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Delta V Series - Operating Manual
Delta V Series - Operating Manual
Operating Manual
Operating Manual
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.
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Fisher Scientific Inc.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) iii
Contents
Index......................................................................................... I-1
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.
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
Contents
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).
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.
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:
• For brevity, expressions such as “choose File > Directories” are used
rather than “pull down the File menu and choose Directories.”
• 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
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:
This manual lists part numbers of key consumables and spare part
items for the instrument.
You can access PDF files of the documents listed above and of this
manual from the data system computer or other electronic storage
devices.
1-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Using this Manual
Reference Documentation
• Forepump
• Turbomolecular pumps
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.
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
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 2-1
Scope of Delivery
Standard System Components
• Turbomolecular pump
• Printed manuals
- Delta V Series Operating Manual
• Multiport
• Microvolume
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
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.
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
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
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.
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.
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
The Vacuum status LED (1 in Figure 3-3) indicates the quality of the
vacuum.
The Main status LED 3 indicates the status of the main pump (analyzer
turbomolecular pump).
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 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 pumps are off or have not yet reached their final
number of revolutions.
Yellow The Penning gauge is on and works properly.
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.
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).
3-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Plug and Measure Concept
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).
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 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
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
The grounding is not necessary for peripheral devices that already run
with a new cable (for example, PreCon device, GP interface).
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.
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
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
2
15A
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.
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
After your computer and the IRMS peripherals have been connected,
switch on the according fuses to operate the devices.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-15
System Description
Connections at the Rear Panel
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.
Compressed Air
3-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Connections at the Rear Panel
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-17
System Description
Connections at the Rear Panel
SUB D Connectors
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
3-18 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet
1
2
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
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
4
1
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-21
System Description
Right Side and Dual Inlet System Cabinet
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
2
6
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.
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
If no Dual Inlet system is available, the fore vacuum pump of the Dual
Inlet system is not installed.
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.
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.
3-24 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Right Side and Dual Inlet System Cabinet
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.
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
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
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 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.
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
The Dual Inlet board controls the Dual Inlet system and options (for
example, a Multiport or a Microvolume). It has the following functions:
Figure 3-25 shows the bellow motors connected to connectors J 205 and
J 206.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-29
System Description
Microvolume Cabinet
The activated sockets are controlled only as groups (as entire shelves of
six, two or two sockets) by the Instrument Control of Isodat.
The activated sockets (1, 3 and 4 in Figure 3-27) provide three groups of
heaters (and/or heatable valves) with energy.
3-30 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Microvolume Cabinet
Make sure that the corresponding button for the socket is activated in
Isodat as well, if you switch on the socket.
3
1
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.
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
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.
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.
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.
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
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.
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.
3-36 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet
• 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.
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.
3-38 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet
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.
Analyzer
Figure 3-37 schematically shows the 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.
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
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°.
m = k H2
---- M
z
with
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-41
System Description
Analyzer Cabinet
m
------- = 110 (10% valley)
m
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.
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
Figure 3-41 shows the aperture of the Delta V instrument with the
turbomolecular pump of the analyzer removed.
3-44 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Analyzer Cabinet
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-45
System Description
Analyzer Cabinet
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).
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.
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.
X-Deflection
Y-Deflection
Extraction
X-Focus
Box
Slit
COM = BDAC
+200..+500 V
COM..-400 V
COM..-400 V
0..+100 V
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-47
System Description
Analyzer Cabinet
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
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.
44 2
45 3
Digital Signal
46 4 Processor (DSP) computer
3 5
8
In the same manner for cup 9 and 10
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).
collector slit
ions
to amplifier
secondary electron
suppression shield
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
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.
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.
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
Figure 3-49 shows collector arrangements for different masses for the
Delta V Advantage and the Delta V Plus instrument.
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
m/z 3 (HD)
m/z 2 (H2)
HD Collector 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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-53
System Description
Analyzer Cabinet
7 6 8
3 9
10
4
1
5
2
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
7 9
6 10
13 8 7
9
6
10
12
12 1 1
2 5
11
3 4
5 2
11
4 3
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
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 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.
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 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.
A right-click on the mass value opens the context menu. Selecting High
Amplification activates/deactivates the second amplifier.
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.
Figure 3-58 shows how several amplifiers are arranged in slots. The
visible green board is amplifier ground plane.
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.
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.
3-60 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Electronics Cabinet
• 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.
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.
• Refill equipment
• Analyzer heater
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-61
System Description
Electronics Cabinet
3-62 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Description
Electronics Cabinet
PCI Fiberline
PC Bus Master
Dual Inlet Board
Power Distribution
Board
Inlet Board
Ion Source
GND Level
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 3-63
System Description
Electronics Cabinet
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-1
Dual Inlet System (Optional)
Layout of the 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.
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.
7
3
4
5
6
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.
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
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.
4-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Valves of the Dual Inlet System
Parts of a Valve
Figure 4-3 shows a pneumatic valve with its high-vacuum side opened.
6
1
5 2
4 3
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.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-7
Dual Inlet System (Optional)
Compressed Air Distributor
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.
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.
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“.
1
2
6
3
5 4
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 4-9
Dual Inlet System (Optional)
Changeover Valve
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.
4 3 2 1
4-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Changeover Valve
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.
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.
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.
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).
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
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.
3 1
Labeled Components: 1=Swagelok™ connector (2 ×), 2=compressed air connection, 3=connecting piece
Figure 4-14. TubeCracker tool
4-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Dual Inlet System (Optional)
Microvolume
3 4
to inlet port
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.
4 5
3
2
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.
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.
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.
3
7
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
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.
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
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
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.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-1
Safety
Safety Symbols and Signal Words in This Manual
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.
5-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Safety Symbols on the Instrument
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-3
Safety
Safety Symbols on the Instrument
5-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Safety
Safety Symbols on the Instrument
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-7
Safety
Intended Use
• 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:
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.
• solvents
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-9
Safety
Safety Instructions for Wearers of Medical Implants
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
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.
1. At the rear panel of the Delta V Series mass spectrometer, turn the
main switch to the Off position. See Figure 5-2.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-11
Safety
Residual Hazards
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.
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.
NOTICE Make sure that only authorized and fully trained operators use this
equipment and that they are fully familiar with these safety notes.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 5-13
Safety
Residual Hazards
Gloves
5-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
6
System Setup
Contents
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
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.
NOTICE A single-phase auxiliary wall outlet must use the same ground as the
instrument.
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
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
6-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Laboratory Conditions
Compressed Air
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.
Temperature
For optimum performance, the instrument should be located in an
air-conditioned room.
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.
6-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation
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.
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
6-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation
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
NOTICE Do not move Delta V Series instruments with any pump turned on.
Remove the belt after transport and before operation is started again.
Before moving the tray with the fore vacuum pumps, remove their
connectors.
6-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation
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.
monitor
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)
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
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.
6-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
System Preparation
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.
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-13
System Setup
Creating an Isodat Backup
backup files
Version Handler
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.
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System Setup
Creating an Isodat Backup
The Version Handler appears listing prior backups. See Figure 6-9.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-15
System Setup
Creating an Isodat Backup
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System Setup
Starting Isodat the Very First Time
Tip Figure 6-12 only appears when starting the system the very
first time, or after a reset of the Delta V Series instrument.
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.
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.
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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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-19
System Setup
Creating a Gas Configuration
The Gas Configuration Editor (Figure 6-17) can be opened from the
Isodat Instrument Control or Isodat Acquisition.
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.
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System Setup
Creating a Gas Configuration
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-21
System Setup
Creating a Gas Configuration
8. Click Yes.
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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.
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.
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.
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.
16. Select the calibration which is valid for the selected cups.
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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.
5. Select Edit > Add Configuration or click this icon to add a new
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.
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.
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System Setup
Creating a Configuration
Figure 6-30 shows the peripheral set added to the Capillary port.
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.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-29
System Setup
Calibrating and Adjusting the System
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System Setup
Calibrating and Adjusting the System
1
2
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-31
System Setup
Calibrating and Adjusting the System
9. Monitor the High Vacuum signal for intermittent spikes and for its
absolute value.
1. Ensure that:
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System Setup
Calibrating and Adjusting the System
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.
7. Wait a few minutes. Monitor the high vacuum level. Perform a time
scan (high vacuum vs. time).
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-33
System Setup
Calibrating and Adjusting the System
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.
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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
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.
9. Introduce the gas into the tubing by successively filling the tubing,
the feed lines and the bellows with gas from the gas reservoir:
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-35
System Setup
Calibrating and Adjusting the System
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.
12. If you do not obtain this pattern, or if an error occurs during peak
center, perform a calibration using CO2.
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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System Setup
Calibrating and Adjusting the System
Figure 6-40 shows the buttons on the Accessories toolbar that are
relevant for high voltage.
2
3
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-37
System Setup
Calibrating and Adjusting the System
Alternatively, after a longer time, the source may have become dirty
and must be dismantled, cleaned and finally reinserted.
2. To turn on the ion source, click this icon. See Figure 6-39.
6. Admit gas into the inlet system. Admit a sufficient amount of gas
into the ion source.
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System Setup
Calibrating and Adjusting the System
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.
In the Set Mass dialog, enter the desired mass to be focused on that
cup (‘44’, for example). See Figure 6-44.
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
❖ To perform a calibration
2. On the right side of the Scan window, select Slow Magnet from the
drop-down list.
3. Click the Start Scan button to start the Magnetic Field scan with
standard parameters. See Figure 6-46.
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.
6-40 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
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:
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.
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.
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.
6-42 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System
5. Click Yes.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-43
System Setup
Calibrating and Adjusting the System
6-44 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
System Setup
Calibrating and Adjusting the System
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.
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.
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System Setup
Calibrating and Adjusting the System
19. Click the Save button in the system bar to save the calibration.
20. Enter the file name for the calibration. See Figure 6-55.
The calibration is saved. This file is not used for mass identification. It
can be used for mass re-calibration, if necessary.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-47
System Setup
Calibrating and Adjusting the System
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System Setup
Calibrating and Adjusting the System
6. Click OK.
9. Click Yes.
The peak center scan starts. See “Peak Center Scan” on page 6-52.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-49
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.
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System Setup
Calibrating and Adjusting the System
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-51
System Setup
Calibrating and Adjusting the System
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.
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System Setup
Calibrating and Adjusting the System
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-53
System Setup
Calibrating and Adjusting the System
7. In the Scan Basic window, click the double arrows next to High
Voltage. See Figure 6-70.
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System Setup
Calibrating and Adjusting the System
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:
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-55
System Setup
Calibrating and Adjusting the System
The result values of the peak center scan are displayed in the
Information window as well. See Figure 6-73.
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System Setup
Calibrating and Adjusting the System
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-57
System Setup
Calibrating and Adjusting the System
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.
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System Setup
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-59
System Setup
Calibrating and Adjusting the System
Crimp Adjustment
Crimp adjustment is only important, if a Dual Inlet system is available.
See also “Crimp Adjustment” on page 9-24.
2. Open the valves that connect the two bellows of the Dual Inlet
system. See Figure 6-81.
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System Setup
Calibrating and Adjusting the System
3. Evacuate the Dual Inlet system using the fore vacuum and high
vacuum pumps.
7. Carefully adjust the crimps. The 10 mbar for CO2 must yield 2 V
on mass 44.
To operate the bellows for the first time, perform a hardware calibration.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-61
System Setup
Calibrating and Adjusting the System
4. Click OK.
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Calibrating and Adjusting the System
5. Click Yes.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-63
System Setup
Calibrating and Adjusting the System
6. Click OK.
In the Set Volume Control window, enter the desired volume ratio
in %. See Figure 6-89.
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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.
Pressure Adjustment
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-65
System Setup
Calibrating and Adjusting the System
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Calibrating and Adjusting the System
The parameters shown in the Focus Delta window are assigned to the
current gas configuration. See Figure 6-91.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-67
System Setup
Calibrating and Adjusting the System
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.
Each focus parameter value of the Focus Delta panel can be adjusted
manually:
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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.
Trap
Electron Energy
Extraction
Extraction Sym.
X-Focus
X-Focus Sym.
Y-Deflection
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-69
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Calibrating and Adjusting the System
Y-Deflection Sym.
SE-Suppression
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
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Resetting the Mass Spectrometer
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).
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 6-73
System Setup
Resetting the Mass Spectrometer
4. To continue the reset, see “Starting Isodat the Very First Time” on
page 6-17.
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7
Operation
Contents
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-1
Operation
Safety Guidelines for Operation
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 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.
7-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Isodat Software Suite
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.
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.
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).
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.
Tip In case the system will not be used for several weeks or months,
Thermo Fisher Scientific recommends only switching off the ion
source.
4. Switch off the pumps at the control panel. See 4 and 5 in Figure 3-3.
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
Before creating a method, you must already have performed the steps
described in the following sections:
7-6 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Creating a New Method
6. Confirm by OK.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-7
Operation
Creating a New Method
Tip The example values and parameters in the tabs of the new
method can usually be accepted.
7-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Creating a New Sequence and Starting Acquisition
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
4. Define the number of samples (3, for example) and click OK. See
Figure 7-6.
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.
Click the table cells of the desired rows to activate the cell. The
green check mark is shown when activated.
11. Select an IRMS method for each sample (H3-Delta V-H2.met, for
example).
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-11
Operation
Creating a New Sequence and Starting Acquisition
7-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
²H/¹H Measurements
²H/¹H Measurements
This section describes 2H/1H measurements and their requirements.
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:
k: H3 factor
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
6. Click OK.
7-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
²H/¹H Measurements
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.
For all other settings, the default values can typically be accepted.
4. Click OK.
7-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
²H/¹H Measurements
6. In the Method column, select the appropriate IRMS method for the
H3 factor determination from the drop-down list. See Figure 7-15.
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
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 %.
1 2 3
• 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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-19
Operation
Dual Inlet System
The second time that can be adjusted is the idle time in the Peripherals
tab. See Figure 7-20.
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
Idle Time
Measure
Integration Time
No
Cycles?
0.015
0.01
0.005
0
0 2 4 6 8 10 12 14
Amplitude
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-21
Operation
Dual Inlet System
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.
1 2
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-23
Operation
Dual Inlet System
7-24 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Dual Inlet System
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
Gas Transfer
p < μVBank Bank to
p > μVAll Microvolume
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.
Standard Bellows to
100%
Switch off
Pump Line and Pump Overlay Time Reference Bottle
Capillary
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
The Change into Advanced mode window opens. See Figure 7-30.
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
5. In the upper left corner of the pane, right-click the icon of your mass
spectrometer.
6. Click Edit.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-29
Operation
Editing a Configuration in Advanced Mode
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
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-31
Operation
Editing a Configuration in Advanced Mode
Events Tab
❖ To configure events for a hardware component
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.
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.
Sequence Tab
❖ To configure sequence for a hardware component
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-35
Operation
Editing a Configuration in Advanced Mode
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.
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.
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.
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.
2. Select File > Open, or click the Open button in the upper left
corner.
7-38 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Editing a Configuration in Advanced Mode
4. Click Open.
The file opens in the Isodat Generic Editor. The system shutdown
parameters are shown. See Figure 7-44.
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.
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
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.
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
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.
The value is calculated from the element delta and the corresponding absolute
element ratio of the standard.
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.
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.
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.
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.
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.
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).
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).
7-46 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results
3. In the File New dialog, select Data Export to create a new export
template. See Figure 7-54.
4. Click OK.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-47
Operation
Exporting Results
5. Select the check boxes for the data you want to include in the export
file:
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-49
Operation
Exporting Results
9. In the Insert Identifier dialog, enter a name for the column. See
Figure 7-57.
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.
7-50 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results
2. In the field File name, enter a name for the export template.
3. Click Save.
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.
5. Click Add.
7-52 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Operation
Exporting Results
The selected export template appears in the list. See Figure 7-64.
8. Click OK to confirm.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 7-53
Operation
Exporting Results
The options specified in the sequence are set. Data acquisition starts.
7-54 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
8
Troubleshooting
Contents
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-1
Troubleshooting
Checking Performance Data
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.
8-2 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Troubleshooting
Absolute Sensitivity
3 × 10-3 3 × 10-3
(Continuous Flow (Continuous Flow
applications) applications)
System Stability 10 ppm 10 ppm
Absolute Sensitivity
Tip Testing Absolute Sensitivity requires a Dual Inlet system.
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
Ionization
- + -
AB + e AB + 2e
n gas
AS = ------------
-
n ion
where:
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
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).
Abundance
Tip Testing Abundance requires a Dual Inlet system.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-5
Troubleshooting
Amplifier Test
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.
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.
Int end
Comp = ---------------
-
Int start
where:
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.
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:
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
Sources of Error
• Resistor values are not configured properly.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-9
Troubleshooting
Resolution
or as:
m
R = --------
m
where:
R Resolution
m Mass of the respective isotope
m Mass difference between neighboring peaks
m a
R = -------- --
m b
where:
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.
Sources of Error
• The slope is usually due to gas consumption during measurement.
However, it should be checked, if an unusual result is obtained.
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:
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 8-11
Troubleshooting
System Stability
8-12 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
9
Maintenance
Contents
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-1
Maintenance
Safety Guidelines for Maintenance
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.
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.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-3
Maintenance
Inspection- and Servicing Plan
9-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Inspection- and Servicing Plan
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-5
Maintenance
Basic Rules for Cleaning
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.
❖ To clean parts
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.
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.
7. To avoid any damage to the skin, rub your fingertips over with a
fatty skin cream when the work is completed.
If the system has been vented (after exchanging parts, for example),
baking removes traces of intruded moisture and water.
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.
9-8 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source
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.
Figure 9-3 shows the connections of the ion source to the ion source
connector board.
2
1
8
5
7 6
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.
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.
The turbomolecular pump of the Dual Inlet system can be left on.
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.
9-10 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source
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.
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
3
1
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
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.
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-13
Maintenance
Ion Source
8. Perform the ion source check. See “Checking the Ion Source” on
page 9-18.
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.
9-14 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source
6
1
7. Carefully insert the new filament carrier along the guide tracks for
up/down. See arrows in Figure 9-8.
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
11. Reinsert the ion source as described at “Reinserting the Ion Source”
on page 9-12.
9-16 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Ion Source
NOTICE Do not use an ultrasonic bath when cleaning the ion source
magnet.
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.
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.
Tip If the halogen lamps are loosely fitted, carefully press their
spring contacts together using small pliers.
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.
• Fore vacuum pump of the Dual Inlet system (rotary vane pump
DUO 2.5)
The turbomolecular pumps are accessible from the left side, and the fore
vacuum pumps from the right side.
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.
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).
❖ To replace oil
1. Before you empty and replace old oil, vent the fore vacuum pumps.
Vacuum System
The main reasons for problems with the vacuum system are leaks and
contaminations.
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.
9-20 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Vacuum System
• Leak detection in the fore vacuum section (if the pressure is too
high for IRMS operation).
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.
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:
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.
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.
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
❖ 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).
1. Open the door at the right side of the Delta V Series instrument to
access to the pressure reducer for compressed air.
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.
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.
2. Push the tubings into the tubing connections until limit stop.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-23
Maintenance
Dual Inlet System
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.
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).
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
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
1. Isolate the pneumatic valve from its pneumatic valve block as shown
in Figure 9-12.
Take care not to scratch the metallic knob with the flat-nose pliers.
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
a. Insert the two tips of the spreader forceps into the two holes 2 of
the circlip.
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
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
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.
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
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.
3
1
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.
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.
a b c
d. Use the spreader forceps to insert the circlip exactly into the
groove of the piston. See arrow in Figure 9-22.
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.
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.
1. As Figure 9-25 shows, insert the pneumatic valve 1 upon the valve
block 2.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-31
Maintenance
Replacing a 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
9-32 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Autocool Refill Device
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.
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.
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
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.
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.
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
1. Make sure that all pipe connections leading to the Dewar vessel of
the Autocool Unit are correctly installed.
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.
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.
For maintaining the stainless steel on/off valve SMOV-1, refer to SGE’s
documentation at www.sge.com.
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
5 3
The cable 6 connects the heater 5 and the activated sockets in the
Microvolume cabinet.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-37
Maintenance
Needle Valves
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.
to Changeover valve
to ion source
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.
2. In the Source Heater panel, click the Inlet Valve Heater button to
switch on the heater. See Figure 6-31.
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:
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.
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.
2. Remove the two screws located on the left and right side.
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
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.
• 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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-41
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries
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.
Within the guide tube, capillaries can be led out towards the external
peripherals. The guide tube inhibits contact between capillaries and
electronics.
9-42 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries
The heating process can be regulated with Isodat: ISL scripts can be
used to create time programs for it.
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).
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-43
Maintenance
Stainless Steel Capillaries and Fused Silica Capillaries
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.
An electric current flows from the brass contact in the center of the
capillary to both ends and bakes it out.
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.
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.
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
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.
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.
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).
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.
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-47
Maintenance
Nickel Capillaries
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.
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.
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.
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 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.
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.
1. Pull away its electronics cylinder (without venting the system). See
Figure 9-38.
9-50 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
Maintenance
Penning Gauge
3. Alternatively, let slightly more gas flow into the ion source to start
the Penning gauge again.
WARNING High Voltage. Risk of injury. High voltages about 3 kV are generated
inside the Penning gauge. Disconnect the Penning gauge.
1
9
8
2
3
4
5
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) 9-51
Maintenance
Penning Gauge
6. Clean the body tube as described at “To clean the body tube” on
page 9-52.
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.
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.
4 3
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.
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
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.
NOTICE Neither touch an amplifier nor its electronic parts (resistors, for
example). This electronic equipment is highly sensitive.
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.
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
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.
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.
4. 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
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.
9-58 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific
A
Legal Documents
Contents
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) A-1
Legal Documents
FCC Compliance Statement
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:
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
Part Number Quantity Material Description Error Description / Reason for Return Return Part Serial No
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
a)
b)
c)
d)
e)
f)
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.
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
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 ampere cm centimeter
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.
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) G-3
Glossary: NCBI–SLAP
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
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.
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
Thermo Scientific Delta V Series Operating Manual (P/N 1174000, Revision E) I-3
Index: S–W
I-4 Delta V Series Operating Manual (P/N 1174000, Revision E) Thermo Scientific