7

Labeled Components: 1=status LED of vacuum quality, 2=status LED of


differential (optional) pump, 3=status LED of main pump, 4=Pump switch,
5=pump switch of Dual Inlet system, 6=status LED of Dual Inlet system pump,
7=adjusting knob for needle valves (optional), 8=status LED of ion source
heater, 9=status LED of emission, 10=status LED of ion source voltage,
11=status LED of power supply and connection to computer
Figure 3-3. Control panel

The Vacuum status LED (1 in Figure 3-3) indicates the quality of the
vacuum.

The Secondary status LED 2 indicates the status of the differential


pump (if available, optional turbomolecular pump).

The Main status LED 3 indicates the status of the main pump (analyzer
turbomolecular pump).

The Pumps switch 4 turns the main pump (analyzer turbomolecular


pump) and the differential pump (if available, optional turbomolecular
pump) on or off.

The Pump switch 5 turns the turbomolecular pump of the Dual Inlet
system (if available) on or off.

The Inlet status LED 6 indicates the status of the turbomolecular pump
of the Dual Inlet system (if available).

The adjusting knob 7 opens and closes the needle valve (optionally up to
three) located at the aluminum-made needle valve heating block close to
the ion source. For details, see “Needle Valves” on page 9-35.

3-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Control Panel

The Heater status LED 8 monitors the ion source heaters (halogen
lamps serving as radiant heaters) that are switched by Isodat.

The Emission status LED 9 monitors the emission of electrons by the


filament.

The Voltage status LED 10 monitors the status of the ion source and the
high voltage.

The Connection status LED 11 monitors the power supply and the
connection to the controlling Isodat computer.

The LEDs at the Control Panel


This section lists the meaning of each LED status at the control panel.
For the position of the LEDs, see Figure 3-3.

Table 3-2 summarizes the statuses of the Vacuum LED.

Table 3-2. Statuses of Vacuum LED


Color of LED Status of Vacuum LED
Off (no color) The Penning gauge is off.

The pumps are off or have not yet reached their final
number of revolutions.
Yellow The Penning gauge is on and works properly.

The set point has not yet been reached.


Green The pressure has fallen below the set point of the
Penning gauge.

Table 3-3 summarizes the statuses of the Main and Secondary pump
LEDs. The Secondary pump LED is active, if the optional
turbomolecular pump is available.

Table 3-3. Statuses of Main and Secondary pump LEDs


Color of LED Status of Pump LEDs
Yellow The device has been switched on.

The final operating state has not yet been reached.


Green The device has reached its final operating state and
works properly.
Red The pump does not work properly due to a technical
problem, defect or another kind of error.
Off (no color) The device is off (the switch to turn on the
corresponding pump has not yet been pressed).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-7
System Description
Control Panel

Table 3-4 summarizes the statuses of the Inlet LED for the
turbomolecular pump of the Dual Inlet system (if available).

Table 3-4. Statuses of Dual Inlet pump LED


Color of LED Status of Dual Inletpump LED
Yellow The device has been switched on.

The final operating state has not yet been reached.


Green The device has reached its final operating state and
works properly.
Red The pump does not work properly due to a technical
problem, defect or another kind of error.
Off (no color) The device has not yet been turned on (for example,
the switch to turn on the corresponding pump has
not yet been pressed).

Table 3-5 summarizes the statuses of the Heater LED.

Table 3-5. Statuses of Ion source heater LED


Color of LED Status of Ion Source Heater
Off (no color) The ion source heater is switched off (or is switched
on, but not working properly).
Green The ion source heater is switched on.

Table 3-6 summarizes the statuses of the Emission LED.

Table 3-6. Statuses of Emission LED


Color of LED Status of Emission LED
Off (no color) The ion source is switched off.

It cannot be switched on because the pumps have not


yet reached their final number of revolutions and/or
the set point of the Penning gauge has not been
reached.

The vacuum quality is not yet satisfactory.


Yellow The vacuum quality is satisfactory, but emission does
not take place.

Possible causes: the filament has not been switched


on or is out of order.
Green All related conditions are in order and therefore
emission takes place.

3-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Plug and Measure Concept

Table 3-7 summarizes the statuses of the Voltage LED.

Table 3-7. Status of ion source and high voltage


Color of LED Status of ion source and high voltage
Off (no color) The ion source is switched off.

It cannot be switched on because the pumps have not


yet reached their final number of revolutions and/or
the set point of the Penning gauge has not been
reached.

The vacuum quality is not yet satisfactory.


Yellow The ion source could be on, but high voltage has not
been switched on.

Possible causes: the vacuum quality is satisfactory, but


the ion source has been switched off automatically
due to a high voltage flashover.

The ion source must be switched on in Isodat.

Table 3-8 summarizes the statuses of the Connection LED.

Table 3-8. Status of power supply and connection to computer


Color of LED Power supply and connection to computer
Off (no color) No power is available.

Possible causes:
• the device is switched off
• the fuses blew
• the main power cable is not plugged in
Yellow Power is available (the main power supply is on and
the main switch is in the On position).

The computer is not connected or switched off.


Green Power is available (the main power supply is on and
the main switch is in the On position).

The computer connection has been established.

Plug and Measure Concept


Up to five peripherals can be connected simultaneously to the five
SUB D connectors. See “SUB D Connectors” on page 3-18 for details.

Each peripheral has its own plug and measure code. This code is
encoded either in the cable to the device or in a plug and measure
adapter.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-9
System Description
Plug and Measure Concept

The instrument automatically recognizes the kind of peripheral and the


SUB D connector used for it, when a configuration requires this device.
Otherwise, and when the device cable is unplugged accidentally, an error
message is displayed.

The Plug and Measure adapter (PnM adapter, Figure 3-4) is used to
connect peripherals. It is pre-configured by Thermo Fisher Scientific for
a defined option, for example, a ConFlo IV interface. Thermo Fisher
Scientific does not recommend a supplementary reconfiguration by the
operator. The PnM adapter is connected to one of the five identical
SUB D ports at the rear panel of the Delta V Series instrument. The
peripheral is then connected to the IRMS via the bottom port of the
PnM adapter.

Jumper J3 Switch S1

Jumper

Cable to
ConFlo IV

Side View:
PnM adapter
configured for
ConFlo IV Jumper J2 Switch S2 to SUB D port

Figure 3-4. Plug and Measure adapter

Peripherals are identified by the settings of the turn switches and the
jumpers. The turn switches are used to specify the PnM ID for the
peripheral (for example, for a ConFlo IV interface, set S1 to 2).

The jumpers are also used to identify the kind of peripheral that is
connected to the IRMS. If indicated, the lowest two contacts of the plug
socket at the PnM adapter (either socket J3 or J2) are cut short from the
outside of the PnM adapter.

Tip Some external options are connected to the SUB D ports without
the PnM adapter.

3-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Plug and Measure Concept

Grounding Cable for Peripherals


Peripherals that are operated by a PnM adapter must be connected to
the IRMS by a green-yellow grounding PE cable. See “PE Connector”
on page 3-18.

The grounding is not necessary for peripheral devices that already run
with a new cable (for example, PreCon device, GP interface).

Configurating Plug and Measure Devices


Five SUB D ports are located at the rear panel of the instrument. For
each port, the electronics recognizes the kind of option connected
(encoded with a PnM ID).

Where indicated in Table 3-9, the lowest two contacts of the plug socket
at the PnM adapter (either socket J3 or J2) are cut short from the
outside of the PnM adapter.

Where indicated in Table 3-9, a new cable is necessary where no PnM


adapter is available.

Table 3-9. Settings for plug and measure devices


Peripheral PnM ID 2nd ID Jumper pin 9/10 New cable
ConFlo IV 0x02 0x03 J3
GCC II/III 0x04 0x05 J3
GasBench II 0x08 0x09
PreCon 0x0A 0x0B Yes
MultiInlet 0x0E 0x0F
acid pump 0x18 0x19 J2
GC/GP 0x10 0x10 Yes
Dual Inlet
MP1
MP2
TC1
TC2 0x12 0x13

The PnM ID is communicated by switches inside the PnM adapter or


by shortcuts inside the cable. A second ID becomes necessary when two
instruments of the same type are installed.

Tip The TubeCracker second bank is applied to two ports of the inlet
board for external options. Therefore, it has a PnM number.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-11
System Description
Connections at the Rear Panel

Connections at the Rear Panel


Figure 3-5 shows a Delta V Series instrument in rear view.

Labeled Components: 1=power panel with main switch, fuses, and power
sockets for peripherals, 2=main power cable, 3=panel with connectors for
computer, compressed air and peripherals
Figure 3-5. Rear view of a Delta V Series instrument

For details on the power supply panel 1, see “Power Supply Panel” on
page 3-13. For details on 2, see “Main Power Cable” on page 3-16.

Figure 3-6 shows the connector panel at the top of the rear panel of your
instrument (3 in Figure 3-5) in detail.

4 3 2

Labeled Components: 1=compressed air inlet, 2=compressed air connection for peripherals, 3=connections for optical
fibers, 4=SUB D connections for peripherals, 5=protective earth connector
Figure 3-6. Connections for computer, compressed air and peripherals

3-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Connections at the Rear Panel

The compressed air connections (1 and 2 in Figure 3-6) are described at


“Compressed Air” on page 3-16.

For details on the optical connections 3, see “Connectors for Optical


Fibers” on page 3-17.

The peripheral connections 4 and 5 are described at “SUB D


Connectors” on page 3-18 and “PE Connector” on page 3-18.

Power Supply Panel


The power supply panel of your Delta V Series instrument is located at
the rear side. See Figure 3-7.

2
15A

Labeled Components: 1=main switch, 2=fuses (15 A, 10 A, 6 A), 3=IEC power


socket (4 × 10 A), 4=IEC power socket (1 × 15 A), 5=PE connector, 6=main
power connection
Figure 3-7. Power supply panel

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-13
System Description
Connections at the Rear Panel

Main Switch

The main switch (1 in Figure 3-7) is located in the top right corner of
the rear panel of the instrument. Figure 3-8 shows the main switch in
Off (left) and On (right) position.

Figure 3-8. Main switch positions

Fuses and Sockets

Thermo Fisher Scientific provides five IEC power sockets to connect


peripherals, a computer or test equipment to the Delta V Series
instrument. The sockets are conform to CE and arranged in two
columns:

• a single 15 A IEC power socket (J7) and

• four 10 A IEC power sockets (J8)

Each column is fed by a separate circuit with a fuse. The sockets


guarantee an adequate, undisturbed power supply of the connected
devices.

3-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Connections at the Rear Panel

Figure 3-9 shows the fuses (see 2 in Figure 3-7) and the sockets at the
rear panel.

15A

Figure 3-9. Fuses (top) and sockets (bottom)

The three fuses provide overcurrent protection for:

• Fuse F1 for the 15 A socket J7 (see 3 in Figure 3-7).


• Fuse F2 for the 10 A sockets J8 (see 4 in Figure 3-7). All four sockets
are designated for connection of IRMS peripherals, such as the
Kiel IV Carbonate Device or the GC/TC device.

• Fuse F3 (6 A) is designated to the Delta V Series instrument.

After your computer and the IRMS peripherals have been connected,
switch on the according fuses to operate the devices.

NOTICE Do not connect recirculating chillers or compressors to the


instrument. Use the country-specific wall outlet instead. See “Power
Supply for Peripherals” on page 6-2.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-15
System Description
Connections at the Rear Panel

Main Power Cable

The main power cable (see 6 in Figure 3-7) leads to the socket wall
outlet. Figure 3-10 shows the main power cable, and the PE connector
that is located directly above the socket on the rear panel.

Figure 3-10. Main power cable and PE connector

A PE connector (Protective Earth connector; for position, see 5 in


Figure 3-7) is provided to additionally connect your Delta V Series
instrument to a separate grounded PE system if it exists in your
building. Electronically, this would imply additional protection for your
system.

Alternatively, in case of several devices within one/the system, these can


be grounded at the PE connector, thereby establishing a local grounding
system.

Compressed Air

Compressed air enters the Delta V Series instrument at the compressed


air inlet 1 in Figure 3-11 (for position, see 1 in Figure 3-6). The air
passes to the pressure reducer where the needed pressure is adjusted (see
also “Pressure Reducer for Compressed Air” on page 3-22) and is led via
an internal distributor to the compressed air connections 2 in
Figure 3-11 (see also 2 in Figure 3-6) where it is distributed to
maximally six peripherals.

Labeled Components: 1=compressed air inlet, 2=compressed air connection


for peripherals
Figure 3-11. Compressed air connections

3-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Connections at the Rear Panel

External IRMS peripherals need compressed air to switch valves and


actuators, such as pneumatic lifters (for example with the ConFlo IV
interface to lift and drop capillaries). Each peripheral must be connected
to one of the compressed air connections.

Usually, the compressed air connections are closed and opened when
you plug in the suitable coupling of a peripheral. When you pull out the
coupling, the connection closes again. A integrated check valve for each
compressed air connection ensures that compressed air only leaves the
Delta V Series instrument when a peripheral is connected.

Tip If the compressed air supply is interrupted, an internal check valve


at the pressure reducer (see Figure 3-18) maintains compressed air
supply for some seconds.

Connectors for Optical Fibers

The connectors for optical fibers (for position, see 3 in Figure 3-6) are
each made up by a pair of a blue and a gray pole. The computer sends
signals to the IRMS via the gray connection and receives signals from
the IRMS via the blue connection. See Figure 3-12.

Labeled Components: 1=two pairs of controlling connections for peripherals


(2 × IN and OUT), 2=connection pair for the controlling Isodat computer
Figure 3-12. Connectors for optical fibers

The connectors 1 in Figure 3-12 are designated to control peripherals.


The connectors 2 in Figure 3-12 are designated for the controlling
Isodat computer.

IRMS peripherals that have an “intelligence of their own” can be


connected via optical fibers (for example, a Kiel IV Carbonate Device or
a Peripheral Controller) so that analog values, such as temperature
values, can be continuously adjusted and read back.

NOTICE Light from extraneous sources, such as sunlight, passes adulterant


signals to the IRMS via the connectors for optical fibers. If no
peripherals are connected, close the unused connectors by plugs. Do
not use red plugs, as red light is primarily responsible for signal
transmission.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-17
System Description
Connections at the Rear Panel

SUB D Connectors

Five 25-pole SUB D connectors are provided to connect peripherals to


the Delta V Series instrument. External peripherals that have a
plug & measure adapter can directly be plugged in here. See 4 in
Figure 3-6.

The valves of the particular peripheral can then be switched on and off
in Isodat. The plug and measure adapter belongs to the cable of the
individual peripheral. The plug and measure concept is described at
“Plug and Measure Concept” on page 3-9.

Tip For peripherals that do not have a plug and measure adapter (such
as the GP interface, PreCon device and LC IsoLink device), the same
functionality has been integrated within their modified plug.

PE Connector

The cables of the peripherals leading to the SUB D connectors are


screened. This avoids both introducing disturbances from outside and
spreading them inside via the cables (electromagnetic compatibility).
Their green-yellow lines must be connected to the PE connector
(Protective Earth connector). See Figure 3-13.

Figure 3-13. PE connector

If additionally a separate grounded PE system exists in your building,


you can connect an extra ground wire. See 6 in Figure 3-6.
Electronically, this would imply additional protection for your system.
Alternatively, in case of several devices within a system, these can be
grounded at the PE connector thereby establishing a local grounding
system.

3-18 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet

Right Side and Dual Inlet System Cabinet


Figure 3-14 shows the right side of the Delta V Series instrument with
the doors removed.

1
2

Labeled Components: 1=Dual Inlet board (optional), 2=fan for turbomolecular


pump of Dual Inlet system (optional), 3=turbomolecular pump of Dual Inlet
system (optional), 4=pressure reducer for compressed air, 5=additional valve
(optional), 6=fore vacuum pump of analyzer, 7=fore vacuum pump of Dual
Inlet system (optional)
Figure 3-14. Components at right side of the IRMS

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-19
System Description
Right Side and Dual Inlet System Cabinet

Figure 3-15 shows the components of the optional Dual Inlet cabinet
located at the right top front of the Delta V Series instrument. See 2 in
Figure 3-1. This cabinet is empty if no Dual Inlet system is available.

1
2

Labeled Components: 1=gas inlet (2 ×), 2=bolt for panel insertion (4 ×),
3=Dual Inlet system (optional)
Figure 3-15. Dual Inlet system cabinet

A variety of sample vials can be attached at both gas inlets (1 in


Figure 3-15). The bolts (2 in Figure 3-15) allow easy re-insertion of the
panels after they have been removed. The Dual Inlet system (3 in
Figure 3-15) is described in detail in Chapter 4, “Dual Inlet System
(Optional).”

The supportive brackets (1 in Figure 3-16) support the connection


between metal and sample vial so that a gas tank can be connected
directly. See 3 in Figure 3-16.

The protective bracket (2 in Figure 3-16) protects the attached sample


vials against being broken away by accident. The protective bracket is
only attached if a Dual Inlet system is available.

The sample vials (4 in Figure 3-16) are attached to the gas inlets via a
Swagelok™ connector (5 in Figure 3-16). The Swagelok connectors are
also used for the TubeCracker. For details, see “TubeCracker” on
page 4-14.

3-20 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet

1
5
2

Labeled Components: 1=support bracket, 2=protective bracket, 3=gas tank


connected, 4=sample vials connected, 5=Swagelok™ connectors
Figure 3-16. Supportive brackets with sample vials attached

Turbomolecular Pump of the Dual Inlet System


The turbomolecular pump of the Dual Inlet system (for position, see 3
in Figure 3-14) is a HiPace™ 80 manufactured by Pfeiffer. It is mounted
next to the Dual Inlet board. See Figure 3-17.

4
1

Labeled Components: 1=connector from additional valve to J 230 on Dual


Inlet board, 2=compressed air distributor, 3=turbomolecular pump of Dual
Inlet system, 4=Dual Inlet board
Figure 3-17. Turbomolecular pump of Dual Inlet system and Dual Inlet
board

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-21
System Description
Right Side and Dual Inlet System Cabinet

To switch the turbomolecular pump (3 in Figure 3-17), press the Pump


button at the Control Panel (see 5 in Figure 3-3). If no Dual Inlet
system is available, this button is inoperable.

The turbomolecular pump is supplied via the power distribution board.


For details on the power distribution board, see “Power Distribution
Board” on page 3-61.

Pressure Reducer for Compressed Air


The pressure reducer for compressed air (for position, see 4 in
Figure 3-14) regulates the pressure of the compressed air needed for
operating the Dual Inlet system and the peripherals. Figure 3-18 shows
details of the pressure reducer.

Labeled Components: 1=adjusting knob, 2=pressure display, 3=oil collection


reservoir, 4=blow-off valve
Figure 3-18. Pressure reducer for compressed air

Oil contained in compressed air is collected within the reservoir 3. The


reservoir can be emptied via the blow-off valve 4.

If the compressed air pressure decreases or breaks down entirely, an


integrated check valve guarantees that the device will still be provided
with compressed air of the adjusted pressure for a limited period of time.

For the compressed air supply of peripherals at the rear side of the
Delta V Series instrument, see “Compressed Air” on page 3-16.

3-22 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet

Fore Vacuum Pumps


Figure 3-19 shows the fore vacuum pumps inside the right cabinet of
the Delta V Series instrument. See also 6 and 7 in Figure 3-14.

2
6

Labeled Components: 1=additional valve, 2=to turbomolecular pump of Dual


Inlet system, 3=belt for transportation lock for fore vacuum pumps, 4=fore
vacuum pump of Dual Inlet system, 5=fore vacuum pump of analyzer, 6=to
waste line of Dual Inlet system
Figure 3-19. Dual Inlet system fore vacuum pump with additional valve

The fore vacuum pump of the Dual Inlet system (4 in Figure 3-19) is
mounted next to the fore vacuum pump of the analyzer 5. Both fore
vacuum pumps are rotary vane pumps, DUO 2.5, manufactured by
Pfeiffer, providing pressures of about 10-3 mbar by a rate of 5 m3/h.

The fore vacuum pump of the analyzer serves as:

• Fore vacuum pump for the turbomolecular pump(s) of the analyzer

• Rough pump for the amplifier housing

After venting the amplifier housing, the rough pump creates a fore
vacuum, before it is possible to connect a turbomolecular pump of
the analyzer.

If a Dual Inlet system is available, the fore vacuum pump of the Dual
Inlet system 4 is mounted next to the fore vacuum pump of the analyzer
5.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-23
System Description
Right Side and Dual Inlet System Cabinet

The fore vacuum pump of the Dual Inlet system serves as:

• Fore vacuum pump for the turbomolecular pump of the Dual Inlet
system

• Rough pump of the Dual Inlet system. It pumps considerable gas


amounts out of the Dual Inlet system.

If no Dual Inlet system is available, the fore vacuum pump of the Dual
Inlet system is not installed.

Movable Tray for Fore Vacuum Pumps

Both fore vacuum pumps are placed on a movable tray. Pump oil that
might leak can be collected there.

NOTICE Do not move Delta V Series instruments with any pump turned on.

Before moving the instrument, both fore vacuum pumps must be


secured (transportation lock) with the provided belt, 3 in Figure 3-19.
Thereby, both fore vacuum pumps can remain in the instrument
during transport.

Remove the belt after transport and before operation is started again.

Before moving the tray with the fore vacuum pumps, remove their
connectors.

The tray is accessible from outside and can be pulled out or pushed
inwards with ease, as the fore vacuum pumps are relatively lightweight.
See Figure 3-20. Rubber pads below the tray prevent scratching the
bottom of the instrument.

Figure 3-20. Movable tray below fore vacuum pumps

3-24 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet

Heat and Exhaust Gas Removal


The exhaust gases of both fore vacuum pumps contain pump oil vapor
and must be removed. The exhaust tube leaves the IRMS underneath its
rear panel doors and is led either outwards or to the exhaust gas
equipment.

Warm ascending air can leave the instrument via the chimney located in
the analyzer cabinet. Air is sucked in via an exhaust device 2 in
Figure 3-21 and led through a chimney 1. See also “Analyzer Cabinet”
on page 3-35.

Labeled Components: 1=chimney, 2=exhaust device


Figure 3-21. Exhaust device and chimney

As the fore vacuum pumps produce heat, the entire pump area is lined
with thermal insulation mats. They prevent other parts of the
instrument from being heated as well. See arrows in Figure 3-22.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-25
System Description
Right Side and Dual Inlet System Cabinet

Figure 3-22. Thermal insulation mats

Additional Valve
The additional valve is only available if the Dual Inlet system is
employed. Figure 3-23 shows the components of the additional valve.

1 2 3

Labeled Components: 1=electrical connector leading to J 230 on Dual Inlet


board, 2=inspection glass showing whether additional valve is open or
closed, 3=connector for compressed air
Figure 3-23. Components of additional valve

3-26 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet

While working as a rough pump, the fore vacuum pump of the Dual
Inlet system cannot be used as a fore vacuum pump for the
turbomolecular pump. The pressure increase at the exit of the
turbomolecular pump of the Dual Inlet system would be too large.

To avoid excessively high pre-pressures at the turbomolecular pump of


the Dual Inlet system, the additional valve has been implemented. It is
located on the fore vacuum pump of the Dual Inlet system (see 5 in
Figure 3-14 and 1 in Figure 3-19) and is controlled by Isodat (see “Dual
Inlet System” on page 7-18).

To open and close the additional valve by Isodat, the connector of the
additional valve is connected to socket J 230 on the Dual Inlet board.
For the position of the socket J 230 on the Dual Inlet board, see 1 in
Figure 3-17.

While the fore vacuum pump of the Dual Inlet system acts as a rough
pump and pumps off large gas amounts, the additional valve is closed.
The turbomolecular pump of the Dual Inlet system operates then
without the fore vacuum pump. This is possible during a limited period
of time.

If no compressed air is available during a longer time, the additional


valve is closed as well. All other valves of the Dual Inlet system are
opened. Operating the Dual Inlet system is impossible.

If no electrical connection has been established to the Dual Inlet board


(the connector of the additional valve has not been stuck into socket
J 230 of the Dual Inlet board), the additional valve is open.

Isodat assures time-controlled that the additional valve is opened again


before the pressure at the exit of the turbomolecular pump becomes too
high. Now, the pump acts as a fore vacuum pump again.

Tip If the turbomolecular pump of the Dual Inlet system does not
operate and repeatedly turns off, the additional valve may be closed.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-27
System Description
Right Side and Dual Inlet System Cabinet

Dual Inlet Board


The Dual Inlet board is located closely to the Dual Inlet system. See 1 in
Figure 3-14. The LEDs for the supply current on the Dual Inlet board
are shown in detail in Figure 3-24.

Figure 3-24. LEDs for supply current on Dual Inlet board

The Dual Inlet board controls the Dual Inlet system and options (for
example, a Multiport or a Microvolume). It has the following functions:

• Control of the valve banks

• Connection of three additional vacuum gauges

• Connection of the operation device for the cooling trap

• Motion control of the bellows

Figure 3-25 shows the bellow motors connected to connectors J 205 and
J 206.

Figure 3-25. Connectors for bellows motors on Dual Inlet board

3-28 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Microvolume Cabinet

Microvolume Cabinet
Figure 3-26 shows the cabinet at the lower right front of the Delta V
Series instrument. For the location, see 3 in Figure 3-1.

2 1

Labeled Components: 1=inspection glass of fore vacuum pump of Dual Inlet


system, 2=position for optional Microvolume and Autocool Unit, 3=inspection
glass of fore vacuum pump of analyzer, 4=panel with activated sockets and
12 V power supply
Figure 3-26. Microvolume cabinet

The Microvolume cabinet allows visual access to the inspection glasses


of the fore vacuum pump of the Dual Inlet system (1 in Figure 3-26)
and the fore vacuum pump of the analyzer (3 in Figure 3-26) to check
the oil levels.

The fore vacuum pumps are described in detail in “Fore Vacuum


Pumps” on page 3-23.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-29
System Description
Microvolume Cabinet

Power Sockets and Plugs


The sockets for heaters (for location, see 4 in Figure 3-26) are shown in
Figure 3-27. They can be switched individually.

Labeled Components: 1=J1110, 2=12 V power supply (S-40-12, 3.5 A),


3=J1112, 4=J1113
Figure 3-27. Activated sockets and 12 V power supply

The activated sockets are controlled only as groups (as entire shelves of
six, two or two sockets) by the Instrument Control of Isodat.

The 12 V power supply (2 in Figure 3-27) is located right to the


activated sockets and provides the ion source heater with the energy
needed to heat out the ion source. See “Replacing the Ion Source
Heaters” on page 9-17.

The activated sockets (1, 3 and 4 in Figure 3-27) provide three groups of
heaters (and/or heatable valves) with energy.

The sockets in group J1110 (1 in Figure 3-27) are assigned to the


following heaters (top to bottom): Dual Inlet system, Multiport,
Multiport Extension, Microvolume, trap (125 VA), and capillary
(185 VA).

The sockets in group J1112 (3 in Figure 3-27, top to bottom) are


assigned to the heaters for Needle valve and Changeover valve. The
sockets in group J1113 (4 in Figure 3-27, top to bottom) are provided
for free use (for example, for a Changeover Extension).

Each plug is labeled: CO for Changeover valve and Changeover


Extension, ST for standard, SA for sample, MV for Microvolume,
MP 10 for Multiport 10, MP 20 for Multiport 20, NV for needle valve.

3-30 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Microvolume Cabinet

Each heater element or valve can individually be switched by the plug of


the device (see 1 in Figure 3-28). When the integrated lamp of an
individual plug is on (see 2 in Figure 3-28), the corresponding socket is
activated.

Labeled Components: 1= plug switch, 2=plug switched on (lamp is on)


Figure 3-28. Plugs with switches and control lamps

Make sure that the corresponding button for the socket is activated in
Isodat as well, if you switch on the socket.

Position of Microvolume and Autocool Unit


Figure 3-29 shows the Dewar vessel containing liquid nitrogen
(Autocool Unit) for operating a Microvolume.

3
1

Labeled Components: 1=Dewar vessel, 2=refill tube for liquid nitrogen,


3=metallic splash guard
Figure 3-29. Position of Microvolume within Microvolume cabinet

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-31
System Description
Ion Source Cabinet

The metallic splash guard 3 protects the activated sockets against liquid
nitrogen that may spill from the Dewar vessel 1.

For a detailed description of Microvolume and Autocool Unit, see


“Microvolume” on page 4-15 and “Autocool Unit” on page 4-17.

Ion Source Cabinet


Figure 3-30 shows the ion source cabinet at the lower left front of the
Delta V Series instrument. For location, see 4 in Figure 3-1. The ion
source cabinet allows access to ion source, amplifiers, and feedthrough.

Labeled Components: 1=ion source (connector board), 2=ion source supply


cable, 3=data logger, 4=shielding cover plate, 5=safety contact for door
Figure 3-30. Ion source cabinet

The ion source 1 is directly accessible and can be removed entirely for
maintenance operations. For details on its maintenance, see “Ion
Source” on page 9-8. The ion source supply cable 2 leads to the ion
source control board. The data logger 3 is accessible from the right
panel.

3-32 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Ion Source Cabinet

If access to the amplifiers is needed, the cover plate 4 can be removed. It


shields up to ten amplifiers as individual electronic boards. For details,
see “Arrangement of Amplifiers” on page 3-33.

The safety contact for the door 5 guarantees that high voltage and
emission are both switched off instantaneously when the door of the ion
source cabinet (4 in Figure 3-1) is opened. The corresponding LEDs at
the control panel are switched off when the door opens so that operator
and ion source are protected from damage.

As soon as the door is closed again, the safety contact is re-established


and the ion source is supplied again.

Figure 3-31. Safety contact for door

Arrangement of Amplifiers
Figure 3-32 schematically shows the arrangement of amplifiers, ground
plane amplifier board, ground plane cup board, 13-fold feedthrough,
and collector system.

amplifiers ground plane ground plane 13-fold collector


(maximum 10) amplifier cup feedthrough system
(green board) (yellow board)

Figure 3-32. Arrangement from amplifier to collector

The amplifiers are mounted onto the ground plane amplifier board. The
ground plane amplifier is located behind the ten amplifiers. This
electronic board guarantees their supply voltages and establishes the
connection to the data logger. The outlets are the transfer points of the
measurement signal (gold spring contacts) to the ground plane cup,
which is arranged below the ground plane amplifier.

The ground plane amplifier board carries the amplifiers and VFCs. It
connects the amplifiers to the data logger. A photo diode switches off
the supply voltage when the lid of the amplifier housing is removed. It
serves as an additional precaution and only works properly when the
workplace is sufficiently illuminated.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-33
System Description
Ion Source Cabinet

NOTICE If the ground plane amplifier needs to be removed, first remove the
data logger because both are connected to each other by a connector.
During re-insertion, first insert the ground plane amplifier and then
the data logger.

The ground plane cup board is mounted below the ground plane
amplifier board upon the 13-fold feedthrough by spring contacts. It
establishes the transfer between the feedthrough and the ten individual
amplifiers. The yellow board is free of lacquer for technical reasons. The
feedthrough is connected to the collector system. For details on the
collector system, see “HD Collector System” on page 3-52.

The up to ten amplifiers are connected to the feedthrough from above.


Usually, only three or five amplifiers are equipped and in use. The upper
amplifiers 6 to 10 are optional. They are designated for special purposes
requiring more than the five mentioned cups (for example for air
measurement).

Assignment of Amplifiers to Cups


Table 3-10 lists the assignment of amplifiers on the ground plane cup
board.

Table 3-10. Amplifiers and m/z values of cups


Amplifier Mass [m/z]
1 2 (HD)
2 28 (N2), 32 (O2), 44 (CO2), 64 (SO2)
3 29 (N2), 33 (O2), 45 (CO2), 66 (SO2)
4 30 (N2), 34 (O2), 46 (CO2)
5 3 (HD)
Generally preset for HD, but
also usable for other gases
6 to 10 Arbitrarily configurable (see for
example Figure 6-63)

The amplifiers are all identical, but have different RC combinations


according to the individual m/z value to be measured. One amplifier can
contain at most two RC combinations. A relay allows selecting different
RC combinations.

Tip On the ground plane cup board, springs and contact pins are
connected via conducting paths. There are longer and shorter
conducting paths. Highly sensitive amplifiers have been connected via
short conducting paths.

3-34 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

Analyzer Cabinet
The left side of the Delta V Series instrument with the panels removed
shows the components of the analyzer. See Figure 3-33.

8 1

4
7

6
5

Labeled Components: 1=Penning gauge, 2=place for turbomolecular pump of


analyzer (optional), 3=turbomolecular pump of analyzer (main pump), 4=fan
for turbomolecular pump(s), 5=three-way valve, 6=cover plate, 7=24 V power
supply, 8=magnet
Figure 3-33. Left side of IRMS

The Penning gauge (1 in Figure 3-33) is an active inverted magnetron


gauge combining head and gauge controller in a single compact unit.
This high vacuum gauge operates as cold cathode ionization gauge, in
which the pressure is measured indirectly as a function of the current
which flows in a Townsend discharge maintained in the body tube.

The ionization of the gas in the vacuum system depends on both the
pressure and the physical properties of the gas. Therefore, the output
signal of the Penning gauge is gas dependent. The output signal voltage
to pressure conversion is applied for nitrogen and dry air. The model
AIM-XL-NW25 is used (BOCE Product No. D14645000). The
measurement range of the similar AIM-S and AIM-SL gauges is
1 × 10-8 mbar to 1 × 10-2 mbar.
The Delta V Series instrument is equipped with at least one
turbomolecular pump, the main pump 3. The main pump evacuates the
entire analyzer system at a rate of 210 L/s. The space 2 is reserved for the
optional turbomolecular pump. For details, see “Turbomolecular Pumps
of the Analyzer” on page 3-37.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-35
System Description
Analyzer Cabinet

A fan 4 cools the analyzer turbomolecular pumps (main pump), and the
optional differential pump.

Behind the cover plate 6, the collector system is arranged. The collector
system is described in detail at “Collector Systems” on page 3-48.

The main power supply 7 (SP480-24, 24 V, 20 A, 480 W) provides


power for the turbomolecular pumps and for several electronic boards,
for example, inlet board, Dual Inlet board (if available), data logger
board, power distribution board.

The magnet 8 is part of the analyzer and is described at “Electromagnet”


on page 3-59. It is controlled by the magnet current regulator which
provides the energy necessary to generate the magnetic field.

Three-Way Valve and Check Valve


The three-way valve (5 in Figure 3-33) allows evacuating the amplifier
area. It can be switched between Fore Vacuum (FV), High Vacuum
(HV), Vent and 0. For details, see “Amplifier Area and Three-Way
Valve” on page 9-55.

A check valve is arranged between three-way valve and analyzer


turbomolecular pump (3 in Figure 3-33). It allows keeping the amplifier
area at vacuum while venting the analyzer.

A Teflon™ tube leads from the three-way valve upwards to the analyzer
turbomolecular pump via the check valve near the three-way valve. See 1
in Figure 3-34. The lower Teflon tube (2 in Figure 3-34) leads from the
three-way valve downwards to the fore vacuum pump of the analyzer.

Labeled Components: 1=to turbomolecular pump of analyzer (required), 2=to


three-way valve and fore vacuum pump of analyzer
Figure 3-34. Check valve near three-way valve

3-36 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

Advantages of the check valve are:

• After the amplifiers have been vented and are now being evacuated
again, they take time to become as stable again as during routine
operation: adsorbed water and gases need time to evaporate and
then to be pumped off.

• The low risk that oil exhalations are sucked in and then intrude the
amplifier area, decreases even further.

Turbomolecular Pumps of the Analyzer


The Delta V Series instrument is equipped with at least one
turbomolecular pump: the main pump, 3 in Figure 3-35 (for position,
see 3 in Figure 3-33).

Labeled Components: 1=flange for optional turbomolecular pump of analyzer


(differential pump), 2=fan for turbomolecular pump(s) of analyzer, 3=required
turbomolecular pump of analyzer (main pump)
Figure 3-35. Turbomolecular pumps of analyzer

The optional turbomolecular pump of the analyzer is not available in


Figure 3-35. Only the flange 1 is shown.

The turbomolecular pump of the analyzer (main pump, 3 Figure 3-35;


Pfeiffer HiPace™ 300) is always required and usually sufficient to
evacuates the entire analyzer system. It has a magnetic screen to be
protected from the magnetic stray field.

A second turbomolecular pump (for position, see 2 in Figure 3-33) may


be used as a supportive option for the main pump. This HiPace 80
pump, manufactured by Pfeiffer, evacuates the analyzer at a rate of
approximately 60 L/s.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-37
System Description
Analyzer Cabinet

As it pumps the ion source area, the main pump must pump less gas,
and the analyzer vacuum is improved. Better abundance, peak shape,
and improved signal-to-background ratio at high ion source pressures
are thereby obtained. This differential pump is used for particular
critical measurements, for example, high-end measurements operating a
Dual Inlet system, when minimal abundance is mandatory.

If a differential pump is available, ion source housing and analyzer


housing are separated by a metallic differential blind. See Figure 3-36. In
this case, analyzer area and ion source housing are pumped off each by a
separate pump.

Figure 3-36. Differential blind

If no differential pump is available, the main alone pump pumps off


both ion source housing and analyzer area.

Working Principle of the Turbomolecular Pumps


The turbomolecular pumps work completely mechanically by rotor
disks imparting momentum to the gas molecules. Baffles or cryogenic
traps are not necessary for retention of pump fluid vapors.

The vacuum system is roughed by rotary pumps through the


turbomolecular pumps. The turbomolecular pumps are started at
atmospheric pressure. This arrangement also obviates the need for a
high vacuum pump valve. The rated capacity of pump speed is available
without restriction at the connecting flange of the source housing.

As the molecular pump principle works in the molecular flow region


only, the turbomolecular pumps require a fore vacuum pump. This
pump is roughing the vacuum system through the turbomolecular
pump down to the upper limit of the turbomolecular pump operating
range.

3-38 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

The turbomolecular pumps installed in the instrument are air-cooled. In


case of a mains failure, there is a delayed venting provided by a venting
valve. When starting the turbomolecular pump, the venting valve is
closed immediately. After stopping (by mains failure or switch-off ),
delayed venting is performed. The vent valve remains open until the
next start cycle of the electronic unit. In absence of current, the valve is
open.

Each turbomolecular pump has an integrated control electronics and


power supply. The pumps are started with the switches on the control
panel. See “Control Panel” on page 3-6. In addition to the LEDs on the
control panel, several LEDs for error indication are directly attached to
the turbomolecular pumps.

For the type of error and details regarding function and design of the
turbomolecular pumps, refer to the Operating Manual of the pump
manufacturer. Both LEDs can easily be monitored by holding a white
piece of paper slantingly beneath the pump.

To drastically increase lifetime during operation at elevated


temperatures, both turbomolecular pumps of the analyzer are protected
by heat sinks.

Analyzer
Figure 3-37 schematically shows the analyzer.

Figure 3-37. Schematic of analyzer

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-39
System Description
Analyzer Cabinet

NOTICE When you turn the switch to the High Vacuum position (HV, see
Figure 9-44) and then turn off the analyzer, the analyzer block stays
evacuated. Do not try to open it.

To avoid damaging of the aluminum-made parts, do not use any


mechanical tool to force opening of flanges. Instead, after first venting
correctly and then loosening the screws, any flange can be easily
removed.

The monolithic analyzer has been milled out of a single aluminum block
(monoblock). This increases stability and facilitates evacuation
compared to an analyzer consisting of several separated blocks.
Figure 3-38 schematically shows the dismounted analyzer block.

7
6
1

5 4

Labeled Components: 1=needle valve controls, 2=position of optional


turbomolecular pump of analyzer (differential pump), 3=ion source,
4=amplifier housing, 5=cup assembly, 6=magnet, 7=position of required
turbomolecular pump of analyzer (main pump)
Figure 3-38. Analyzer block - dismounted

The gaseous sample is fed into the ion source via the inlet system. In the
ion source, ions are generated in a high vacuum by the impact of
electrons. The ions are then accelerated to energies of up to 3 keV and
focused by electrostatic lenses to form a beam.

3-40 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

The ion beam exits the ion source into the magnetic field through a slit
with a fixed width of 0.2 mm. It enters the magnetic field boundary at
an angle of 26.5° and traverses the 90° magnetic sector field. Part of the
ion beam exits at the same angle of 26.5°.

Due to shaping and dimensions of the magnet, not only a focusing in


X-direction, but also in Y-direction is achieved. The refraction power
(X-direction) is half as much as compared to the same magnet without
shaping it. The focal length decreases and its value is the same for X-
and Y-direction. Consequently, mass dispersion increases compared to
the conventional arrangement, where the beam enters and exits the field
normal to the boundaries. The 9 cm-radius system has the same mass
dispersion as the conventional 18 cm arrangement (where the beam
enters and exits the field normal to the boundaries with a sector radius
of 18 cm).

The magnetic sector field is generated by an electromagnet with a


maximum field strength of 0.75 T. It covers a mass range up to m/z = 80
for the Delta V Advantage instrument and m/z = 96 for the Delta V Plus
instrument at full accelerating voltage.

The mass setting is achieved by varying magnetic field strength and/or


accelerating voltage. The relation between mass number m/z of the ions
reaching the ion collector and magnetic field strength H is given by:

m = k  H2
---- M
z

with z the number of charges on the ion, and


2
r
= --------
kM -
2U

with

r: nominal radius of ion path (r = 9 cm = const.)


U: accelerating voltage.

Due to the variable accelerating voltage U, kM is not a constant value as


well, but a function of U.

U and H can be varied to allow different species to be analyzed. A


specialty of this instrument is to allow for fast switches between gas
species (jump calibration). During a measurement, U and H are kept
constant to allow for a single gas species to enter the cups.

Example: For the special case of U = 3 kV, kM = 1.35 × 10-6 m2/V


results.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-41
System Description
Analyzer Cabinet

Usually, Universal Triple detectors are used. The HD collectors are


positioned in the housing of the collector systems. Their exit slit width
is 2 mm. For the middle narrow cup, the resolution below results:

m
------- = 110 (10% valley)
m

In the special case of C, N, O, and S-collectors (in short CNOS


collectors), MEMCO detectors are applied. Their collector slit width is
1.4 mm for the middle cup of the Universal Triple collector. See also
“Collector Systems” on page 3-48.

Analyzer Heater
The aluminum-made analyzer is equipped with a heater
(power-controlled, 200 W). Turning it on heats out the analyzer.
Substances adsorbed on the aluminum surface, primarily water, but also
hydrocarbons (for example, if pump oil has intruded the analyzer in case
of an accident), desorb and are removed.
Usually, for example after cleaning the ion source, the analyzer heater
does not need to be used. After extensive maintenance or service
operations however, turning it on facilitates regaining vacuum: typically,
vacuum first worsens before it improves. The initial pressure value is
regained or even outreached not until the heater is finally turned off. If
no gas has been let in, pressures up to 5 × 10-8 mbar can be obtained
within the analyzer after heating it out. If the pressure is much too high,
peaks become rounded and skew.

The MS State window in Instrument Control of Isodat is used to turn


the analyzer heater on and off. The appropriate temperature is then
automatically reached (maximally about 40 °C to 50 °C). If the analyzer
heater is on, mostly the ion source heater should be on as well, because
then both increase temperature.

Tip Isodat switches off the analyzer heater after 12 h. This prevents
the electronics from damage due to permanent heating.

3-42 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

Ion Source
The ion source is mounted on the front flange for easy maintenance.
Correct alignment of the ion source relative to the analyzer tube is
achieved by fitting the surface to the analyzer head. Figure 3-39 shows
how the Dual Inlet system is coupled to the ion source.

Figure 3-39. Coupling of Dual Inlet system to ion source (Delta V Advantage
instrument)

The ion source of the Delta V Series instrument is designed for high
sensitivity (due to high gas density) and linearity. To ensure high
sensitivity, the ion source is of gas-tight design. The sample gas enters
the ionization chamber through the Changeover valve or the manually
operated needle valve. It leaves it only via small apertures, which are
required as a passage for the electron beam and the ions exiting into the
analyzer. The aperture limits the width of the ion beam and guides it. So
the beam can be focused and hits the magnet accurately.

In case of the Delta V Plus instrument, the ion beam is wider. The focus
quad allows utilizing a larger portion of the original ion beam coming
from the ion source, therefore increasing peak shape, sensitivity and
resolution.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-43
System Description
Analyzer Cabinet

The Delta V Advantage and Delta V Plus instruments are equipped


with different apertures. Figure 3-40 shows the aperture of the Delta V
Advantage instrument on the left, and of Delta V Plus on the right.

Figure 3-40. Dismounted apertures

Figure 3-41 shows the aperture of the Delta V instrument with the
turbomolecular pump of the analyzer removed.

Figure 3-41. Aperture of Delta V Plus - implemented

The conductivity of these openings is much lower than the pumping


speed of the vacuum pumps. The pressure within the ionization
chamber is about 100 times higher than outside, which leads to high ion
yields. The ions are generated in the source by electron impact
ionization. The ionizing electrons are emitted by a thermionic cathode.
The emission current is held constant by the ion source control board.

Two small permanent magnets are mounted to the ionization chamber,


generating a magnetic field parallel to the electron beam. Due to the
magnetic field, the electrons are focused to a defined part of the
ionization volume. The probability to generate an ion with the aid of
one single electron increases.

The energy of the ionizing electrons is determined by the potential


difference between cathode and ionization chamber. It has a range
between 70 eV and 124 eV. The electron beam leaves the ionization

3-44 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

chamber via a small opening opposite to the cathode. It is collected in


the electron trap, which is held on a positive potential relative to the
ionization chamber.

Extraction plates accelerate ions out of the ionization chamber. The


following lens system consisting of different lenses focuses the ion beam
onto the ion source slit. Mechanical tolerances might cause a slight
out-of-axis deflection of the ion beam. Some of the lenses are half
sections, which are insulated from each other. This construction allows
for compensation by applying different potentials to the halves of the
lenses.

In Isodat, continuous values for the ion accelerating voltage can be set. If
the accelerating voltage is changed, the lens potentials are changed
proportionally with the exception of those of the trap and cathode
voltages.

Setting the accelerating voltage to lower values results in an


enhancement of the mass range beyond 80 for the Delta V Advantage
instrument, and beyond 96 for the Delta V Plus instrument. For
example, setting it to 2.0 kV results in a mass range up to 106 for the
Delta V Advantage instrument and up to 129 for the Delta V Plus
instrument.

Ion Generation
Ions are formed in the ionization housing from neutral gas atoms by
bombardment with electrons. The electrons in turn are formed on a
filament by electric heating. The amount of electrons is determined by
the emission current. See parameter Emission in Figure 3-42.

Figure 3-42. Focus Delta panel in Isodat

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-45
System Description
Analyzer Cabinet

This value can be adjusted in Acquisition or Instrument Control of


Isodat (between 0 and 1.5 mA). Higher values result in higher cup
readings but shorter lifetime of the filament.

The electrons are accelerated towards the ionization volume with a small
voltage traditionally called Electron Energy. This value can be adjusted
between 70 and 150 V. Higher energies yield more ions but may
generate multiply charged ionic species that interfere on certain masses
(for example, He2+ interferes with H2).

After leaving the ionization volume, the electrons are collected on an


electrode called Trap with a potential more positive than the ionization
volume. This potential can be adjusted between 0 and 40 V. Higher
values correspond to higher collection efficiency but also higher energy
spread of the ion beam.

Trap Current and Box Current


To control the quality of ion generation, two separate electron currents
in the source are continuously monitored and displayed in the MS
window. See right part of Figure 3-43.

Figure 3-43. Monitoring two separate electron currents

The Box current is the part of the electron current that hits the
ionization housing. The Trap current is the portion of the electron
current that reaches the trap (as intended). A ratio of the Box current
and Trap current of approximately 1:1, or further in favor of the Trap
current, indicates an effective electron collection.

Deviations from these values indicate upcoming problems concerning


the filament.

3-46 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

Lenses
The ion source of the Delta V Series instruments contains four pairs of
lenses: two pairs in front of the beam-defining slit and two pairs behind
this slit. See Figure 3-44.

ion beam line towards the cups

X-Deflection

Y-Deflection
Extraction

X-Focus
Box

Slit
COM = BDAC

+200..+500 V
COM..-400 V

COM..-400 V

0..+100 V

Figure 3-44. Lens arrangement and ion source potentials

The lenses are named starting from the ionization volume Extraction.
Their purpose is to form the ion beam and to guide it through the ion
optical system (magnet, flight tubes) towards the cups.

The first two pairs of lenses (Extraction and Focus) have the purpose to
form an ion beam and produce a focal point in the position of the slit.
These lenses define the beam strength at the point of the slit and further
down the beam towards the cups. They can be adjusted absolutely in
voltage, and a voltage difference between the lenses of a pair can be
adjusted.

The X-Deflection and Y-Deflection lenses are used to fine-adjust the


complete beam into the flight tube. The effect is smaller than that for
the above mentioned lenses, and larger changes in voltage must be
applied to induce an effect on the beam.

As is denoted by the respective names, the X-Deflection lens (unipolar -


only one lens plate can be adjusted) is used to move the beam in the
plane of magnetic deflection, whilst the Y-Deflection is used to move the
beam perpendicular to that plane. The Y-Deflection has an important

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-47
System Description
Analyzer Cabinet

additional purpose: setting an absolute voltage on these plates causes the


beam to change its focal point in the Y-direction (perpendicular to the
plane of magnetic deflection).

The Delta V Plus instrument additionally contains a quadrupole lens to


fine-adjust focal lengths in X-direction and Y-direction.

Collector Systems
Several configurations of collector systems for ion detection are
available, the MEMCO and the Universal Triple system. User-tailored
collector systems can be installed as well.

The collector system is installed within the collector system housing. For
HD isotope analysis, an optional collector system with two Faraday cups
and amplifiers is available. The HD collector system is also installed
within the collector system housing.

Each collector cup has its own amplifier, and the feedback resistor of the
amplifier can be matched to the abundance of the isotope to be collected
in this cup. Each collector cup and its amplifier are connected to a
Voltage-to-Frequency Converter (VFC). Up to ten amplifiers can be
used to support up to ten cups. They are allotted to one of the ten
counters, forming a measuring channel. See Figure 3-45.

U/I Current
Amplifier 50 V Divider 1/5 10 V --> 4.4 μA to Frequency Line Driver

Figure 3-45. Components forming a measuring channel

3-48 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

The converters transform the analog ion current signals into pulses. The
pulses are fed to counters for a pre-selected integration time. At the end
of each integration interval, the number of counts is read and the ion
current ratios are calculated. See Figure 3-46.

mass cup amplifier VFC counter


HD CO2
2 1

44 2

45 3
Digital Signal
46 4 Processor (DSP) computer

3 5

8
In the same manner for cup 9 and 10

Figure 3-46. Schematic of ion detection system

The collector systems cover the mass range from m/z 10 to m/z 80 for
the Delta V Advantage instrument (and to m/z 96 for the Delta V Plus
instrument) at 3 kV accelerating voltage, allowing a resolution of
m/m = 110 (10% valley) for both instruments. Owing to the high
dispersion of the analyzer system, the distance between the collectors is
extremely large (for example, approximately 4 mm between m/z 44 and
m/z 45).

The Faraday collectors have been designed as deep, shielded buckets


with integrated secondary electron suppression shields. See Figure 3-47.

collector slit
ions

to amplifier

secondary electron
suppression shield

Figure 3-47. Layout of a Faraday collector cup

Effects that might degrade the ion current measurement are eliminated.
In most cases, Universal Triple collectors consisting of a narrow and two
wide cups are used. On demand, a MEMCO collector system is
delivered.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-49
System Description
Analyzer Cabinet

Only in case of a Universal Triple collector and a Universal Triple


collector plus H/D, the pin positions are predefined.

Depending on the special application, completely different, individual


cup configurations may be reasonable when, for example, not all of the
ten amplifiers need to be used. Or if several gases or ions are to be
measured simultaneously, special collectors may be needed with more
than five amplifiers. Examples for these particular or combinative
applications are:

• atmospheric measurements of CO2, N2, Ar

• simultaneous measurement of SO/SO2

• additional measurement of H2, SF6, Kr

When operating with more than five amplifiers, a closing plate must
be mounted above the uppermost amplifier. It shields magnetic fields
and enables switching between amplifiers.

Universal Triple Collector System

The Universal Triple collector system is suitable for N2, O2, CO2 and
SO2 measurement. It consists of one small and two wide, individually
shielded deep Faraday cups. See Figure 3-48.

Figure 3-48. Schematic of Universal Triple system

The Universal Triple collector system can be accessed together with the
optional HD collector system during one experiment (for example, for
background checks).

3-50 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

The Delta V Advantage instrument offers switchable amplifiers. When


switching from one gas to another, the resistors are changed and
adjusted with Isodat (including high voltage). See Table 3-11.
Table 3-11. Cup assignment of Universal Triple collector system
Gas Cup 2 Cup 3 Cup 4
N2 28 29 30
O2 32 33 34
CO2 44 45 46

Figure 3-49 shows collector arrangements for different masses for the
Delta V Advantage and the Delta V Plus instrument.

Figure 3-49. Collector arrangements and masses

MEMCO Collector System

The MEMCO collector system comprises three up to six identical cups.


The 3-cup version allows simultaneous measurement of two isotope
ratios from the same sample (for example, 13C/12C and 18O/16O of
CO2).

Tip Different gases may jointly use one cup to reduce the total
number of cup measuring channels.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-51
System Description
Analyzer Cabinet

Universal CNOSH Detector

The Universal CNOSH detector is a 5-cup detector (3-cup with


additional HD cups). Figure 3-50 shows a schematic.

Universal CNOSH Detector

m/z 3 (HD)

m/z 2 (H2)

 m/z 44, 45, 46


 m/z 28, 29, 30
 m/z 32, 33, 34
 m/z 64, 66

Figure 3-50. Universal CNOSH detector

HD Collector System

The HD collector system is a dual Faraday collector assembly for


hydrogen isotope measurement on the same ion path, operating in
parallel to the MEMCO or Universal Triple systems. The HD collector
is located in the common collector system housing. The collector cups
are designed like those of the MEMCO system.

3-52 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

Figure 3-51 shows the implemented collector system with its important
parts.

1
6

4
3 2

Labeled Components: 1=feedthrough to amplifiers (and ground plane cup and


ground plane amplifier), 2=SE feedthrough, 3=feedthrough for retarding
voltage, 4=24 V power supply, 5=SE wires, 6=collectors (arranged below)
with retaining screws, 7=SE suppression voltage distributor
Figure 3-51. Collector - implemented

Figure 3-52 shows the dismounted collector system in top view.

Figure 3-52. Collector system (dismounted) in top view

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-53
System Description
Analyzer Cabinet

Figure 3-53 shows a schematic of the collector system in side view.

Labeled Components: 1=H2 collector (m/z = 2), 2=Universal Triple collector


(m/z = 28, m/z = 46), 3=HD collector (m/z = 3), 4=retarding lens connector
Figure 3-53. Schematic of collector system in side view

Figure 3-54 shows the assignment of the amplifier numbers 1 to 10 to


the cups.

7 6 8

3 9

10
4

1
5
2

Figure 3-54. Feedthrough to amplifier number

The view in Figure 3-54 is from inside from the cup housing towards
the feedthrough. The arrow is directed upwards. The cup for m/z 28 is
assigned to amplifier No. 2. The cup for m/z 29 is assigned to amplifier
No. 3. The cup for m/z 30 is assigned to amplifier No. 4.

3-54 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

NOTICE To avoid damaging of the aluminum-made parts, do not use any


mechanical tool to force flanges to open. After first venting correctly
and then loosening the screws, any flange can easily be removed.

Figure 3-55 shows the numbers 1 to 13 of the individual pins of the


feedthrough.

view from inside view from outside


8 13

7 9

6 10
13 8 7
9
6
10
12
12 1 1
2 5
11
3 4
5 2
11
4 3

Figure 3-55. Feedthrough of ion source

The ion source connector board indicates which electrical connector


leads to which lens plate within the ion source. To locate the ion source
connector board, see Figure 3-30. For connectors to the ion source
connector board, see Figure 9-3. See also “Lenses” on page 3-47.

Amplifiers and VFCs


The DC amplifiers have 100% inverse feedback. Their output voltage
(50 V maximum) is the product of the input current and a feedback
resistor. The feedback resistor must match the abundance of the isotope
to be collected in the respective collector cup. Table 3-12 shows the
resistor values to be used for isotopes of different gases.

Table 3-12. Resistor values matching natural abundance of isotopes


Gas Mass [m/z] Resistor [ Capacity [pF]
H2 2 1 × 109 150

3 1 × 1012 2
N2 28 3 × 108 470

29 3 × 1010 5

30 1 × 1011 2

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-55
System Description
Analyzer Cabinet

Table 3-12. Resistor values matching natural abundance of isotopes,


Gas Mass [m/z] Resistor [ Capacity [pF]
8
O2 32 3 × 10 470

33 1 × 1012 2

34 1 × 1011 2
8
CO2 44 3 × 10 470

45 3 × 1010 5

46 1 × 1011 2
8
SO2 64 3 × 10 470

66 1 × 1010 15

The product R × C is approximately a constant equaling the time


constant of the amplifier. Usually, it amounts about 0.1 to 0.2 seconds.

The amplifiers of the Delta V Series instrument allow for two settings of
amplification factors. They are switched and controlled in the Cup
Settings window of the Configurator of Isodat. See Figure 3-56.

Figure 3-56. Cup settings window

Tip In the Acquisition of Isodat, you set the cup readings in the Gas
Configuration Editor.

3-56 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

For details on the amplifiers and resistors, see “Amplifiers and VFCs” on
page 3-55.

The column Resistors in Figure 3-56 is always used. The column


Resistor 2 can additionally be switched as an option. This is stored in
the Gas Configuration as well.

The black triangle next to the mass value in Figure 3-57 shows that the
second resistor is switched on. When no triangle is shown, only the first
resistor is active.

Figure 3-57. Indicator for active second resistor

A right-click on the mass value opens the context menu. Selecting High
Amplification activates/deactivates the second amplifier.

Arrangement of Several Amplifiers


The resistors and a capacitor form a RC combination. Usually, an
amplifier contains one specifically chosen RC combination to
accomplish a particular amplification according to the individual
measurement problem. However, RC combinations can be arranged in
parallel. The additional RC combination enables switching between
amplifiers which is handled by Isodat. See “Amplifiers and VFCs” on
page 3-55.

The gold-made contact is the transfer point for the ion current (from
cups to amplifier board). The offset potentiometer controls the offset.
When the amplifier was calibrated, the potential was set to 0 V. The
attenuation potentiometer controls the time constant and yields the
optimal characteristic of the RC combination as it avoids over- and
undershooting.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-57
System Description
Analyzer Cabinet

NOTICE Do not touch the surface of the high-impedance resistors. Even a slight
touch of a fingertip contaminates the resistors resulting in signal
instability. If you accidentally touched a resistor, clean it with
methanol.

Do not change the offset potentiometer. It has already been adjusted


by Thermo Fisher Scientific.

The amplifier housing is a component of the analyzer block. Space for


ten amplifiers offer increased flexibility for simultaneous measurement
of several gases.

Figure 3-58 shows how several amplifiers are arranged in slots. The
visible green board is amplifier ground plane.

Labeled Components: 1=connectors between amplifier and ground plane


(5 ×), 2=contacts to the collectors (5 ×), 3=13-fold feedthrough,
4=arrangement of amplifiers
Figure 3-58. Arrangement of amplifiers

When operating with more than five amplifiers, a closing plate must
be mounted above the uppermost amplifier. It shields magnetic fields
and enables switching between amplifiers. Do not remove this closing
plate.

3-58 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet

Electromagnet
The magnetic field providing the ion deflection is generated by an
electromagnet (8 in Figure 3-33) with a maximum field strength of
0.75 T. The selection of the different masses is achieved by changing the
magnetic field. In addition, the covered mass range can be extended by
continuously varying the accelerating voltage.

The magnet is directly sealed into the aluminum block behind the
analyzer. See Figure 3-59.

Figure 3-59. Position of magnet behind analyzer

Its two magnetic coils have been arranged in a shape reminding of


spectacles. This shape reduces the stray field and saves space compared
to one large magnetic coil.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-59
System Description
Electronics Cabinet

Electronics Cabinet
The electronics cabinet is located at the rear of the Delta V Series
instrument and contains complicated circuits.

NOTICE Only qualified, skilled electronics engineers should perform servicing.


Keep the rear panel doors closed. They may only be opened by a
Thermo Fisher Scientific field service engineer in case of severe
electronic problems. A dedicated tool is required. Opening the
electronics cabinet is only allowed for maintenance purposes by
qualified personnel.

Thermo Fisher Scientific recommends calling a Thermo Fisher


Scientific field service engineer if servicing is required. Before calling,
try to localize the defect. A precise description of the defect eases the
repair and reduces costs.

Thermo Fisher Scientific recommends using Thermo Scientific spare


parts only, because many parts are specially selected. When replacing
fuses, only use the correct type.

Focus Quad Power Supply Board


The Focus Quad power supply board is available only in the Delta V
Plus instrument.

The Focus Quad power supply board provides a DC voltage between


-20 V and +20 V. As with the other lens voltages, the value of the Focus
Quad voltage can be adjusted and focused between -100%, 0 and
+100% in the Instrument Control or Acquisition of Isodat. See
Figure 3-60.

Figure 3-60. Focus Quad with Delta V Plus instrument

3-60 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Electronics Cabinet

As ion focusing is facilitated, the sensitivity of the IRMS increases, and


the peak shape is enhanced.

Power Supply for Amplifiers and VFC


The power supply for amplifiers and Voltage-Frequency Converter
(VFC) is a 55 V power supply. It provides the different supply voltages
for the amplifiers.

Power Distribution Board


The power distribution board (also called power distributor) regulates
major parts of the IRMS, because it:

• maintains vacuum safety as it controls fore vacuum pumps,


turbomolecular pumps and control panel.

• switches the relays of heaters.

• controls the Penning gauge by reading out its set trip: when the
pressure falls below the set trip, the ion source control board is
switched on.

• controls the magnetic field.

To change the magnetic field, Isodat sends a signal along the serial
data link cable. This signal is transformed into a voltage on the
power distribution board. This voltage in turn regulates the magnet
current regulator. Finally, the magnet current regulator provides the
energy that is necessary to create a new magnetic field.

Additional vacuum gauges can be connected to the vacuum sensors


without affecting vacuum security. The connection to the Penning
gauge for high vacuum measurement is important for vacuum security.

The connections of the 230 V consumers are connected to the


following:

• Mains from fuse and main switch

• 24 V power supply, not switched

• 55 V power supply (socket J503), not switched

• Refill equipment

• Inlet valve heater (socket J1112)

• Ion source control board (socket J322)

• Analyzer heater

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-61
System Description
Electronics Cabinet

• Ion source heating

• Inlet system heater (socket J1110)

• Inlet pump (socket J1109)

• Pump source and analyzer (socket J1108)

• Source heater (socket J1113)

Figure 3-61 shows the controls for refill equipment.

Figure 3-61. Controls for refill equipment

The settings of trimmers determine trigger thresholds:

• LED “N2 OFF” is on when liquid nitrogen has reached maximum


level.

• LED “N2 ON” is on when liquid nitrogen has fallen below


minimum level.

• LED “N2ALERT” is on when liquid nitrogen has reached a critical


level.

• LED “REFILL” is on when refill is switched on.

3-62 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Electronics Cabinet

Electronic Components for Data Acquisition


Some electronics components are located outside the electronics cabinet.
They are mainly related to data acquisition. Figure 3-62 outlines the
communication between the computer and several electronic boards.

PCI Fiberline
PC Bus Master
Dual Inlet Board

Power Distribution
Board

Bus Repeater (on


Inlet Board) Ion Source
High Level

Inlet Board
Ion Source
GND Level

Figure 3-62. Communication between computer and boards

Grounding of the Delta V Series Instrument


The yellow-green ground wires shown in Figure 3-63 shield against
high-frequency disturbances into or from the IRMS in accordance with
the criteria of electromagnetic compatibility (EMC).

Labeled Components: 1=ground bolt


Figure 3-63. Ground wires

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-63
System Description
Electronics Cabinet

At several grounding points within the instrument, ground wires are


connected to metallic parts with low-impedance. The ground wires are
installed by Thermo Fisher Scientific. The ground bolt of the electronic
cabinet (1 in Figure 3-63) is shown as an example. For details, see “PE
Connector” on page 3-18.

For the grounding of the instrument, yellow-green ground wires must


be used exclusively.

3-64 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
4
Dual Inlet System (Optional)

This chapter describes functional units of the optional Dual Inlet system
(valves, Multiport, Microvolume, Changeover valve, and Changeover
Extension, for example).

Contents

• Layout of the Dual Inlet System on page 4-2

• Working Principle of the Dual Inlet System on page 4-4

• Valves of the Dual Inlet System on page 4-5

• Compressed Air Distributor on page 4-8

• Changeover Valve on page 4-8

• Changeover Extension on page 4-12

• Multiport on page 4-12

• Microvolume on page 4-15

• Autocool Refill Device on page 4-19

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-1
Dual Inlet System (Optional)
Layout of the Dual Inlet System

Layout of the Dual Inlet System


Figure 4-1 schematically shows the Dual Inlet system.

Figure 4-1. Schematic of Dual Inlet system

The Dual Inlet system is controlled by the Dual Inlet board. See “Dual
Inlet Board” on page 3-28.

The Dual Inlet system only needs one fore vacuum pump (fore vacuum
pump of Dual Inlet system). See “Fore Vacuum Pumps” on page 3-23.

The components of the Dual Inlet system (valve blocks, Changeover


valve, Changeover Extension, Multiport, Microvolume, for example) are
heated by the inlet heaters. The inlet heaters are provided with energy by
arbitrary sockets of the socket group 1 in Figure 3-27.

4-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Layout of the Dual Inlet System

Figure 4-2 shows the Dual Inlet system mounted in the Delta V Series
instrument. Left and right bellow are shown. The descriptions are
applicable for both bellows.

left bellow right bellow

7
3

4
5
6

Labeled Components: 1=stainless steel capillary, 2=compressed air


connector, 3=Swagelok™ connector, 4=pressure transducer, 5=connector
leading to Dual Inlet system (stainless steel capillary, only with
Microvolume), 6=connector leading to Changeover valve (stainless steel
capillary, only with Microvolume), 7=brass contact in center of capillary for
current entry
Figure 4-2. Dual Inlet system in front view (behind upper door)

The stainless steel capillary (1 in Figure 4-2) leading to the Changeover


valve is surrounded by an insulating silicone tube and is connected with
a Swagelok™ connector 3.

Compressed air is connected at 2. The pressure transducer 4 measures


the actual pressure within the individual bellows.

The connector 5 for a stainless steel capillary leads to the Dual Inlet
system and is only available if a Microvolume is installed. The connector
6 for a stainless steel capillary leads to the Changeover valve and is only
available if a Microvolume is installed.

An alligator crimp can be connected to the brass contact 7 in the center


of the capillary. The current from a connected power supply unit can
enter and heat out the capillary. For details, see “Baking Stainless Steel
Capillaries” on page 9-42.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-3
Dual Inlet System (Optional)
Working Principle of the Dual Inlet System

Working Principle of the Dual Inlet System


The Dual Inlet system of the Delta V Advantage instrument has been
symmetrically designed and allows alternating measurements of a
sample and a standard gas. If the instrument is equipped with a Dual
Inlet system, the configuration is identical for the sample side and the
standard side, which enables balanced flow. Each inlet side has two ports
and a variable volume (bellow) with the respective inlet capillary leading
to the Changeover valve. For very small samples, a Microvolume with its
own capillary can be installed.

Before measurements can be performed and results be compared, equal


gas conditions for pressure and flow must be provided for both, sample
and standard gas, to obtain a balanced ion beam intensity. Pressure
adjustment for sample and standard gas is performed in reservoirs
(bellows), which are adjustable in volume. These variable volumes are
operated by software-controlled bellow motors.

An automated procedure balances the volumes to such an extent that


the ion beam intensity of a selected mass attains a preset value. As it is
not possible with Isodat in some cases, balancing of the volumes can also
be performed separately. The bellows are adjustable from about 3.5 to
40 mL each.

Precise isotope ratio determination with Dual Inlet measurement


requires a stable gas flow into the ion source. To obtain this, bellow
balancing of both sides is essential. Bellow balancing is called Pressure
Adjust in Isodat. See “Pressure Adjustment” on page 6-65. If sample gas
flows into the ion source, an equal amount of a standard gas is evacuated
simultaneously by the waste line pump system or vice versa so that the
flow conditions remain identical during measurement.

Flow conditions are also matched by adjusting the flow resistance


through the capillaries to the ion source. The flow resistance is set to
equal conditions by crimping the capillaries in front of the inlet port of
the Changeover valve. The crimps of the capillaries are factory-set, but
must be set anew when a capillary is replaced. How to crimp a capillary
to a specific flow resistance is described at “Baking Stainless Steel
Capillaries” on page 9-42 and at “Replacing Capillaries” on page 9-45.

The bellows adjust the pressure for larger samples (> 50 bar × μL). Very
small samples, as low as 5 bar × μL, can be analyzed with the optional
Microvolume. For details, see “Microvolume” on page 4-15.

To avoid any condensation, to remove impurities, or to measure SO2,


the Dual Inlet system including the Changeover valve and the ion
source can be heated up to 80 °C.

4-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Valves of the Dual Inlet System

Valves of the Dual Inlet System


The Dual Inlet system is operated by pneumatic valves with a nominal
closing pressure of 5 bar (500 kPa; 73 psi). Although the valves are made
of stainless steel, check them for wear after long-term operation. All the
valves base upon the same construction principle.

Parts of a Valve
Figure 4-3 shows a pneumatic valve with its high-vacuum side opened.

6
1

5 2

4 3

Labeled Components: 1=gold plunger, 2=stainless steel membrane,


3=Swagelok connector for gas inlet, 4=knife (gas exhaust), 5=gold gasket,
6=hole (gas inlet), 7=stainless steel valve block
Figure 4-3. Valve of Dual Inlet system

The stainless steel membrane (2 in Figure 4-3) is turned down by 180°


and then laid onto the gold gasket 5, with the gold plunger 1 oriented
downwards. The plunger fits exactly to the edge. The gold gasket seals
the valve block against the membrane.

The Swagelok™ connector for gas inlet 3 is laterally welded on the valve
block. The knife 4 is located in the center of the valve block and also
serves as gas exhaust. The hole 6 acts as gas inlet to the valve.

The parts of such a valve, see Figure 4-4, are made of stainless steel.

5 4 3 2

Labeled Components: 1=screws for cap (4 ×), 2=covering cap, 3=actuator for
compressed air, 4=stainless steel membrane, 5=valve block
Figure 4-4. Parts of a Dual Inlet system valve

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-5
Dual Inlet System (Optional)
Valves of the Dual Inlet System

The screws 1 in Figure 4-4 fasten the covering cap 2 to the valve block 5.
The actuator for compressed air 3 usually lies within the rear side. For
details, see “Operating Pneumatic Valves” on page 4-10. The valve plug
of the stainless steel membrane 4 closes the valve. A sleeve not shown
here is attached to its rear side.

Arrangement in Valve Blocks


Compressed air is either supplied by an optional compressor connected
to the IRMS or by a laboratory pressure air line. The metal valves are
equipped with gold gaskets and gold seats acting on knife-edges. Up to
six valves are machined into one monoblock, thus considerably reducing
the volume in plumbing as well as possible leakage of the installation.

This monoblock type of valve block is used throughout all inlet


modules. Figure 4-5 shows a schematic of a monoblock.

Figure 4-5. Double valve block

For plumbing, the valve blocks are fitted with 1/4 inch Swagelok™
connectors. Compressed air is fed to the pneumatically operated valves
by solenoid valves. These are controlled by dedicated electronics linked
to the computer.

4-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Valves of the Dual Inlet System

Manifold Block with Solenoid Valves


Four of the solenoid three-way valves are located on a manifold block.
See Figure 4-6. The solenoid valves are operated by a voltage of 24 V.
The voltage is supplied by the Dual Inlet board and the connector 2 in
Figure 4-6.

Labeled Components: 1=LED for individual switching status (on/off) (4 ×),


2=connector to Dual Inlet board
Figure 4-6. Manifold block with four solenoid valves

The solenoid valves are normally open (with the exception of


TubeCracker). The working condition is signaled by a red LED located
on the printed circuit board. The actuators for compressed air transform
a signal A into another signal B and switch an electrical signal generated
at the Dual Inlet board into a compressed air signal. Thereby,
compressed air is provided which forcefully switches the actual valves.

Tip In case of a power failure, all solenoid valves open automatically


(with the exception of TubeCracker, where they close automatically).
The pneumatic valves in the entire Dual Inlet system close, avoiding
contamination.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-7
Dual Inlet System (Optional)
Compressed Air Distributor

Compressed Air Distributor


The compressed air distributor, Figure 4-7, is part of the Dual Inlet
system. Therefore, it is only available when a Dual Inlet system is
installed.

Labeled Components: 1=connection where compressed air enters, 2=blind


plug, 3=tubing connection
Figure 4-7. Compressed air distributor

The compressed air connections of the distributor are all equivalent


ones. Compressed air enters at 1 in Figure 4-7 and is then distributed to
all compressed air valves.

The number of compressed air valves of the system depends on which


particular options for the Dual Inlet system are available. If only a few
compressed air valves are connected to the compressed air distributor,
you should close the unused connections tightly with blind plugs 2.

Changeover Valve
The Changeover valve allows maintaining a continuous flow of gas as it
switches between reference gas flow and sample gas flow in the range of
some tens to some hundred mbar × L × s-1 each. Alternately, one gas
flow is continuously led into the ion source (evacuated by the
turbomolecular pump of the analyzer), whereas the other gas flow is
continuously pumped off by the turbomolecular pump of the Dual Inlet
system.

Layout of the Changeover Valve


The Changeover valve consists of a single block attached to the analyzer
housing and accepts the coupling of capillaries for sample and standard
gas. It is operated either automatically by Isodat, or directly with the
monitor display of the inlet schematic.

4-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Changeover Valve

Figure 4-8 shows the position of the Changeover valve upon the
analyzer.

Figure 4-8. Changeover valve

Made of two metallic blocks which contain four individual valves each,
the Changeover valve allows repeatedly alternating between sample gas
and reference gas. Switch between “no gas into the ion source“, “gas
from the right bellow into the ion source“, and “gas from the left bellow
into the ion source“.

Figure 4-9 show the layout of a Changeover valve.

1
2

6
3

5 4

Figure 4-9. Schematics of Changeover valve

The capillaries from the bellows of the Dual Inlet system (or from a
Microvolume) are connected at 1 and 3. 2 connects to the IRMS source
inlet. 4 leads to the turbomolecular pump.

Alternatively to 1, the capillaries can be connected to 6. Alternatively to


3, the capillaries can be connected to 5.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-9
Dual Inlet System (Optional)
Changeover Valve

Operating Pneumatic Valves


A cylinder on top of the valve is actuated by compressed air. The
gold-made plunger (1 in Figure 4-3) presses a membrane (2 in
Figure 4-3) underneath and tightens the valve. Gas transfer is
impossible.

Without compressed air, the cylinder is not actuated. The plunger does
not press the membrane and does not tighten the valve. Gas transfer is
possible.

Figure 4-10 shows the parts of a pneumatic valve.

4 3 2 1

Labeled Components: 1=guide sleeve (made of Pertinax, arranged above


O-ring seal), 2=O-ring seal (seals compressed air plunger against sleeve),
3=compressed air plunger, 4=outer sleeve (compressed air plunger moves
within it)
Figure 4-10. Parts of a pneumatic valve

Connecting Dual Inlet Peripherals Using Stainless Steel Capillaries


By default, Dual Inlet peripherals are connected to the Changeover valve
via stainless steel capillaries. The stainless steel capillaries
(ID = 0.15 mm) have a crimping position.

4-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Changeover Valve

Figure 4-11 shows the connection of a stainless steel capillary to the


Changeover valve.

Labeled Components: 1=heating cartridge, 2=crimping screw (4 ×),


3=stainless steel capillary, 4=crimping position
Figure 4-11. Capillary connections at Changeover valve

A heating cartridge is positioned at 1. Several cartridges are located in


the metal block. They serve to heat out the Changeover valve and
usually do not need to be maintained or replaced.

The crimping screws 2 hold the stainless steel capillary 3. A crimping


position is shown as 4.

Connecting Dual Inlet Peripherals Using Nickel Capillaries


This section describes the alternative option to use pure nickel capillaries
for the connection. Nickel capillaries (ID = 0.127 mm) are available
ready-to-use from Thermo Fisher Scientific.

Besides the Dual Inlet system, a Multiport, a Microvolume, a Kiel


Carbonate IV Device and a Reference Gas Refill Device are among the
Dual Inlet peripherals that can be connected via nickel capillaries. The
Dual Inlet applications include different gases, for example H2, O2,
CO2, and SO2. The use of nickel capillaries is independent of the mass
spectrometer. So far, nickel capillaries have been tested only with CO2.

Nickel capillaries are widely spread in the clumped isotopes technique,


for example when measuring stochastically distributed 13C and 18O in
CO2 samples. They are produced by electroforming. This process
implies highly reproducible inner diameters.

To maintain nickel capillaries, see “Nickel Capillaries” on page 9-47.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-11
Dual Inlet System (Optional)
Changeover Extension

Changeover Extension
The Changeover extension is advantageous when it is required to
automatically switch between various external peripherals. It may be
added to the Changeover valve as an optional extension module. See
Figure 4-12.

Figure 4-12. Changeover extension attached to Changeover valve

The Changeover extension is flanged to the Changeover valve by


1/4 inch Swagelok™ connectors. It provides two additional inlet ports
allowing coupling of further inlet system options (Kiel IV Carbonate
Device, for example).

Additional sample gases can be switched via the two ports. External
peripherals (for example, a ConFlo IV interface) can be connected to it
instead of connecting them to a needle valve.

The Changeover extension is controlled by Isodat, whereas a needle


valve can only be switched manually.

Multiport
The Multiport is a sample manifold inlet system consisting of one or
two banks of 10 ports each. It may be optionally equipped with a
TubeCracker. When employing a Multiport as an inlet system, the
Multiport is connected directly to the sample side of the Inlet System
valve 12 (left inlet port). The valves of the Multiport are operated either
automatically by Isodat, or manually by the monitor display, as is the
Dual Inlet system.

If a Dual Inlet system is available, the Delta V Advantage instrument


may additionally contain a Multiport 10 (10 ports) and/or a Multiport
Extension (10 ports) each. Together they provide 20 additional ports
(“Multiport Extension”).

4-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Multiport

A Multiport allows easily switching between various inlet ports for gases.
The degree of automation is higher than in case of a Dual Inlet system.
In case of gas change, it is not necessary to repeatedly connect new
sample vials at the front side and start measurement manually. Instead,
connect different sample vials to the Multiport at the same time and
then simply start automatic successive measurement with Isodat.

If no Multiport is available, only the two inlet ports of the Dual Inlet
system can be used to let gases flow into the system. If more than two
ports are needed however, a Multiport is required (for example, in case
of automatic successive measurement of different gases after
offline-preparation).

Dismantling the Multiport


Figure 4-13 shows the implemented Multiport 10.

2
6

3
4

Labeled Components: 1=Multiport Extension, 2=socket screws (2 ×), 3=Multiport 10, 4=fixture
Figure 4-13. Top view of installed Multiport

The Multiport Extension 1 is shown in top view. The Multiport 10 is


the lower row of ports 3.

On the right side, both the Multiport Extension and the Multiport 10
are fastened by socket screws 2. On the left side, they are simply attached
to the fixture 4 without screws.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-13
Dual Inlet System (Optional)
Multiport

TubeCracker
The TubeCracker tool (see Figure 4-14) is an option for the Multiport.
After gases have been prepared offline and stored within melted-off glass
ampules, the TubeCracker automatically breaks the ampules at a
pre-determined breaking point. As the TubeCracker is mounted upon a
Multiport, the gas enters the system this way. See also “Multiport” on
page 4-12.

On either side of the TubeCracker, the rubber-sealed Swagelok™


connectors 1 enable holding and cracking glass tubes of any length. The
glass tubes would jut out of the TubeCracker on either side.

3 1

Labeled Components: 1=Swagelok™ connector (2 ×), 2=compressed air connection, 3=connecting piece
Figure 4-14. TubeCracker tool

On the left side of Figure 4-14, the TubeCracker is shown in rest


position. Compressed air is connected at 2. The connecting piece 3 is
protected by a plastic bag. The TubeCracker is mounted onto one of the
Multiport positions.

On the right side of Figure 4-14, the TubeCracker is shown in extended


position after it was operated with compressed air. The glass tube would
have been cracked. The fracture is always located inside the
TubeCracker.

Reference Gas Refill


When working with a Multiport inlet system, a reference gas refill may
be necessary to avoid running out of reference gas during measurements.
The reference gas refill provides the reference gas supply to the inlet
system.

4-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Microvolume

The reference gas refill (Figure 4-15) is a hardware option. It consists of


a metal tank 1 with a manual valve 2 that is connected by a capillary 3 to
one of the inlet ports on the standard side.

3 4
to inlet port

Labeled Components: 1=metak tank, 2=manual valve, 3=capillary, 4=crimping


piece
Figure 4-15. Schematic of reference gas refill

The capacity of the metal tank is about 5 L. With the reference gas refill
selected, the standard side of the inlet system is completely pumped out
before it is filled again for the next measurement sequence.

Microvolume
The Microvolume is an optional inlet module for very small sample
amounts. It may be installed in combination with a Dual Inlet system or
a Multiport. In both cases, the Microvolume is connected to the left
port (valve 12) of the Dual Inlet system.

The Microvolume (Figure 4-16) consists of a cooling finger 1, a valve


block, an Autocool Unit and a separate capillary that leads to the
Changeover valve. The Microvolume contains two valves and a
pumping device.

4 5
3
2

Labeled Components: 1=cooling finger, 2=gasket (gold), 3=washer, 4=copper


rod, 5=fitting
Figure 4-16. Parts of Microvolume - to be inserted into Autocool unit

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-15
Dual Inlet System (Optional)
Microvolume

The total volume in front of the capillary crimp (the “cooling finger”
volume plus the connections including the capillary) is about 145 L.
Due to the viscous flow conditions which require a pressure of at least
15 mbar in front of the capillary, a sample of 3 bar×L to 50 bar×L
must be concentrated into a small volume.

The cooling finger volume can be reduced for even smaller samples by
inserting small steel spheres. The concentration in a Microvolume is
achieved by freezing the small sample using liquid nitrogen and
expanding it again by subsequent heating.

Depending on the gas to be measured, two different types of


Microvolume can be used: for CO2, a smaller Microvolume is used,
whereas a larger one is required for N2. The larger one contains a
molecular sieve to freeze out N2 at liquid nitrogen temperature.
The valves of the Microvolume are operated in the same way as the
other components of the Dual Inlet system (automatically by Isodat or
manually by monitor display). With the Autocool Unit, the temperature
can be set individually within a range of about -180 °C to +155 °C.

The sample gas to be measured (for example, CO2) moves to the cold
cooling finger, which is the coldest place in the tubing system, and is
frozen out.

Then, the valves are closed, and the Microvolume is heated. The sample
gas expands and considerably increases the pressure within the small
volume. Now, measurement by standard-sample comparison is possible,
with the sample in the small Microvolume, and the standard within the
equally small volume between valve 25, valve 26 and the capillary
(shown by the highlighted area in Figure 8-1).

4-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Microvolume

Autocool Unit
The Autocool Unit is an automatic cooling unit for the cooling finger
that supersedes the manual procedure. It is controlled by Isodat: the
temperature of the Autocool Unit is set among the Micro Volume
settings in the Peripherals tab of a method. See Figure 4-17.

Figure 4-17. Microvolume settings in the Peripherals tab of a method

The temperature settings can also be changed directly in the


Microvolume panel. See Figure 4-18.

Figure 4-18. Entering temperature for Autocool Unit

The temperature range between -180 °C and +155 °C can be covered.


The time to get from +50 °C down to -180 °C is less than 2 min. The
time to get from -180 °C up to +50 °C is about 1 min.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-17
Dual Inlet System (Optional)
Microvolume

All parts of the assembly are made of a material with high thermal
conductivity and are placed in close thermal contact to each other,
enabling a quick temperature change. To heat the Microvolume to a
defined temperature, the heater element is activated. The heating phase
is controlled by the temperature sensor.

The Microvolume fits into a thermal contact pipe (2 in Figure 4-19)


attached to the lid of a Dewar vessel. The Dewar vessel contains liquid
nitrogen. An electrical heater element 7, a temperature sensor 1 and a
cascaded arrangement of three small bowls 3 are fitted to the contact
pipe.

3
7

6 maximum water level

minimum water level

Labeled Components: 1=temperature sensor, 2=thermal contact pipe,


3=cascaded arrangement of bowls, 4=hood and standpipe, 5=immersed
heater element, 6=level sensor with three thermistors, 7=heater element
Figure 4-19. Schematic of Autocool Unit

To cool the Microvolume, another electrical heater element immersed in


liquid nitrogen 5 is activated and causes both evaporation and agitation.

Above the heater element, a funnel-shaped hood of a standpipe is


positioned (see 4) which leads to the uppermost bowl of the cascaded
arrangement. This arrangement enables about one droplet of liquid
nitrogen per second to be carried by the stream of evaporated nitrogen.

The level sensor 6 consists of three sensing thermistors, one each for the
maximum, the minimum and the alert level. They are Pt 100 resistors
(100 ).

Small holes in the bottom of the bowls yield a constant trickle of liquid
nitrogen back into the Dewar vessel. The continuous flow of liquid
nitrogen rapidly cools the Microvolume.

4-18 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Autocool Refill Device

By suitably balancing the liquid nitrogen flow and heating the


Microvolume, any temperature within the range can be obtained.

Due to the very small quantity of liquid nitrogen held in the cascaded
bowl arrangement the Microvolume temperature rises very quickly
when the immersion heater is switched off and the pipe heater is
switched on. A constant liquid nitrogen level in the Dewar vessel is
maintained by the liquid nitrogen refill device.

Autocool Refill Device


The Autocool Refill device provides a constant level of liquid nitrogen in
the Dewar vessel of the Autocool unit. It consists of a Dewar vessel of
75 L or 25 L capacity and is equipped with the safety devices, valves and
pressure gauges required for handling liquid nitrogen safely.

Figure 4-20 schematically shows the Autocool Refill device. The 75 L


Dewar vessel is equipped with a level indicator that monitors the liquid
nitrogen content.

level indicator
refill valve electronic
Liquid Fill and (N12)
pressure gauge control board
Decant Valve
relief and pressure control
burst membrane regulator

Trycock/vent
valve
gas use valve pressure-
raising valve

pressure
raising tube
level
sensor

Dewar vessel
Autocool Unit

Figure 4-20. Schematic of Autocool Refill device

The transfer line to the Dewar vessel of the Autocool unit is controlled
by a solenoid-operated refill valve (N 12). The refill valve is directly
connected to the liquid fill and decant valve of the Autocool Refill
device.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-19
Dual Inlet System (Optional)
Autocool Refill Device

The Autocool Refill device is activated by a level sensor installed in the


Dewar vessel of the Autocool Unit. See “Autocool Unit” on page 4-17.
The power distribution board of the Autocool Refill device evaluates the
signals of the sensors and activates the refill valve to start or to end the
nitrogen transfer.

Working Principle
The transfer of liquid nitrogen is affected by a pressure build-up in the
self-pressurizing Dewar vessel of the Autocool Refill device. The
pressure builds up by vaporization of liquid nitrogen in a coiled pressure
raising tube located in the vacuum interspace of the Dewar vessel when
the gas vent valve is closed and the pressure raising valve is opened.

A pressure gauge monitors the pressure. A pressure of 0.35 bar (35 kPa;
5 psi) should be sufficient to transfer liquid nitrogen. A pressure of
0.7 bar (70 kPa; 10 psi) transfers liquid at about 10 L/min. A higher
pressure is not necessary and even wasteful.

As soon as a preset pressure is reached, the pressure regulator installed in


the circulation cuts the flow through the coiled pressure raising tube.
The blow-off valve is set to a limit of about 1.5 bar (150 kPa; 22 psi).
An additional burst membrane prevents building up a dangerous
pressure. The gas vent valve allows bleeding excessive pressure, if
necessary.

Refill Tube for Liquid Nitrogen


The refill tube for liquid nitrogen (for position, see 2 in Figure 3-29) has
been isolated and provides the Microvolume. It is connected to the
liquid nitrogen refill tank (external LN2 tank of 50 L or 100 L).
Depending on the fill level in the Dewar vessel, a refill valve at the refill
tank are opened or closed. Resistor cascades are monitoring three
different fill levels (lower level, middle level and final switch-off ) within
the Dewar vessel.

NOTICE As it cannot be heated, do not allow the cooling finger to be in contact


with liquid nitrogen. The fill level must end well beneath the cooling
finger.

Protective Tube for Fill Level Controller


The fill level controller (6 in Figure 4-19) is protected by a metallic tube.
Otherwise, the fill level controller could repeatedly be switched on or off
by swashing liquid nitrogen.

4-20 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
5
Safety

This chapter contains information that is important for your own safety
or the safety of others, and that prevents damage to the instrument,
Read this chapter carefully before you install or operate the instrument
and its accessories, or come into contact with it.

Contents

• Safety Symbols and Signal Words in This Manual on page 5-2

• Safety Symbols on the Instrument on page 5-3

• Rating Plate on page 5-6

• Intended Use on page 5-7

• Electric Safety Precautions on page 5-9

• Safety Instructions for Wearers of Medical Implants on page 5-10

• In Case of Emergency on page 5-11

• Residual Hazards on page 5-12

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-1
Safety
Safety Symbols and Signal Words in This Manual

Safety Symbols and Signal Words in This Manual


Notices concerning the safety of the personnel operating the Delta V
Series mass spectrometer appear different from the main flow of text.
Safety notices include the following:

Always be aware of what to do with and the effect of safety


information.

CAUTION Points out a hazardous situation that can lead to minor or medium
injury if not avoided.

WARNING Points out a hazardous situation that can lead to severe injury or death
if not avoided.

DANGER Points out a hazardous situation that will lead to severe injury or death
if not avoided.

Observing This Manual


This manual must always be kept near the instrument to be available for
quick reference.

Be sure to read and comply with all precautions described in this


manual.

System configurations and specifications in this manual supersede all


previous information received by the purchaser.

5-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Safety Symbols on the Instrument

Safety Symbols on the Instrument


Table 5-1 lists all safety labels on the instrument and their respective
positions. See the indicated safety notices to prevent risk of harm to the
operator and to protect the instrument against damage. If present, read
and follow the instructions on the labels.

Table 5-1. Safety labels on the instrument


Label Description Label Position
Two labels are attached next to the power
panel at the rear side of the instrument:

The upper label indicates the presence of


electric current inside the instrument.

The lower label attached next to the power


panel at the rear side of the instrument
indicates that the instrument may only be
opened by qualified personnel.

This label is attached to the left side of the


instrument in the upper right corner.

For details, see “Removing the Blind to Access


the Capillaries” on page 9-40.

The label indicates the presence of hot


surfaces.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-3
Safety
Safety Symbols on the Instrument

Table 5-1. Safety labels on the instrument, continued


Label Description Label Position
This label is attached on the left side below the
top cover of the instrument.

The label indicates the presence of electric


current inside of the instrument.

This label is attached to the housing of the


amplifier power supply inside the analyzer
cabinet at the left side of the instrument.

The label indicates the presence of electric


current inside of the instrument.

This label is attached to the heater sockets


panel inside the Microvolume cabinet at the
lower right front of the instrument.

The label indicates the presence of electric


current inside of the instrument.

This label is attached to the ion


source control board inside the electronics
cabinet at the back of the instrument.

This label is explained in the label attached to


the protecting pane at the back of the
instrument inside the electronics cabinet next
to the first label.

The labels indicate the presence of high


voltage.

5-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Safety Symbols on the Instrument

Table 5-1. Safety labels on the instrument, continued


Label Description Label Position
This label is attached near the magnet of the
instrument.

The label indicates that the electromagnet


might affect the function of cardiac
pacemakers, implanted heart defibrillators and
medical implants that might contain
ferromagnetic materials (clips or prostheses,
for example).

If you wear these devices, keep a sufficient


safety distance to the magnet.

See “Safety Instructions for Wearers of


Medical Implants” on page 5-10.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-5
Safety
Rating Plate

Rating Plate
To identify correctly the instrument when you contact Thermo Fisher
Scientific, always have the information from the rating plate available.
The rating plate is attached to the power column at the rear side of the
instrument. It contains the serial number, which is important in any
type of communication with Thermo Fisher Scientific.

See Figure 5-1 as an example for a Delta V Plus instrument.

Figure 5-1. Rating plate of a Delta V Plus instrument

5-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Intended Use

Intended Use
The Delta V Series mass spectrometer is a stand-alone instrument for
isotope ratio mass spectrometry (IRMS) applications.

Observe the following usage guidelines when you operate your


Delta V Series mass spectrometer:

• The instrument is designed to be placed inside the laboratory. It is


not designed for the use outdoors.

• The instrument is designed for laboratory research use only. It is


not designed for use in diagnostic or medical therapeutic
procedures.

If the Delta V Series mass spectrometer is used in a manner not


specified by Thermo Fisher Scientific, the protection provided by the
instrument could be impaired. Thermo Fisher Scientific assumes no
responsibility and will not be liable for instrument damage and/or
operator injury that might result.

Whenever the safety protection of the mass spectrometer has been


compromised, disconnect the instrument from all power sources and
secure the unit against unintended operation.

Notice on the Susceptibility to Electromagnetic Transmissions

Your instrument is designed to work in a controlled electromagnetic


environment. Do not use radio frequency transmitters, such as mobile
phones, in close proximity to the instrument.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-7
Safety
Intended Use

Qualification of the Personnel

Only employees of Thermo Fisher Scientific or personnel acting on


behalf of Thermo Fisher Scientific are allowed to install the Delta V
Series mass spectrometer.

Personnel that install or operate the Delta V Series mass spectrometer


must have the following qualifications:

• Electrical Connections
The electrical installation must be carried out by qualified and
skilled personnel (electrician) according to the appropriate
regulations (for example, cable cross-sections, fuses, grounding
connection). Refer to the Gas Isotope Ratio MS Pre-Installation
Requirements Guide for the specifications.

• Installation
Only employees of Thermo Fisher Scientific or personnel who act
on behalf of Thermo Fisher Scientific are allowed to install the
Delta V Series mass spectrometer.

• General Operation
The Delta V Series mass spectrometer is designed to be operated
by qualified laboratory personnel. Before starting, all users must be
instructed about the hazards presented by the instrument and the
used chemicals. The users must be advised to read the relevant
Material Safety Data Sheets (MSDSs).

• Decommissioning
Only employees of Thermo Fisher Scientific or personnel who act
on behalf of Thermo Fisher Scientific are allowed to
decommission the Delta V mass spectrometer.

Permitted Materials
The Delta V Series mass spectrometer is designed to be operated with
the following materials:

• standard reference gases and samples gases


- carbon monoxide (CO), nitrogen (N2), carbon dioxide (CO2),
oxygen (O2), sulfur dioxide (SO2), helium (He, carrier)
- With special collectors, other gases are possible.

• fore vacuum pump oil


- used for cooling, lubrication, and sealing of the fore vacuum
pump(s).

5-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Electric Safety Precautions

NOTICE Only use the fore vacuum pump oil indicated on the name plate of
the pump. In case other oils are used, the manufacturer rejects all
responsibility should any trouble occur.

• calibration compounds, samples

• solvents

Electric Safety Precautions


WARNING High Voltage. Risk of electric shock. High voltages up to 3.3 kV are
used in the instrument.

Observe the following safety precautions when operating or


performing service on your instrument:

• The instrument is properly grounded in accordance with


regulations when shipped. You do not need to make any changes
to the electrical connections or to the chassis of the instrument to
ensure safe operation.

Do not change the external or internal grounding connections.


Tampering with or disconnecting these connections could
endanger you and/or damage the system.

• Do not run the system without the housing on. Permanent


damage can occur. Do not remove the protective covers from
plugs, cables, and other parts. Do not touch the magnet current
regulator, the transformer or any other boards.

When leaving the system, make sure that all protective covers and
doors are properly connected and closed, and that heated areas are
separated and marked to protect unqualified personnel.

Do not rig or override any safety switches or safety functions. Risk


of electric shock, burn hazard or damage to your system can occur.
• Do not turn the instrument on if you suspect that any kind of
electrical damage has incurred. Instead, disconnect the power cord
of the mass spectrometer and contact a Thermo Fisher Scientific
field service engineer for a product evaluation.

Do not attempt to use the instrument until it has been evaluated.


Electrical damage may have occurred if the system shows visible
signs of damage, or has been transported under severe stress.

• Do not place any objects upon the instrument, especially not


containers with liquids, unless it is requested by the user
documentation. Leaking liquids might get into contact with
electronic components and cause a short circuit.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-9
Safety
Safety Instructions for Wearers of Medical Implants

Safety Instructions for Wearers of Medical Implants


HF/RF magnetic field emitting instruments may
influence active and passive body implants, such
as pacemakers, infusion pumps, hip joint
replacements, etc.
If you are wearing a cardiac pacemaker, an implanted heart defibrillator
or medical implants that might contain ferromagnetic materials (clips or
prostheses, for example), read and follow these safety instructions.

WARNING Magnetic and Electromagnetic Radiation. The electromagnet might


affect the function of cardiac pacemakers, implanted heart
defibrillators and medical implants that might contain ferromagnetic
materials (clips or prostheses, for example). If you wear these devices,
keep a sufficient safety distance to the magnet.

Parts of a pump or a gauge emit electromagnetic radiation. This


radiation can interfere with the operation of cardiac pacemakers and
implanted heart defibrillators, possibly causing death or serious injury.
If you wear these devices, keep a sufficient safety distance to the pump
or gauge.

Current static magnetic field guidelines restrict exposures for wearers


of cardiac pacemakers to 0.5 mT. To avoid exposure to stray fields,
restrict access to personnel with pacemakers or other implanted
electronic devices to a minimum distance from the edge of the magnet
coil assemblies.

Medical implants (clips or prostheses, for example) that may contain


ferromagnetic materials, would be subject to strong attractive forces
near to the magnet. All people with such implants should be excluded
from the laboratory rooms and appropriate warning signs be
displayed.

Strong magnetic fields might affect the operation of electronic


components. They can cause permanent damage of magnetically
sensitive devices.

Strong attractive forces can cause metal objects to move uncontrollably


towards them. Do not bring compressed gas cylinders, tools, or other
metal objects near to the magnet. Keep computers, credit cards and
other magnetically sensitive devices sufficiently far away from the
instrument.

To avoid hazards from flying metal objects, do not insert items, such as
tools made of magnetically permeable material, in the gap between
upper and lower magnet coil assemblies when the magnet circuit is
switched on.

5-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
In Case of Emergency

Read the Operating Manual of your instrument to get comprehensive


information about the specific hazards that are presented by it. The
manual also provides information about the necessary
countermeasures (safety distances, for example).

If not stated otherwise in the Operating Manual, carriers of active


implants must keep a safety distance of at least 30 cm (12 in) to the
magnet, magnet coil or pump.

In Case of Emergency
This section describes the emergency shutdown, not the regular system
shutdown. For the regular system shutdown, see “Shutting Down the
Instrument” on page 7-5.

❖ To shut down the system in case of emergency

1. At the rear panel of the Delta V Series mass spectrometer, turn the
main switch to the Off position. See Figure 5-2.

Figure 5-2. Main switch at rear panel of mass spectrometer

All power to the mass spectrometer, including the internal vacuum


pumps, is shut off.

2. Pull the mains plug out of the power socket.

3. Switch off the computer by pressing its On/Off switch.

WARNING Electric Current. Electric shock hazard. Capacitors inside the


instrument might still be charged, even if the instrument is turned
off.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-11
Safety
Residual Hazards

4. Close the compressed air supply.

5. Switch off all peripherals.

6. Close all gas supplies, except the helium supply.

7. Close the liquid nitrogen supply.

8. After about two hours, close the helium supply.

9. Secure the mains switch against being switched on by using a lock.


Fill in and sign the card. See Figure 5-3.

Figure 5-3. Main switch secured against being switched on again

10. Inform your local service organization.

Residual Hazards
Pay attention to the following residual hazards:

WARNING High Voltage. Risk of injury. Some parts of the Delta V Series
instrument are at high voltage. Opening the electronics cabinet is only
allowed for maintenance purposes by qualified service personnel.

CAUTION Hazardous Chemicals. Risk of intoxication. Samples and solvents


might contain toxic, carcinogenic, mutagenic, or corrosive/irritant
chemicals. Avoid exposure to potentially harmful materials. Always
wear protective clothing, gloves, and safety glasses when you handle
solvents or samples. Also contain waste streams and use proper
ventilation. Refer to your supplier's Material Safety Data Sheet
(MSDS) for proper handling of a particular compound.

5-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Residual Hazards

CAUTION Hot Surface. Risk of burns. Parts of the instrument might be very hot
and might cause severe burns if touched. Allow hot components to
cool before servicing.

Safety Instructions for the Autocool Unit


Before operating the Autocool Refill device, carefully read these notes as
well as the handling instructions of the manufacturer.

NOTICE Make sure that only authorized and fully trained operators use this
equipment and that they are fully familiar with these safety notes.

CAUTION Cold Liquid. Risk of frostbite. The Autocool device contains


extremely cold liquid gas. Careless handling might cause severe
personal injury including frostbite. Only use the cryogenic liquid
specified on the label on the Autocool Refill device. Wear protective
clothing when operating this equipment, including protective gloves
and face shield. Do not overfill or tilt the device. Prevent spills.

WARNING Noxious Gases. Risk of suffocation. Use the device only in


well-ventilated areas. Poor ventilation might cause suffocation. Follow
correct First Aid procedures. If gas was inhaled, remove the victim to
fresh air. If necessary, give artificial respiration and seek medical
assistance immediately.

Personal Protective Equipment


This manual can only give general suggestions for personal protective
equipment (PPE), which protects the wearer from hazardous substances.
Refer to the Material Safety Data Sheets (MSDSs) of the chemicals
handled in your laboratory for advice on specific hazards or additional
equipment.

Eye Protection

The type of eye protection required depends on the hazard. For most
situations, safety glasses with side shields are adequate. Where there is a
risk of splashing chemicals, goggles are required.

Protective Clothing

When the possibility of chemical contamination exists, protective


clothing that resists physical and chemical hazards should be worn over
street clothes. Lab coats are appropriate for minor chemical splashes and
solids contamination, while plastic or rubber aprons are best for
protection from corrosive or irritating liquids.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-13
Safety
Residual Hazards

Gloves

For handling chemical compounds and organic solvents, Thermo Fisher


Scientific recommends white nitrile clean room gloves. For handling hot
objects, gloves made of heat-resistant materials (for example, leather)
should be available.

5-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
6
System Setup

This chapter describes how to set up a Delta V Series mass spectrometer.

It is your responsibility as the operator to provide a suitable location, a


source of power of acceptable quality, a suitable operating
environment, and a proper exhaust system.

Contents

• Laboratory Conditions on page 6-2

• System Preparation on page 6-7

• Creating an Isodat Backup on page 6-14

• Starting Isodat the Very First Time on page 6-17

• Creating a Gas Configuration on page 6-20

• Creating a Configuration on page 6-25

• Source Heater on page 6-28

• Calibrating and Adjusting the System on page 6-29

• Resetting the Mass Spectrometer on page 6-73

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-1
System Setup
Laboratory Conditions

Laboratory Conditions
This section gives an overview of important requirements for the
laboratory where the Delta V Series mass spectrometer is placed. For
details, refer to the Gas Isotope Ratio MS Pre-Installation Requirements
Guide.

Power Supply

Power Requirements

Table 6-1 summarizes the power requirements of the Delta V Series


instruments (basic systems) during operation and bakeout.

Table 6-1. Basic power requirements of Delta V Series instruments


Specification Value
Input Nominal 230/400 V; 50/60 Hz AC
voltage Dedicated line voltage, must be
free of spikes
Supply system Three-phase, 5-wire system in ‘Y’
configuration (neutral wire must
be connected to earth)
Voltage ±10%
fluctuation
Internal fuses Phases fused with 15 A (L1), 10 A
(L2), 6 A (L3)a
Output 1× 230 V AC, 50/60 Hz, max. 15 A
4× 230 V AC, 50/60 Hz, max. 10 Ab
a
One 15 A fuse for one bigger socket (J7); one 10 A fuse for all four sockets; one 6 A fuse for the
IRMS
b
The four outputs (J8) are secured with one 10 A fuse, that is, the sum of the output currents
must not exceed 10 A.

NOTICE To ensure trouble-free operation of the Delta V Series instrument, the


maximum allowable voltage between neutral and ground must be less
than 1 V.

Power Supply for Peripherals

When connecting external peripherals or computer equipment, take


care that the overall current does not exceed 10 A (fuse F2) or 15 A
(fuse F1) respectively. If the overall current exceeds these values, the
IRMS will not be turned off as it has a fuse of its own (fuse F3).

6-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Laboratory Conditions

Tip Additional devices can be noisy, and they blow warm air into the
room. See “Air Conditioning System” on page 6-5. It is advisable to
install those devices outside the laboratory.

Additional single-phase 230 V (or 110 V) AC outlets are needed for


some peripherals or test equipment, such as compressors. Provide
sufficient spare 230 V (110 V) AC outlets behind the system and close
to the workbench space within your laboratory to accommodate your
system setup.

NOTICE A single-phase auxiliary wall outlet must use the same ground as the
instrument.

It is your responsibility to have the outlets installed by your electrician


before the instrument is installed.

Establishing the Power Supply

❖ To establish the power supply for the instrument

1. Connect your Delta V Series instrument to the power supply.

Tip At the rear panel of the Delta V Series instrument, five sockets
are arranged to connect peripherals and computer equipment (see
3 and 4 in Figure 3-7). For first tests, the IRMS can be checked
without any peripheral connected.

2. Turn on the IRMS by setting the main switch to position On. The
main switch is located at the rear side of Delta V Series instrument.
See Figure 3-7.

Gas Supply
Your system can require large amounts of gases during daily operation. It
is essential that the gases are delivered with the necessary pressure and
purity. You must provide all gases needed for specification measurements
(international standards).

This section informs about the purity and pressure of gases that your
system requires. For information about the purity and pressure of gases
that your peripherals require, refer to the Gas Isotope Ratio MS
Pre-Installation Requirements Guide.

NOTICE Do not store gas cylinders where they can damage cables or gas lines,
and secure them in accordance with standard safety practices.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-3
System Setup
Laboratory Conditions

NOTICE Contaminations introduced during installation of house lines used for


gas delivery may cause damage to the system. Ensure that all gas lines
used with your system have been cleaned of all particulates and oils.
You are responsible for any damage to the instrument caused by
contaminations introduced from your gas delivery system.

Gas Samples for Dual Inlet Instrument Setup

Depending on the type of collector system, you must provide either


CO2 or H2 gas samples for the installation of your instrument. The inlet
system of a Delta V Series instrument terminates in 1/4 inch
connectors.

Gases for Continuous Flow Peripherals

The Delta V Series instrument uses helium as carrier gas in continuous


flow configurations. The helium supply must be ultra-high purity 5.0
(99.999 %). Because particulate filters can be a source of
contamination, Thermo Fisher Scientific does not recommend using
them.

Continuous flow applications require also reference gases such as CO2,


N2, H2, SO2. The need of the gas depends on your application and cup
configuration. Refer to the Gas Isotope Ratio MS Pre-Installation
Requirements Guide for the gases required and for their purity.

Gas lines for helium and reference gases should be made of stainless
steel. All gas lines should be free of oil and preferably flame dried.
Helium gas supply lines should terminate with 1/8 inch female
Swagelok™ connectors.

The gas tanks should be located in the same room as the Delta V Series
instrument to ensure best results due to minimal temperature
fluctuations.

NOTICE Do not shut off the helium gas. A continuous flow of helium is
required for optimum performance of the mass spectrometer. Thermo
Fisher Scientific recommends installing a separate helium supply for
the Delta V Series instrument that is independent of a possibly
available centralized supply.

Argon

During installation, a bottle of argon is needed for leak checking.


99.5 % welding argon is sufficient.

6-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Laboratory Conditions

Compressed Air

Compressed air must be provided by the distribution unit of your


laboratory. The pressure should be in the range between 6 and 10 bar
(600 and 1 MPa; 87 and 145 psi).

The compressed air supply of the laboratory needs to be connected to


the compressed air unit of the Delta V Series instrument using the
6 × 1 mm tubing. The tubing is part of the Installation Kit.

The compressed air connection should be 1/4 inch. The remaining gas
connections are 1/8 inch. Teflon™ reducing ferrules are provided to
reduce to 1/16 inch. You may want to have reducing unions from
1/4 inch to 1/8 inch and from 1/8 inch to 1/16 inch at hand for each
gas depending on the outlet of their regulators.

The pressure of compressed air for the instrument and the connected
peripherals is regulated by a secondary distributor inside the IRMS. The
value for the secondary distributor is 5 bar (500 kPa; 73 psi) as default
factory setting.

Connect your compressor (for compressed air) to the compressed air


inlet at the rear side of the IRMS (1 in Figure 3-11) using the 6 × 1 mm
tubing.

At least 5 bar (500 kPa; 73 psi) is internally necessary, whereas 6 bar


(600 kPa; 87 psi) is recommended. Usually, the pressure reducer for
compressed air (Figure 3-18) is factory-set via the rotary adjusting knob
to display 5 bar (500 kPa; 73 psi).

Temperature
For optimum performance, the instrument should be located in an
air-conditioned room.

The laboratory room temperature must be maintained between 18 and


24 °C (64 and 75 °F). The temperature should not vary more than
±1 °C per hour.

Operating at temperatures above those recommended may cause


premature failure of transistors and integrated circuits.

Air Conditioning System


Thermo Fisher Scientific recommends installing an air conditioning
system if the specified limits will be exceeded due to unfavorable
climatic conditions.

The instrument and the magnet should not be placed directly below the
cold air stream of the air conditioning system.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-5
System Setup
Laboratory Conditions

Humidity
The relative humidity of the operating environment should not exceed
40 to 60%, with non-condensing and non-corrosive atmosphere.
Thermo Fisher Scientific recommends equipping your laboratory with a
temperature/humidity monitor to ensure that your laboratory is always
within the required temperature and humidity specifications.

NOTICE Operating the Delta V Series system at very low humidity might cause
accumulation and discharge of static electricity, which can shorten the
life of electronic components. Operating the system at high humidity
might cause condensation, oxidation and short circuits, and also
blocks the filters of the cooling fans.

Exhaust System
The exhaust port of the rotary pump should be connected to an exhaust
gas line leading out of the building. The inner diameter of the tube
should be at least 1.5 cm.

Lay the waste gas tube (at the output of the pumps) outdoors to prevent
accumulation of oil mist and perilous gases (for example, CO or H2).
Connect it to the exhaust vent of your laboratory.

CAUTION Noxious Material. Risk of injury. If your system is used to analyze


hazardous materials, the effluent from the open-split interface and the
exhaust from the rotary pumps must be connected to an adequate
exhaust system.

Floor and Vibration


The floor in the laboratory must be level (unevenness less than 10 mm).

The floor must be a solid floor (concrete screed) with a compressive


strength of 1.5 t/m2 being able to carry the weight of the Delta V Series
instrument. Consider the additional weight of the data system as well as
any option or peripheral delivered together with the instrument.

NOTICE Hollow chamber floors (“twin-wall constructions”) are not capable of


carrying the weight and must not be used.

Tip Thermo Fisher Scientific recommends placing the mass


spectrometer on a protective surface to safeguard the floor of your
laboratory.

6-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation

The floor must be free of mechanical vibration caused by equipment in


adjoining locations. The maximum acceptable amplitude is 10 m
(peak to peak) movement for all frequencies above 30 Hz.

Radio Frequencies
If strong radio transmitters are operating close to your laboratory,
contact your local sales representative for advice. Because of the
complexity of such influences, no general suggestion can be given in this
manual.

Magnetic Fields
The instrument site must be free of interfering magnetic fields. The
maximum acceptable field amplitude (AC) for any frequency is
5 × 10-6 T.

System Preparation
This section explains hardware-related steps to be performed before any
measurement can be started.

Placing the Instrument


Table 6-2 lists the dimensions and the weight of the Delta V Series
instrument.

Table 6-2. Dimensions of Delta V Series instrument


Width Depth Height Weight
81 cm 78 cm 92 cm 300 kg
(31.9 in) (30.7 in) (36.2 in) (660 lbs)

Add additional space around the instrument (80 cm/3 ft) on each side
to allow access to components or for maintenance work and to facilitate
heat dissipation.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-7
System Setup
System Preparation

Figure 6-1 shows the space requirements of the Delta V Series


instrument in front view.

81.0 cm (31.9 in)

92.0 cm (36.2 in)


Figure 6-1. Space requirements of Delta V Series IRMS - front view

Figure 6-2 shows the space requirements of the Delta V Series


instrument in side view.

98.3 cm (38.7 in)

81.2 cm (32.0 in)


78.0 cm (30.7 in)
85.5 cm (33.7 in)
6.3 cm (2.5 in)

Figure 6-2. Space requirements of Delta V Series IRMS - side view

6-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation

Figure 6-3 shows the space requirements of the Delta V Series


instrument in top view (with doors).

81.0 cm (31.9 in)

78.0 cm (30.7 in)


17.0 cm (6.7 in)

38.0 cm (15.0 in)


door door

Figure 6-3. Space requirements of Delta V Series IRMS - top view

Figure 6-4 shows the dimensions of the Delta V Series instrument with
the optional peripherals table in front view.

120 81

92
92

Figure 6-4. Delta V Series instrument and peripherals table - front view

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-9
System Setup
System Preparation

Figure 6-5 shows the dimensions of the Delta V Series instrument the
optional peripherals table in top view.

4
82
78

99
120 81

17
Figure 6-5. Delta V Series instrument and peripherals table - top view

Moving the Instrument

The Delta V Series instruments are equipped with two fixed


(non-adjustable) casters and two rotatable casters to be easily movable
within the laboratory. The instruments can be locked in place by four
screws.

NOTICE Do not move Delta V Series instruments with any pump turned on.

Before moving the instrument, both fore vacuum pumps must be


secured (transportation lock) with the provided belt, 3 in Figure 3-19.
Thereby, both fore vacuum pumps can remain in the instrument
during transport.

Remove the belt after transport and before operation is started again.

Before moving the tray with the fore vacuum pumps, remove their
connectors.

❖ To move your instrument within your laboratory

1. Take care that all pumps are turned off.

2. Secure both fore vacuum pumps (transportation lock).

3. Use a forklift or a lifting truck to transport your instrument as near


as possible to its final place within the laboratory.

4. Carefully roll the instrument on its casters to its final place.

5. Lock the instrument in its place by arresting the four screws.

You can leave the casters unlocked during operation.

6-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation

Placing the Data System

Thermo Fisher Scientific recommends using a workbench with the


minimum dimensions of 1 × 1.20 m (3 × 4 ft) to hold the data system
computer and the monitor. Take care to provide sufficient additional
space for an optional printer on this workbench. The workbench must
be capable of supporting the weight of the data system (about 20 kg;
44 lbs) plus the optional printer.

The fiber optic data cable connecting your computer to the fiber optic
connectors at the rear panel of your IRMS is about 6 m (20 ft) long.
This allows you to place the computer on a table outside the direct
vicinity of the mass spectrometer.

Figure 6-6 shows the typical hardware components of the data system.

120 cm (47.2 in)

monitor

Ethernet switch computer

Ethernet

76 cm (29.9 in)
communication
cables (used for wall outlet for data system components 230 V AC
optional GC, (from the same power supply as for IRMS)
GC-MS or HPLC
communication)

Figure 6-6. Typical hardware components of data system

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-11
System Setup
System Preparation

Table 6-3 lists the space requirements and weights of the typical
hardware components of the data system. The printer is not delivered
with the system. All values depend upon your equipment.

Table 6-3. Typical data system hardware components space and load
requirements
Module Height Width Length Weight
cm in cm in cm in kg lb
Monitor 36 14 41 16 18 7 6 13
Mini tower 48 19 18 7 43 17 14 30
computer
Laser printer 20 8 41 16 46 18 7 16

If optional peripherals use LAN connections, the cables must be no


longer than 3 m (10 ft) each. Therefore, the workbench holding the
data system must be located near the peripheral that requires this
connection.

Tip To ensure compliance with safety and EMC regulations, use


category 5, shielded Ethernet cables no longer than 3 m (10 ft) in
length.

Preparing the Pumping System


Before starting the pumping system, it is assumed that:

• the fore vacuum pumps are filled with oil

• the fore vacuum pumps are connected to the power supply

• the gas ballast of the fore vacuum pumps is shut

The fill level of the oil must range between the upper and the lower line,
optimally at half height of the level indicator. Thermo Fisher Scientific
recommends a total oil exchange once a year. Refer to the manufacturer’s
manual and to www.pfeiffer-vacuum.com.

The gas ballast is shut by turning the switch to position 0. The switch is
located at the side. Refer to the manufacturer’s manual and to
www.pfeiffer-vacuum.com.

❖ To start the pumping system

1. Press the Main (and Secondary) Pumps switch (4 in Figure 3-3) to


switch on the turbomolecular pump(s) of the analyzer.

2. If a Dual Inlet system is employed, additionally press the Inlet


Pump switch (5 in Figure 3-3).

6-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation

If no Dual Inlet system is available, this switch has no function.

The pump LEDs are yellow when they are switched on. After
15 minutes, the Main LED (3 in Figure 3-3) and, if a differential
pump is available, Secondary LED (2 in Figure 3-3) must be green.
See Table 3-3 for LED statuses.

If one of the turbomolecular pumps does not reach 80% of the


rotational speed after a specific period of time, the pumping system
shuts down. After 20 minutes, the security threshold should be
reached. The ion source can then be switched on. The red LEDs
Main, Secondary or Inlet indicate errors concerning the
turbomolecular pumps (for example, if after 15 minutes the security
threshold of  3 × 10-5 mbar has not been reached).

Connecting the Computer to the IRMS


❖ To connect the data system computer to the IRMS

1. To enable data transfer between the IRMS and the computer,


connect the fiber line to the respective port at the rear side of the
computer.

2. Connect the other end of the fiber line to the IRMS by inserting the
blue plug into the blue connector and the gray plug into the gray
connector. See Figure 3-12.

The Connection status LED (11 in Figure 3-3) is green once everything
is connected, Isodat is running and the power supply is on.

If the Connection status LED is not green when Isodat is started, no


connection between IRMS and computer could be established. Check
the plug connections and fiber lines.

Connecting Peripherals to the IRMS


❖ To connect peripherals to the IRMS

1. Connect your peripherals to the SUB D ports of the IRMS. See


Figure 3-6.

2. Establish the compressed air supply.

3. Establish the power supply for the peripherals, preferably via the
built-in connector (see 3 and 4 in Figure 3-7), or use an external
power supply.

Once the configuration for the peripheral is created (see “Creating a


Configuration” on page 6-25), peripherals are identified
automatically after they are connected.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-13
System Setup
Creating an Isodat Backup

Creating an Isodat Backup


Isodat backups can be created and restored using the Version Handler.
This tool is part of Isodat. The Version Handler as well as the backup
files are stored in the folder C:\Isodat_Backups. See Figure 6-7.

backup files

Version Handler

Figure 6-7. Location of Version Handler and backup files

NOTICE A backup created using the Version Handler does not include the User
folder. This implies that all measurement data (configurations,
methods, sequences and result files, with the exception of ISL scripts)
are not saved.

Therefore, save the User folder and all measurement data before
starting the installation of Isodat.

Tip Isodat 3.0 can still open and operate methods and sequences
created with older version of Isodat that do not include GC or LC
devices.

Already existing methods and sequences for GC and LC devices


become incompatible when changing from Trace GC.ocx to
Foundation GC drivers.

❖ To create an Isodat backup

1. Shut down Isodat.

2. On your desktop, double-click the folder Isodat 3.0.

6-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Creating an Isodat Backup

3. Double-click the Version Handler shortcut. See Figure 6-8.

Figure 6-8. Double-clicking Version Handler shortcut

The Version Handler appears listing prior backups. See Figure 6-9.

4. Click the Create Backup icon in the top left corner.

Figure 6-9. Prior backups listed in Version Handler

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-15
System Setup
Creating an Isodat Backup

The backup starts reminding you that all measurement data


(configurations, methods, sequences and result files, with the
exception of ISL scripts) are not saved. See Figure 6-10.

Figure 6-10. Backup starts

5. Wait until the backup is finished.

The backup just created is listed as a new entry in the Version


Handler. See Figure 6-11.

Figure 6-11. Backup listed as new entry in Version Handler

6. Close the Version Handler.

6-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Starting Isodat the Very First Time

Starting Isodat the Very First Time


❖ To start Isodat

1. Double-click this icon to open the Configurator of Isodat.

The Select Isotope MS window opens. See Figure 6-12.

Figure 6-12. Selecting Delta V Series instrument as mass spectrometer

Tip Figure 6-12 only appears when starting the system the very
first time, or after a reset of the Delta V Series instrument.

2. Select your Delta V Series instrument.

3. Confirm with OK.

The Optional Hardware window opens. See Figure 6-13.

Figure 6-13. Selecting optional hardware

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-17
System Setup
Starting Isodat the Very First Time

4. De-select ForeVacuum.

5. Click OK.

The Cup Settings window opens. See Figure 6-14.

Figure 6-14. Default cup settings

Tip The default cup configuration installed on your Delta V


Series system is shown on the Collector Configuration Sheet
supplied with your instrument. The Collector Configuration
Sheet can also be requested from Thermo Fisher Scientific
(Bremen).

6. Read the instructions in the Cup Settings window (see Figure 6-14)
and also refer to the cup configuration in your purchase order and
other instrument documentation.

7. In the Installed column, check whether the cups are selected.

8. Check the Peak Center option of the cups.

9. Check the values for Resistor [Ohm] of the cups.

10. Check the values for Resistor 2 [Ohm] of the cups.

11. Click OK.

6-18 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Starting Isodat the Very First Time

12. In the Gas Configuration Editor (see Figure 6-15), check for your
particular configuration whether the masses are correctly assigned to
the cups.

Figure 6-15. Gas Configuration Editor

Check Calibration, Ratio Groups, Magnet position and PC-Offset.

The default values for Magnet position are averaged experience


values that cannot be checked and edited here, but later during
calibration.

At Mass Info, the number of required cups (for example, 3 in


Figure 6-15), is displayed with the corresponding masses (for
example, 44, 45, 46).

13. Click this icon.

14. Confirm with OK to complete the process of resetting the mass


spectrometer. See Figure 6-16.

Figure 6-16. Shutdown of Isodat to complete reset

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-19
System Setup
Creating a Gas Configuration

Creating a Gas Configuration


A gas configuration is a parameter set that contains all necessary settings
to optimally receive ions of all interesting masses of one gas species in
the respective cups.

In this parameter set, mass to cup dependencies are stored, as well as


focus settings, the mass calibration, amplifier settings, and peak center
offset.

The Gas Configuration Editor (Figure 6-17) can be opened from the
Isodat Instrument Control or Isodat Acquisition.

Figure 6-17. Gas Configuration Editor

A gas configuration determines a combination of masses which are


collected in the cups for evaluation of ratios and eventually  values.
The gas configuration is specific for the particular gas and is combined
with a magnet field value taken from the mass calibration of your IRMS.
The ratio groups determine the reported ratios of predefined masses.

For a carbon measurement, a gas configuration must be available for


m/z 44 (12C16O16O), m/z 45 (13C16O16O) and m/z 46. Otherwise, it
must be created as follows.

Before defining this gas configuration, ensure that the connected IRMS
has the cups for the simultaneous detection of m/z 44, m/z 45 and
m/z 46, and that the mass calibration for these cups has already been
performed.

6-20 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Creating a Gas Configuration

❖ To create a gas configuration

1. Double-click the Isodat icon in the Windows™ taskbar to close all


open Isodat applications.
2. Double-click this icon to open the Acquisition of Isodat.

3. Click Editors. Select Gas Configuration Editor. See Figure 6-18.

Figure 6-18. Selecting Gas Configuration Editor

Tip The Gas Configuration Editor is only available, if neither an


acquisition nor a scan are running.

As default, CO2 is created as the first gas configuration. See


Figure 6-19.

Figure 6-19. Creating gas configuration

4. In the Gas Configuration Editor window, click Add to add a new


gas configuration.

5. In the New Gasconfiguration window, enter N2 at Name. See


Figure 6-20.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-21
System Setup
Creating a Gas Configuration

6. Select a template for your gas configuration from the drop-down


list. The default Template is CO. See Figure 6-20.

Figure 6-20. Entering name of new gas configuration

7. Confirm with OK.

A dialog window opens. See Figure 6-21.

Figure 6-21. Confirming formula

8. Click Yes.

The gas configuration N2 is added to the Configurations table. See


Figure 6-22.

Figure 6-22. N2 is added to the configurations

6-22 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Creating a Gas Configuration

9. In the column Ratio Groups, check the entry for the gas
configuration created.

10. In the column Ratio Groups, select the cell you want to change.

11. Click the cell again.

The Ratio Groups window opens. See Figure 6-23.

Figure 6-23. Changing the ratio groups

Tip You can also open this Ratios Groups window by clicking No
instead of Yes in the Confirm Formula window (see Figure 6-21).

12. For the Evaluations you want to change, click the cell in the Enable
column.

A check mark is shown. Click the cell again to deactivate it.

13. Confirm with OK.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-23
System Setup
Creating a Gas Configuration

The Ratio Groups entry for the gas configuration is changed. See
Figure 6-24.

Figure 6-24. Gas Configuration and corrected Ratio Groups entry

Tip Figure 6-24 shows a common cup configuration as used in


most Delta V Series mass spectrometers. If you have a special cup
configuration, the respective masses are collected in other cups.

14. In the Calibration column, select your current calibration file.

If no calibration file has been created yet, accept the Current


(Default) option.

15. Enter the correct masses to the appropriate cups specific for your
IRMS.
Select a row in the table to show the number of cups required for
measurement and the assigned masses. See Figure 6-25.

Figure 6-25. Required cups and masses

16. Select the calibration which is valid for the selected cups.

17. Click this button.

6-24 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Creating a Configuration

Creating a Configuration
Before operating, a configuration containing the Delta V Series
instrument needs to be created in Isodat Configurator.

❖ To create a configuration for a Delta V Series instrument

1. Double-click this icon to open the Configurator of Isodat.

2. Click Interfaces. Select Comport to set the port to Active.

3. Click Interfaces. Select Comport Extended to set the port to


Active.

4. Click Interfaces. Select Fiberline to set the port to Active.

5. Select Edit > Add Configuration or click this icon to add a new
configuration.

Isodat creates a new configuration. See Figure 6-26.

Figure 6-26. New configuration created

6. Enter a name for the configuration, for example,


ConFlo IV + Generic EA (HF I). See Figure 6-27.

Figure 6-27. New name for configuration

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-25
System Setup
Creating a Configuration

7. Click this symbol to show source port and capillary port. See
Figure 6-28.

Figure 6-28. New configuration showing source and capillary port

8. In the right pane, click the corresponding tab (Elemental Analyzer


Sets - ConFlo IV, for example) to display the available peripheral
sets.

9. Drag and drop the suited peripheral set from the right pane to the
Capillary port of your configuration on the left pane (for example,
ConFlo IV + Generic EA (HF I)). See Figure 6-29.

Figure 6-29. Drag and drop of peripheral set to Capillary port

6-26 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Creating a Configuration

Depending on the peropheral set you selected, the Optional


Hardware window opens (with GasBench II device or
GC IsoLink II device, for example). Select the optional hardware
required and confirm with OK.

Figure 6-30 shows the peripheral set added to the Capillary port.

Figure 6-30. Peripheral set added to Capillary port

10. Close the Configurator. All settings are saved automatically.

11. Create a method as described at “Creating a New Method” on


page 7-6.

12. Create a sequence as described at “Creating a New Sequence and


Starting Acquisition” on page 7-9.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-27
System Setup
Source Heater

Source Heater
The source heater consists of halogen lamps near the ion source. The
lamps serve as radiant heaters. When the source heater is turned on, the
Heater status LED (8 in Figure 3-3) must be on. Otherwise, one of the
heaters might be defective.

❖ To switch on the source heater

1. Open the Instrument Control of Isodat.

2. In the MS State window, click the respective button to turn on the


individual heater. See the MS State panel, Figure 6-31.

Figure 6-31. Turning on individual heaters in MS sate panel

A green button indicates that the heater is on. A gray button


indicates that the heater is off.

Tip The Inlet Valve Heater heats the needle valve where
peripherals are connected (about 80 °C), as well as the Changeover
valve/Changeover Extension. It is provided with energy by
arbitrary sockets of the socket group 3 in Figure 3-27.

3. Click the Inlet Valve Heater button to switch on the heater of the
Changeover valve and/or the heater of the needle valve in case of
Continuous Flow applications. This prevents water condensation.

Tip The Inlet Heater heats the Dual Inlet system, if available. The
Analyzer Heater heats the analyzer block.

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System Setup
Calibrating and Adjusting the System

Calibrating and Adjusting the System


To be able to work with your system, adjust and calibrate it using the
Instrument Control and the Configurator of Isodat as follows:

• “Checking the Vacuum” on page 6-30

• “Introducing Gas into the Continuous Flow System” on page 6-32

• “Introducing Gas into the Dual Inlet System” on page 6-33

• “High Voltage Supply - Adjusting Potentials” on page 6-37

• “Magnet Steps and Mass Selection” on page 6-39

• “Magnet Calibration” on page 6-39

• “Mass Calibration” on page 6-41

• “Jump Calibration for Elemental Analyzer Applications” on


page 6-48
• “Peak Shapes” on page 6-50

• “Peak Center Scan” on page 6-52

• “Peak Center Offset” on page 6-57

• “Electronic Offset” on page 6-59

• “Crimp Adjustment” on page 6-60

• “Calibrating the Bellows” on page 6-61

• “Focus Settings of the IRMS” on page 6-66

• “Auto Focusing” on page 6-70

• “Manual Focusing - Tune Scan” on page 6-71

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System Setup
Calibrating and Adjusting the System

Checking the Vacuum


Once the instrument is started, check the quality of the vacuum. This
should be a part of the daily routine.

❖ To check the vacuum

1. Open Instrument Control of Isodat.

The Scan window opens. See Figure 6-32.

Figure 6-32. Scan window of Instrument Control

The Scan windows allows performing different scans (for example,


signal over time, high vacuum over time, signal over magnet field,
signal over high voltage).
2. Select your configuration from the drop-down list (for example,
ConFlo IV + Generic EA (HF I)). See “Creating a Configuration”
on page 6-25 for details on creating a configuration.
3. Select your gas configuration from the drop-down list (for example,
CO2).

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Calibrating and Adjusting the System

4. The value displayed at Vac in the MS panel indicates the quality of


the vacuum. See 2 in Figure 6-33.

1
2

Labeled Components: 1=Box and Trap values, 2=high vacuum


Figure 6-33. High vacuum displayed in MS panel

The MS panel furthermore displays the values of the Box and Trap
current (1 in Figure 6-33).

5. To monitor the vacuum with the scan feature, select Time for the
X-axis and High Vacuum for the Y-axis in the Scan window. See
Figure 6-34.

Figure 6-34. Selecting Y-axis for Scan window

6. Click the Options button.

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The Scan Parameter window opens. See Figure 6-35.

Figure 6-35. Scan Parameter window

7. Enter the desired Scan Time in seconds. Usually, one hour is


sufficient. Leave the Integration Time at the default value of 0.1 s.

8. Click the Start Scan button to start the scan.

9. Monitor the High Vacuum signal for intermittent spikes and for its
absolute value.

Typical pressure values after 24 hours of pumping without any gas


supplied (needle valve closed or Dual Inlet system with no gas) and
no heating of the analyzer are about 2 × 10-7 mbar or lower.

Introducing Gas into the Continuous Flow System


This section describes the steps needed to introduce the helium flow
through the needle valve into the mass spectrometer during installation.
The information below may be helpful as well, when you are starting the
instrument after a longer pause.

❖ To introduce gas into the Continuous Flow system

1. Ensure that:

a. the needle valve is closed

b. the capillaries are connected to the needle valve

c. typical reference and sample capillaries from the ConFlo IV


interface are used.

Thermo Fisher Scientific further recommends having the system


under vacuum for more than 24 hours with the ion source heaters
and the inlet valve heaters on.
2. Open Instrument Control of Isodat.

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Calibrating and Adjusting the System

3. Check the vacuum level.

With the needle valve closed, the vacuum should be in the range of
1-5 × 10-7 mbar.
4. Make sure that filament and high voltage are off and that the MS
panel shows no green bar for HV, and 0 mA for the Box and Trap
currents.

5. Make sure that a flow of helium through all the capillaries is


installed. Refer to the Operating Manual of the connected
peripheral.

6. Open the needle valve counterclockwise by 1/2 to 3/4 turn.

7. Wait a few minutes. Monitor the high vacuum level. Perform a time
scan (high vacuum vs. time).

8. As soon as the vacuum is stable and the analyzer pressure is below


3.5 × 10-5 mbar, turn on high voltage.

If this range cannot be reached, a leak along the capillaries


connected to the needle valve may exist:

• Do not turn on high voltage (blocked by Isodat), because you


would risk to damage the filament.

• Close the needle valve.

• Check the capillaries from the peripheral or from the ConFlo IV


interface to the needle valve.

• Check the ferrule in the needle valve.

Introducing Gas into the Dual Inlet System


All gas paths in the Dual Inlet system must be successively evacuated
before use.

❖ To introduce gas into the Dual Inlet system

1. Open the Instrument Control of Isodat.

2. If the Dual Inlet panel is not shown, right-click next to the


Accessories icons. See Figure 6-36.

Figure 6-36. Administrate Panels

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-33
System Setup
Calibrating and Adjusting the System

3. From the context menu, select Administrate Panels....

The Accessories dialog opens. See Figure 6-37.

Tip In the Accessories dialog, all panels available for the current
configuration as well as several general panels (such as File Browser
or ISL Scripts) are listed. All panels with activated Visible column
are shown in the Instrument Control or Acquisition of Isodat.

4. To show the Dual Inlet panel, click the column Visible in the row
Dual Inlet.

5. Confirm by OK.

Figure 6-37. Accessories dialog

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System Setup
Calibrating and Adjusting the System

6. On the Dual Inlet panel, click the Pop-out button to open the
panel in a separate window. See Figure 6-38.

4
1

Labeled Components: 1=valve to external gas supplies, 2=rough pump valve,


3=turbomolecular pump valve, 4=valve to external gas supplies, 5=Login
button
Figure 6-38. Dual Inlet panel

The size of this panel can now be adjusted. The content dynamically
changes with the size.

7. Evacuate the Dual Inlet system and the connected tubing from the
reference gas supply to the Dual Inlet system by using the rough
vacuum pump.

The valve to the external gas supply (see 1 and 4 in Figure 6-38)
needs to stay closed. Commonly used reference gas supply is a 1 L
bottle with manual valve regulator.

8. Close the rough pump valve (2 in Figure 6-38).

9. Introduce the gas into the tubing by successively filling the tubing,
the feed lines and the bellows with gas from the gas reservoir:

Begin at the outside and proceed inwards from valve to valve.


Thermo Fisher Scientific does not recommend letting the gas flow
directly into the ion source.

The MS panel shows the intensity pattern characteristic for CO2.


See Figure 6-39. The intensity for m/z 44 is smaller than the one on
m/z 45, which in turn is smaller than the one on m/z 46.

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System Setup
Calibrating and Adjusting the System

NOTICE Before starting a measurement, after pumping for 15 min, an


analyzer pressure between the lower 10-6 mbar and the upper
10-7 mbar range should be reached. This pressure should even
drop between the lower 10-7 mbar and the upper 10-8 mbar range
while pumping continues for a longer time (if all valves are closed).

If after 15 min of pumping a pressure of 10-5 mbar cannot be


reached, a leak may exist. As a safety measure, the cathode turns
off at pressures above 3 × 10-5 mbar.

10. To turn on the ion source, click this icon. See Figure 6-39.

11. If you got a signal on all cups, click this icon to perform a peak
center.

The signal intensities should yield the pattern shown in Figure 6-39.

Figure 6-39. Intensity pattern for CO2

12. If you do not obtain this pattern, or if an error occurs during peak
center, perform a calibration using CO2.

If you calibrated the IRMS before, a peak center may be sufficient.

Principle of a Peak Center

In this subtle HVDAC scan, only the high voltage (HVDAC value) is
changed. The magnet jumps to a specified BDAC value (10145 BDAC
steps, for example). As a result, the magnet exactly finds the peak of
interest. The BDAC values of a particular gas (12071 BDAC steps in
case of CO2, for example) have been stored in the gas configuration
(CO2, for example). The peak center runs according to the BDAC
values specified there. For each mass, at least one peak center is
performed. Default value is three peak centers for each mass.

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Calibrating and Adjusting the System

High Voltage Supply - Adjusting Potentials

WARNING Electric Current. Risk of an electric shock. Opening the electronics


cabinet is only allowed for maintenance purposes by qualified
personnel.

Figure 6-40 shows the buttons on the Accessories toolbar that are
relevant for high voltage.

2
3

Labeled Components: 1=button Source Off, 2=button Source On, 3=button


Reset HV
Figure 6-40. Power supply buttons

Clicking button 1 in Figure 6-40 switches off the power supply of the
ion source control board. High Voltage and Emission current are turned
off. The high voltage unit provides the ion accelerating voltage.

Clicking button 2 in Figure 6-40, switches on the power supply of the


ion source control board. High Voltage and Emission current are turned
on. See Figure 6-41 and Figure 3-42. High Voltage controls the kinetic
energy of the ion beam and important ion optical properties such as
resolution and dispersion.

Increasing high voltage (per click and drag) allows for higher
transmission and smaller energy width of the emerging ion beam.
Drawbacks are more frequent sparks and a smaller mass range of the
IRMS. See “Electromagnet” on page 3-59.

Figure 6-41. Changing the value of high voltage

Clicking button 3 in Figure 6-40 resets high voltage (after a flashover,


for example).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-37
System Setup
Calibrating and Adjusting the System

NOTICE Switching off the high voltage unit in case of an overload is a


protective measure. Perform troubleshooting. A short circuit in the
feed line of the ion source may have occurred (after cleaning or
reinserting the ion source, for example).

Alternatively, after a longer time, the source may have become dirty
and must be dismantled, cleaned and finally reinserted.

❖ To adjust the potentials

1. Open Instrument Control of Isodat.

2. To turn on the ion source, click this icon. See Figure 6-39.

3. In the Scan window, select Tune Scan.

4. Click the Start Scan button to start the Tune Scan.

5. Wait until the Tune Scan is completed. See Figure 6-42.

Figure 6-42. Performing a Tune Scan

6. Admit gas into the inlet system. Admit a sufficient amount of gas
into the ion source.

7. To adjust the potentials, continue with “Focus Settings of the


IRMS” on page 6-66.

6-38 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

Magnet Steps and Mass Selection


Individual masses are selected by controlling the current in the magnet
at a given high voltage (HV).

❖ To set the magnet

1. Open Instrument Control of Isodat.

2. In the MS panel of Isodat, click and drag the field Magnet [Steps]
to adjust the value to your needs. See Figure 6-43.

Figure 6-43. Selecting the value for the magnet

Alternatively, right-click on one of the current cup readings (44, for


example) and select Jump to Mass from the context menu.

In the Set Mass dialog, enter the desired mass to be focused on that
cup (‘44’, for example). See Figure 6-44.

Figure 6-44. Setting mass

Magnet Calibration
To determine and store the important relation between magnet current
and selected mass, perform a calibration. It is required to have a stable
CO2 gas signal from the source, for example.

In case of a Dual Inlet measurement, fill one bellow with gas and open
the respective side to the source.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-39
System Setup
Calibrating and Adjusting the System

In case of a Continuous Flow measurement, inject reference gas into the


source.

❖ To perform a calibration

1. Open Instrument Control of Isodat.

2. On the right side of the Scan window, select Slow Magnet from the
drop-down list.

In the field left to it, Magnetic Field is automatically displayed. See


Figure 6-45.

Figure 6-45. Selecting parameters for a Magnetic Field scan

3. Click the Start Scan button to start the Magnetic Field scan with
standard parameters. See Figure 6-46.

Figure 6-46. Starting a Magnetic Field scan

When the scan is finished, the Calibration button in the left pane of
the Scan window becomes active.
4. Click the Calibration button to perform an automatic calibration.

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Calibrating and Adjusting the System

Mass Calibration
The mass calibration of Delta V Series instruments is performed in
Instrument Control. It is assumed that the mass spectrometer is coupled
either with a Dual Inlet system or a ConFlo IV device to supply the
required reference gas:

• With a ConFlo IV interface, the pressure of the supplied gases is set


to 5 bar (500 kPa; 73 psi), and at 1 bar (100 kPa; 15 psi) at its
internal regulators, respectively.

Set the sample dilution to maximum to avoid any effects from the
sample side of the ConFlo IV interface. See also “Introducing Gas
into the Continuous Flow System” on page 6-32.

• Using a Dual Inlet system as the gas source for calibration requires
to fill one of the bellows with reference gas. See also “Introducing
Gas into the Dual Inlet System” on page 6-33.

Performing a Mass Calibration

During a mass calibration, a mass scan over the selected mass range is
performed. An approximate pattern of the gases present in the mass
spectrometer results. Delta V Series instruments propose positions of
the gases. These positions need to be checked, adjusted and accepted,
before the mass calibration can be finished.

During the very first calibration, the proposals usually must be


corrected. The calibration masses are assigned to their peaks by drag and
drop, snapping the lines to the mass peaks.

Once the calibration is completed, perform a Peak Center Offset and


pass this offset value to the gas configuration. For details, see “Peak
Center Offset” on page 6-57.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-41
System Setup
Calibrating and Adjusting the System

In Figure 6-47, the offset is 0, and the peak center and the cursor
position are matching.

Figure 6-47. Peak center offset determination

❖ To perform a mass calibration

1. Open Instrument Control of Isodat.

2. Select your configuration and gas configuration required for the


calibration. See Figure 6-48 as an example.

Figure 6-48. Selecting configuration and gas configuration

A mass calibration is usually performed using CO2 as reference gas,


but it is also possible to calibrate on other gases. If you want to use
another gas than CO2, make sure that you know all the mass peaks
that this gas produces in the ion source.

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System Setup
Calibrating and Adjusting the System

3. Select Scan > Calibrate. See Figure 6-49.

Figure 6-49. Calibrate command in Scan menu

A message window opens. See Figure 6-50.

4. Make sure that the reference gas is open.

5. Click Yes.

Figure 6-50. Message window to ensure that reference gas is opened

6. In the Set Calibration Parameter window, enter 200 at Start [Steps]


and 12500 at Stop [Steps].

These parameters define the range of the magnet scan with CO2 as
calibration gas. See Figure 6-51.

7. Enter 2 at Step [Steps] to catch the correct peak height for the
various peaks. See Figure 6-51.

8. Confirm with OK.

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System Setup
Calibrating and Adjusting the System

Figure 6-51. Set Calibration Parameter window

The mass scan starts.

Wait until it is finished. See Figure 6-52.

Figure 6-52. Mass calibration finished

9. Click the Calibration button.

6-44 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

The calibration window opens. See Figure 6-53.

Labeled Components: 1=plot area, 2=calibration area


Figure 6-53. Proposal of peak positions

The mass proposals are shown in the calibration area (2 in


Figure 6-53): CO2 masses at 44, 28, and 12 for the selected
reference gas as well as some water masses 16, 17, 18. The masses
12, 28 and 44 need to be identified to proceed. A proposal about
their position is then offered.

On demand, additional masses can be added to the proposal list. If


the positions do not match satisfactorily, they are slightly moved
later.

10. Click anywhere in the calibration area 2 to activate this area.

11. Above the plot area 1, double-click Cup 3 to select the center cup.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-45
System Setup
Calibrating and Adjusting the System

12. Click the Info button to check your selection of masses for
consistency. See Figure 6-54.

Figure 6-54. Controlling mass proposals

The curve in Figure 6-54 shows the quadratic dependence of the


magnetic field (proportional to mass units) generated by the current.
The latter is given in steps of the DAC that controls the current in
the magnet.

13. Identify the masses 44, 28 and 12 in the plot area of the scan.

14. Adjust the proposed values by dragging and dropping the vertical
lines to the correct values.

15. When you finished the corrections, click the Finish Cal. button.

The calibration takes approximately 15 min.

Isodat now attempts to scan the peaks in detail to determine the


exact positions on the magnet current scale. In the calibration
window and in the peak list, check that the peak height shown there
matches the mass number selected.

Tip If the calibration has been successful, the calibration window


shows a new picture where the mass position markers no longer
coincide with the mass peaks. This reflects the magnet hysteresis, a
physical effect that is inherent to the magnet and that cannot be
avoided.

When the calibration is finished, the Save Calibration window


opens.

6-46 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

16. Mark the check box Pass Calibration to the current


Gasconfiguration.

17. Enter a calibration name.

18. Click Save.

The calibration is saved as an Isodat Calibration file (not as a single


file) and passed to the particular gas configuration. The gas
configuration is loaded together with this particular calibration
information.

19. Click the Save button in the system bar to save the calibration.

The Save As window opens.

20. Enter the file name for the calibration. See Figure 6-55.

21. Click Save.

Figure 6-55. Saving the calibration

The calibration is saved. This file is not used for mass identification. It
can be used for mass re-calibration, if necessary.

Tip Check the Gas Configuration Editor (see “Creating a Gas


Configuration” on page 6-20) for the selected calibration. The same
calibration can be used multiple times, and for more than one gas
configuration. On the other hand, several calibrations can be used for
one gas configuration.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-47
System Setup
Calibrating and Adjusting the System

Jump Calibration for Elemental Analyzer Applications


For C/N or H/O analysis with Elemental Analyzer applications, a jump
calibration must be performed.

❖ To perform a jump calibration

1. Open Instrument Control of Isodat.

2. Make sure that both your Elemental Analyzer configuration and


your gas configuration are selected.

3. Select Scan > Jump Calibration. See Figure 6-56.

Figure 6-56. Selecting Jump Calibration

4. In the Available Jump Calibrations window, click the New button.


See Figure 6-57.

Figure 6-57. Available Jump Calibrations window

5. In the Create Jump Calibration window, select the suitable gas


configurations from the drop-down lists. Enter the appropriate
values. See Figure 6-58.

6-48 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

6. Click OK.

Figure 6-58. Creating Jump Calibration

7. A message window opens. See Figure 6-59.

Figure 6-59. Preparing reference port

Depending on the selected gas configurations, Isodat reminds you to


open the respective reference port.

8. Open the respective port.

9. Click Yes.

The peak center scan starts. See “Peak Center Scan” on page 6-52.

The fast peak jump calibration starts for the duration of


approximately 10 to 15 min.

10. Wait until the jump calibration is finished.

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System Setup
Calibrating and Adjusting the System

Peak Shapes
The term “peak shape” refers to the ion optical image of the slit on the
respective cup. This term is used to denote the quality of the ion optical
system as well as the quality of cup alignment.

A peak shape is obtained by electrically or magnetically moving the slit


image over the respective cup. Isodat offers a standard way of scanning
the peak shape with the Scan window of Instrument Control.

❖ To perform a peak shape scan

1. Open Instrument Control of Isodat.

2. In the Scan window, select Peak Shape. See Figure 6-60.

Figure 6-60. Selecting Peak Shape scan

3. Click the Start Scan button to start.

The individual peak shape of your instrument depends on the


selected cup arrangement. In the CO2 scan (Figure 6-61), the
smallest mass occurs first in the Scan window. The bigger masses
appear later.

Figure 6-61. CO2 scan using an Universal Triple Collector

6-50 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

Due to cup geometry - and contrary to the CO2 scan - in the N2


scan (Figure 6-62), the biggest mass occurs first. The smaller masses
appear later.

Figure 6-62. N2 scan using an Universal Triple Collector

As an example for a special customized collector arrangement,


Figure 6-63 shows a scan of a simultaneous N2-NO-N2O-CO2
measurement.

Figure 6-63. Scan of a simultaneous measurement

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System Setup
Calibrating and Adjusting the System

Peak Center Scan


A peak center scan is an electric scan where the physical ion beam is
electrically moved across the cup by changing the accelerating voltage.

The purpose of the peak center scan is to obtain a value for the statistical
center of the ion beam, given in HVDAC steps. If no proper peak can
be detected (if the peak is too small or ends outside the Scan window,
for example), the function assumes the value -1.

Figure 6-64 shows the Center Scan button on the Accessories toolbar.

Figure 6-64. Center scan button in Accessories toolbar

❖ To preset Center Scan parameters

1. Open Instrument Control of Isodat.

2. On the toolbar of Instrument Control, click the arrow next to


Editors and select Gas Configuration Editor. See Figure 6-65.

Figure 6-65. Opening Gas Configuration Editor

The Gas Configuration Editor window opens. See Figure 6-66.

Figure 6-66. Gas Configuration Editor window

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Calibrating and Adjusting the System

3. Right-click somewhere in the row for a gas configuration to open


the context menu. See Figure 6-67.

4. From the menu, select Peak Center.

Figure 6-67. Context menu of Gas Configuration Editor

The Scan Basic window opens. See Figure 6-68.

5. Click the double arrows next to Intensity.

Figure 6-68. Scan Basic window - I

The Scan Integration Unit window opens. See Figure 6-69.

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System Setup
Calibrating and Adjusting the System

6. Set an appropriate integration time. Click OK.

Figure 6-69. Setting integration time

7. In the Scan Basic window, click the double arrows next to High
Voltage. See Figure 6-70.

Figure 6-70. Scan Basic window - II

The Scan ScaleHv window opens. See Figure 6-71.

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System Setup
Calibrating and Adjusting the System

8. Change the values as appropriate. Click OK.

Figure 6-71. Setting High Voltage

9. Click OK to close the Scan Basic window.

10. Click Save & Close to close the Gas Configuration Editor.

The parameters for the peak center scan have now been set. The peak
center scan can now be performed:

❖ To perform a peak center scan

1. Open Instrument Control of Isodat.

2. On the Accessories toolbar, click the Center Scan button.

The Peak Center window opens. See Figure 6-72.

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System Setup
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The peak center scan begins.

Figure 6-72. Peak Center procedure

The result values of the peak center scan are displayed in the
Information window as well. See Figure 6-73.

Figure 6-73. Result values of peak center scan

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Calibrating and Adjusting the System

Peak Center Offset


A peak center offset allows adjusting the ion beam aside the center of the
peak found. See “Peak Center Scan” on page 6-52.

After each peak center scan, the obtained peak center value is corrected
by the fixed peak center offset value (given in HVDAC steps). See PC
Offset of the gas configuration in Figure 6-66.

❖ To perform a peak center offset

1. Open Instrument Control of Isodat.

2. On the Accessories toolbar, click the Peak Center Offset button.


See Figure 6-74.

Figure 6-74. Peak Center Offset button on Accessories toolbar

The Peak Center Offset Determination window opens. A Peak


Shape scan is performed. See Figure 6-75.

Figure 6-75. Peak Shape scan is performed

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System Setup
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3. Enter the desired the peak center value in the field Offset, or adjust
the value by dragging and dropping the Offset line. See Figure 6-76.

Figure 6-76. Adjusting the desired peak center offset value

4. Click OK to confirm the Peak Center Offset value.

The Peak Center Offset value is transferred into the gas


configuration. See the PC Offset column in Figure 6-77.

Figure 6-77. Peak Center Offset transferred into gas configuration

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Calibrating and Adjusting the System

Peak Center Offset is especially useful when ratios for such species must
be determined that do not match the current cup configuration.

The parameters used in the Peak Shape scan (Start, Stop and Steps) are
stored at Peak Shape in the file IsoScanMacro.iso in the folder
C:\Thermo\IsodatNT \Global\Databases. In most cases, the file does
not need to be edited. Before editing this file, create a backup.

Electronic Offset
The electronic offset is used to calibrate the counting channels
associated with the cup amplifiers. It cannot be used for standard
applications.

❖ To perform an electronic offset

1. Open Instrument Control of Isodat.

2. On the Accessories toolbar, click the Electronic Offset button. See


Figure 6-78.

Figure 6-78. Electronic Offset button on Accessories toolbar

The Electronic Offset window opens. It shows the current values of


the electronic offsets for all channels. See Figure 6-79.

Figure 6-79. Current values of electronic offsets

3. Click the Reset button to reset the values to N/A.

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Calibrating and Adjusting the System

4. Click the Measure button to measure the current counting rate on


each amplifier channel.

The base count rate generated by the voltage-to-frequency counters


plus additional electronic noise is measured. The resulting offset
value is then subtracted from all readings. This results in a zero
reading when no current enters the respective cups.

5. To calibrate the counter zero setting for all channels simultaneously,


switch off High Voltage on the Accessories toolbar. See Figure 6-80.

Emission is automatically switched off as well.

Figure 6-80. Switching off power supply on Accessories toolbar

Crimp Adjustment
Crimp adjustment is only important, if a Dual Inlet system is available.
See also “Crimp Adjustment” on page 9-24.

❖ To perform a crimp adjustment

1. Open Instrument Control of Isodat.

2. Open the valves that connect the two bellows of the Dual Inlet
system. See Figure 6-81.

Figure 6-81. Visualization of Dual Inlet system

6-60 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

3. Evacuate the Dual Inlet system using the fore vacuum and high
vacuum pumps.

4. Switch off the pumps.

5. Admit approximately 10 mbar of CO2 into each bellow.


6. Wait for at least 3 minutes to allow for equilibration of the gas.

7. Carefully adjust the crimps. The 10 mbar for CO2 must yield 2 V
on mass 44.

8. To check the current signal level, switch the Changeover valve


repeatedly between the left and right bellow. Allow for the signal to
settle a few seconds before taking the reading. The difference
between the two inlet capillaries should be less than 50 mV.

Calibrating the Bellows


The purpose of the bellows (variable volumes) is to compress or expand
gas samples to adjust proper gas flows for the two capillaries leading to
the Changeover valve.

Before a Dual Inlet measurement, a bellow hardware and a bellow signal


calibration must be performed. It is presumed that the ion source has
been switched on and focusing has already been performed.

To operate the bellows for the first time, perform a hardware calibration.

NOTICE A hardware calibration deletes a signal calibration. Hardware


calibration must always be followed by signal calibration.

Signal calibration establishes a relationship between the position of the


bellows and the signal on the cups. Since signal calibration needs to set
percentage values (25% and 75%) of bellows extension, hardware
calibration must always be performed before signal calibration.

During automated operation, if the bellows are controlled via scripts, or


during acquisition, Isodat uses an algorithm that allows direct setting of
signal amplitudes. For this to be possible, a signal calibration must be
performed.

NOTICE Signal calibration requires a signal intensity of at least 3 V.

If signal calibration has not been performed, the Diagnosis tests


cannot be run.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-61
System Setup
Calibrating and Adjusting the System

Hardware Calibration of the Bellows

❖ To perform a hardware calibration of the bellows

1. Open Instrument Control of Isodat.

2. On the Accessories toolbar, click the Calibrate Bellows button. See


Figure 6-82.

Figure 6-82. Calibrate Bellows button on Accessories toolbar

3. In the Calibrate Bellows window, select Hardware. See Figure 6-83.

Figure 6-83. Calibrate Bellows - Hardware

4. Click OK.

A message window opens. See Figure 6-84.

Figure 6-84. Calibrate bellows - hardware message

6-62 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

5. Click Yes.

The bellows are opened to 100% and closed again (0%).

Another message window informs that the hardware calibration has


been completed. See Figure 6-85.

Figure 6-85. Calibrate bellows - hardware calibration completed

6. Continue with “To perform a signal calibration” on page 6-63.

Signal Calibration of the Bellows

❖ To perform a signal calibration

1. Open Instrument Control of Isodat.

2. Let an amount of gas into the bellows that results in a pressure of


about 10-20 mbar on each side.

This gas amount is necessary to obtain a certain signal intensity. If


the gas amount is either too small (less than 10 mbar) or too large
(more than 20 mbar), warning messages appear.

3. Close valve 14 and valve 24.

4. On the Accessories toolbar, click the Calibrate Bellows button. See


Figure 6-86.

Figure 6-86. Calibrate Bellows button on Accessories toolbar

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-63
System Setup
Calibrating and Adjusting the System

5. In the Calibrate Bellows window, select Signal. See Figure 6-87.

Figure 6-87. Calibrate Bellows window - Signal

6. Click OK.

A message window (Figure 6-88) informs that the calibration of the


right and left bellow starts.

Figure 6-88. Calibrate bellows - hardware message

The signal intensity of the gas is measured depending on the volume


of the bellows.

7. After the calibration has been performed, right-click the bellow


symbol in the Dual Inlet window.

In the Set Volume Control window, enter the desired volume ratio
in %. See Figure 6-89.

Figure 6-89. Setting volume of bellows

6-64 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System

The arrows below the bellows value on the right in Figure 6-89
allow for increasing or decreasing the volume by a single step at the
respective bellows motor.

Alternatively, click on the bellows symbol (right in Figure 6-89) and


drag your mouse up or down to the desired volume.

Pressure Adjustment

During automated operation, a number of parameters are used to


control the movement of the bellows. They are summarized in the
Peripherals tab of a Dual Inlet method. See Figure 6-90.

Figure 6-90. Parameters for Pressure Adjust

An automated pressure adjustment can only be carried out after the


signal calibration has been successfully performed.

Without bellows calibration, pressure adjustment and Diagnosis tests


are impossible. After the bellows have been calibrated however, the
Diagnosis tests can be run. For details, see Chapter 8,
“Troubleshooting.” .

After performing Diagnosis tests, a measurement of a Dual Inlet


acquisition can be started. For details, see Chapter 7, “Operation.” .

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-65
System Setup
Calibrating and Adjusting the System

Focus Settings of the IRMS


Focusing reduces or increases sensitivity, or optimizes linearity. Focusing
has to be performed to overcome:

• minimal remaining mechanical tolerances

• the gradual degradation of the ion source (due to metal deposition


by sputtering, for example)

• the different ion-optical properties of various gases (for H2, a slightly


different focusing compared to CO2 yields better results, for
example)

Typically, an Auto Focus procedure as described at “Auto Focusing” on


page 6-70 needs to be performed to optimize the Focus Delta settings of
your Delta V Series instrument for your gas configuration.

Isodat additionally offers a manual focusing procedure. See “Manual


Focusing - Tune Scan” on page 6-71.

Tip If you are not experienced with focusing, Thermo Fisher


Scientific recommends performing the Auto Focus procedure.

A first type of manual focusing, intensity focusing (also called peak


shape focusing or sensitivity focusing) is performed only in case of
Dual Inlet measurements. Sensitivity and peak shape are improved,
when the extraction voltage (Extraction and Extraction Sym.) is
decreased.

In the vast majority of cases however, the so-called linearity focusing is


performed as another type of manual focusing. It requires relatively high
extraction voltages (high values of Extraction and Extraction Sym.) to
extract the ions out of the ionization housing.

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System Setup
Calibrating and Adjusting the System

The parameters shown in the Focus Delta window are assigned to the
current gas configuration. See Figure 6-91.

Figure 6-91. Parameters on Focus Delta window

Tip Thermo Fisher Scientific recommends specific focus settings for


each gas configuration.

Context Menu of Focus Delta Window

The context menu of the Focus Delta window offers additional


functions. See Figure 6-92.

Figure 6-92. Context menu of Focus Delta window

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-67
System Setup
Calibrating and Adjusting the System

Table 6-4 lists the commands of the context menu.

Table 6-4. Context menu of the Focus Delta panel


Menu Item Description
Load Opens a Focus Settings document (*.fcs).

Used to load previously saved parameters.


Save Opens the Save As dialog to save the current
focus settings as an *.fcs document (for example,
in the folder C:\Thermo\Isodat NT\Global\Focus
Settings).
Pass to Assigns the current focus settings to the active gas
Gasconfiguration configuration.

This command replaces previously assigned focus


settings.
Autofocus Opens the AutoFocusDelta dialog box.
Enables to select the Autofocus parameters and to
start the Autofocus procedure.
Create Focus Creates a *.csv report in the folder
Parameter Report C:\Thermo\Isodat NT\Global\Focus Settings.

❖ To open the context menu

1. Open Instrument Control of Isodat.

Alternatively, you can use Isodat Acquisition.

2. Right-click the Focus Delta window, or click the Menu button (see
8 in Figure 7-1) to open the context menu (see Figure 6-92).
See Table 6-4 for details about the context menu.

Editing Focus Parameter Values

Each focus parameter value of the Focus Delta panel can be adjusted
manually:

• either continuously by clicking and dragging up or down

• or using a context menu.

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System Setup
Calibrating and Adjusting the System

Dragging changes the value according to the step selected for this field.
A right-click opens the context menus shown in Table 6-5.

Table 6-5. Focus Delta context menus on value side


Context Menu Focus Parameter
Emission

Trap

Electron Energy

Extraction

Extraction Sym.

X-Focus

X-Focus Sym.

Y-Deflection

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System Setup
Calibrating and Adjusting the System

Table 6-5. Focus Delta context menus on value side, continued


Context Menu Focus Parameter
X-Deflection

Y-Deflection Sym.

SE-Suppression

Tip Only experienced users should perform manual focusing.

❖ To edit focus parameter values

1. Open Instrument Control of Isodat.

2. In the Focus Delta panel, move the mouse over the value to be
changed.

The mouse changes its appearance to arrows or, at the end of each
row, to a plus sign. For each click with the plus sign, the value
changes according to the step selected in the context menu. See
Table 6-5.

3. If you want to change the value continuously, click and drag the
mouse when the mouse shows the arrows.

4. Right-click the value and select Edit from the context menu, if you
want to enter the new value directly. The colored part of a field
increases and diminishes with the parameter value.

Auto Focusing
❖ To perform Auto Focusing

1. Open Instrument Control of Isodat.

The Scan window opens. See Figure 6-32.

2. Click this button to start Auto Focus.

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System Setup
Calibrating and Adjusting the System

The Auto Focus Delta window opens. See Figure 6-93.

Figure 6-93. Auto Focus Delta window

3. Click OK, because the default settings can typically be accepted.


The potentials (see Figure 6-91) are adjusted accordingly.

By de-selecting one of the variable potentials however, you decrease


the possibility of changing the signal. This is very useful for fine
tuning. If you know, for example, your desired focus voltage, set it
manually, then de-select the Focus Voltage option in the Autofocus
window, and finally perform the Auto Focus.

4. Save the focus settings or Pass to Gas Configuration. See


Figure 6-92 and Table 6-4.

Manual Focusing - Tune Scan


The instrument has been focused ex-factory during the testing
procedure. You only need fine tuning according to your needs.

Tip Only experienced users should perform manual focusing. Be


careful. In case of doubt, preferably perform Autofocusing. Manual
focusing and Autofocusing can also be performed in turn (for
example, beginning with a rough manual focusing that is followed by a
fine Autofocusing).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-71
System Setup
Calibrating and Adjusting the System

All or only selected potentials might be varied. It may be advantageous


to set some potentials to default values, for example as Table 6-6 shows.
Table 6-6. Setting potentials to default values
Potential Set it to
Trap maximum
Electron Energy maximum
Emission maximum (or lower)
Extraction about 80% (for linearity focusing)

Do not change the parameter SE Suppression. It is pre-set to about


80-90% (about 200 V).

❖ To perform manual focusing

1. Open Instrument Control of Isodat.

The Scan window opens. See Figure 6-32.

2. In the Scan window, select Tune Scan. See Figure 6-94.

Figure 6-94. Selecting Tune Scan

6-72 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Resetting the Mass Spectrometer

A Tune scan monitors the course of intensity over time while


changing the parameters in the Focus window. It continues during
the complete focusing process.

Tip For this Tune scan, it does not matter which cup is used.
Focusing aims at gaining the maximum intensity value, which is
obtained by the Tune scan. In case of Dual Inlet, 100 mV
approximately correspond to 1 mbar.

3. Select a particular cup (for example, mass 44, mass 45 or mass 46).

The intensity of this mass/cup is monitored over time.

4. Change the values to your needs as described at “Editing Focus


Parameter Values” on page 6-68.

5. Click the Start Scan button.

The Tune scan begins.

6. After scanning, Save the focus settings or Pass to Gas


Configuration. See Figure 6-92 and Table 6-4.

Resetting the Mass Spectrometer


For some cases, it may be necessary to reset the mass spectrometer.

NOTICE Thermo Fisher Scientific recommends running the Version Handler of


Isodat to save your configurations and result data before resetting the
instrument. See “Creating an Isodat Backup” on page 6-14.

When resetting the mass spectrometer, all configurations including the


cup settings are deleted. Remember these for later re-configuration.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-73
System Setup
Resetting the Mass Spectrometer

❖ To reset the mass spectrometer

1. Open the Configurator of Isodat.

2. Select Edit > Reset Isotope MS. See Figure 6-95.

Figure 6-95. Selecting Reset Isotope MS

A message window opens. See Figure 6-96.

3. Confirm with Yes.

Figure 6-96. Reset deletes all configurations

4. To continue the reset, see “Starting Isodat the Very First Time” on
page 6-17.

6-74 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
7
Operation

This chapter describes basic operations and measurements of your


Delta V Series instrument.

Contents

• Safety Guidelines for Operation on page 7-2

• Isodat Software Suite on page 7-2

• Starting Up the Instrument on page 7-4

• Shutting Down the Instrument on page 7-5

• Creating a New Method on page 7-6

• Creating a New Sequence and Starting Acquisition on page 7-9

• ²H/¹H Measurements on page 7-13

• Dual Inlet System on page 7-18

• Editing a Configuration in Advanced Mode on page 7-27

• Viewing Results on page 7-40

• Exporting Results on page 7-46

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-1
Operation
Safety Guidelines for Operation

Safety Guidelines for Operation


When operating the Delta V Series instrument, pay attention to the
following general safety guidelines.

WARNING High Voltage. Risk of injury. Some parts of the Delta V Series
instrument are at high voltage. Opening the electronics cabinet is only
allowed for maintenance purposes by qualified service personnel.

WARNING Electric Current. Risk of electric shock. Do not remove the cover
before or during operation, for example, at the ion source. Voltages of
at least 220 V are prevalent inside.

WARNING Explosive Gas. Risk of injury. Ethanol vapors are explosive. Do not
smoke or handle with open fire. During leak detection, ventilate the
laboratory carefully.

CAUTION Hot Surface. Risk of burns. Temperatures of about 75 °C or higher


may be reached at the metallic surface of valves that are baked out. Do
not touch any surface of a valve you are baking out.

CAUTION Cold Liquid. Risk of frostbite. The Autocool Refill device contains
extremely cold liquid gas. Careless handling might cause severe
personal injury including frostbite. Only use liquid nitrogen as cooling
agent.

WARNING Noxious Material. Risk to health. Hazardous compounds introduced


into the system may be dissolved in the pump oil. Use only
locally-approved containers and procedures for waste oil disposal.
Notice that contaminated pumps must be emptied and
decontaminated before they are sent back to Thermo Fisher Scientific
for repair or exchange.

Isodat Software Suite


Isodat is the software suite for system control, data acquisition and data
evaluation being an integral part of the system architecture.

All aspects of the mass spectrometer are controlled by Isodat, including


ion generation, mass separation and ion detection. Control of the ion
source allows manual tuning, autotuning, as well as storage and retrieval
of ion source parameters.

Different configurations representing different analytical setups can be


stored and retrieved. Up to eight simultaneous data acquisition streams
are supported.

7-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Isodat Software Suite

The system is designed to fully automatically execute predefined


procedures and run sequences of analyses, including customized
reporting.

Isodat Script Language (ISL) is the tool giving the expert user full access
to the mass spectrometer, the inlet systems and additional user-supplied
devices. An input-output module allows connection and control of up
to five interfaces. Scripts can be developed for customized applications.

Isodat provides a comprehensive set of customizable data evaluation


routines. Standard report forms are provided according to the
application. In addition, reports can be easily customized in the Result
Workshop of Isodat. This section describes the most basic buttons of the
Isodat modules Instrument Control and Acquisition.

The Accessories toolbar (1 in Figure 7-1) is located at the top of the


panels.

1
2 3 4

9 7
8

Labeled Components: 1=Accessories toolbar, 2=Hide button, 3=Pop out button, 4=Shrink button, 5=Editors, 6=Redo
button, 7=Undo button, 8=Menu button, 9=Focus Delta context menu
Figure 7-1. Accessories toolbar and panel buttons

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-3
Operation
Starting Up the Instrument

For details about the Focus Delta panel, see “Focus Settings of the
IRMS” on page 6-66.

Table 7-1 lists the function available on the Accessories toolbar.


Table 7-1. Functions available on Accessories toolbar
Icon Name Comment
File Search Allows searching for Isodat files.

Center Scan Starts a peak center procedure.

Electronic Offset Allows measuring and/or resetting an


electronic offset.
Peak Center Offset Starts determining the peak center
offset.

Auto Focus Allows selecting the auto focus


parameters and starting the auto
focus procedure.
Calibrate Bellows Only visible if a Dual Inlet
configuration is loaded.

Allows the hardware calibration or


signal calibration of the bellows.
Reset HV Resets the HV voltage.

Source On Switches on the source electronics.

Source Off Switches off the source electronics.

Starting Up the Instrument


Before starting measurements, switch on the Delta V Series instrument
as follows.

The first startup of the system is described at “System Preparation” on


page 6-7.

❖ To start up the instrument

1. Make sure that compressed air is connected to the instrument. See


also “Compressed Air” on page 6-5.

This is especially important, if you operate a Dual Inlet system.

2. Check that the needle valve is closed.

7-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Shutting Down the Instrument

You can close the needle valve using the adjusting knob (7 in
Figure 3-3).

3. Switch off the system by turning the main switch (1 in Figure 3-7).

4. Switch on the computer.

5. Start Isodat.

6. Switch on the pumps at the control panel. See 4 and 5 in Figure 3-3.

7. In the MS State panel of Isodat, switch on all heaters you need. See
Figure 6-31.

8. On the Accessories toolbar of Isodat (in Instrument Control or


Acquisition), click this button to switch on the ion source.

The instrument is stable and ready for operation, when the


operating vacuum is reached. This usually takes 24 to 48 hours.

Shutting Down the Instrument


The Delta V Series instrument should only be shut down as follows for
maintenance.

Tip In case the system will not be used for several weeks or months,
Thermo Fisher Scientific recommends only switching off the ion
source.

❖ To shut down the instrument

1. On the Accessories toolbar of Isodat (in Instrument Control or


Acquisition), click this button to switch off the ion source.
2. In the MS State panel of Isodat, switch off all heaters. See
Figure 6-31.

3. Wait for approximately 30 minutes.

4. Switch off the pumps at the control panel. See 4 and 5 in Figure 3-3.

5. Wait approximately 3 to 10 minutes for the system to vent. The


venting can be heard.

6. Switch off the system by turning the main switch (1 in Figure 3-7).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-5
Operation
Creating a New Method

Creating a New Method


All parameters relevant for data acquisition of a sample are stored in a
method. This section describes how to create a new method.

Thermo Fisher Scientific provides a set of predefined configurations,


methods and sequences for dedicated system configurations.

Before creating a method, you must already have performed the steps
described in the following sections:

• “Creating a Gas Configuration” on page 6-20

• “Creating a Configuration” on page 6-25

Before defining a new gas configuration, ensure that the connected


IRMS has the cups set for the simultaneous detection of masses 44, 45
and 46 (see “Starting Isodat the Very First Time” on page 6-17) and that
the mass calibration for these cups has already been performed (see
“Mass Calibration” on page 6-41).

❖ To create a new method

1. Open the Acquisition of Isodat.

2. Select the configuration for your application (Dual Inlet, for


example).
3. Select the suitable gas configuration (CO2., for example).

4. Click this button.

The File New dialog opens. See Figure 7-2.

Figure 7-2. File New dialog box

7-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Creating a New Method

5. Select the Method icon.

6. Confirm by OK.

7. Check the values and parameters of the Instrument tab of the


method. See Figure 7-3.

Figure 7-3. Instrument tab of new method

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-7
Operation
Creating a New Method

8. Check the values and parameters of the Peripherals tab. See


Figure 7-4.

Figure 7-4. Peripherals tab of new method

Depending on the system configuration, different options are


shown. In this example, a Dual Inlet Multiport system configuration
has been selected.

Tip The example values and parameters in the tabs of the new
method can usually be accepted.

9. Click this button.

7-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Creating a New Sequence and Starting Acquisition

The Save As window opens.

10. Enter a name for the method.

11. Click Save.

12. To start a measurement, proceed with “Creating a New Sequence


and Starting Acquisition” on page 7-9.

Creating a New Sequence and Starting Acquisition


A measurement is performed with a sequence that in turn is based on a
method designed for your system configurations.

Before starting an acquisition, make sure that:

• Electronic offset has been measured and saved. See “Electronic


Offset” on page 6-59.

• All peripherals have been configured. See “Creating a


Configuration” on page 6-25.

• The mass calibration for all gases to be measured has been


performed. See “Mass Calibration” on page 6-41.

• In case of a Dual Inlet application, the bellows calibration has been


performed. See “Calibrating the Bellows” on page 6-61

• In case of Elemental Analyzer application for C/N or H/O analysis,


the jump calibration has been performed and saved. See “Jump
Calibration for Elemental Analyzer Applications” on page 6-48.

• In case of a liquid autosampler, the COM port and the other


parameters have been set. Refer to the Operating Manual of the
autosampler for details.

See “Calibrating and Adjusting the System” on page 6-29 for a detailed
description of system preparation.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-9
Operation
Creating a New Sequence and Starting Acquisition

❖ To create a new sequence and to start acquisition

1. Open the Acquisition of Isodat.

2. Click this button.

The File New dialog opens. See Figure 7-5.

Figure 7-5. File New dialog of Isodat

3. Select the Sequence icon and click OK.

4. Define the number of samples (3, for example) and click OK. See
Figure 7-6.

Figure 7-6. Defining number of samples

7-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Creating a New Sequence and Starting Acquisition

5. The sequence opens. See Figure 7-7. In the Method column, select
the appropriate IRMS method from the drop-down list.

Figure 7-7. Editing the sequence list

Edit the sequence list as required:

Click the table cells of the desired rows to activate the cell. The
green check mark is shown when activated.

6. Select this button to perform a peak center before the measurement.

7. Select this button to check reference dilution.

8. Select this button to activate H3 Stability.

9. Select this button to activate H3 Factor.

10. Enter text in column Identifier 1 to identify the sample.

11. Select an IRMS method for each sample (H3-Delta V-H2.met, for
example).

12. Click the Start button.

13. Enter a file name. See Figure 7-8.

The file extension .seq is added automatically.

14. Click Save.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-11
Operation
Creating a New Sequence and Starting Acquisition

Figure 7-8. Saving a sequence

The Start Sequence dialog opens. See Figure 7-9.

Figure 7-9. Defining sequence parameters

7-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
²H/¹H Measurements

15. Select parameters for Results, Export, Printout, Properties, and


Sequence Scripts.

16. Click OK to start the sequence.

²H/¹H Measurements
This section describes 2H/1H measurements and their requirements.

Determining the H3 Factor


H3+ ions formed in the ion source interfere with DH+ ions in the mass
spectrum. The H3+ portion of the m/z ion beam is determined as
H3 factor. The H3 factor is used to correct the H3+ contribution to the
m/z 3 signal. A low and stable H3 factor is desirable. It must be
determined before measuring samples and is basically a linearity
measurement.
Formation of H3+ ions is due to the ion-molecule reaction inside the ion
source:
+ +
H2 + H2  H3 + H

The number of H2 molecules and the number of H2+ ions are both
proportional to the partial pressure of H2 gas in the ion source. Hence,
the H3+ ion formation rate is proportional to the square of the H2 partial
pressure in the ion source. As a result, the measured ion current ratio can
be written as:

+ + + 2
DH + H 3 DH + k   H 2 
+
I(3)
--------- = ----------------------------
- = -----------
- ------------------------
-
I(2) + + +
H2 H2 H2

with:

I(2): measured ion current on m/z 2

I(3): measured ion current on m/z 3

k: H3 factor

This leads to:


+
DH = I(3) – k  I(2)
-----------
+
- ---------
H2 I(2)

To minimize the H3+ ion formation rate, the ion source is usually
operated at 100% extraction voltage. This minimizes the residence time
of hydrogen ions in the ionization volume of the ion source.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-13
Operation
²H/¹H Measurements

Creating a Method for H3 Factor Determination


❖ To create a method for H3 factor determination

1. Open Acquisition of Isodat.

2. Select the configuration for your application,


ConFlo IV + Generic EA (HF I), for example.
3. Select the gas configuration (H2, for example).

4. Click this button.

The File New dialog opens. See Figure 7-10.

5. Select the Method icon.

6. Click OK.

Figure 7-10. File New dialog of Isodat

The new method opens with its Instrument tab.

7-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
²H/¹H Measurements

7. In the Instrument tab of the method, select H2 at


Gasconfiguration. See Figure 7-11.

Figure 7-11. Instrument tab of method for H3 factor determination

8. Click the folder icon for Acquisition Script.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-15
Operation
²H/¹H Measurements

9. Select the script Linearity determination acq.isl in the folder for your
system configuration, for example. See Figure 7-12.

Figure 7-12. H3 determination script folder

For all other settings, the default values can typically be accepted.

10. Click this button.

The Save As window opens.

11. Enter a name for the method.

12. Click Save.

Creating a Sequence for H3 Factor Determination and Starting Acquisition


1. Open Acquisition of Isodat.

2. Click this button.

The File New dialog opens. See Figure 7-13.

3. Select the Sequence icon.

4. Click OK.

7-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
²H/¹H Measurements

Figure 7-13. File New dialog

5. Define the number of samples. Click OK. See Figure 7-14.

Figure 7-14. Defining number of samples

6. In the Method column, select the appropriate IRMS method for the
H3 factor determination from the drop-down list. See Figure 7-15.

Figure 7-15. Selecting IRMS method

7. Select this check box for the appropriate sequence lines to determine
the H3 factor. See Figure 7-16.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-17
Operation
Dual Inlet System

Figure 7-16. Activating H3 factor determination

8. Edit the sequence list as required.

9. Click the Start button.

Dual Inlet System


The Dual Inlet window in Instrument Control or Acquisition of Isodat
schematically shows all relevant valves, pressure values and pump
statuses of the system. See Figure 7-17.

Labeled Components: 1=crimp position of capillary (1 × left and 1 × right), 2=turbomolecular pump of Dual Inlet system,
3=fore vacuum pump of Dual Inlet system
Figure 7-17. Dual Inlet window

7-18 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Dual Inlet System

The values at the top left and top right of the Dual Inlet window show
the current pressure of the left and right side of the Dual Inlet system,
respectively in millibar.

The value at the lower part of the Dual Inlet window shows the current
pressure value of the fore vacuum pump in millibar.

The values below the left and right green bellows show the volume
proportion of each bellow in %.

Switching Positions of the Changeover Valve


The Changeover valve (for its position in the Dual Inlet window, see
Figure 7-17) can be switched to three different positions. See
Figure 7-18.

1 2 3

Figure 7-18. Switching positions of Changeover valve

• In 1 in Figure 7-18, the left side capillary is opened to the ion source
while the right side capillary is opened to the turbomolecular pump
of the Dual Inlet system.

• In 2 in Figure 7-18, the right side capillary is opened to the ion


source while the left side capillary is opened to the turbomolecular
pump of the Dual Inlet system.

• In 3 in Figure 7-18, both capillaries are pumped by the


turbomolecular pump of the Dual Inlet system.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-19
Operation
Dual Inlet System

Changeover Valve in Dual Inlet Measurement


Two important times can be adjusted in the Dual Inlet method. The
first is the integration time in the Instrument tab. See Figure 7-19.

Figure 7-19. Setting integration time

The second time that can be adjusted is the idle time in the Peripherals
tab. See Figure 7-20.

Figure 7-20. Setting idle time

Usually, the Changeover valve is controlled by Isodat to accomplish a


Dual Inlet measurement.

Figure 7-21 shows a flow chart of the basic Dual Inlet measurement.
“Measure” is the measurement of ion current during the integration
time.

7-20 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Dual Inlet System

No
Microvolume

Close V15 Open V15


Close V25 Open V25
Switch to:
Sample
Switch to:
Standard Idle Time

Idle Time Measure


Integration Time
Measure
Integration Time Switch to:
Standard

Idle Time

Measure
Integration Time

No
Cycles?

Figure 7-21. Dual Inlet measurement loop

Shot Noise Limits of Precision in Dual Inlet Measurements


Figure 7-22 shows how precision (one  value) varies when integration
time and amplitude are changed.

Shot Noise Limit


0.04
0.035 16 s integration time
0.03 8 s integration time

0.025 4 s integration time


1  Limit

0.02 32 s integration time

0.015
0.01

0.005
0
0 2 4 6 8 10 12 14
Amplitude

Figure 7-22. Shot noise limits of precision

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-21
Operation
Dual Inlet System

Higher amplitudes and longer integration times lead to enhanced


measurement precision, with low standard deviation of the n repetitions
(with n selected at Number of Cycles in Figure 7-20; for example,
n = 8).

This consideration can be used to select a reasonable integration time


for a given measurement and to calculate the precision that can be
expected.

The diagram contains the results of a calculation for the shot noise
(statistical noise) on a cup, taking into account the integration time, the
resistor of the cup and the signal height on that cup. The sample
calculation is performed for the middle cup and is true for  13C. For
 18O roughly multiply the results by 1.4.

The internal precision value is shown for Standard Deviation in the


output table. The internal precision is not the value shown for Standard
Error, although in discussions both are often confused.

The standard error is a value that is generally smaller, because it takes


into account the repetitions of the measurement (number of cycles,
usually set to 8). The standard error is also shown in the output table
and represents the error in determining the average of a distribution (in
our case the average -value of the n repetitions of individual
measurements).

Switching Positions of the Changeover Extension


The Changeover Extension enhances the capabilities of the standard
Changeover valve by adding two ports usable for two additional
peripherals.

Similar to the Changeover valve, in Isodat the Changeover Extension


can be switched to five different positions. Figure 7-23 shows the first
two of them, and Figure 7-24 the remaining three ones.

1 2

Figure 7-23. Positions of Changeover Extension - I

7-22 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Dual Inlet System

In 1 in Figure 7-23, the left side capillary is opened to the ion source
while the right side capillary is opened to the turbomolecular pump of
the Dual Inlet system.

In 2 in Figure 7-23, the right side capillary is opened to the ion source
while the left side capillary is opened to the turbomolecular pump of the
Dual Inlet system.

3 4 5

Figure 7-24. Positions of Changeover Extension - II

In 3 in Figure 7-24, the left side capillary of the Changeover Extension is


opened to the ion source while all other capillaries are opened to the
turbomolecular pump of the Dual Inlet system.

In 4 in Figure 7-24, the right side capillary of the Changeover Extension


is opened to the ion source while all other capillaries are opened to the
turbomolecular pump of the Dual Inlet system.

In 5 in Figure 7-24, all capillaries of the Changeover valve and the


Changeover Extension are pumped by the turbomolecular pump of the
Dual Inlet system.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-23
Operation
Dual Inlet System

Combined Multiport-Microvolume Measurement


The parameters of both Microvolume and Multiport can be set in the
Peripherals tab of a Dual Inlet method. See Figure 7-25.

Figure 7-25. Setting Microvolume and Multiport parameters

7-24 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Dual Inlet System

Figure 7-26 schematically shows a combined Multiport-Microvolume


measurement.

p sample pressure
MpExp Multiport Expansion Threshold
MpDirect Multiport Bellow Direct Threshold
p μVBank Microvolume Freeze Bank Threshold
μVAll Freeze All Threshold
Expansion Mode as described in the method for Microvolume

Expansion
p > MpExp Bank to Bellow

Gas Transfer
p < MpDirect Bank to Bellow

p < MpDirect Expansion


p > μVBank Mode

Gas Transfer
p < μVBank Bank to
p > μVAll Microvolume

Gas Transfer Dual Inlet


p < μVAll Sample to Measurement
Microvolume Cycle

Figure 7-26. Combined Multiport-Microvolume measurement

The sample pressure p is measured. If p is too high to be measured


directly with the bellows, the gas is expanded to the bellows, and the
remaining gas is pumped off.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-25
Operation
Dual Inlet System

Reference Refill
If a Reference Refill device is installed and configured, the Reference
Refill parameters can be set in the Instrument tab of the Dual Inlet
method. See Figure 7-27.

Figure 7-27. Setting Reference Refill parameters

Figure 7-28 schematically shows the Reference Refill process.

Standard Bellows to
100%

Pump Line with Open Reference to


FV Threshold Bellows
Roughing Pump

Pump Line with HV Pump Time Fill Bellows Refill Time


Turbo Pump

Connect to Switch Bellows to


Reference Bottle COV

Switch off
Pump Line and Pump Overlay Time Reference Bottle
Capillary

Close all Dual Inlet


Valves

Figure 7-28. Reference Refill process

A fore vacuum threshold (FV Threshold) can be set to be used while the
bellows and adjacent volumes are pumped off. The respective volumes
are pumped off for the duration of the HV Pump Time with the Dual
Inlet turbomolecular pump.

During the Pump Overlay Time, the volumes and the connected
Reference Refill volume are pumped off together to avoid that used gas
enters the bellows.

The actual refill of the bellows takes place for the duration of the Refill
Time.

7-26 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

Editing a Configuration in Advanced Mode


This section describes how to edit a configuration in Advanced mode.

Tip Editing configurations is only possible in Advanced mode. Only


personnel trained by Thermo Fisher Scientific should perform this.

❖ To edit a configuration in Advanced Mode

1. Open the Configurator of Isodat.

2. Select Edit > Advanced mode. See Figure 7-29.

Figure 7-29. Selecting Advanced Mode

The Change into Advanced mode window opens. See Figure 7-30.

Figure 7-30. Entering Advanced mode

3. Confirm by OK.
4. Click the Devices tab.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-27
Operation
Editing a Configuration in Advanced Mode

The mass spectrometer you selected earlier is shown in the right


pane together with all peripherals. See Figure 7-31.

Figure 7-31. Instruments and peripherals in Device tab

5. In the upper left corner of the pane, right-click the icon of your mass
spectrometer.

6. Click Edit.

The Device Editor opens.

7. Continue with “Device Editor” on page 7-29.

Tip The Edit command that allows editing a configuration is only


accessible via the Devices tab in the Advanced mode.

7-28 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

Device Editor
The hardware database provides a pool of all available hardware
elements. During installation of Isodat, the hardware database is
checked for new hardware. As a subset, the installed hardware
components of the device are listed here.

The device is addressed with the Plug Measure ID which is the internal
board address. The board can manage more than one device.

Figure 7-32 shows the Device Editor for the currently edited device.

Figure 7-32. Device Editor

The Edit Mode allows modifying a device by adding additional


hardware components from the hardware database.

The Plug Measure ID is the ID assigned to the current device (for


example, 0 for your mass spectrometer).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-29
Operation
Editing a Configuration in Advanced Mode

❖ To modify a device by adding hardware components

1. In the Configurator of Isodat, enter the Advanced mode.

2. Open the Device Editor of your mass spectrometer. See “Editing a


Configuration in Advanced Mode” on page 7-27.

3. In the Device tab, select the check box Edit Mode. See Figure 7-33.

The window is divided in two panes, a left one and a right one.

The left pane in Figure 7-33 shows all hardware components that
could be added. The right pane displays only the installed
hardware components.

You can now add hardware components from the hardware database
to the list of already installed components.

4. In the left pane, mark the particular hardware component you want
to add (for example, Valve). See Figure 7-33.

all installed
hardware
components

all hardware
components that
could be added

Figure 7-33. Edit Mode activated

7-30 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

5. Drag and drop the particular hardware component you want to add
into the right pane (for example, Valve). See Figure 7-34.

The newly added hardware component (for example, Valve) is


added to the right pane. See Valve 1 in Figure 7-34.

Figure 7-34. Hardware component added

6. Configure the added new hardware component as follows:

a. Double-click the new hardware component (for example,


Valve 1).

The Hardware window opens. See Figure 7-35.

b. Enter the appropriate values in the fields.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-31
Operation
Editing a Configuration in Advanced Mode

c. Confirm with OK.

Figure 7-35. Properties of new hardware component

The hardware component is now defined in Isodat.

7. Continue with “Events Tab” on page 7-32.

Events Tab
❖ To configure events for a hardware component

1. In the Configurator of Isodat, enter the Advanced mode.

2. Open the Device Editor of your mass spectrometer. See “Editing a


Configuration in Advanced Mode” on page 7-27.

3. Click the Events tab for the currently edited device. See Figure 7-36.

7-32 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

4. Drag and drop a hardware component from the left pane (“Available
Items”) to the right pane (“Events”), Valve 1, for example.

Figure 7-36. Events tab

5. Right-click on the item newly added to the right pane.

The context menu opens. See Figure 7-37.

From the context menu:

• Select Rename to rename an item.

• Select Delete to delete an item.

If you selected Delete, a message window opens.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-33
Operation
Editing a Configuration in Advanced Mode

Confirm with Yes. The item is deleted from the right pane.

Figure 7-37. Deleting or renaming the selected item

After you changed events by adding, renaming or deleting them,


you must create new methods and sequences. In general, after
changing a database, create new methods and sequences.

6. If you added or changed an item, continue with “Sequence Tab” on


page 7-34.

Sequence Tab
❖ To configure sequence for a hardware component

1. In the Configurator of Isodat, enter the Advanced mode.

2. Open the Device Editor of your mass spectrometer. See “Editing a


Configuration in Advanced Mode” on page 7-27.

7-34 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

3. Click the Sequence tab for the currently edited device. See
Figure 7-38.

Figure 7-38. Sequence tab

4. Drag and drop an item from the left pane (“Available Items”) to the
right pane (“Sequence Items”) to add it to the Sequence Items list.

• Select Sequence Flag to activate or deactivate an action


(Interface Pump Control, for example).

• Select Sequence File and define method files (for autosampler


or GC, for example). These methods can then be selected in a
sequence.

• Select Sequence Text to add a text column (for a comment, for


example).

By dragging and dropping, add as many flags as you like to a


sequence. They are read out in the particular measurement scripts.
By activating/deactivating the sequence items, certain parameters
defined in the measurement script are set or not (delays or flow
rates, for example).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-35
Operation
Editing a Configuration in Advanced Mode

Often, for the first sample within a sequence, a flag is activated. It is


deactivated for the following samples of the sequence.

These basic parameters are set only once and kept constant for the
following samples. This ensures, for example, working with a
constant flow rate during the entire sequence. The same is true for
performing a peak center.

Monitor Parameter Tab


The right pane of the Monitor Parameter tab shows the parameters that
are constantly read out and monitored (the status of the acid pump -
blocked or not - or the status of the six-port valve, for example). See
Figure 7-39.

Figure 7-39. Monitor Parameter tab

System Start Values Tab


❖ To set system start values

1. In the Configurator of Isodat, enter the Advanced mode.

2. Open the Device Editor of your mass spectrometer. See “Editing a


Configuration in Advanced Mode” on page 7-27.

7-36 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

3. Click the System Start Values tab for the currently edited device.

The right pane of the System Start Values tab lists parameters that
are set to a certain value (the system start values) during the start of
Isodat. Individual components of the interface can be switched into
an intended status (switching the acid pump off, for example) while
Isodat is started. See Figure 7-40.

Tip The shutdown parameters of the system can be edited in the


Isodat Generic Editor. See “To use the Isodat Generic Editor” on
page 7-38.

4. Drag and drop an item (Source Heater, for example) from the left
pane (“Available Items”) to the right pane (“Parameter”). See
Figure 7-40.

Figure 7-40. System Start Values tab

5. In the right pane, right-click the newly added item.

6. From the context menu, select Properties.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-37
Operation
Editing a Configuration in Advanced Mode

7. From the drop-down list of Source Heater - State, select On. See
Figure 7-41.

Figure 7-41. Properties of added item

Every time Acquisition or Instrument Control starts, the source


heater is switched on.

Tip If the source heater has been on before starting Isodat,


nothing changes: the source heater stays on.

❖ To use the Isodat Generic Editor

1. In the folder C:\Thermo\IsodatNT \Global\bin, double-click the file


IsodatEditor.exe.

The Isodat Generic Editor opens. See Figure 7-42.

Figure 7-42. Isodat Generic Editor opens

2. Select File > Open, or click the Open button in the upper left
corner.

3. Browse to the folder C:\Thermo\Isodat NT \Global\Databases.

7-38 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode

Therein, select the file System ShutDown Parameters.iso. See


Figure 7-43.

4. Click Open.

Figure 7-43. Selecting file containing system shutdown parameters

The file opens in the Isodat Generic Editor. The system shutdown
parameters are shown. See Figure 7-44.

Figure 7-44. System shutdown parameters in Isodat Generic Editor

5. Edit the shutdown parameters of particular system components


(acid pump, oxidation reagent pump, purge, for example) according
to your needs.

NOTICE After editing shutdown parameters, a restart of Isodat is necessary for


the parameters to take effect. This feature is used for security. Some
parameters are set in a way not to damage the interface or the IRMS
during system startup and shutdown.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-39
Operation
Viewing Results

Viewing Results
In Continuous Flow applications, peak areas are calculated and shown
in the results window of Isodat. For Dual Inlet applications, intensity
values are determined.

After a measurement, a graphical presentation of the results and a table


containing the values are given in the Acquisition module. See
Figure 7-45 as an example for the results of a continuous flow
measurement with a Thermo Scientific™ Flash HT Plus elemental
analyzer.

Figure 7-45. Display of measurement results - example

You can define a peak or the background by clicking the Def Bgd and
the Def Peak button, respectively.

You can scan a selected area by clicking the Scan button, or delete single
or all occurrences.

7-40 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Viewing Results

During an acquisition, the Stop button is activated, and the sequence


line currently measured is highlighted. See Figure 7-46.

Figure 7-46. Sequence during measurement

The result table contains several tabs, each presenting a different set of
result data.

Representation of Data
• A red value indicates that during integration the timeout criterion
was reached.

Red numbers are only shown for intensities in the columns <m/z>
Sample and <m/z> Reference.
• Only for Dual Inlet measurements: A black value on a pink
background is an outlier relating to the particulars given in the
Outlier Test area of the Evaluation tab.

Re-evaluating these data with None for Outlier Test on the


Evaluation tab (see “Recalculation” on page 7-45) cancels the
emphasis of the values. See Figure 7-47.

Figure 7-47. Values changing color

•  values (for example, d 13C/12C vs. V-PDB, or d18O/16O vs.


VSMOW) are shown as black values on green. These values fall into
the k-fold of the  values.

Table 7-2 lists the columns shown on the Raw <gas configuration> tab
of the continuous flow measurement. For a Dual Inlet measurement, the
columns slightly differ.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-41
Operation
Viewing Results

Table 7-2. Columns of the Raw Data tab


Value Description
Peak Nr. Number of peaks found
Start [s] Start time in seconds
Rt [s] Retention time in seconds
Width [s] Width of peak in seconds
Sample Dilution [%] Sample dilution in %
Ampl. <m/z> [mV] Amplitude of a particular mass in mV.
A separate column is provided for each mass.
BGD <m/z> [mV] Background for a particular mass in mV.
A separate column is provided for each mass.
Area All [Vs] Sum of all (peak) areas for all isotope traces
Amt% [%] Atomic percentage value of the heavier isotope
The percentage is calculated from the  Mean value (for example, Atom-% of 13C is
calculated from  [13C/12C]).
R <m2/z>/<m1/z> Ratio of the intensities of two masses (for example, R 45/44)
rR <m2/z>/<m1/z> Raw Ratio of the intensities of two masses (for example, rR 45/44)
rd <m2/z>/<m1/z> Raw delta value of two molecular masses in ‰ vs. a secondary customary standard

The values are calculated from the raw ratios.

Example: rd [45 CO2/44 CO2] vs. CO2_zero


d <m2/z>/<m1/z>  value of two element isotopes (in ‰) vs. a primary standard

The values are calculated from the true element sample ratios and the true element
standard ratios. The true element standard ratios are read from primary standards
defined in the primary standard database.

Examples: d [13C/12C] vs. VPDB, or d [18O/16O] vs. VSMOW


Delta/Delta  value of two element isotopes (in ‰) vs. a primary standard.
<m2/z>/<m1/z> [‰]
These values are element deltas and are calculated from the true element sample
ratios and the true element standard ratios. The true element standard ratios are read
from primary standards defined in the primary standard database.

Example: Delta [13C/12C] vs. V-PDB or Delta [18O/16O] vs. V-SMOW


AT % Atomic percentage value of an isotope.

The value is calculated from the element delta and the corresponding absolute
element ratio of the standard.

Examples: At % [13C] or At % [18O]

7-42 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Viewing Results

Graphical Representation
Each mass finding is presented with a different color. The context menu
offers additional functions to change the appearance of the plot (Ratio
Options, for example). See Figure 7-48.

Figure 7-48. Context menu of graphical presentation

The menu items currently selected are shown with a check mark. It is
also possible to add labels or to re-scale the current view.

The acquisition values are shown in a table below the graphical


presentation. See Figure 7-49.

Figure 7-49. Table view of result data tab Raw Sample

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-43
Operation
Viewing Results

For the table view, the context menu offers the functions shown in
Figure 7-50.

Figure 7-50. Context menu for table view

If Calculate is selected from the context menu, the Calculate Results


dialog opens. See Figure 7-51.

Figure 7-51. Calculate Results dialog

Dedicated values may be changed or calculated with the aid of the


Calculator that opens with this button.

7-44 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Viewing Results

Recalculation
For some parameters of the method selected before measurement start,
values may be changed to be recalculated.

❖ To start recalculation

1. On the toolbar of the result window, click the Edit Method button
(Continuous flow measurement) or the Show Method button (Dual
Inlet measurement) to open the Method dialog.

Some tabs allow editing the settings for re-evaluation (Evaluation


Type or Standard Parameters, for example). See Figure 7-52.

Figure 7-52. Method dialog - opened from results (for a Continuous flow measurement)

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-45
Operation
Exporting Results

For the method, only those values that can be recalculated are
activated for editing. The Instrument tab does not offer values for
recalculation.

2. To change the standard parameter settings, select the new standard


from the drop-down list. See Figure 7-53.

Figure 7-53. Standard parameter for recalculation

3. Click OK to save the settings and to close the Method dialog.


4. To start recalculation, click the Start Re-Eval button for
Continuous flow measurements, or the Recalc button for Dual Inlet
measurements.

5. Wait until the re-evaluation/recalculation is finished.

The new values are shown in the result data view.

Exporting Results
Measurement parameters and results can be exported as a Microsoft™
Excel™ spreadsheet file. The export can easily be tailored to your needs.
Rules must be established to determine how to perform the export.
These export rules are described in an export template (a *.wke file).

Various selectors, which group Identifiers, are used to create an export


template. For an export, more than one template can be selected.
Multiple templates can be used simultaneously. Every single template
(*.wke file) finally leads to the export file wk1. Every wk1 file is created
according to the rules of the file.

Although measurement data are stored in one result file, the data
concerning every single gas type can be exported separately to an export
file of their own (multigas measurement, for example).

Single parts of a measurement can be exported to an export file of their


own (only the method parameters, for example).

Some types of data can be specified further in query tabs, where


sophisticated export properties are defined (peak-relevant data, for
example).

7-46 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results

Creating an Export Template


❖ To create an export template

1. Open Acquisition of Isodat.

2. Click this button to create a new document.

3. In the File New dialog, select Data Export to create a new export
template. See Figure 7-54.

4. Click OK.

Figure 7-54. Creating an export template

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-47
Operation
Exporting Results

The Data Export dialog opens. See Figure 7-55.

Figure 7-55. Main filter page of data export

5. Select the check boxes for the data you want to include in the export
file:

For Acquisition Mode, as default both parameter types are selected.


If you select Dual Inlet or Continuous Flow, only those parameters
relevant for the selected acquisition mode are presented.

If you select Gas Configuration, select a gas configuration from the


drop-down list.

7-48 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results

If you select Included String, enter the string in the edit box and
click Apply. Only data including this string are shown in the
Available Columns list.

6. Select the check box Data Type and select the check boxes of the
data to include these for export.

With Disable All, all check boxes are deselected. With Enable All,
all check boxes are selected.

7. Drag and drop the columns to be shown in the export file from the
left pane “Available Columns” to the right pane “Columns to
export”. See Figure 7-56.

Figure 7-56. Defining columns for export

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-49
Operation
Exporting Results

A column is added to the Preview table for each identifier.

Tip Selectors are always combined by an AND relation. The


selection can be changed during template creation. The export
columns are not affected.

8. To add a customized column that contains no data, drag and drop


the Custom Identifier from the left pane to the right pane.

9. In the Insert Identifier dialog, enter a name for the column. See
Figure 7-57.

10. Click OK.

Figure 7-57. Confirm deletion of Identifier

The new column is added to the Preview table. This is useful, for
example, to later import data into this column.

11. To delete an entry in the right pane, right-click the entry and select
Delete Identifier from the context menu. See Figure 7-58.

Figure 7-58. Deleting an Identifier

12. Click Yes to confirm. See Figure 7-59.

Figure 7-59. Confirm deletion of Identifier

7-50 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results

13. Continue until all columns are defined.

14. Proceed with “To save an export template” on page 7-51.

❖ To save an export template

1. On the toolbar of the Acquisition, click this button.

The Save As dialog opens with the folder Export Templates


pre-selected. See Figure 7-60.

Figure 7-60. Saving an export template

2. In the field File name, enter a name for the export template.
3. Click Save.

The export template is saved with the file extension wke.

Applying an Export Template


Several samples can be bundled into a single export file.

❖ To apply an export template

1. Open Acquisition of Isodat.

2. Create a new sequence as described at “Creating a New Sequence


and Starting Acquisition” on page 7-9.

3. Click the Start button to start the sequence.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-51
Operation
Exporting Results

For Export, the Format is set to None if no file format has been
selected yet.

4. In the Export part of the Start Sequence dialog, click Modify


Template List. See Figure 7-61.

Figure 7-61. Modifying template list

A dialog opens. See Figure 7-62.

5. Click Add.

Figure 7-62. Add export template

6. In the Open dialog, select your export template (wke file).

7-52 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results

7. Click Open. See Figure 7-63.

Figure 7-63. Selecting export template

The selected export template appears in the list. See Figure 7-64.

Figure 7-64. Export Template listed

8. Click OK to confirm.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-53
Operation
Exporting Results

The Format is set to Excel (*.xls). See Figure 7-65.

Figure 7-65. Export Format is set to Excel

9. Confirm with OK.

The options specified in the sequence are set. Data acquisition starts.

Tip The export is performed during the measurement. This is


different from a Re-evaluation, where the export takes place after a
measurement.

7-54 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
8
Troubleshooting

This chapter describes diagnostic criteria for operating the Delta V


Series mass spectrometer.

Contents

• Checking Performance Data on page 8-2

• Absolute Sensitivity on page 8-3

• Abundance on page 8-5

• Amplifier Test on page 8-6

• Compression Factor on page 8-7

• Linearity on page 8-7

• Peak Flatness on page 8-8

• Relative Sensitivity on page 8-8

• Resolution on page 8-9

• Signal Stability on page 8-11

• System Stability on page 8-11

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-1
Troubleshooting
Checking Performance Data

Checking Performance Data


Thermo Fisher Scientific has developed several test routines to check the
performance of the Delta V Series mass spectrometers. These test
routines are included in the Diagnosis module of Isodat and are
described in the following sections. They require specific technical
knowledge of the instrument. Successful execution of some of the tests
depends upon the preconditions of the instrument.

When running the test routines, highly sensitive focusing of the Delta V
Series instruments yields the best specification results. For details on
focusing the ion source, see “Focus Settings of the IRMS” on page 6-66.

Reference gas for all performance data is CO2. Make sure you have
properly filled CO2 reservoirs attached to the inlet system before
starting the Diagnosis module.

Table 8-1 lists values of some of the Diagnosis parameters.


Table 8-1. Values of some Diagnosis parameters
Diagnosis parameters Delta V Advantage Delta V Plus
Absolute Sensitivity 1200 molecules/ion 800 molecules/ion
(sensitivity focusing) (sensitivity focusing)
1500 molecules/ion 1100 molecules/ion
(linearity focusing) (linearity focusing)
Amplifier Test 0.005 0.005
(for R = 3 × 108 ) (for R = 3 × 108 )
0.02 0.02
(for R = 1 × 109 ) (for R = 1 × 109 )
0.03 0.03
(for R = 3 × 1010 ) (for R = 3 × 1010 )
0.06 0.06
(for R = 1 × 1011 ) (for R = 1 × 1011 )
0.3 0.3
(for R = 1 × 1012 ) (for R = 1 × 1012 )
Linearity 0.066‰/V 0.066‰/V
(for CO2; 13C) (for CO2; 13C)

0.066 ‰/V 0.066 ‰/V


(for CO2; 18O) (for CO2; 18O)
Resolution 110 110

8-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Troubleshooting
Absolute Sensitivity

Table 8-1. Values of some Diagnosis parameters, continued


Diagnosis parameters Delta V Advantage Delta V Plus
-4
Signal Stability 3 × 10 3 × 10-4
(Dual Inlet (Dual Inlet
applications) applications)

3 × 10-3 3 × 10-3
(Continuous Flow (Continuous Flow
applications) applications)
System Stability 10 ppm 10 ppm

Table 8-2 lists some more important parameters.

Table 8-2. Values of other important parameters


Parameter Delta V Advantage Delta V Plus
End Vacuum 1 × 10-7 mbar 1 × 10-7 mbar
(without differential (without differential
pump) pump)

7 × 10-8 mbar 7 × 10-8 mbar


(with differential pump) (with differential pump)
Mass Range 1 to 80 Da 1 to 96 Da
H3 Factor 10 ppm/nA 10 ppm/nA
Stability of 0.03 ppm/nA/h 0.03 ppm/nA/h
H3 Factor

Absolute Sensitivity
Tip Testing Absolute Sensitivity requires a Dual Inlet system.

Absolute Sensitivity is defined as the number of molecules needed to


generate an ion which is then registered at the collector (for example,
one ion of m/z 44 at the corresponding collector cup).

Based on a defined volume, the ion current is determined during a


defined period of time as a function of sample consumption (sample
loss). The small defined volume is located between valve 25 of the inlet
system and the inlet capillary. It amounts to approximately 145 L.

Integrating the ion current over time yields the number of ions. From
the signal drop during measurement, the number of molecules necessary
to generate this ion amount is calculated. To obtain Absolute Sensitivity,
the number of molecules is divided by the number of ions.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-3
Troubleshooting
Absolute Sensitivity

Positively charged ions are produced in the ion source by electron


bombardment. This Electron Impact (EI) ionization is described by:

Ionization
- + -
AB + e  AB + 2e

Ionization and dissociation


- + -
AB + e  A + B + 2e

Definition of Absolute Sensitivity AS (in molecules/ion)

n gas
AS = ------------
-
n ion

where:

ngas Sample gas consumption


nion Number of detected ions

The number of consumed sample molecules ngas is calculated via the


ideal gas law:

p  v = n gas  R  T

where:

p Pressure difference
v Volume (here 250 L)
ngas Number of consumed sample molecules
R Universal gas constant
T Temperature

The amount of detected ions nion in the collector cup can be calculated
via the electrons needed to neutralize the positive ions:

t2
Q =  I dt
t1

where:

Q Charge
I Intensity
t Time

8-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Troubleshooting
Abundance

Principle of Testing Absolute Sensitivity


Measurement starts determining pressure and intensity. The volume is
reduced to the defined volume of 145 L that is enclosed between
valve 25, valve 26 and the capillary by closing valve 25 of the Dual Inlet
system. See highlighted area in Figure 8-1.

Figure 8-1. Defined volume enclosed between valves and capillary

The system is in a waiting position until start pressure and intensity are
reached. The ion current is measured for the preset time (500 s, for
example).

Tip Absolute Sensitivity should be about 1500 molecules CO2 per


mass 44 at the collector cup.

Abundance
Tip Testing Abundance requires a Dual Inlet system.

Abundance describes the contribution of a mass to a neighboring mass


(the amount of ions for m/z 44 falling into the m/z 45 cup, for example).
The intensity of a mass (m/z 44, for example) is compared to the
intensity of the neighboring peak (m/z 45, for example).

In case of CO2, the amount of ion current of mass 44 falling into the
m/z 45 cup is divided by the ion current of m/z 44 falling into the
m/z 44 cup.

Measured as ratio of two ion currents, Abundance is dimensionless and


quoted in % or ppm. It should not exceed 2 × 10-6 for a Delta V
Advantage instrument with a Dual Inlet system. The Abundance test is
performed with CO2, and the device must be calibrated. A peak center
is performed on the narrow cup 3 (middle cup of Universal Triple
collector) before measurement starts.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-5
Troubleshooting
Amplifier Test

Principle of Testing Abundance


Signal height (intensity) on m/z 44 is determined in the appropriate
collector cup (cup 3, for example). The background signal on m/z 45 is
measured (electronic noise with no gas) from m/z 44 to m/z 45.5.

With CO2 as sample gas, high voltage (HV) is scanned from m/z 44 to
m/z 45.5, and the intensities are measured on the neighboring cup of
m/z 45 (cup 4, for example), with bigger resistor value to keep the signal
in the detection range.

The Abundance of m/z 44 onto m/z 45 from the signal to the left and to
the right of the m/z 45 peak is extrapolated.

Sources of Error
• Resistor values are not configured properly.

• Due to electrons on the left and on the right side of the peak, a
negative signal may result. This problem can be overcome by
manual adjustment.

Amplifier Test
The Amplifier Test checks the ion detection performance of the IRMS
with no ions present. It informs about the background noise of
electronic devices.

As the amplifier baseline must be determined without an interfering


signal, the ion source is switched off (the ion current is zero) before
measurement starts. The signal intensity of every cup is individually
measured at least 200 times for 300 seconds of integration time. Finally,
mean and standard deviation are calculated.

8-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Troubleshooting
Compression Factor

Compression Factor
Tip Testing Compression Factor requires a Dual Inlet system.

The Compression Factor is only important in case of a Dual Inlet


system as it measures bellows compression. This intensity ratio is
dimensionless [mV/mV]:

Int end
Comp = ---------------
-
Int start

where:

Intend Intensity at the end of measurement


Intstart Intensity at the start of measurement

The Compression Factor determines the dynamic range of the two


bellows informing about their tightness and linearity. The ion signal
intensity is measured at different bellows compressions: an intensity vs.
volume diagram results. The standard deviation around the mean of the
signal is calculated.

NOTICE The bellows must be calibrated before performing the test.

To test this parameter, the peak intensity for a mass (m/z 44, for
example) is measured starting at the maximum (100%) down to the
minimum (0%). A minimum death volume of about 3 mL is still
remaining at 0% volume. A certain level (200 mV, for example) serves as
starting point of the measurement. The signal for the bellow expanded
to maximum should be at this level. If not, the inlet system is expanded
and pumped automatically until the reference level is reached.

Tip The Compression Factors should be about the same for both
bellows: at least 1:10 or higher.

Linearity
With the Linearity test, synonymously called Ratio Linearity, signal
linearity is checked vs. beam intensity (intensity of main ion current)
over a range of varying signals. Signal intensity is measured, and the
isotope ratios are displayed vs. beam intensity. Linearity is calculated as
slope of the regression line [‰/V]. The ratios are monitored between
2 V and 8 V in 1 V steps. For each data point, the background is
subtracted.

Source of Error
• Resistor values are not configured properly.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-7
Troubleshooting
Peak Flatness

Peak Flatness
As slope of the peak plateau, Peak Flatness reflects the quality of the ion
stream. A correction is necessary to eliminate effects of descending peak
plateau with increasing high voltage. This is done by measuring the peak
twice, first with increasing and then with decreasing high voltage. The
resulting peak represents the mean values of both runs.

The measured intensity is a function of the acceleration voltage (ion


energy). During a high voltage scan, the intensity is slightly affected by
this effect. To overcome this, an “energy correction” is performed. The
ion intensity at the top of the peak is measured. Peak Flatness can be
determined for different gases and different collector cups (for example,
for a CO2 peak at m/z 45 at cup 2).

Two results are obtained:

• Maximum intensity deviation divided by the intensity

• Slope of the regression line [1/Da]

Relative Sensitivity
Relative Sensitivity Srel describes the dependency of signal intensity or
ion current on the ion source pressure. It is given in A/mbar:

1 1 U
S rel = ----------  ------  ----
0.69 p R

where:

U Voltage measured at the amplifier of the collector cup (Cup 3,


mass 44, for example)

R Resistor value (3 × 108  for mass 44, for example).


This value is the same for N2 and CO2 as reference gases. It needs to be
changed in special cases only.

D p Pressure difference between a measurement with and without


reference gas.

0.69 Correction factor for CO2.

The ion gauge is calibrated with N2, however, which has a different
ionization probability. The correction factor takes this into account. To
calculate it, intensities (ion currents) and pressures are measured with
and without reference gas.

8-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Troubleshooting
Resolution

Tip Two different Relative Sensitivity values exist depending on


whether the instrument is equipped with a differential pumping
system or not. The difference is due to different pressure readings at
the same flow. The Absolute Sensitivity (given in molecules/ion)
however, is the same.

After a cycle of, for example, three measurements and calculations of


Relative Sensitivity, a mean value is displayed. This value should be
about 0.2 A/mbar for a standard system and about 0.5 A/mbar for a
differentially pumped system. It depends on the pumping capacity of
the turbomolecular pumps. Each cup (each mass) has a Relative
Sensitivity value of its own.

Different values of Relative Sensitivity can only be compared, if


pumping speed, conductance, location of the ion gauge etc. are
identical. Therefore, it is senseless to compare different types of
instruments.

Sources of Error
• Resistor values are not configured properly.

• Relative Sensitivity depends on the accuracy of the high vacuum


pressure gauge, which is limited.

Resolution
Resolution describes the masses that can be separated from each other,
or the minimal relative distance between two masses that can be
resolved. In mass spectrometry, different definitions of resolution are
used.

The 10% valley definition is commonly used for double focusing sector
field mass spectrometers. See Figure 8-2.

R = m/m

100%

or

10%
5%
m m
m m

Figure 8-2. 10% valley definition of Resolution

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-9
Troubleshooting
Resolution

Resolution can be defined as:

• Mass divided by the mass difference of two neighboring peaks, if the


valley between peaks drops to 10% of the peak height.

or as:

• Mass divided by the peak width (in Da) at 5% of peak height.

According to the 10% valley definition, the value is dimensionless:

m
R = --------
m

where:

R Resolution
m Mass of the respective isotope
m Mass difference between neighboring peaks

In Dual Peak mode, the distance between peak centers of two


neighboring peaks is measured [Da]. The peak width of one peak is
measured at 5% peak height.

In Single Peak mode, the distance between neighboring peaks is set to


1 Da. In both modes, Resolution R can be calculated as follows (the
mass difference is usually 1 Da):

m a
R = --------  --
m b

where:

a Distance between peak centers


b Peak width of the isotope of interest

When determining Resolution, choose intensity focusing. See “Focus


Settings of the IRMS” on page 6-66. Use the narrowest cup available,
usually cup 3, m/z 45 in the middle of the Universal Triple collector.

Example
For a resolution of 88 and m/z 44, a peak with a distance of
(44/88) Da = 0.5 Da could be resolved using the 10% criterion.

Start mass and end mass of the magnetic field scan can be edited. In case
of CO2, the mass ranges from about 43 to 45.5. The magnet steps values
referring to m/z 44 and m/z 45 are determined, and Resolution is
calculated.

8-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Troubleshooting
Signal Stability

Signal Stability
Signal Stability describes intensity peak height stability. Intensity on top
of the peak is measured for a limited period of time (5 minutes, for
example). Notice the similarity to System Stability, but here, the stability
is not measured at the peak flank, but at the peak center. Signal Stability
should be ~2 × 10-4 for 5 minutes.

Two results are obtained:

• Slope of the regression line (normalized by the intensity).

• Standard deviation of the regression line (normalized by the


intensity).

Tip Testing Signal Stability requires a signal of 3 V or more.

Sources of Error
• The slope is usually due to gas consumption during measurement.
However, it should be checked, if an unusual result is obtained.

• Instabilities of the emission may cause an unstable signal although a


stable high voltage and magnetic field are given.

• Pressure fluctuations (check oil of the fore vacuum pumps) or


temperature fluctuations, particularly at the crimps.

System Stability
System Stability describes high voltage stability and thus magnetic field
stability. Already small variations of high voltage or magnetic field
dramatically influence signal intensity: they cause peak shifts. The
fluctuations of high voltage or the magnetic field strength are measured
at the peak flank, because they exert a much higher impact on peak
intensity at the flank than on top. The System Stability test comprises
the following steps:

• Peak center and peak flanks are determined.

• Magnetic field is set to 50% of peak height (at peak flank).

• Signal intensity (high voltage fluctuation) at the peak flank is


measured for a defined period of time (15 minutes, for example).

• A new peak center takes place.

• Calculation of System Stability [min-1] and Relative Mass Drift


[min-1] (either electronic or to magnetic drift) using the slope of the
peak flank.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-11
Troubleshooting
System Stability

Tip Testing System Stability requires a signal of 3 V or more.

Two results are obtained:

• Slope of relative mass drift vs. time (time drift)

• Standard deviation of this slope (scatter of the mass)

A value of 5 × 10-4 measured over a period of 15 minutes reflects good


System Stability.

8-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
9
Maintenance

This chapter describes maintenance procedures the user must perform


to ensure optimum performance of the Delta V Series mass
spectrometer.

Contents

• Safety Guidelines for Maintenance on page 9-2

• General Advice for Maintenance on page 9-3

• Inspection- and Servicing Plan on page 9-4

• Basic Rules for Cleaning on page 9-6

• Baking the System on page 9-7

• Ion Source on page 9-8

• Vacuum Pumps on page 9-19

• Vacuum System on page 9-20

• Pressure Reducer for Compressed Air on page 9-23

• Dual Inlet System on page 9-24

• Replacing a Pneumatic Valve on page 9-25

• Autocool Refill Device on page 9-33

• Needle Valves on page 9-35

• Stainless Steel Capillaries and Fused Silica Capillaries on page 9-39

• Nickel Capillaries on page 9-47

• Penning Gauge on page 9-50

• Amplifier Area and Three-Way Valve on page 9-55

• Thermo Fisher Scientific Service on page 9-58

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-1
Maintenance
Safety Guidelines for Maintenance

Safety Guidelines for Maintenance


When performing maintenance on the Delta V Series system, pay
attention to the following general safety guidelines.

Because the Delta V Series instrument contains elaborate and


expensive components, only qualified and skilled personnel should
perform servicing. If there are any uncertainties or if difficulties arise,
contact your Thermo Scientific service. Thermo Fisher Scientific
further recommends using original Thermo Scientific spare parts only.
Notice that many adjustments can be carried out only with special
tools and instruments, which are not supplied with the system. See the
references within this manual.

Before starting maintenance and repair, read the appropriate chapters


of this manual. Before calling your Thermo Scientific service, try to
localize the defect. A precise description of the defect eases repair and
reduces costs.

WARNING High Voltage. Risk of injury. Some parts of the Delta V Series
instrument are at high voltage. Opening the electronics cabinet is only
allowed for maintenance purposes by qualified service personnel.

WARNING Explosive Gas. Risk of injury. Ethanol vapors are explosive. Do not
smoke or handle with open fire. During leak detection, ventilate the
laboratory carefully.

CAUTION Hot Surface. Risk of burns. Temperatures of about 75 °C or higher


may be reached at the metallic surface of valves that are baked out. Do
not touch any surface of a valve you are baking out.

WARNING Electric Current. Risk of electric shock. Do not remove the cover
before or during operation or when performing minor servicing, for
example, at the ion source. Voltages of at least 220 V are prevalent
inside.

WARNING Noxious Material. Risk to health. Hazardous compounds introduced


into the system may be dissolved in the pump oil. Use only
locally-approved containers and procedures for waste oil disposal.
Notice that contaminated pumps must be emptied and
decontaminated before they are sent back to Thermo Fisher Scientific
for repair or exchange.

CAUTION Cold Liquid. Risk of frostbite. The Autocool Refill device contains
extremely cold liquid gas. Careless handling might cause severe
personal injury including frostbite. Only use liquid nitrogen as cooling
agent.

9-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
General Advice for Maintenance

General Advice for Maintenance


When performing maintenance on the Delta V mass spectrometer,
observe the following advice:

• Accurate results can be obtained only, if the system is in good


condition and properly calibrated.

• Preventive maintenance must begin with installation and must


continue during the warranty period to maintain the warranty.
Thermo Fisher Scientific offers maintenance and service contracts.
Contact your local Thermo Fisher Scientific representative for more
information. Routine and infrequent maintenance procedures are
listed in Table 9-1.

• The user maintenance procedures described in this chapter do not


require removing the instrument housing. Thermo Fisher Scientific
assumes no responsibility and will not be liable for instrument
damage and/or operator injury that might result from using the
instrument without the housing attached. Therefore, a Thermo
Fisher Scientific field service engineer must be called, if removal of
the instrument housing is required.

• To successfully carry out the procedures described in this chapter,


observe the following rules:
- Proceed methodically
- Always wear clean, talc-free, and lint-free gloves when handling
the components of the ion optics, mass analyzer, and ion
detection system. See “Personal Protective Equipment” on
page 5-13 for a specification of the required gloves.
- Always place the components on a clean, lint-free surface.
- Do not overtighten a screw or use excessive force.
- Dirty tools contaminate your system. Keep the tools clean and
use them exclusively for maintenance and service work at the
mass spectrometer.
- Do not insert a test probe (for example, an oscilloscope probe)
into the sockets of female cable connectors on PCBs.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-3
Maintenance
Inspection- and Servicing Plan

Inspection- and Servicing Plan


Table 9-1 lists routine and infrequent maintenance procedures to be
performed by the user.

Table 9-1. Maintenance procedures


MS Component Procedure Frequency Page
Instrument Baking As required page 9-7
Check the instrument for leaks After baking, and as page 9-21
required
Ion Source Dismount the ion source As required page 9-9
Reinsert the ion source As required page 9-12
Replace the cathode unit As required page 9-14
Clean the ion source When the values of the page 9-16
diagnostic criteria
described in Chapter 8,
“Troubleshooting.” can
no longer be obtained.
Replace the ion source heaters As required page 9-17
Check the ion source As required page 9-18
Vacuum Pumps Check the oil level Quarterly page 9-19
Exchange the oil Every four years, refer to page 9-20
oil color chart
Vacuum System Perform leak detection at the mass As required page 9-21
spectrometer
Perform leak detection at the fore vacuum As required page 9-21
section
Clean the vacuum components As required page 9-22
Pressure Reducer Check the oil reservoir Yearly page 9-23
Empty the oil reservoir As required page 9-23
Adjust the pressure value Yearly page 9-23
Remove the tubing As required page 9-23
Insert the tubing As required page 9-23
Dual Inlet Adjust the crimps As required page 9-24
Insert the pneumatic valve As required page 9-28

9-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Inspection- and Servicing Plan

Table 9-1. Maintenance procedures, continued


MS Component Procedure Frequency Page
Autocool Refill device Check the Autocool Refill device As required page 9-33
Check the evaporation rate As required page 9-33
Check the Dewar vessel As required page 9-34
Enable automated and As required page 9-35
computer-controlled refill operation
Fill the Dewar vessel Before starting page 9-35
measurement, and as
required
Microvolume Adjust the capillaries As required page 9-46
Needle Valve Remove the heater (for maintenance As required page 9-36
operation)
Connect new peripheral As required page 9-38
Bake out the needle valve When a new peripheral page 9-39
has been connected
Stainless steel capillaries Remove the blind (to access capillaries) As required page 9-40
Bake out the capillaries As required page 9-42
Replace the capillaries As required page 9-45
Adjust the capillaries As required page 9-46
Nickel capillaries Cut the capillaries As required page 9-48
Bake out the capillaries As required page 9-48
Install the capillaries As required page 9-48
Crimp the capillaries As required page 9-49
Penning gauge Put the Penning gauge back to operation As required page 9-50
(rough-and-ready)
Disconnect and clean the Penning gauge As required page 9-51
Adjust the set point of the Penning gauge As required page 9-53
Amplifier area and Vent the amplifier housing As required page 9-57
three-way valve
Evacuate amplifier housing with evacuated As required page 9-57
analyzer
Evacuate amplifier housing with vented As required page 9-57
analyzer

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-5
Maintenance
Basic Rules for Cleaning

Basic Rules for Cleaning


Tip Do not economize with the cleaning agent. Renew the cleaning
bath frequently.

❖ To check highly volatile cleaning agents (for example, cyclohexane,


acetone)

1. Dip a polished metal plate into the bath and take it out again so that
as much liquid as possible remains behind on the plate.

2. Preferably, bend the plate to a concave shape.

3. Allow the bath liquid to evaporate.

No residuals should be left on the plate. Otherwise, change the bath


liquid.

❖ To clean parts

NOTICE Use slightly contaminated bath liquids for preliminarily washing


severely contaminated parts. Do not rinse with water if using volatile
cleaning agents. Rinse with a lot of water if using cleaning agents in
aqueous solution. Use warm water, finally rinse with distilled or
deionized water.

1. Dry the parts which have been rinsed in water well in a dust free
area, preferably in a vacuum drying oven.

In the case of drying ovens with forced air circulation, the air must
be free of dust.

If necessary, wrap the parts loosely in tissue paper and place them in
the oven.

As contaminations on ceramic parts consist of physically adsorbed


metal layers, they cannot be removed with volatile cleaning agents.

2. Using an ultrasonic bath increases the probability of a successful


removal of contaminations. Successful removal of contaminations
from ceramic parts may not always be possible. In this case, replace
these parts.

3. If new parts are not available, remove strongly adhering layers by


filing down with a diamond file. After filing, wash the parts. The
diamond file can easily be cleaned using an erasing rubber.

4. If new parts are not available, remove strongly adhering layers by


annealing at red heat in a propane-oxygen flame. Too high
temperature may cause distortion of ceramic parts. Therefore, avoid
the white heat range.

9-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Baking the System

NOTICE Do not wash any parts after they have been annealed. Ceramic
parts that cannot be disconnected from metal parts must not be
annealed.

5. When re-assembling, do not touch the washed parts with naked


hands. Use non-fibrous gloves and clean tools.

6. In case of difficult assembly jobs, it may be necessary to work


without gloves. Then thoroughly wash your hands and remove any
fat or grease from your fingertips with a solvent. The parts should
then be touched only with degreased fingertips.

7. To avoid any damage to the skin, rub your fingertips over with a
fatty skin cream when the work is completed.

Baking the System


It may be necessary to bake the following parts of the system: ion source,
analyzer block, needle valve, and valve blocks of the optional Dual Inlet
system.

If the system has been vented (after exchanging parts, for example),
baking removes traces of intruded moisture and water.

If the system has been contaminated, the contaminations may lead to


disturbing interferences. Baking removes contaminating compounds.

If sulfur measurements have been performed, they may lead to


interferences with CO2. Baking removes sulfur-containing compounds.

❖ To bake the system

1. In the Acquisition or Instrument Control of Isodat, open the MS


State panel.

2. In the MS State panel, click the respective button to turn on the


individual heater. See Figure 9-1.

Figure 9-1. Controlling activated sockets in Isodat

A green button indicates that the heater is on. A gray button


indicates that the heater is off. For details, see “Source Heater” on
page 6-28.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-7
Maintenance
Ion Source

3. Remove the door on the lower right front of your Delta V Series
instrument to get access to the sockets of the heaters. See also
“Microvolume Cabinet” on page 3-29.

4. Make sure that the cables of the heaters are properly connected to
their respective socket blocks.

5. Keep pumping all the instrument sections as long as you are baking.

6. Leave the heaters on for about 10-12 hours (over night, for
example). In case of the Inlet Valve Heater, a shorter heating time as
well as less frequent heating may be sufficient.

Ion Source
When the front panel is opened, the ion source is turned off
automatically for safety reasons, and the corresponding LED at the
control panel stays off. Conversely, you cannot turn on the ion source,
if the door is not properly closed.

Maintenance operations at the ion source are frequently necessary.


Figure 9-2 shows an explosion drawing of the ion source.

Figure 9-2. Explosion drawing of ion source

9-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source

Accessing the Ion Source


The ion source is quickly and easily accessible. Before starting any
maintenance operation, it can be dismantled as a whole together with
the ion source connector board still attached to it. Only three
connectors must be unplugged.

The entire unit together with the ion source connector board can then
be positioned upright on a work bench for maintenance. This procedure
prevents mistakes (related to wiring, for example). After maintenance,
the ion source can be reinserted as a whole.

Dismounting the Ion Source


Dismounting the ion source is necessary to exchange the cathode or
heaters, and to clean ion source parts.

Figure 9-3 shows the connections of the ion source to the ion source
connector board.

2
1

8
5

7 6

Labeled Components: 1=connector for ion source heater, 2=metallic claw


(4 ×), 3=connector for low-lying ion source potentials (ground
potential < V < 500 V), 4=spacer (4 ×), 5=resistors on ion source connector
board, 6=ion source connector cable, 7=connector for high-lying ion source
potentials (V  3 kV), 8=connectors to ion source connector board (13-fold
feedthrough)
Figure 9-3. Ion source and ion source connector board

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-9
Maintenance
Ion Source

The connector for the ion source heater (1 in Figure 9-3) is coming from
the 12 V power supply. Four metallic claws 2 fasten the flange to the
housing. The connector for low-laying ion source potentials 3 is fed
from the ion source connector cable 6.

The spacers 4 allow for placing the ion source upright on a work bench
for maintenance operations. The resistors on the ion source connector
board 5 damp possible flashovers within the ion source. Only very small
currents flow towards the ion source connector board. Possible damage
is minimized.

When dismounting or inserting the ion source, it is not necessary to


loosen or disconnect the 13 connectors (see 8): rather, the ion source can
be dismounted as a whole together with the ion source connector board
attached to it.

NOTICE To avoid damaging the aluminum-made parts, do not use any


mechanical tool to force the opening of flanges. Instead, after first
venting correctly and then loosening the screws, any flange can be
easily removed manually.

❖ To dismount the ion source

1. Switch off the ion source.

2. If available, close the Changeover valve of the Dual Inlet system.

Afterwards, the Dual Inlet system can be operated while the rest of
the instrument is being vented. This is advantageous for filament
exchange, for example.

3. Switch off the pump system of the main instrument.

The turbomolecular pump of the Dual Inlet system can be left on.

4. Vent the analyzer. See “Venting the Amplifier Housing” on


page 9-57.

5. Pull out the three green connectors 1, 3, and 7 in Figure 9-3.

6. Loosen all four claws (see 2 in Figure 9-3) using a screw wrench.

Tip Before handling the ion source, see Figure 9-5 for its
important mechanical parts.

7. Carefully pull out the ion source.

9-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source

8. Arrange the ion source on the spacers (5 in Figure 9-4) to place it on


your work bench. See Figure 9-4.

1
6

Labeled Components: 1=guide ring, 2=gas inlet into ion source, 3=supporting
surface for ion source, 4=halogen lamp as ion source heater (2 ×), 5=spacer
(4 ×), 6=slit for guide pin of ion source
Figure 9-4. Dismounted ion source placed on workbench

9. If you plan to remove the ion source for a longer period of time (for
cleaning, for example), close the opening of the analyzer head by
suitable means. This prevents foreign particles from entering the ion
source.

10. Perform the intended maintenance of the ion source.

11. To reinsert the ion source, see “Reinserting the Ion Source” on
page 9-12

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-11
Maintenance
Ion Source

Reinserting the Ion Source


Figure 9-5 shows important mechanical parts of the ion source.

3
1

Labeled Components: 1=ceramic pin (4 ×), 2=metallic bolt (2 ×), 3=spring (4 ×)


Figure 9-5. Mechanical parts of ion source

Like the four springs (3 in Figure 9-5), also the metallic bolts 2 which
are inserted perpendicularly between the ceramic pins 1, ensure
mechanical stability.

9-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source

Figure 9-6 shows the empty ion source housing.

Labeled Components: 1=gas inlet, 2=aperture, 3=aperture sheet, 4=guide pin


of ion source, 5=thread for metallic claw
Figure 9-6. Empty ion source housing

For details on the apertures of the Delta V Series instruments, see


Figure 3-40 and Figure 3-41.

NOTICE In seldom cases, the guide pin may be canted within the ion source or
may fall out completely. When reinserting the ion source, make sure
that the guide pin is still present and not canted. The ion source must
be easily movable and not get stuck during reinsertion.

❖ To reinsert the ion source

1. Carefully inspect the edge sealing for absence of scratches and lint.

2. Place the Viton™ O-ring upon the flange of the analyzer head.

3. Insert the ion source into the analyzer head.

When inserted, ion source flange and making flange should be


aligned in parallel.

NOTICE Due to the elastic Viton O-ring, it is sufficient to fasten the four
metallic claws hand-tight. Screwing them on too tight might
damage the aluminum-made analyzer block.

4. Carefully press the ion source in the direction of the analyzer.


Tighten the four metallic claws (2 in Figure 9-3) hand-tight.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-13
Maintenance
Ion Source

5. Check for short circuits.

6. Re-adjust the ion source potentials if necessary (for example, after


exchanging the cathode unit and/or dismantling the ion source).

7. Plug in the three green connectors (1, 3, and 7 in Figure 9-3).

8. Perform the ion source check. See “Checking the Ion Source” on
page 9-18.

Replacing the Cathode Unit


If a filament (cathode) has burnt through, it must be replaced. This is
probably the most often occurring maintenance operation of the ion
source. Buy new filaments at Thermo Fisher Scientific.

Tip Always stock a filament as this restricts dead times. Thermo Fisher
Scientific recommends replacing a filament twice a year. Use lint-free
gloves and clean tools.

❖ To replace the cathode unit

1. Dismantle the ion source as described at “Dismounting the Ion


Source” on page 9-9.

2. Place the ion source upright onto a work bench.

3. Unscrew the mechanical connections (1 and 6 in Figure 9-7).


4. Unscrew the supply connections 3 and 4.

5. Disconnect the supply lines 2 and 5.

6. Carefully pull out the filament.

9-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source

6
1

Labeled Components: 1=mechanical connection, 2=supply line, 3=supply


connection, 4=supply connection, 5=supply line, 6=mechanical connection
Figure 9-7. Ion source showing cathode unit

7. Carefully insert the new filament carrier along the guide tracks for
up/down. See arrows in Figure 9-8.

Figure 9-8. Inserting filament carrier along guide tracks

8. Align the filament carrier along the guide tracks for left/right. See
arrows in Figure 9-9.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-15
Maintenance
Ion Source

This ensures that the filament fits correctly.

Figure 9-9. Proper adjustment of filament

9. Fasten the screws of the supply connections 3 and 4.


10. Reconnect the supply lines 2 and 5.

11. Reinsert the ion source as described at “Reinserting the Ion Source”
on page 9-12.

Cleaning the Parts of the Ion Source


Because the ion source and/or its parts gets dirty by and by, it must be
cleaned from time to time. Either send the ion source to Thermo Fisher
Scientific or clean it as described below.

❖ To clean metallic and/or ceramic parts

1. Carefully dismount the ion source as described at “Dismounting the


Ion Source” on page 9-9.

2. Carefully disassemble the ion source into its components.

3. Grind all contaminated and discolored metal parts with aluminum


oxide powder (600 grain) or use a soft emery paper with a 600 grain.

This mechanical cleaning must be followed by a chemical cleaning:

9-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source

4. Clean all parts made of stainless steel in a detergent solution at


60 °C for about 1 or 2 hours.

5. Clean all parts in a bath. An ultrasonic bath improves and


accelerates the cleaning procedure.

NOTICE Do not use an ultrasonic bath when cleaning the ion source
magnet.

6. Rinse the metallic parts with deionized water.

7. Remove the residues of water with pure ethanol or acetone.

8. To eliminate solvent residuals, dry the parts using a fan or a drying


oven.

Replacing the Ion Source Heaters


Thermo Fisher Scientific recommends using Osram Starlite halogen
lamps (No. 64432 S of 35 W, 12 V and GY 6.35) which are of high
quality and durability. See product catalog at www.osram.com.

It may be advantageous to replace the ion source heaters as well when


the filament is being replaced. Two commercial halogen lamps of 12 V
serve as ion source heaters. See 4 in Figure 9-4.

The halogen lamps are provided with energy by the 12 V power supply
(see 2 in Figure 3-27) and are run with undervoltage so that their
lifetime is drastically increased.

Tip The halogen lamps may not imply an infrared protection, as those
mainly would emit visible light and their heating power would be
decreased. Halogen lamps without an infrared protection emit more
infrared radiation and are therefore better suited as heaters.

❖ To replace the halogen lamps (ion source heaters)

1. Dismount the ion source as described at “Dismounting the Ion


Source” on page 9-9.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-17
Maintenance
Ion Source

2. Carefully pull the halogen lamps (1 and 2 in Figure 9-10) with pliers
or use a cloth or gloves.

Labeled Components: 1,2=halogen lamp


Figure 9-10. Halogen lamps of ion source

3. Insert the new halogen lamps.

Tip If the halogen lamps are loosely fitted, carefully press their
spring contacts together using small pliers.

4. Reinsert the ion source as described at “Reinserting the Ion Source”


on page 9-12.

Checking the Ion Source


Carefully check the position of the connection wires. The wires must
neither contact each other, neither the ionization housing, nor the ion
source plates.

❖ To check the ion source

1. Check the filament of the cathode unit.

2. Check the edge sealing surfaces of the ion source flange for radial
scratches before inserting the ion source into the analyzer head.

3. Make sure all contacts of the 13-fold feedthrough to the ion source
control board (see 8 in Figure 9-3) are connected.

9-18 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Vacuum Pumps

Vacuum Pumps
The Delta V Series instrument is equipped either with or without a
differential pumping system. The high vacuum status of the pumping
system is monitored by a Penning gauge attached to the left side of the
ion source housing. The fore vacuum is controlled by a Pirani gauge
located at the Dual Inlet system.

The Delta V Series instrument is equipped with the following analyzer


pumps manufactured by Pfeiffer:

• A fore vacuum pump (rotary vane pump DUO 2.5).

• A turbomolecular main pump HiPace™ 300

• An optional differential pump HiPace™ 80.

For details about handling and maintenance, refer to the Operating


Manual of the pump supplier.

Furthermore for a Dual Inlet system, the following pumps


manufactured by Pfeiffer may be in use:

• Fore vacuum pump of the Dual Inlet system (rotary vane pump
DUO 2.5)

• Turbomolecular pump of the Dual Inlet system (HiPace 80)

The turbomolecular pumps are accessible from the left side, and the fore
vacuum pumps from the right side.

For all maintenance operations, refer to the Operating Manual of the


manufacturer and to www.pfeiffer-vacuum.com.

Tip Replace pump oil of turbomolecular pumps and of fore vacuum


pumps every four years. Because the Delta V Series instrument must
be vented before, Thermo Fisher Scientific recommends performing
the replacement as part of an overall check of all pumps.

Checking Oil Levels

NOTICE The oil levels must not drop below a certain level. On the other hand,
do not fill in more oil than is indicated by the calibration mark.

❖ To check oil levels

1. Quarterly check the oil levels in the inspection glasses of both fore
vacuum pumps.

2. If the oil levels are too low, fill in a sufficient amount, but not too
much new oil.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-19
Maintenance
Vacuum System

Filling in new oil (in case of too low oil levels) is even possible while
the pumps are running. It is not necessary to vent the fore vacuum
pumps.

Replacing Oil
For details about oil replacement of a turbomolecular pump of the
analyzer, refer to the manual of the manufacturer. Even the
turbomolecular pump of the Dual Inlet system has been mounted in a
way that eases direct access to it (for oil level control, oil exchange or
other maintenance operations, for example).

WARNING Noxious Material. Risk to health. Hazardous compounds introduced


into the system may be dissolved in the pump oil. Use only locally
approved containers and procedures for waste oil disposal. Notice that
contaminated pumps must be emptied and decontaminated before
they are sent back to Thermo Fisher Scientific for repair or exchange.

❖ To replace oil

1. Before you empty and replace old oil, vent the fore vacuum pumps.

2. To vent the instrument as seldom as possible, empty and replace the


oil of both the fore vacuum pumps and the turbomolecular pumps
simultaneously within one session once a year.

Vacuum System
The main reasons for problems with the vacuum system are leaks and
contaminations.

NOTICE Be careful when servicing the vacuum system. Abrupt opening to


atmospheric pressure might damage filaments, multipliers, heaters,
slits and other sensitive parts.

Detecting Leaks
Leak detection is rather time-consuming. Carefully check all flange
connections and assemble them properly during service. Additionally,
monitor the pressure during the cooling period after baking. If
necessary, re-tighten the flanges.

Leaks may be caused:

• If flange connections and/or sealings are improperly treated during


service operations.

• Accidentally during cooling periods after baking.

9-20 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Vacuum System

• If heavily treated sealing components are worn out.

Thermo Fisher Scientific recommends two different methods for leak


detection:

• Mass spectrometric leak detection

This method can be applied if the leak permits IRMS operation


(p ~6 × 10-4 mbar).

• Leak detection in the fore vacuum section (if the pressure is too
high for IRMS operation).

❖ To perform mass spectrometric leak detection

1. Use a container with a suitable test gas (argon, for example).

2. Connect the reducing valve to a PVC tube and the open end of the
tube to a fine capillary (glass or metal tubing, for example).

3. Using a sensitive cup, set the IRMS to the argon peak of m/z 40, and
blow a fine argon beam onto the parts where leaks are suspected.

❖ To perform leak detection in the fore vacuum section

WARNING Explosive Gas. Risk of injury. Ethanol vapors are explosive. Do not
smoke or handle with open fire. During leak detection ventilate the
laboratory carefully.

1. Use a small washing bottle with ethanol and spray a fine ethanol
beam onto the connections where a leak is suspected.

2. When hitting the leak, after a short delay, the pressure first decreases
and afterwards increases rapidly. Use the Penning gauge for pressure
reading.

Contaminations
Contaminations may be caused by:

• Water vapor stemming from the sample preparation devices

• Using improper elastomer gaskets, especially at elevated


temperatures. Thermo Fisher Scientific recommends ordering spare
gaskets from Thermo Scientific only.

• Introducing solvents that are not removed carefully after cleaning.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-21
Maintenance
Vacuum System

Check the final pressure daily. About 24 hours after start, without
sample inflow, the pressure should be in the 10-8 mbar range.

NOTICE Do not use silicon greases or silicon oils. Silicon layers lead to surface
charges and are difficult to eliminate.

Viton Gaskets
The Viton™ of the Viton gasket must be of good and preheated quality.
Thermo Fisher Scientific recommends ordering spare gaskets from
Thermo Scientific only.

Before inserting the gasket, ensure that sealing surfaces and gasket are
clean and that the gasket surfaces are not damaged. For cleaning, wipe
the gasket using clean paper.

NOTICE Do not use vacuum grease. Do not clean Viton gaskets with solvents.
Viton must not be operated at temperatures above 150 °C.

Cleaning Vacuum Components


For general remarks, see “Basic Rules for Cleaning” on page 9-6.
Cleaning the parts of the ion source is described at “Cleaning the Parts
of the Ion Source” on page 9-16.

For cleaning parts of the fore vacuum region, Thermo Fisher Scientific
recommends using cyclohexane as solvent. The best cleaning is obtained
with a hot ultrasonic bath. Observe the following recommendations.

❖ To clean parts of the fore vacuum region

1. Use pure solvents only.

2. When cleaning with solvents, use a hood.

3. Pay attention to the safety regulations of your country.

4. After cleaning, carefully dry the parts.

5. Do not touch the cleaned parts with your fingers. Use lint-free
gloves.

9-22 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Pressure Reducer for Compressed Air

Pressure Reducer for Compressed Air


Compressed air may contain oil that is collected in a reservoir.

❖ To check and empty the oil reservoir of the pressure reducer for
compressed air

1. Open the door at the right side of the Delta V Series instrument to
access the pressure reducer for compressed air.

2. Visually check the oil level in the reservoir. See 3 in Figure 3-18.

3. Turn the blow-off valve (4 in Figure 3-18) to the right to drain the
condensate from the reservoir (3 in Figure 3-18).

4. Clean the filter, if required.

Tip Check the oil level of the reservoir once a year.

❖ To adjust the pressure reducer to a particular pressure value

1. Open the door at the right side of the Delta V Series instrument to
access to the pressure reducer for compressed air.

2. Pull the adjusting knob (1 in Figure 3-18) upwards to unlock it.

3. Turn the adjusting knob until the desired pressure value is shown at
the pressure display (2 in Figure 3-18). Usually, the pressure reducer
has been adjusted to 5 bar (500 kPa; 73 psi) as default factory
setting.

4. Push the adjusting knob down to lock the pressure reducer at this
particular pressure value.

Tip Thermo Fisher Scientific provides the pressure reducer in the


locked state.

❖ To remove tubings from tubing connections

1. Switch off compressed air.

2. Push the gray plastic ring (for example, 3 in Figure 4-7) towards the
brass part of the compressed air distributor using an open-ended
spanner. At the same time, pull the tubing out. The manufacturer
SMC provides a tool to do this.

❖ To insert tubings into tubing connections

1. Switch off compressed air.

2. Push the tubings into the tubing connections until limit stop.

3. Slightly redraw the tubings.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-23
Maintenance
Dual Inlet System

Dual Inlet System


WARNING Electric Current. Risk of an electric shock. Do not remove the cover
before or during operation or when performing minor servicing (at the
ion source, for example). Voltages of at least 220 V are prevalent
inside.

CAUTION Hot Surface. Risk of burns. Do not remove the cover before or during
operation or when performing minor servicing (at the ion source, for
example). Temperatures above 60 °C are prevalent inside.

NOTICE Only in case of maintaining the Dual Inlet system (if a seal must be
replaced, for example), a Thermo Fisher Scientific field service
engineer may remove the cover.

Crimp Adjustment
Crimp adjustment ensures an approximately constant and slight gas
flow into the source. Gas consumption is low. In most cases, crimp
adjustment ensures the same flow from both bellows.

Adjusting this flow is essential for high performance operation of the


Dual Inlet system and has to be done with utmost care. Crimp
adjustment is typically performed on CO2.

At the time of installation, crimping is performed by the Thermo Fisher


Scientific field service engineer, and there is no reason to change it.
However, after some time of operation, it might be necessary to bake the
instrument and subsequently to control the crimping of the inlet
capillaries. See Figure 9-11.

Figure 9-11. Crimp adjustment

❖ To adjust the crimps

1. Open the entire Dual Inlet system (bellows 100%).

2. Let 10 mbar of CO2 flow into each bellow (equilibration).

Tip If the crimps are not adjusted, the system might reach signal
limits at 50 mV.

9-24 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Replacing a Pneumatic Valve

3. Carefully adjust the crimps for each inlet port until the bellows
pressure leads to a signal of 2 to 2.2 V on both sides (standard side
and sample side).

In case of CO2, about 10 mbar correspond to a signal of 2 V.

Replacing a Pneumatic Valve


A pneumatic valve block comprises several (one, two, up to seven)
pneumatic valves. Pneumatic valves are used, for example, in the
Changeover valve and in the Dual Inlet. For an overview, see “Valves of
the Dual Inlet System” on page 4-5, “Arrangement in Valve Blocks” on
page 4-6, and “Operating Pneumatic Valves” on page 4-10.

Figure 9-12 shows a pneumatic valve 5 as part of its pneumatic valve


block. The screwed plate 2 seals the pneumatic valve towards the
surrounding air by exerting a pressure upon the gold seal 7. Compressed
air is connected at 3 and 4.

6
1
5
2

4 3 a b c

Labeled Components: 1=screw (4×), 2=plate, 3,4=compressed air connector, 5=pneumatic valve, 6=gold plunger of
pneumatic valve, 7=gold seal of valve block
Figure 9-12. Isolating a pneumatic valve from its pneumatic valve block

• The gold plunger 6 of the pneumatic valve needs to be replaced, if a


gas unintentionally enters the system.

• The gold seal 7 of the valve block needs to be replaced, if


surrounding air enters the system.

• The pneumatic valve 5 as a whole needs to be replaced, if it does not


switch (close) at all anymore. An internal leak (high argon leakage)
occurs.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-25
Maintenance
Replacing a Pneumatic Valve

Figure 9-13 shows an isolated pneumatic valve from above (a; with the
metallic knob 1) and from below (b; with the gold plunger 2 inside the
membrane 3).

1 2

a b

Labeled Components: 1=metallic knob, 2=gold plunger, 3=membrane


Figure 9-13. Pneumatic valve - view from above (a) and from below (b)

Disassembling a Pneumatic Valve


❖ To disassemble a pneumatic valve

1. Isolate the pneumatic valve from its pneumatic valve block as shown
in Figure 9-12.

2. Use flat-nose pliers to separate the pneumatic valve (1 in


Figure 9-14) into the pneumatic plunger 2 and its lower part 3 as
follows:

Take care not to scratch the metallic knob with the flat-nose pliers.

a. Protect the pneumatic valve by covering its metallic knob with a


piece of cloth.

b. Carefully grab the protected metallic knob with the flat-nose


pliers and pull the pneumatic plunger away.

1 2 3

Labeled Components: 1=pneumatic valve, 2=pneumatic plunger (with a Pertinax™ ring and a Viton™ O-ring inside),
3=lower part
Figure 9-14. Separating pneumatic valve into pneumatic plunger and lower part

9-26 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Replacing a Pneumatic Valve

3. Remove the circlip, 3 in Figure 9-15, with the spreader forceps 1 as


follows:

The spreader forceps is not included in the Tool kit.

a. Insert the two tips of the spreader forceps into the two holes 2 of
the circlip.

b. Press the two handles of the spreader forceps together.

This opens the tips of the spreader forceps so that the circlip is
released. Below the circlip, eight washers 4 are arranged against
each other in a batch.

3
4

Labeled Components: 1=spreader forceps, 2=holes of circlip, 3=circlip, 4=washers


Figure 9-15. Removing the circlip

Figure 9-16 shows the pneumatic valve disassembled into its parts.

4 5 6 7
3

1 2

Labeled Components: 1=pneumatic plunger, 2=circlip, 3=washer (8×), 4=housing, 5=membrane, 6=piston, 7=gold
plunger
Figure 9-16. Parts of a pneumatic valve

The gold plunger 7 is located on the rear side of the membrane 5 and the
piston 6.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-27
Maintenance
Replacing a Pneumatic Valve

Reassembling a Pneumatic Valve


After replacing the membrane (together with the gold plunger),
reassemble the pneumatic valve as follows.

❖ To reassemble a pneumatic valve

Reassemble the pneumatic valve on the clean, smooth and even surface
of a desk. Avoid that the surface has a pattern as this pattern may
impair the gold seal.

1. As Figure 9-17 shows, carefully lead the piston 2 of the membrane 1


through the hole of the housing 3.

Labeled Components: 1=membrane, 2=piston, 3=housing


Figure 9-17. Leading piston of membrane through hole of housing

2. Grab the plate springs in the correct order as follows:

Figure 9-18a shows that the plate springs are not flat, but slightly
curved. This leads to spacings between the plate springs when
arranging several of them alternating, opposed to each other. This is
the correct order. When the plate springs are compressed, they act
like a spring. See Figure 9-18b.

b
a

Figure 9-18. Correct arrangement of plate springs

9-28 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Replacing a Pneumatic Valve

Do not arrange the plate springs such that an inwards curved plate
spring is followed by an inwards curved one. See Figure 9-19. This
is the wrong order. The resulting batch is flat and does not act like
a spring.

Figure 9-19. Wrong arrangement of plate springs

3. Thus, arrange the eight curved plate springs as a batch, opposed to


each other, in your hand. According to Figure 9-18, any inwards
curved plate spring must be followed by an outwards curved one.

4. Stick the batch of opposed plate springs as a whole around the


piston 2 of the membrane. See 3 in Figure 9-20.

3
1

Labeled Components: 1=batch of plate springs, 2=piston, 3=opposed plate


springs arranged around piston
Figure 9-20. Arranging plate springs in batch around piston

5. If the circlip is worn out, replace it (or at least bend the circlip
carefully back until it is tensioned again).

A worn out circlip will not fit exactly into the groove of the piston,
as is necessary in step d.

6. Reinsert the circlip upon the batch of plate springs as follows:

a. Insert the tips of the spreader forceps into the holes of the
circlip. See Figure 9-21a.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-29
Maintenance
Replacing a Pneumatic Valve

b. Grab the circlip with the spreader forceps. With the tips of the
spreader forceps, slightly press down the batch of plate springs.
See Figure 9-21b.

c. Slightly push the handles of the spreader forceps apart to arrange


the circlip around the piston, on top of the plate springs. See
Figure 9-21c.

a b c

Figure 9-21. Arranging circlip around piston

d. Use the spreader forceps to insert the circlip exactly into the
groove of the piston. See arrow in Figure 9-22.

gold plunger from below

Figure 9-22. Inserting circlip exactly into groove

7. Make sure that the circlip is fitted exactly into the groove.

8. Grease the guide sleeve (made of Pertinax™; see arrow in Figure 9-23
as well as 1 in Figure 4-10) of the pneumatic plunger inside and
outside.

Grease the O-ring seal (made of Viton™; see 2 in Figure 4-10)


located inside the guide sleeve as well.

Figure 9-23. Guide sleeve of pneumatic plunger

9-30 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Replacing a Pneumatic Valve

9. By using the tool, 1 in Figure 9-24, press the guide sleeve exactly
into the pneumatic plunger.

Labeled Components: 1=tool


Figure 9-24. Pressing guide sleeve into pneumatic plunger using a tool

Reinserting a Pneumatic Valve into its Valve Block


After a defective pneumatic valve has been replaced, it must be
re-assembled into its valve block as follows.

❖ To reinsert a pneumatic valve into its valve block

1. As Figure 9-25 shows, insert the pneumatic valve 1 upon the valve
block 2.

Labeled Components: 1=pneumatic valve, 2=valve block


Figure 9-25. Inserting pneumatic valve upon valve block

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-31
Maintenance
Replacing a Pneumatic Valve

2. As Figure 9-26 shows, arrange the plate 1 exactly upon the


pneumatic valve 2. The four bore holes 3 of the plate must coincide
with the four bore holes of the valve block.

Labeled Components: 1=plate, 2=pneumatic valve, 3=bore holes (4×)


Figure 9-26. Arranging plate upon pneumatic valve

3. Insert two screws into two opposite bore holes. Tighten them
alternately a bit by hand. See Figure 9-27b.

4. Insert the two remaining screws into the two remaining opposite
bore holes. Tighten them alternately a bit by hand. See
Figure 9-27c.

a b c

Figure 9-27. Tightening pairs of opposite screws

9-32 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Autocool Refill Device

Autocool Refill Device


Regularly check the components of the Autocool Refill device for
damage or freeze-up.

CAUTION Cold Liquid. Risk of frostbite. The Autocool Refill device contains
extremely cold liquid gas. Careless handling may cause severe personal
injury including frostbite. Only use liquid nitrogen as cooling agent.

❖ To check the Autocool Refill device

1. Check the components of the Autocool Refill device for damage or


freeze-up.

2. Dry and clean the items (or replace them, if necessary).

3. Make sure that the items are thoroughly degreased and dried,
because moisture or lubricants freeze at cryogenic temperatures. Use
PTFE tape or other approved oxygen-safe compounds.

Do not use thread-sealing compounds.

4. Occasionally, increase the pressure up to the relief valve setting to


ensure satisfactory functioning of this safety device.

Checking the Liquid Nitrogen Evaporation Rate


If you suspect that the evaporation rate of the Autocool Refill device is
excessive, write down the decrease of the liquid nitrogen level for some
time.

❖ To check the liquid nitrogen evaporation rate

1. Close the pressure-raising valve. See Figure 4-20.

2. Open the Trycock/vent valve.

3. After the contents are fully vented to atmospheric pressure, measure


the boil-off rate using a flowmeter.

The normal boil-off rate for nitrogen is 1 L/min for gas, that is
about 2 L of liquid per day.

The reason for a higher rate might be abnormal cold or frost formation
at the lower dished end of the outer casing, which should be removed.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-33
Maintenance
Autocool Refill Device

Maintaining the Dewar Vessel


Before handling the Dewar vessel, check the vessel.

NOTICE Do not use the Dewar vessel when its glassy surface is damaged until it
is repaired, because it may implode due to mechanic or thermal strain.

❖ To check the Dewar vessel

1. Thoroughly inspect the glassy surface of the Dewar vessel for


damages such as scratches, cracks, dents and flaws.

2. If its protective shell is damaged, replace the Dewar vessel.

3. Check the screws that connect the upper and lower section. If the
screws are damaged, do not use the Dewar vessel until it is repaired.

4. When liquid nitrogen has totally evaporated, water remains in the


Dewar vessel. Inspect the Dewar vessel for remaining water. Pour it
out to avoid formation of ice in the Dewar vessel.

Working With Liquid Nitrogen


As a quick reference, Table 9-2 lists the arrangement of the valves of the
external LN2 tank for filling, dispensing and storage of liquid nitrogen.
Table 9-2. Valve statuses during operation
Operation Liquid Fill Gas Use Pressure-Raising Trycock/Vent
and Decant Valve Valve Valve
Valve
Automatic open closed closed closed
Refill during
operation
Dispensing open open closed closed
liquid
Pressure closed closed closed open
withdrawal
Storage closed closed closed open

Tip See Figure 4-20 for a schematic and the names of the different
valves.

Before operating the Microvolume, check the fill level of the Autocool
Refill device.

9-34 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Needle Valves

❖ To enable the automated and computer-controlled refill operation

1. Make sure that all pipe connections leading to the Dewar vessel of
the Autocool Unit are correctly installed.

2. Close the Trycock/vent valve.

3. Open the liquid fill and decant valve.

4. Open the pressure-raising valve.

5. Close the pressure-raising valve as soon as the operating pressure is


reached (at least 0.7 bar; 70 kPa; 10 psi).

The Autocool Refill device is now connected to the Dewar vessel of the
Microvolume.

The flow is controlled by the refill valve N12 (see Figure 4-20). The
pressure-raising valve may be closed when the working pressure is
reached, or it may remain open, provided the pressure regulator is set to
a suitable working pressure. If necessary, open and close the
pressure-raising valve several times until the working pressure is stable.

❖ To fill the Dewar vessel

1. Close the Trycock valve.

2. Make sure that the pressure-raising valve is closed.

3. Open the liquid fill and decant valve.

The Dewar vessel of the Autocool Unit is filled automatically with


liquid nitrogen to roughly the required level.

Needle Valves
Up to three equivalent needle valves (stainless steel on/off valve
SMOV-1 manufactured by SGE) are used to control peripherals. The
needle valves are located at the aluminum heating block, close to the ion
source.

The needle valve can also be controlled using the control panel: up to
three adjusting knobs (7 in Figure 3-3) open and close the valves.
Thereby, gas transfer (a mixture of helium and sample gas) from a
peripheral to the ion source is enabled or disabled.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-35
Maintenance
Needle Valves

NOTICE Open and close needle valves with caution. Operate the adjusting
knobs sensitively. To open a needle valve, turn the corresponding
adjusting knob only once or maximally twice counterclockwise.

If you open a valve too far, leaks may result. In extreme cases, the
needle valve might be totally unscrewed from the Swagelok™
connector, which leads to venting of the analyzer. Turning an adjusting
knob one or maximally two revolutions clockwise closes the
corresponding needle valve again.

Any arbitrary peripheral can be connected to any of the three needle


valves (a GasBench II device, an LC IsoLink device, a ConFlo IV
interface, or a GC-Combustion interface, for example). When a
peripheral is not used, keep the corresponding needle valve closed. Open
it to use the peripheral for measurements.

Tip Even though up to three peripherals can simultaneously be


connected, only one should be active and controlled by its adjusting
knob at a time. Furthermore, do not apply too high gas pressures to
the ion source.

For maintaining the stainless steel on/off valve SMOV-1, refer to SGE’s
documentation at www.sge.com.

Removing the Needle Valve Heater

CAUTION Hot Surface. Risk of burns. Temperatures of about 75 °C or above


may be reached at the metallic surface of valves that are baked out. Do
not touch any surface of a valve you are baking out.

The needle valve heater is the same for Dual Inlet devices and
Continuous Flow devices. The heater comprises a heating cartridge to
uniformly heat the needle valves either during specific operational time
intervals or during the entire operation. This keeps the valves clean,
particularly water-free. Temperature is about 60 to 80 °C, but below
100 °C.

9-36 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Needle Valves

Figure 9-28 shows the parts of the needle valve heater.

5 3

Labeled Components: 1=connector for fused silica capillaries of peripheral,


2=needle valve, 3=cylindrical connector, 4=slot screws (2×, second screw see
detail), 5=heating block, 6=connection of heater to activated sockets in the
Microvolume cabinet
Figure 9-28. Heating block for needle valves

Peripherals are connected via fused silica capillaries at 1. The cylindrical


connector 3 for the needle valves 2 is fixed with two screws. The
movable shafts allow for compensation of differences in length. They are
direct connections to the three adjusting knobs at the control panel. See
“Control Panel” on page 3-6.

The cable 6 connects the heater 5 and the activated sockets in the
Microvolume cabinet.

❖ To remove the heater for maintenance operations

1. Loosen the slot screws 4 in Figure 9-28.

2. Remove the heating block 5.

After removal, only the inlet distributor remains. It establishes the


connection to the ion source and to the Changeover valve.

Leaks at the Needle Valves


Needle valves might become leaky by and by. For maintaining the
stainless steel on/off valve SMOV-1, refer to SGE’s documentation at
www.sge.com.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-37
Maintenance
Needle Valves

Connecting a New Peripheral


Depending on your measurement type, connecting another peripheral
might become necessary.

❖ To connect a new peripheral

1. Switch off the instrument.

2. If you want to connect a new or a second needle valve, vent the


instrument.

You do not need to vent the instrument, if you only change


capillaries.

CAUTION Hot Surface. Risk of burns. The needle valve heating block may be
hot. Wait a sufficient time to allow the parts to cool before touching
them.

3. Carefully remove the needle valve heating block. See “Removing the
Needle Valve Heater” on page 9-36.

4. Remove the locking cap (2 in Figure 9-29).

to Changeover valve

to ion source

Labeled Components: 1=manifold, 2=locking cap, 3=nut


Figure 9-29. Inlet distributor

5. Screw on the new needle valve.

6. Remove the nut (3 in Figure 9-29).

Tip To avoid unscrewing the entire valve, hold a screw wrench


against it.

7. Insert the ferrule with the two capillaries coming from the
peripheral into the nut 3.

9-38 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

8. Carefully stick the capillaries through until they touch the ground at
the valve.

9. Begin to tighten the nut until the capillaries are no longer movable
within the ferrule.

10. Open the ferrule a little and pull back the capillaries a bit.

Tip When pulling back the capillaries a bit, mark this position by
a small piece of adhesive tape.

11. Carefully tighten the nut again.

12. Connect the new peripheral to a SUB D connector (4 in Figure 3-6)


and to a compressed air connector (2 in Figure 3-6) at the rear panel
of the IRMS.

13. Switch on the IRMS again.

Baking a Needle Valve


After you have connected the new peripheral, bake the corresponding
needle valve as follows.

❖ Tobake a needle valve

1. Re-mount the needle valve heater block.

2. In the Source Heater panel, click the Inlet Valve Heater button to
switch on the heater. See Figure 6-31.

3. Perform a leak check. See “Detecting Leaks” on page 9-20.

Stainless Steel Capillaries and Fused Silica Capillaries


Fused silica capillaries are used to connect Continuous Flow peripherals
to the Delta V Series instrument.

All stainless steel capillaries have a central brass contact for the current
entry and are surrounded by an insulating silicone tube. They are used
to connect:

• a Changeover valve to a Dual Inlet system

• a Changeover valve to a Kiel IV Carbonate Device (if available)

• a Changeover valve to a Microvolume (if available).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-39
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

NOTICE Take care that hot stainless steel capillaries do not touch plastics parts
during and after they are baked out.

Fused silica capillaries are fragile although their stability has been
increased by a polyimide coating.

Removing the Blind to Access the Capillaries


The removable blind (2 in Figure 9-30) on the left side of the Delta V
Series instrument allows quick access to for example the needle valves
and the Penning gauge. In most maintenance cases, the peripheral
placed upon the cover plate does not need to be removed.

Labeled Components: 1=cover plate, 2=removable blind, 3=side panel


Figure 9-30. Removable blind on left side of a Delta V Series instrument

The capillaries are easily accessed from outside after removing the blind
on the left side.

Tip Remove the blind for easy access in case of more complex
maintenance operations.

❖ To remove the blind

1. Remove the left side panel (3 in Figure 9-30) by grasping it at the


top and at the bottom and then lifting it up and out.

2. Remove the two screws located on the left and right side.

3. Pull the blind outwards.

4. If you need more space, pull away the electronics cylinder of the
Penning gauge. See Figure 9-38.

9-40 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

Putting Capillaries through


In this section, putting through fused silica capillaries, but also stainless
steel capillaries, is described. Two mechanisms have been realized to lead
both types of capillaries from the Delta V Series instrument towards the
peripherals positioned outside of it. This allows for arranging and
connecting the peripherals flexibly and saves capillary length:

• putting capillaries through via blinds with slits

• putting capillaries through via a guide tube

Putting Capillaries through via Blinds with Slits

Removing the blind on the left side is described at “Removing the Blind
to Access the Capillaries” on page 9-40. At the right side, another blind
with slits at both ends is arranged. It cannot be removed as easily as the
blind on the left side.
The slits are used as throughputs for capillaries. See 2 in Figure 9-31.
Thereby, the capillaries may stay connected even when the blind is
removed.

Labeled Components: 1=cover plate, 2=capillary throughput, 3=blind


Figure 9-31. Capillary throughput via blinds with slits

Depending on the peripheral to be connected, different slits are used:

• Generally, the rear slits are used for all peripherals except the Kiel IV
Carbonate Device. They are more often used than the front slits.

• The slits on the left side are used more often than those on the right
side. In the usual case of a peripheral positioned left to the IRMS,
this keeps the distance between capillaries that are restricted in
length, and the analyzer smallest.

• The Kiel IV Carbonate Device is placed besides the IRMS. Its


stainless steel capillary is mostly led through the front slits.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-41
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

Tip Any other peripheral however, is placed on top of the IRMS,


upon the cover plate. The capillaries are then led out preferably via the
left rear slits. This is true also in case of operating several peripherals
which are not placed on top, but left to the Delta V Series instrument.

Putting Capillaries through via a Guide Tube

Top right at the rear side, a hollow guide tube made of plastic is
arranged between the two outer walls of the IRMS. See 1 in Figure 9-32.

Labeled Components: 1=guide tube


Figure 9-32. Capillary throughput via guide tube

Within the guide tube, capillaries can be led out towards the external
peripherals. The guide tube inhibits contact between capillaries and
electronics.

Baking Stainless Steel Capillaries


Thermo Fisher Scientific recommends baking stainless steel capillaries
when they are contaminated (by impurities or water, for example).
Stainless steel capillaries conduct electric current quite well. Figure 9-33
shows the capillary heating transformer that provides the energy for the
heating process.

9-42 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

Labeled Components: 1=main switch (on/off), 2=input of 0 V, 3=input of 7.7 V


(12 A), 4=input of 0 V, 5=input of 7.7 V (12 A)
Figure 9-33. Capillary heating transformer

The heating process can be regulated with Isodat: ISL scripts can be
used to create time programs for it.

During the start phase of heating, signal intensity increases, but


decreases and stabilizes later. The best results for decontaminating
capillaries are achieved by baking them for approximately 6 to 8 hours.

With stabilized signal intensity lower than the first signal, a successful
decontamination can be assumed. The result can be checked by a
zero-measurement (measuring the same gas on the sample and the
standard side).

❖ To bake a stainless steel capillary

1. Before heating the capillary, heat the surrounding of the capillary to


approximately 80 °C for about 30 to 60 minutes.

The surrounding comprises the valves of the inlet system (including


the valves of a Multiport, if in use), the Changeover valve, the ion
source and the analyzer housing.

During the heating period, all valves must be open. Swagelok™


connectors should be heated separately with a flame or a heat gun
for a short while.

2. Enable gas transfer through the capillaries to be baked. Let CO2


flow through the capillaries during the entire process.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-43
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

Impurities within the capillaries (water, for example) are


continuously transported to the waste line together with the gas and
are removed by the waste line pump. The Dual Inlet system must be
closed.

3. Connect the 0 V inputs (2 and 4 in Figure 9-33) of the capillary


heating transformer to the banana jack. See 1 in Figure 9-34.

Figure 9-34. Fixing alligator crimps to the capillaries

4. Connect one of the 7.7 V inputs of capillary heating transformer


(positive pole; 3 or 5 in Figure 9-33) to the brass contact in the
center of one capillary (for example, 2 in Figure 9-34) with alligator
crimps.

5. Connect the other 7.7 V input of the capillary heating transformer


to the brass contact in center of the other capillary (for example, 3 in
Figure 9-34).

NOTICE After the capillary has been wired, make sure that the capillary
(with or without insulation) has no contact to any plastic surface
of tubes, housings, cables etc. to avoid melting or smoldering
caused by a hot capillary.

6. Turn on the capillary heating transformer by pressing its main


switch (1 in Figure 9-33).

An electric current flows from the brass contact in the center of the
capillary to both ends and bakes it out.

7. Control the heating phase by monitoring signal intensity of H2O


(m/z 18, measured on the channel for m/z 45).

9-44 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

8. Bake out the capillaries for half an hour while CO2 continuously
passes through them.

NOTICE Heat the crimped part of the capillary separately for a few minutes
with a flame or a heat gun. Before removing the upper crimp
block, mark the parts of the crimping device to avoid mismatch
when reassembling.

9. Remove the upper crimp block and heat separately.

10. When re-fitting the crimp block, make sure that the capillary is
placed exactly in the grove of the base and the die of the upper block
in the crimp of the capillary. See Figure 9-35.

Figure 9-35. Crimping device at the end of a capillary

11. After baking the capillary, the flow resistance of the crimp needs to
be checked and reset to 1 V per 10 mbar if required. See “Replacing
Capillaries” on page 9-45.

Replacing Capillaries
Replacing an inlet capillary may become necessary in case of
contamination or mechanical damage. After replacement, the flow rate
of the new capillary needs to be set by crimping. The crimping device
consists of two metal blocks. The base is attached to the end piece of the
new capillary, which has to be fitted to the Changeover valve. The
second block, to be bolted on top of the base block, holds a metal pin in
a spacing, which squeezes the capillary when bolting the two blocks
together.

❖ To replace a capillary

1. Make sure that all valves are closed before venting the surrounding
area of the capillary, which is to be exchanged.

2. Vent the parts of the inlet system and the Changeover valve, which
are connected by the capillary.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-45
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries

3. Loosen the Swagelok™ fittings holding both end pieces of the


capillary to be exchanged. New capillaries are delivered with close
ends. Use a diamond file to cut a capillary end at opposite sides
before breaking off the tip. Then smoothen the end of the capillary.

4. Fasten the end pieces of the new capillary with the Swagelok
connectors. Connect the end piece with the crimp block to the
Changeover valve. Fasten the upper crimp block loosely onto the
base with the capillary.

Adjusting Capillaries
Each time after a capillary has been replaced (see “Replacing Capillaries”
on page 9-45), the flow through it must be adjusted. It is reasonable to
do this from time to time, even if no capillary has been replaced.

❖ To adjust the capillaries

1. Pump out the Dual Inlet system.

2. Let a proper amount of CO2 flow into the Dual Inlet system, so that
the storage reservoir pressure is about 20 mbar on both capillary
sides.
3. Start Instrument Control of Isodat.

4. Activate the Scan window. See Figure 9-36.

5. From the rightmost drop-down list, select Tune Scan.

6. Click the Start Scan button.

Figure 9-36. Scan window

9-46 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Nickel Capillaries

7. Carefully tighten the screws of the crimp block and squeeze the
capillary until the output signal reaches 1 V per 10 mbar (with CO2
used for measurement).

8. Bake the capillary. See “Baking Stainless Steel Capillaries” on


page 9-42.

Nickel Capillaries
This section describes how to handle, insert, cut, bake and crimp nickel
capillaries. To connect Dual Inlet peripherals using nickel capillaries, see
“Connecting Dual Inlet Peripherals Using Nickel Capillaries” on
page 4-11.

Handling Nickel Capillaries


The advantageous laminar flow and diffusion characteristics of the 18%
narrower nickel capillaries lead to both higher precision and accuracy
especially in case of small sample amounts. The bellow compression
factors are improved as well.

Nickel capillaries have a smoother inner surface compared to stainless


steel capillaries. Water residues can therefore easier be pumped down.

Nickel capillaries however, lead to a smaller absolute sensitivity value at


8 V signal, if determined via the Diagnosis module of Isodat. This is due
to the algorithm of the software. The sensitivity of the analyzer stays the
same. At lower signal values, for example 1-2 V, the absolute sensitivity
reached with nickel capillaries is increased.

The power function signal vs. time is more linear at lower voltages
(pressure dependence). In case of stainless steel capillaries, absolute
sensitivity is calculated by means of linear regression. Nickel capillaries
however, require an exponential regression for calculating absolute
sensitivity.

The CO2 sample decrease signal (m/z 44) vs. the CO2 pressure is a
power function. Its characteristics depends on the pressure, the
dimension of the crimp hole, material properties, the dimensions of the
capillary tubing and the source pressure.

To determine absolute sensitivity, a linear relationship between bellow


pressure and intensity is assumed. The real absolute sensitivity value
(molecule per ion) of the device is always slightly lower than the
absolute sensitivity value computed by the software.

Use a magnet to differentiate between a stainless steel capillary (not


magnetic) and a pure nickel capillary (magnetic).

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-47
Maintenance
Nickel Capillaries

Installing Nickel Capillaries


As a general guideline for installing capillaries, see “Replacing
Capillaries” on page 9-45.

If you have a Microvolume, Thermo Fisher Scientific recommends


installing two nickel capillaries at the Changeover valve and one at the
input of the Microvolume.

The nickel capillary package contains one spare nickel capillary which
can be used to run an additional Dual Inlet peripheral. Maximal two
Dual Inlet peripherals can be run. Additional single capillaries can be
ordered from Thermo Fisher Scientific.

Cutting Nickel Capillaries

NOTICE Nickel capillaries need extra care when cutting them with a diamond
file. Do not reduce the inner diameter by cutting or bending.

As nickel shears off very easily, the capillaries tend to form cracks or
even break off. Handle them very carefully and avoid contact with
edges.

A protective cover made of stainless steel prevents the nickel capillary


from shearing off and breaking.

❖ To cut nickel capillaries

1. File the capillary from the outside until the cut extends around its
entire circumference.

2. Carefully bend the end of the capillary such that the nickel capillary
is fully open.

Baking Nickel Capillaries


As a general guideline for baking capillaries, see “Baking Stainless Steel
Capillaries” on page 9-42.

Due to the different material properties and capillary dimensions


however, baking of nickel capillaries differs considerably from baking
stainless steel capillaries.

Due to its higher resistance at 12 A, pure nickel gets hotter than stainless
steel. Therefore, nickel capillaries need to be baked only during a short
period of time. Connect the transformer directly to the UPS, if
available.

9-48 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Nickel Capillaries

NOTICE Do not bake a contaminated nickel capillary longer than 5 min to


prevent the heating transformers (12 A, 7 V) and the fuses from
damage. Bake only one nickel capillary at a time.

Crimping Nickel Capillaries


As a general guideline for crimping Dual Inlet capillaries, see “Replacing
Capillaries” on page 9-45.

Due to the different material properties however, crimping of nickel


capillaries differs from crimping stainless steel capillaries.

NOTICE Due to the considerable ductility of pure nickel, handle the capillary
especially careful when crimping it. If you reduce the inner diameter at
the crimping position too much, the capillary may irreversibly be
closed. It must then be replaced.

Do not cut the capillary at the edge of the crimp position (full metal
block). Do not change the inner diameter of the capillary by bending
it.

During crimping, reduce the inner diameter of the nickel capillary at the
crimping position as described at “Replacing Capillaries” on page 9-45.
This is achieved by very carefully fixing two screws alternately by using
an hex key. During crimping nickel capillaries, check the signal to
pressure ratio more often than in case of stainless steel capillaries. This
avoids overtightening the crimp holes of the nickel capillaries.

For CO2, adjust the crimping position such that a signal of 2 V is


obtained with a pre-pressure of 10 mbar. For hydrogen due to its lower
conductance, a lower signal to pressure ratio can be expected (10 mbar
H2 to 10 V).
After crimping, determine the sensitivity of the mass spectrometer.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-49
Maintenance
Penning Gauge

Penning Gauge
This section describes maintenance and dismantling of the Penning
gauge. Refer also to the Instruction Manual of Edwards and to
www.edwardsvacuum.com.

The design of the Penning gauge allows to easily clean the cathode tube
(7 in Figure 9-37), the cathode plate 6 and the anode assembly 3 that
may get dirty.

Labeled Components: 1=magnet housing, 2=collar, 3=anode assembly,


4=O-ring seal, 5=body tube, 6=cathode plate, 7=cathode tube, 8=circlip
Figure 9-37. Parts of Penning gauge - schematic

Putting the Penning Gauge Into Operation Again


If the Penning gauge does not spark during an evacuation, it may be
necessary to clean it. Before cleaning it, try the following
“rough-and-ready” procedure.

❖ To put the Penning gauge into operation again (“rough-and-ready”)

1. Pull away its electronics cylinder (without venting the system). See
Figure 9-38.

Figure 9-38. Pulling away electronics cylinder of Penning gauge

9-50 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Penning Gauge

2. Re-connect the Penning gauge.

3. Alternatively, let slightly more gas flow into the ion source to start
the Penning gauge again.

4. If the problem remains, clean the Penning gauge. See


“Disconnecting and Cleaning the Penning Gauge” on page 9-51.

Disconnecting and Cleaning the Penning Gauge


If the “rough-and-ready” procedure described at “Putting the Penning
Gauge Into Operation Again” on page 9-50 does not put the Penning
gauge into operation again, it must be cleaned. A contaminated Penning
gauge may read out wrong pressures.

WARNING High Voltage. Risk of injury. High voltages about 3 kV are generated
inside the Penning gauge. Disconnect the Penning gauge.

❖ To disconnect the Penning gauge

1. Disconnect the cable from the Penning gauge.

2. Pull away the electronics cylinder (9 in Figure 9-39) of the Penning


gauge.

1
9

8
2

3
4
5

Labeled Components: 1=needle-nosed pliers, 2=collar, 3=circlip, 4=body tube,


5=O-ring seal, 6=anode assembly, 7=cathode plate, 8=cathode tube,
9=electronics cylinder
Figure 9-39. Dismantled parts of Penning gauge

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-51
Maintenance
Penning Gauge

3. To unlock the bayonet fitting, turn the body tube 4 anti-clockwise


(viewed from the vacuum flange).

4. Vent the system.

5. Remove the body tube 4 from the vacuum system.

6. Clean the body tube as described at “To clean the body tube” on
page 9-52.

❖ To clean the body tube

1. After disconnecting the Penning gauge as described in “To


disconnect the Penning gauge” on page 9-51, use the pliers (1 in
Figure 9-39) to unscrew the collar 2.

2. Insert the needle-nosed pliers into both eyelets of the circlip 3. Pull
out the circlip.

3. Use fine sandpaper or Al2O3 to remove dirt from the metal parts
(predominantly from the cathode tube 8, the cathode plate 7, and
the anode assembly 6).

After you have re-installed the Penning gauge, adjust its set point (“set
trip“) as described at “Adjusting the Set Point of the Penning Gauge” on
page 9-53.

Measurement Points for the Penning Gauge

WARNING High Voltage. Risk of injury. Some parts of the Delta V Series
instrument are at high voltage. Opening the electronics cabinet is only
allowed for maintenance purposes by qualified service personnel.

The Penning gauge is controlled by the Power Distribution board.


Three measurement points MP 11, MP 12 and MP 13 located on this
board are relevant for the Penning gauge. See Figure 9-40.

4 3

Labeled Components: 1=MP13, 2=MP12, 3=MP11, 4=connection to Penning


gauge
Figure 9-40. Measurement points on power distribution board

9-52 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Penning Gauge

The value between ground (GND), MP 13, and MP 11 is the set point
(1 × 10-5 mbar, for example). When the pressure falls below the set
point, vacuum is considered to be sufficient. The Penning gauge then
enables electronics and Isodat, so that ion source and high voltage can be
switched on.

However, when the actual pressure exceeds the set point, security
mechanisms become active. The Penning gauge induces a shutdown of
ion source and high voltage. The set point must be adjusted as described
at “Adjusting the Set Point of the Penning Gauge” on page 9-53.

The value between ground (GND), MP 13, and MP 12 is the actual


voltage value read out by the Penning gauge. This output voltage
represents a pressure (the actual vacuum status) and can be checked on
the power distribution board.

As various types of Penning gauges have a voltage-pressure characteristic


of their own, Isodat converts this measured voltage value into its
appropriate pressure value (for example, 1 × 10-5 mbar may correspond
to 6.8 V for a particular type of Penning gauge).

Adjusting the Set Point of the Penning Gauge


The set point of the Penning gauge (set trip) is the particular voltage at
which the set point output signal goes on. In the very rare case of
defective electronics of the Penning gauge, or if you bought a new
electronics for it at Edwards, adjust its set point.

Tip For your instrument, Thermo Fisher Scientific has adjusted the
set point of the Penning gauge.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-53
Maintenance
Penning Gauge

Figure 9-41 shows a schematic of the Penning gauge parts.

Labeled Components: 1=end cap, 2=vacuum flange, 3=body tube, 4=magnet


housing, 5=cable connector plug, 6=set point potentiometer, 7=Penning
gauge connector socket
Figure 9-41. Schematic of Penning gauge parts

❖ To adjust the set point of the Penning gauge

1. Turn the set point potentiometer using a fine screwdriver.

The set point potentiometer is accessible through a hole in the


end-cap of the Penning gauge. See arrow in Figure 9-42.

Figure 9-42. Penning gauge

2. Turn the set point potentiometer clockwise to increase the voltage.


Turn it anti-clockwise to decrease the voltage.

9-54 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Amplifier Area and Three-Way Valve

WARNING High Voltage. Risk of injury. Some parts of the Delta V Series
instrument are at high voltage. Opening the electronics cabinet is only
allowed for maintenance purposes by qualified service personnel.

3. Simultaneously measure the set point as the voltage between the


pins MP 11 and MP 13 on the power distribution board. See
Figure 9-43.

Figure 9-43. Voltage measurement on power distribution board

4. Adjust the set point to 6.2 V.

Amplifier Area and Three-Way Valve


If you need access to the amplifier area for maintenance, vent the
amplifier housing beforehand by turning the switch to the Vent
position. See “Venting the Amplifier Housing” on page 9-57.

When capacitors or resistors at the amplifiers cause problems, they need


eventually be replaced. For example, fingerprints on the resistor may
cause a rather noisy signal. Dismantle the resistor and carefully wipe it
with pure ethanol.

NOTICE Neither touch an amplifier nor its electronic parts (resistors, for
example). This electronic equipment is highly sensitive.

To avoid damaging an amplifier, do not replace it while the power


supply is switched on.

To avoid damaging the aluminum-made parts, do not use any


mechanical tool to force the opening of the flanges. Instead, after first
venting correctly and then loosening the screws, any flange can be
easily removed manually.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-55
Maintenance
Amplifier Area and Three-Way Valve

The three-way valve (Figure 9-44) allows evacuating the amplifier area
to the millibar range. Evacuation provides thermal insulation and leads
to a stable signal due to elimination of cosmic radiation.

Labeled Components: 1=to turbomolecular pump of analyzer, 2=to fore


vacuum pump of analyzer
Figure 9-44. Switching positions and layout of three-way valve

Table 9-3 lists the switching positions of the three-way valve.

Table 9-3. Switching positions of three-way valve


Switching position Designation
0 Off
FV Amplifier area is connected to fore vacuum.
HV Amplifier area is connected to high vacuum.
Vent Amplifier area is vented.

At its bottom, the three-way valve contains a punched sheet plate


(diameter of hole 0.15 mm). An O-ring seal is positioned on the sheet
plate. The white Teflon™ tube that leads to the fore vacuum pump of the
analyzer is arranged upon the O-ring seal. The Teflon tube is equipped
with a supporting sheath on its inside. On the outside, the usual
Swagelok™ cone is arranged.

Tip When mounting the Teflon tube on the right side, push it in
tightly before and while you fasten it with the screw. Thereby, the
Teflon tube seals up against the O-ring seal.

9-56 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Amplifier Area and Three-Way Valve

Venting the Amplifier Housing


This procedure allows venting the amplifier area without affecting the
analyzer vacuum.

Tip The amplifier area is not vented automatically when the IRMS is
vented.

To vent even the amplifier area, turn the three-way valve to the Vent
position. See Figure 9-44 and Table 9-3.

Evacuating the Amplifier Housing with an Evacuated Analyzer


The amplifier housing can be evacuated without affecting the analyzer
vacuum.

❖ To evacuate the amplifier housing

1. Turn off the ion source to prevent the filament from any damage.

2. Switch the three-way valve to the FV position. See Figure 9-44 and
Table 9-3.

3. Wait for at least two hours, but not longer than four hours.
This waiting time is necessary because pumping the amplifier
housing proceeds along a considerably narrow restriction.

Tip If the turbomolecular pumps of the analyzer have been shut


down, use the switches at the control panel (4 and 5 in Figure 3-3)
to turn the pumps on again.

If then the turbomolecular pumps are shut down again, probably a


leak is present at the amplifier area, or the seal fits improperly due
to impurities.

4. Switch the three-way valve to the HV position. See Figure 9-44 and
Table 9-3.

Evacuating the Amplifier Housing with Vented Analyzer


When all pumps are switched off (control panel switch 4 in Figure 3-3),
this procedure allows to evacuate the amplifier housing.

To evacuate the amplifier housing with vented analyzer, switch the


three-way valve to the HV position. See Figure 9-44 and Table 9-3.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-57
Maintenance
Thermo Fisher Scientific Service

Thermo Fisher Scientific Service


This section contains information concerning maintenance work that
must be performed by Thermo Fisher Scientific personnel.

Health and Safety Form

Hazardous Chemicals. Hazardous material might contaminate


certain parts of your system during analysis. To protect our employees,
we ask you to adhere to special precautions when returning parts for
exchange or repair.

If hazardous materials have contaminated mass spectrometer parts,


Thermo Fisher Scientific can only accept these parts for repair if they
have been properly decontaminated.

Materials that due to their structure and the applied concentration


might be toxic or which are reported in publications to be toxic are
regarded as hazardous. Materials that will generate synergetic
hazardous effects in combination with other present materials are also
considered hazardous.

Parts contaminated by radioisotopes must not be returned to Thermo


Fisher Scientific, neither under warranty nor within the exchange part
program. If unsure about parts of the system possibly being
contaminated by hazardous material, make sure that the Thermo
Fisher Scientific field service engineer is informed before the engineer
starts working on the system.

Your signature on the Health and Safety Form confirms that the
returned parts have been decontaminated and are free of hazardous
materials. The form is provided in this manual. See “Health and Safety
Form” on page A-5. You can also request the Health and Safety Form
stand-alone from the Thermo Fisher Scientific field service engineer.

Services to be Performed by Thermo Fisher Scientific Service Only


Table 9-4 lists services that must be performed by a Thermo Fisher
Scientific field service engineer or personnel trained by Thermo Fisher
Scientific. Depending on the actual workload of your Delta V mass
spectrometer, you may increase the maintenance frequency.

Table 9-4. Thermo Fisher Scientific service procedures


MS Component Procedure Frequency
Pump System Full service Yearly
Ion Source Complete cleaning of all ion source Yearly
parts

9-58 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
A
Legal Documents

Contents

• FCC Compliance Statement on page A-2

• WEEE Compliance on page A-3

• Declaration of Conformity on page A-4

• Health and Safety Form on page A-5

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) A-1
Legal Documents
FCC Compliance Statement

FCC Compliance Statement


This equipment has been tested and found to comply with the limits for
a Class B digital device, pursuant to Part 15 of the FCC Rules. These
limits are designed to provide reasonable protection against harmful
interference in a residential installation. This equipment generates, uses
and can radiate radio frequency energy and, if not installed and used in
accordance with the instructions, may cause harmful interference to
radio communications. However, there is no guarantee that interference
will not occur in a particular installation. If this equipment does cause
harmful interference to radio or television reception, which can be
determined by turning the equipment off and on, the user is encouraged
to try to correct the interference by one or more of the following
measures:

• Reorient or relocate the receiving antenna.

• Increase the separation between the equipment and receiver.


• Connect the receiver into an outlet on a circuit different from that
to which the equipment is connected.

• Consult the dealer or an experienced radio/TV technician for help.

A-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Legal Documents
WEEE Compliance

WEEE Compliance
This product is required to comply with the European Union’s Waste
Electrical & Electronic Equipment (WEEE) Directive 2012/19/EU. It
is marked with the following symbol:

Thermo Fisher Scientific is registered with B2B Compliance


(B2Bcompliance.org.uk) in the UK and with the European Recycling
Platform (ERP-recycling.org) in all other countries of the European
Union and in Norway.

If this product is located in Europe and you want to participate in the


Thermo Fisher Scientific Business-to-Business (B2B) Recycling
Program, send an email request to weee.recycle@thermofisher.com with
the following information:

• WEEE product class

• Name of the manufacturer or distributor (where you purchased the


product)

• Number of product pieces, and the estimated total weight and


volume

• Pick-up address and contact person (include contact information)

• Appropriate pick-up time

• Declaration of decontamination, stating that all hazardous fluids or


material have been removed from the product

This recycling program is not for biological hazard products or for


products that have been medically contaminated. You must treat these
types of products as biohazard waste and dispose of them in
accordance with your local regulations.

RoHS
For information about the Restriction on Hazardous Substances
(RoHS) Directive for the European Union, search for RoHS on the
Thermo Fisher Scientific European language websites.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) A-3
Legal Documents
Declaration of Conformity

Declaration of Conformity

A-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Health and Safety Form
Health and Safety Form Legal Documents
Health and Safety Form
This Decontamination Declaration Form must be completed for all materials returned to Thermo Fisher Scientific. It
should be sent to the destination by e-mail, with approval from an authorized person. A signed hardcopy should be
attached to the outside of the package with shipping paperwork and a further copy should be placed inside the
packaging. The receiving Thermo Fisher Scientific office can help with this form and supply a return number, shipping
address and e-mail address. This form can be used to request warranty. Use the text "not used" to indicate a field not
being used. Where a Thermo Scientific part number is not known, add the supplier name (as for the examples below).

1. General information

Thermo Fisher Scientific contact name for delivery


Thermo Fisher Scientific receiving site
Customer Instrument type
Address Instrument SN
Order number
Phone Return number
E-Mail Medical Device Research Use Only
SAP Service Notification

Part Number Quantity Material Description Error Description / Reason for Return Return Part Serial No

2. Condition of the material or instrument


Has the material or instrumentation been removed from the Tick the applicable check box.
shipping packaging or in contact with
- pump fluids Yes Æ go to section 3
- service fluids
- samples No Æ go to section 5
- standard solutions
- other chemicals
- hazardous materials

3. Contamination
Use the check boxes to state any contaminants the material/instrumentation been exposed to. Contaminated materials
must not be shipped to Thermo Fisher Scientific. If any exposure boxes are ticked, select ‘Yes’, if none, select ‘No’.
serious health
toxic flammable corrosive oxidizing
hazard
hazardous to gas under other harmful
explosive
environment pressure substances
biological radioactive
contaminated contaminated

Yes Æ go to section 4
Thermo Scientific
No Æ go to section 5
Delta V Series Operating Manual (P/N 1174000, Revision E) A-5

Health and Safety Form (P/N 1342350, Revision H) Page 1 of 2


Legal Documents
Health and Safety Form
Health and Safety Form
4. Description of process substances and/or compounds
Which substances have been in contact with the material or instrumentation? (trade name and/or chemical term of service
fluids and substances; properties of substances or compounds according to the Material Safety Data Sheet; e.g. toxic,
flammable, corrosive, radioactive)

Part Number Trade Name Chemical / Substance Name / Properties

a)

b)

c)

d)

e)

f)

5. Legally binding declaration

Has the material/instrument undergone a decontamination process? Yes Æ go to section 6 No


Is the material/instrument safe to handle for Thermo Fisher Scientific and Yes No
third-party personnel?

Components, materials and/or instruments that have been contaminated to a harmful level by whatever substances and/or compounds
as stated in sections 3. and 4. above will not be accepted without written evidence of proper decontamination.
I hereby declare that the instrument has undergone successfully all required decontamination procedures and is safe to handle for
Thermo Fisher Scientific and/or third-party service personnel or suppliers such as Pfeiffer Vacuum, Leybold Vacuum, Edwards Vacuum
products, or others.
I confirm that all information, which is supplied on this form, is accurate, complete and sufficient to judge any contamination level. I
acknowledge and agree that I will be liable for any personal injury or any other damage, which might result from a false, inaccurate or
incomplete statement and that I will indemnify and defend Thermo Fisher Scientific and/or any other concerned third party for and
against any liabilities, claims, losses, and/or damages of all kinds arising out of and/or caused by such false, inaccurate or incomplete
statements.
Thermo Fisher Scientific reserves the right not to process refunds or returns where the declared or observed use or previous
contamination of the product/material has by Thermo Fisher Scientific judgement impacted its integrity.

6. Detailed description of the decontamination process used

Part Number Serial Number Describe the decontamination process

Return Number Name of authorized person (block letters) Date Signature Company stamp

A-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific

Health and Safety Form (P/N 1342350, Revision H) Page 2 of 2


G
Glossary
This section lists and defines terms used in this manual. It also includes acronyms, metric prefixes, symbols, and
abbreviations.

A B C D E F G H I J K L M N O P Q R S T U V W X Y Z

A CID collision-induced dissociation

A ampere cm centimeter

ac alternating current cm3 cubic centimeter

ADC analog-to-digital converter Continuous-Flow (CF) Automated preparation device


and mass spectrometer in which sample analysis is
AP acquisition processor conducted in a continuous stream of helium carrier gas.
API atmospheric pressure ionization CPLD Complex Programmable Logic Device
ASCII American Standard Code for Information CPU central processing unit (of a computer)
Interchange
CRC cyclic redundancy check
B CRM consecutive reaction monitoring
b bit CSIA Compound Specific Isotope Analysis
B byte (8 b) <Ctrl> control key on the terminal keyboard
baud rate data transmission speed in events per second
D
BBOT 2,5-Bis 5-Tert-Butyl-Benzoxazol-2-Yl Thiophene
d depth
BEST Brightly Enhanced Sample Transfer
Da dalton
BF backflush
DAC digital-to-analog converter
C dc direct current
°C degrees Celsius driver A device-specific control program that enables a
computer to work with a particular device.
CE European conformity. Mandatory European marking
for certain product groups to indicate conformity with DS data system
essential health and safety requirements set out in
European Directives. DSP digital signal processor

cfm cubic feet per minute DSQ™ Dual Stage Quadrupole

CI chemical ionization

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) G-1
Glossary: Dual Inlet (DI)–ICP

Dual Inlet (DI) Inlet method in which a pure gas sample FWHM Full Width at Half Maximum
is admitted into an isotope ratio mass spectrometer
(IRMS) by a variable volume bellows. A reference gas is G
admitted into the IRMS via a second variable volume
bellows. The bellows are balanced to provide sample and g gram
reference signal responses of equal intensity.
G Gauss; giga (109)
E GC gas chromatograph; gas chromatography
EA Elemental Analyzer GC/MS gas chromatograph/mass spectrometer
EA-IRMS Elemental Analyzer Isotope Ratio Mass GFCI Ground Fault Circuit Interrupter: this term is
Spectrometry mainly used in North America. As a synonym, the term
Residual Current Device (RCD) is used in Europe.
ECD Electron Capture Detector
GISP Greenland Ice Sheet Precipitation. International
EI electron ionization
reference standard for hydrogen and oxygen isotopes.
Elemental Analyzer (EA) Automated sample preparation
See also SLAP and VSMOW.
instrument in which samples are automatically
converted into pure gases for isotope ratio analysis. An GLT Glass Lined Tubing
elemental analyzer contains the following elements: (i)
furnace for combustion, reduction or pyrolysis of sample GUI graphical user interface
material; (ii) chemical traps for analyte gas purification;
(iii) gas chromatography for time separation of these H
analyte gases.
h hour
EMBL European Molecular Biology Laboratory
h height
EMC Electromagnetic Compatibility
HF high flow
<Enter> Enter key on the terminal keyboard
HFCS High Fructose Corn Syrup
ESD electrostatic discharge
HOT OC High Oven Temperature Cold On-Column
ESI electrospray ionization
HPLC High Performance Liquid Chromatography.
eV electron volt Standalone liquid chromatography system (or inlet for
mass spectrometry detector).
F
HTC High Temperature Conversion
-15)
f femto (10
HV high voltage
°F degrees Fahrenheit
Hz hertz (cycles per second)
FID Flame Ionization Detector
I
FM flow meter

forepump The pump that evacuates the foreline. A IAEA International Atomic Energy Agency
rotary-vane pump is a type of forepump. ICIS™ Interactive Chemical Information System
ft foot ICL™ Instrument Control Language™
FTP file transfer protocol ICP inductively coupled plasma

G-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Glossary: ICP-OES–Natural Abundance

ICP-OES inductively coupled plasma optical emission log file A text file, with a .log file extension, that is used
spectroscopy to store lists of information.

ID inside diameter LVSL Large Volume Splitless Injector

IEC International Electrotechnical Commission m micro (10-6)

IEEE Institute of Electrical and Electronics Engineers


M
in. inch
m meter
I/O input/output
m milli (10-3)
ion optics Focuses and transmits ions from the ion source
to the mass analyzer. M mega (106)

ion source A device that converts samples to gas-phase M+ molecular ion


ions.
MB Megabyte (1048576 bytes)
irm isotope ratio monitoring
MCD Microchannel Device
IRMS Isotope Ratio Mass Spectrometer
MH+ protonated molecular ion
K min minute

k kilo (103, 1000) mL milliliter

K kilo (210, 1024) mm millimeter


KEGG Kyoto Encyclopedia of Genes and Genomes MP measuring point
kg kilogram MS mass spectrometer; mass spectrometry

L MS MSn power: where n = 1

MS/MS MSn power: where n = 2


l length

L liter MSn MSn power: where n = 1 through 10

LAN local area network MSDS Material Safety Data Sheet

lb pound MTBE methyl tert-butyl ether

LC Liquid chromatography. A process that separates a MVFC multifunctional valve cluster


chemical mixture carried by liquid into components as a
m/z Mass-to-charge ratio. An abbreviation used to denote
result of differential distribution of the solutes as they
the quantity formed by dividing the mass of an ion (in
flow around or over a stationary or solid phase.
u) by the number of charges carried by the ion.
LC/MS liquid chromatograph / mass spectrometer For example, for the ion C7H72+, m/z=45.5.

LED light-emitting diode


N
LF low flow
n nano (10-9)
LN2 liquid nitrogen
Natural Abundance The concentration of isotopes as
found in nature.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) G-3
Glossary: NCBI–SLAP

NCBI National Center for Biotechnology Information R


(USA)
RAM random access memory
NIST National Institute of Standards and Technology
(USA) RCD Residual Current Device: this term is mainly used
in Europe. As a synonym, the term Ground Fault
noise Any random disturbance that obscures the clarity of Circuit Interrupter (GFCI) is used in North America.
a signal
relative standard deviation A measure of the dispersion
NPD nitrogen/phosphorous detector of a group of measurements relative to the mean of the
group. Relative standard deviation is expressed as a
O percentage of the average value. The percent relative
standard deviation is calculated as:
OC On-Column
SD
% RSD = 100  -------
OD outside diameter x
where SD is the standard deviation and is the
OS open split
sample mean.
W ohm
RF radio frequency
outlier A calibration data point that does not appear to
correlate to other calibration data points within RMS root mean square
experimental error.
RoHS Restriction of Hazardous Substances. EU directive
on the restriction of the use of certain hazardous
P substances in electrical and electronic equipment.

p pico (10-12) ROM read-only memory


Pa pascal rotary-vane pump A mechanical vacuum pump that
creates the vacuum necessary for the proper operation of
PCB printed circuit board the turbomolecular pump. Also called roughing pump
PDD Pulsed Discharge Detector or forepump.

PE protective earth RS-232 An accepted industry standard for serial


communication connections. This Recommended
PEEK polyether ether ketone Standard (RS) defines the specific lines and signal
characteristics used by serial communications controllers
PID proportional/integral/differential to standardize the transmission of serial data between
devices.
P/N part number

P/P peak-to-peak voltage S


PPE personal protective equipment s second

ppm parts per million serial port An input/output location (channel) for serial
data transmission.
psig pounds per square inch, gauge
SIM selected ion monitoring
PU polyurethane
SLAP Standard Light Antarctic Precipitation;
PTV Programmable Temperature Vaporizing international reference standard for hydrogen and
oxygen isotopes.

G-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Glossary: SPME–WEEE

See also VSMOW. U


SPME Solid Phase Micro Extraction u atomic mass unit
SRM selected reaction monitoring UHV ultra high vacuum
SS stainless steel
V
SSL Split/Splitless
V volt
standard deviation In statistics, the standard deviation
SD is a measure of the dispersion of a group of V AC volts alternating current
measurements. For example, masses, times, or
intensities. Standard deviation is calculated as follows: V DC volts direct current

VFC voltage-frequency converter


n

  xi – x 
2
vol volume
 = SD = i=1
---------------------------
-
n–1 VCDT Vienna Canyon Diablo Troilite; international
reference standard for sulfur isotopes.
See also relative standard deviation.
VPDB Vienna Pee Dee Belemnite; international reference
T standard for carbon and oxygen isotopes.

TCD Thermal Conductivity Detector VSMOW Vienna Standard Mean Ocean Water;
international reference standard for hydrogen and
TCP/IP transmission control protocol / Internet protocol oxygen isotopes.

TIC total ion current See also SLAP.

Torr A unit of pressure, equal to 1 mm of mercury and


133.32 Pa. W

turbomolecular pump A vacuum pump that provides a w width


high vacuum for the mass spectrometer and detector
W watt
system.
WEEE European Union Waste Electrical and Electronic
Equipment Directive. Provides guidelines for disposal of
electronic waste.

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) G-5
Glossary: WEEE–WEEE

G-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
I
Index
A signal calibration 6-63
box current 3-46
Absolute Sensitivity 8-3
testing 8-5
Abundance 8-5
sources of error 8-6 C
testing 8-6 calibration 6-29
Accessories toolbar 7-3 capillaries
acquisition access 9-40
start 7-9 adjustment 9-46
adjustment of potentials 6-37 replacement 9-45
Advanced mode 7-27 throughput 9-41
configuring a sequence 7-34 throughput via blinds 9-41
configuring events 7-32 throughput via guide tube 9-42
Device Editor 7-29 cathode unit
modification of a device 7-30 replacement 9-14
monitoring parameters 7-36 Changeover extension 4-12
setting system start values 7-36 switching positions 7-22
air conditioning system 6-5 Changeover valve 4-8
amplifier 3-55 in Dual Inlet measurement 7-20
amplifier area maintenance 9-55 layout 4-8
amplifier arrangement 3-33, 3-57–3-58 switching positions 7-19
amplifier assignment to cups 3-34 check valve 3-36
amplifier housing 3-58 checking performance data 8-2
evacuation with evacuated analyzer 9-57 cleaning rules 9-6
evacuation with vented analyzer 9-57 cleaning vacuum components 9-22
venting 9-57 collector arrangement 3-51
Amplifier Test 8-6 collector systems 3-48
analyzer 3-39 combined multiport microvolume measurement 7-24
turbomolecular pump 3-37 compressed air connection 3-16
analyzer block 3-40 compressed air distributor 4-8
analyzer cabinet 3-35 Compression Factor 8-7
analyzer heater 3-42 configuration
auto focusing 6-70 creation 6-25
Autocool Refill device 4-19 connection to computer 6-13
automated refill operation 9-35 connection to peripherals 6-13, 9-38
checking liquid nitrogen evaporation rate 9-33
contaminations 9-21
maintenance 9-33
Continuous Flow measurement
working principle 4-20
gases 6-4
Autocool Unit 4-17
introduction of gas 6-32
position 3-31
control panel 3-6
safety instructions 5-13
LEDs 3-7
crimp adjustment 6-60, 9-24
cup settings 6-18
B
baking 9-7
bellows D
calibration 6-61
data system
hardware calibration 6-62
dimensions 6-11–6-12
pressure adjust 6-65

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) I-1
Index: E–I

placing 6-11 G
workbench 6-11
gas configuration
Declaration of Conformity A-4
creation 6-20
Delta V Advantage vs. Delta V Plus 3-3
Gas Configuration Editor 6-19–6-20
Dewar vessel
gas requirements
filling 9-35
argon 6-4
maintenance 9-34
compressed air 6-5
Diagnosis parameters 8-2
gas supply 6-3
Dual Inlet board 3-28
ground bolt 3-64
Dual Inlet measurement
grounding 3-63
gas samples 6-4
grounding cable 3-11
introduction of gas 6-33
scheme 7-21
shot noise limits of precision 7-21
Dual Inlet system 4-1 H
additional valve 3-26 H3 factor
layout 4-2 determination 7-13
maintenance 9-24 method 7-14
operation 7-18 sequence 7-16
solenoid valves 4-7 starting acquisition 7-16
turbomolecular pump 3-21 HD collector 3-52
valve blocks 4-6
Health and Safety Form 9-58, A-5
valves 4-5
heat removal 3-25
working principle 4-4
high amplification 3-57
Dual Inlet system cabinet 3-19
humidity 6-6
HVDAC scan 6-36
hydrogen measurement 7-13
E
electric safety precautions 5-9
electromagnet 3-59 I
electronic components for data acquisition 3-63
IEC power sockets 3-14
electronic offset 6-59
inspection- and servicing plan 9-4
electronics cabinet 3-60
instrument 3-2
emergency 5-11
front panel 3-4
Ethernet 6-11 rear panel 3-12
exhaust fume 6-6 right side panel 3-19
exhaust gas removal 3-25 safety symbols 5-3
side panels 3-5
intended use 5-7
F ion detection system 3-49
Faraday collector cup 3-49 ion generation 3-45
FCC Compliance Statement A-2 ion source 3-43
access 9-9
fill level controller 4-20
check 9-18
focus parameter values 6-68, 6-70
cleaning 9-16
Focus Quad power supply board 3-60
dismounting 9-9
focus settings 6-66 maintenance 9-8
fore vacuum pumps 3-23 reinsertion 9-12
movable tray 3-24 ion source cabinet 3-32
fused silica capillaries ion source heater 6-28
maintenance 9-39
ion source heaters 9-17
fuses 3-14
ion source potentials 3-47
Isodat 7-2
Cup Settings window 3-56
Dual Inlet panel 6-35

I-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Index: J–R

Focus Delta panel 3-45 O


very first start 6-17
oil
Isodat Generic Editor 7-6, 7-38
level check 9-19
replacement 9-20
Operating Manual
J safety symbols 5-2
jump calibration 6-48 signal words 5-2
optical fibers 3-17
optional hardware components 6-17
optional system components 2-2
L
laboratory conditions 6-2
laboratory temperature 6-5
leak detection 9-20
P
fore vacuum section 9-21 pacemakers 5-10
mass spectrometer 9-21 peak center offset 6-57
lenses 3-47 peak center principle 6-36
Linearity 8-7 peak center scan 6-52
sources of error 8-7 Peak Flatness 8-8
liquid nitrogen 9-34 peak shape scan 6-50
liquid nitrogen refill tube 4-20 Penning gauge
adjustment of set point 9-53
cleaning 9-51
disconnection 9-51
M maintenance 9-50
magnet calibration 6-39 measurement points 9-52
magnetic fields 6-7 putting into operation again 9-50
main switch 3-14 permitted materials 5-8
manual focusing 6-71 personal protective equipment (PPE) 5-13
mass calibration 6-41 plug and measure concept 3-9, 3-11
measuring channel 3-48 pneumatic valve
medical implants 5-10 disassembly 9-26
MEMCO collector 3-48, 3-51 operatiion 4-10
method creation 7-6 reassembly 9-28
Microvolume 4-15 reinsertion into valve block 9-31
cabinet 3-29 replacement 9-25
position 3-31 power cable 3-16
Multiport 4-12 power distribution board (power distributor) 3-61
dismantling 4-13 power sockets 3-30
power supply 3-61, 6-2
power supply panel 3-13
pressure reducer 3-22, 9-23
N adjusting pressure 9-23
needle valve oil reservoir 9-23
bakeout 9-39 protective earth connector (PE connector) 3-18
heater removal 9-36
pumping system 6-12
leak 9-37
maintenance 9-35
nickel capillaries 4-11, 9-47
bakeout 9-48 Q
crimping 9-49 qualification of personnel 5-8
cutting 9-48
handling 9-47
installation 9-48
R
radio frequencies 6-7

Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) I-3
Index: S–W

rating plate 5-6 system preparation 6-7


ratio groups 6-24 System Stability 8-11
Reference Refill 4-14
parameters 7-26
process 7-26
T
Relative Sensitivity 8-8
sources of error 8-9 technical data 1-vii
reset 6-74 Thermo Fisher Scientific service 9-58
residual hazards 5-12 third party manuals 1-5
Resolution 8-9 three-way valve 3-36
10% valley definition 8-9 maintenance 9-55
results trap current 3-46
applying an export template 7-51 TubeCracker 4-14
calculation 7-44 tubings
creating an export template 7-47 insertion 9-23
export 7-46 removal 9-23
raw data 7-42 turbomolecular pump 3-38
recalculation 7-45
representation of data 7-41
saving an export template 7-51
viewing 7-40, 7-43
U
Universal CNOSH detector 3-52
Universal Triple collector 3-48, 3-50
user-tailored collector 3-48
S
scope of delivery 2-1
sequence creation 7-9
setting the magnet 6-39
V
shutdown 7-5 vacuum check 6-30
Signal Stability 8-11 vacuum system maintenance 9-19–9-20
sources of error 8-11 Version Handler 6-15
stainless steel capillaries 4-10 vibration 6-6
bakeout 9-42 Viton gaskets 9-22
maintenance 9-39 voltage to frequency converter (VFC) 3-55
standard system components 2-2
starting the system 7-4
SUB D connectors 3-18 W
susceptibility to electromagnetic transmissions 5-7
WEEE Compliance Statement A-3

I-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific

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