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Control Number ZN5SQVE-00

Trace Elemental Analyzer


NSX-5000V

Operation Manual
For
Sulfur Measurement

CAUTION
To use the unit correctly, read this operation manual before use.
Keep the manual at hand.

Nittoseiko Analytech
Introduction 1

Introduction
Thank you for purchasing our Trace Elemental Analyzer Model NSX-5000V. This system
measures sulfur in samples using a vertical furnace.
This operation manual is for the Trace Elemental Analyzer Model NSX-5000V.
To use the unit efficiently and safely, read this operation manual and fully understand the
functions and the operation methods before use.
This operation manual describes preparation before starting the system and
measurement operations. It contains the description of simultaneous measurement of
nitrogen and sulfur that is performed by connecting the nitrogen detector ND-500.
The NSX-5000 system consists of an injector, an electric furnace, and a detector. These
units are combined according to each measurement. Read the instruction manuals of the
component units with care and perform measurement operation by following their
operation manuals.
Some unit combinations may not be supported. When changing the configuration of the
units, update the unit software and application software.

Before Use

Take care of the following points about this operation manual.

(1) Do not reprint this manual wholly or partially without permission.

(2) The contents may be changed without notice.

(3) Though this manual was prepared carefully, contact our local distributor when
mistakes, omissions, or missing pages are found.
The application software in this manual may be different depending on the version
of the software.

(4) For any consequences of used results, we do not take any responsibility regardless
of (3).

(5) Assign specific operators and supervisors when using this unit.

(6) Always follow the contents in this operation manual. When problems or damages
occur by neglecting the contents in this manual, we do not guarantee the system
even within the guarantee period.

Nittoseiko Analytech has the copyrights of this manual and the unit software.
Microsoft and Windows are registered trademarks of Microsoft Corporation.
Other company and product names are their trademarks and registered trademarks.

NSX-5000V
2 Introduction

About This Manual

About Composition

This operation manual is composed as follows.


 Section 1 : Preparation
 Section 2 : Basic Operations
 Section 3 : Advanced Operations

About Indications

The elements of windows are expressed as follows.


 The names of menus, windows, icons, and items are expressed with double
quotations marks. The button names are expressed with brackets.
Example: Click [OK].
Click “File”-“New”-“Folder” of the menu.
 Keyboard keys are expressed with angle brackets.
Example: Press <F5> key.
 The title of a reference chapter is expressed with double quotation marks.
Example: Refer to “3-1. Disconnection and Connection”.

The selection of a menu, button, or icon is expressed as follows.


Example: Click [OK].
Click “File”-“New”-“Folder” of the menu.

Refer to “SAFETY PRECAUTIONS” for the indication of warnings and cautions.

About Terms

The following terms are used in the manual.


 Application software: Software that operates the system from a PC
 Schedule: File that sets the contents and order of measurement and contains
results
 Method: File that sets parameters of each unit

NSX-5000V
SAFETY PRECAUTIONS 1

SAFETY PRECAUTIONS
To use this unit correctly, read this operation manual and the instruction manual of each
unit with care before use.
Always read safety precautions before use.
Security cannot be assured if the unit is operated without following the instructions in this
manual.
Keep this operation manual at hand.

Indication of Safety Precautions

This operation manual uses several indications to highlight critical precautions. The items
with these indications are important for the safe use of the unit. Always observe them.
The following indications are used for safety precautions.

WARNING
Information under this sign explains critical operations which the contain
risk of death or serious casualties caused by wrong handing.

CAUTION
Information under this sign explains critical operations which contain the
risk of human casualties or property damages caused by wrong handing.

Other Indications

Besides the safety precaution indications, this operation manual uses the following
indication to show an important or useful thing for measurement with this unit. The items
with this indication are important for the safe use of the unit. Be sure to read them before
use.

POINT
Information under this sign explains important items and tips for
measurement with this unit.

NSX-5000V
2 SAFETY PRECAUTIONS

Warnings and Cautions

Cautions

Read the following cautions carefully to use the unit correctly and safely.

WARNING Prohibition of unattended


operation
Do not use this unit without attendance at night or other situations.
The unit is designed for attended operation. If there is no one around when
an error occurs, appropriate measures cannot be taken promptly, which
may lead to a serious accident.

WARNING Combustibles and combustible


gas
Keep the system off the combustibles and combustible gas.
The electric furnace of the system is hot during operation. Do not let
combustibles contact directly with the electric furnace or combustible liquid
drop around it. Doing so may cause a fire.

WARNING Power plug


Do not touch the power plug with wet hands.
Failure to do so may lead to electric shock.

WARNING Power cable


Do not bundle the power cable or use it with physical force applied to it. Do
not heat the power cable.
A hot or broken power cable may lead to a fire or electric shock.
Do not use a power cable under the rating or modified or broken one.
Use a power cable based on our specification.

NSX-5000V
SAFETY PRECAUTIONS 3

WARNING Cables and connectors on the


rear of the unit
Do not touch the cables and connectors on the rear of the unit during use
of the unit.
Doing so may cause poor communication or a fire due to errors.

WARNING For protection


When handling chemicals, always wear protectors.
Failure to do so may lead to physical damage, such as chemical injury or
blindness. When handling chemicals, always check the safety data sheet
and wear protectors, such as safety goggles and safety gloves.

WARNING Gas Leak Check


Never check for gas leakage while the temperature of the electric furnace
is raised. Doing so may cause burns.
When gas flow is less than the preset value, gas may be leaking. If
measurement is performed in that state, a serious accident may result. Be
sure to check for gas leakage.

WARNING Hot electric furnace and


combustion tube
Do not touch a hot electric furnace and combustion tube.
Doing so may cause burns. Never touch them and its surroundings.

WARNING “WARNING” indication


When “WARNING” is displayed in the PC monitor, this indicates risk of
serious accidents.
When these messages are displayed, deal with the problems immediately.

NSX-5000V
4 SAFETY PRECAUTIONS

WARNING Microsyringe to use


Always use a microsyringe specified by us.
Failure to do so may break the microsyringe or cause a fire due to
abnormal combustion.

WARNING Measurement parameters and


unit condition
If the condition of the units is different from the measurement parameters
set by the application software, the units may be damaged and explosive
combustion may cause a fire.
Particularly, if the parameters of the injector are different, a serious
accident may result. Be sure to check measurement parameters and the
condition of the units before starting measurement.

WARNING Cooling of the electric furnace


Do not stop the power supply until the temperature of the electric furnace
drops to 300 degrees Celsius or lower because the electric furnace needs
to be cooled by the fan. Do not shut down the application software while
the electric furnace is hot. Doing so makes it impossible to check the
temperature of the electric furnace.

CAUTION Prevention of glass breakage


Combustion tube is glass. Handling it roughly may cause it to break.
Take care in handling.

CAUTION Combustion tube devitrification


When a combustion tube is devitrified, it may break due to lowered
mechanical strength.
The term "devitrification" refers to the condition of a combustion tube where
the color has turned white. When a combustion tube is devitrified,
especially when fine cracks are in the devitrified part, the mechanical
strength is low. Change it immediately with a new one.

NSX-5000V
SAFETY PRECAUTIONS 5

CAUTION Check of O-ring


When setting an O-ring, check that it is not damaged. If it is damaged,
change it immediately.

CAUTION Disconnection of lower line from


combustion tube outlet
Before platinum catalyst treatment, be sure to remove the female ball joint.
When a new platinum catalyst or a platinum catalyst that has not been
used for a long time is used, the moisture contained in the platinum catalyst
may ooze out. Place a beaker under the outlet of the combustion tube.
Platinum catalyst treatment may generate acid gas.

CAUTION Problems during measurement


If any problems occur during measurement, click the “Abort” icon in a PC
window to stop measurement and the unit. Suspended measurement
(step) can not be continued. Create a new step.
Resolve the cause of the problem and check that the unit is in proper
condition. Then, resume measurement.

CAUTION Maximum injection volume


The maximum injection volume of a sample is 200 µL.
Never inject a volume exceeding the maximum injection value.

CAUTION Error during continuous run


If an error occurs during continuous schedule run, the operation of the unit
stops, but the application software may not show that it is stopped.
If the application software is running the unit even when the unit is stopped
due to an error, click the “Cancel” icon to stop it and properly deal with the
error. Then, click the “Start” icon again.

NSX-5000V
6 SAFETY PRECAUTIONS

CAUTION Solvent for dilution


Select a solvent for dilution that easily dissolves the sample and has no
impact on measurement.
If a solvent that deposits or adheres as the result of mixing is selected, the
syringe or the ASC-550L unit may be damaged. In addition, if the solvent
has an impact on measurement, correct measurement results cannot be
shown.

CAUTION Cover of the unit


Do not remove the cover of the unit except for our servicemen.
Doing so may cause a fault or electric shock.

CAUTION Unit supervisors and operators


Assign specific operators and supervisors for the system.
The system needs to be installed and used with due care. The supervisors
should manage and supervise the operators of the system.

NSX-5000V
Table of Contents 1

Table of Contents

Introduction ...................................................................................................................... 1
Before Use ................................................................................................................ 1
About This Manual .................................................................................................... 2
About Composition ........................................................................................... 2
About Indications .............................................................................................. 2
About Terms ..................................................................................................... 2
SAFETY PRECAUTIONS ................................................................................................ 1
Indication of Safety Precautions ............................................................................... 1
Other Indications ....................................................................................................... 1
Warnings and Cautions............................................................................................. 2
Cautions............................................................................................................ 2
Section 1: Preparation ................................................................................................. 1-1
1-1. Unit Composition ........................................................................................... 1-1
1-2. Preparation of Combustion Tube ................................................................... 1-2
1-2-1. Washing of Combustion Tube ............................................................ 1-2
1-2-2. Preparation of Inner Combustion Tube ............................................... 1-3
1-2-3. Preparation of Outer Combustion Tube .............................................. 1-4
1-2-4. Assembly of Inner and Outer Combustion Tubes ............................... 1-5
1-3. Setting of Combustion Tube to Vertical Furnace ........................................... 1-5
1-4. Combustion Tube Outlet Connection ............................................................. 1-7
1-5. Platinum Catalyst Treatment of Outer Combustion Tube .............................. 1-7
Section 2: Basic Operations ........................................................................................ 2-1
2-1. Start Up ......................................................................................................... 2-1
2-1-1. Maintenance, Inspection, and Preliminary Preparation for Measurement
............................................................................................................ 2-1
2-1-2. Power and Gas Supply ....................................................................... 2-1
2-1-3. Start .................................................................................................... 2-1
2-1-4. Logon Window .................................................................................... 2-2
2-1-5. Mode Selection Window ..................................................................... 2-3
2-1-6. Logon and Connection ....................................................................... 2-4
2-2. Initial Window Composition ............................................................................ 2-4
2-3. Schedule and Method Preparation ................................................................ 2-6
2-3-1. Flow of Schedule Preparation in Advanced ........................................ 2-6

NSX-5000V
2 Table of Contents

2-3-2. Setup Window (Advanced) ................................................................ 2-7


2-3-3. New Method Preparation ................................................................... 2-8
2-3-4. New Schedule Preparation ................................................................ 2-9
2-3-5. Template Registration ...................................................................... 2-10
2-3-6. Schedule Preparation with Template (Advanced) ............................ 2-10
2-3-7. Setup Window (Simple) ................................................................... 2-12
2-3-8. Schedule Preparation (Simple) ........................................................ 2-13
2-4. Measurement Preparation .......................................................................... 2-14
2-4-1. System Window ............................................................................... 2-14
2-4-2. Measurement Preparation ............................................................... 2-15
2-4-3. Gas Leak Check .............................................................................. 2-15
Inspection When Gas is Leaking ........................................ 2-16
2-4-4. Measurement Window ..................................................................... 2-17
2-4-5. Parameter Check ............................................................................. 2-18
2-4-6. Vertical Furnace Parameter Settings ............................................... 2-19
2-4-7. Sulfur Detector Parameter Settings ................................................. 2-20
2-4-8. Rule Window .................................................................................... 2-20
2-4-9. Concentration Calculation ................................................................ 2-21
Absolute Amount Calculation for Calibration Curves ......... 2-21
Sample Concentration Calculation ..................................... 2-22
2-4-10. Step Editor Window ....................................................................... 2-22
2-4-11. ASC Program Setting Window ....................................................... 2-25
2-4-12. Settings for Blank Measurement .................................................... 2-26
2-4-13. Standard Measurement Setting ..................................................... 2-26
2-4-14. Sample Measurement Setting........................................................ 2-27
2-4-15. Injection Status Check ................................................................... 2-28
2-5. Measurement Operations ........................................................................... 2-29
2-6. Results ........................................................................................................ 2-31
2-6-1. Result Window ................................................................................. 2-31
2-6-2. Blank Results Window ...................................................................... 2-33
2-6-3. Calibration Results Window ............................................................. 2-34
Calibration Types ............................................................... 2-35
2-6-4. Sample Results Window .................................................................. 2-36
2-6-5. Re-analysis Window ........................................................................ 2-37
2-7. Print ............................................................................................................ 2-39

NSX-5000V
Table of Contents 3

2-7-1. Report Settings Window ................................................................... 2-39


2-7-2. Printing ............................................................................................. 2-40
2-8. Post-Measurement Operations .................................................................... 2-41
2-8-1. Shutdown Window ............................................................................ 2-41
2-8-2. Shutdown ......................................................................................... 2-42
Section 3: Advanced Operations ................................................................................. 3-1
3-1. Disconnection and Connection ...................................................................... 3-1
3-1-1. Communication Disconnection ........................................................... 3-1
3-1-2. Unit Connection .................................................................................. 3-1
3-2. User Settings ................................................................................................. 3-2
3-2-1. User Management Window ................................................................ 3-2
3-2-2. Edit User Account Window ................................................................. 3-3
3-3. Column Display Setting ................................................................................. 3-4
3-4. Import and Export .......................................................................................... 3-5
3-4-1. Import and Export of a Schedule ........................................................ 3-5
Export of a Schedule ............................................................ 3-5
Import of a Schedule ............................................................. 3-6
3-4-2. Import and Export of a Method ........................................................... 3-7
Export of a Method ............................................................... 3-7
Import of a Method ................................................................ 3-7
3-5. Registration and Read ................................................................................... 3-8
3-5-1. Blank Registration .............................................................................. 3-8
3-5-2. Blank Read ......................................................................................... 3-9
3-5-3. Calibration Curve Registration .......................................................... 3-11
3-5-4. Calibration Curve Read .................................................................... 3-12
3-6. Continuous Schedule Run ........................................................................... 3-13
3-6-1. Continuous Run Schedule Setting Window ...................................... 3-13
3-6-2. Continuous Run Schedule Setting .................................................... 3-14
3-7. Spike Standard ............................................................................................ 3-16
3-8. Automatic Syringe Dilution ........................................................................... 3-17
3-8-1. Method and Schedule Setting .......................................................... 3-18
3-8-2. Step Editor Window (Automatic Syringe Dilution) ............................. 3-18
3-8-3. Calibration Measurement with Automatic Syringe Dilution ............... 3-19
3-8-4. Sample Measurement with Automatic Syringe Dilution .................... 3-20

NSX-5000V
4 Table of Contents

NSX-5000V
Preparation 1-1

Section 1: Preparation
This section describes the preparation of the NSX-5000V system. For the installation of
a unit and the measurement preparation of injector, refer to the respective instruction
manuals.

1-1. Unit Composition

Operate the NSX-5000V system by adding an injector to the vertical furnace (VF-500)
and sulfur detector (SD-500). Select the most appropriate injector according to the
purpose and sample type. It is also possible to connect the nitrogen detector (ND-500)
as a detector to measure nitrogen simultaneously. Fig. 1-1 shows an example of the NSX-
5000V system and Table 1-1 shows examples of NSX-5000V unit composition.

ASC-550L

SD-500 VF-500

Fig. 1-1. Example of NSX-5000V System

Table 1-1. Examples of NSX-5000V Unit Composition

Sample type Injector Electric Detector


furnace
Non-aqueous Automatic sampler for liquid: ASC-550L
liquid Vertical Sulfur
Volatile liquid Automatic injector for liquefied petroleum furnace Detector
Gas gas (LPG) : GI-560 : VF-500 : SD-500
LPG

NSX-5000V
1-2 Preparation

1-2. Preparation of Combustion Tube

Although the injector composition varies according to the sample type, the combustion
tube composition is the same. Check the combustion tube composition by referring to
“Table 1-2. Combustion Tube Composition”, and prepare an appropriate combustion tube.
To measure nitrogen and sulfur simultaneously, apply platinum catalyst treatment to the
outer combustion tube as needed. For platinum catalyst treatment of the outer
combustion tube, refer to “1-5. Platinum Catalyst Treatment of Outer Combustion Tube”.

Table 1-2. Combustion Tube Composition

Sample type Injector Combustion tube composition Parts


number
Non-aqueous ASC-550L Inner combustion tube 22 L227 TS8QPN
liquid
Outer combustion tube 30, L375 FN2QPG
Volatile liquid GI-560 Inner combustion tube 22 L227 TS8QPN
Gas Outer combustion tube 30, L375 FN2QPG
LPG

1-2-1. Washing of Combustion Tube

Before using a new combustion tube, wash and dry it. Visually check the condition of the
combustion tube in use every month. If it is contaminated, wash it. However, combustion
tubes are easily devitrified after measurement of alkaline or metal-containing samples. In
this case, check the combustion tube more frequently. Wash the combustion tube as
follows.

CAUTION Prevention of glass breakage


Combustion tube is glass. Handling it roughly may cause it to break.
Take care in handling.

CAUTION Combustion tube devitrification


When a combustion tube is devitrified, it may break due to lowered
mechanical strength.
The term "devitrification" refers to the condition of a combustion tube where
the color has turned white. When a combustion tube is devitrified,
especially when fine cracks are in the devitrified part, the mechanical
strength is low. Change it immediately with a new one.

NSX-5000V
Preparation 1-3

(1) If you already use a combustion tube, remove the quartz wool and filler from the
combustion tube.
(2) Brush the combustion tube with neutral detergent. When contamination cannot be
removed by brushing, immerse the combustion tube in detergent overnight or longer,
and then wash it.
(3) After washing, rinse with pure water and dry it.

1-2-2. Preparation of Inner Combustion Tube

This section describes the preparation of the inner combustion tube. Fill quartz wool into
the inner combustion tube as follows. Refer to “Fig. 1-2. Preparation of Inner Combustion
Tube”. Do not touch any part that will be hot with bare hands because fingerprints put on
the combustion tube burn when it becomes hot. If there are parts touched with bare hands,
wipe them with an ethanol-soaked cloth to remove the sebum.

POINT Change of quartz wool


The quartz wool in the inner combustion tube needs to be changed
regularly because substances that are not vaporized by furnace heat (such
as salts and metals) accumulate in the quartz wool. The change frequency
depends on the measurement frequency. However, change the quartz
wool once every week when samples contain a lot of salts and/or metals.
Otherwise, change it once every 3 to 4 weeks. Regardless of the above, if
the quartz wool looks stiff by visual inspection, change it.

(1) Ball 0.2 g of quartz wool. Do not ball it tightly, but loosely.
(2) Fill the balled quartz wool into the projection of the inner combustion tube with the
quartz wool poker while ensuring that there is no gap.

0.2 g

Fig. 1-2. Preparation of Inner Combustion Tube

NSX-5000V
1-4 Preparation

1-2-3. Preparation of Outer Combustion Tube

This section describes the preparation of the outer combustion tube. Fill quartz wool and
combustion tube filler (alumina balls) into the outer combustion tube as follows. Refer to
“Fig. 1-3. Preparation of Outer Combustion Tube”. Do not touch any part that will be hot
with bare hands because fingerprints put on the combustion tube burn when it becomes
hot. If there are parts touched with bare hands, wipe them with an ethanol-soaked cloth
to remove the sebum.

POINT Change of quartz wool


If the quartz wool looks stiff by visual inspection, change it.

(1) Ball 0.5 g of quartz wool and fill it into the outer combustion tube in such a way that
its height is about 25 mm.
(2) Fill about 30 g of combustion tube filler (alumina balls) into the outer combustion
tube filled with the quartz wool, in such a way that its height is about 50 mm.
(3) Ball 0.4 g of quartz wool and fill it into the outer combustion tube filled with the
combustion tube filler (alumina balls), in such a way that its height is about 30 mm.

0.4 g, about 30 mm

About 30 g, about 50 mm

0.5 g, about 25 mm

Fig. 1-3. Preparation of Outer Combustion Tube

NSX-5000V
Preparation 1-5

1-2-4. Assembly of Inner and Outer Combustion Tubes

This section describes the procedure for assembling the inner and outer combustion
tubes. Assemble the inner and outer combustion tubes as follows. Refer to “Fig. 1-4.
Assembly of Outer and Inner Combustion Tubes”. Do not touch any part that will be hot
with bare hands because fingerprints put on the combustion tube burn when it becomes
hot.

(1) Put 2. inner combustion tube 22 L227 into 1. outer combustion tube 30 L375 while
ensuring that the claw positions are aligned.
(2) Fix them with 3. springs for combustion tube.

2.

3.

1.

Fig. 1-4. Assembly of Outer and Inner Combustion Tubes

1-3. Setting of Combustion Tube to Vertical Furnace

Set the assembled combustion tube to the vertical furnace as follows. Refer to “Fig. 1-5.
Combustion Tube Setting” and “Fig. 1-6. Electric Furnace Top”.

WARNING Turning off the electric furnace


When handling combustion tube parts, always turn off the heater switch
and wait until the furnace temperature is room-temperature.
Failure to do so may cause burns.

CAUTION Check of O-ring


When setting an O-ring, check that it is not damaged. If it is damaged,
change it immediately.

NSX-5000V
1-6 Preparation

CAUTION Glass breakage


Combustion tube is glass. By tightening it too tightly, it may be broken.
Take care in handling.

POINT Cleaning of outer combustion


tube
Before setting a combustion tube, wipe the outside of the outer combustion
tube with an ethanol-soaked cloth. Contamination accelerates
devitrification of the combustion tube and the life may be shortened.

(1) Operate the electric furnace hook on the right of the electric furnace to open it.
(2) Put 1. O-ring holder on the top of the inner combustion tube or combustion tube
adapter, and then put 2. O-ring P16.
(3) Hold the bottom of the combustion tube and slowly raise it upward to insert it into
the hole of the flange.
(4) Tighten the O-ring holder to fix the top of the inner combustion tube or combustion
tube adapter. At this time, turn the branch tube of the outer combustion tube to the
front.
(5) Close the electric furnace and operate the electric furnace hook on the right of the
electric furnace to fix it.
(6) Connect 3. gas supply line to the outer combustion tube and 5. female ball joint
12.5 with 4. straight connector 6/4. Connect 5. female ball joint 12.5 and the
branch tube male ball joint and fix them with 6. clip 12 for ball joint.
(7) Put 7. shield plates by turning the chamfered surfaces upward and align them so
that they surround the combustion tube.

3. 4. 5. 6. 7.
2.

1.

Fig. 1-5. Combustion Tube Setting Fig. 1-6. Electric Furnace Top〇

NSX-5000V
Preparation 1-7

1-4. Combustion Tube Outlet Connection

This section describes the connection of the outlet of the combustion tube set to the
electric furnace. Connect 1. female ball joint 18 to the outlet of the combustion tube and
fix it with 2. clip 18 (long). Refer to “Fig. 1-7. Fixing of Female Ball Joint”.

1. 2.

Fig. 1-7. Fixing of Female Ball Joint

1-5. Platinum Catalyst Treatment of Outer Combustion Tube

To measure nitrogen and sulfur simultaneously, apply platinum catalyst treatment to the
outer combustion tube as needed, and then fill regular combustion tube filler (alumina
balls). Apply platinum catalyst treatment to the outer combustion tube as follows. For the
preparation of the outer combustion tube for platinum catalyst treatment, refer to “Fig. 1-
8. Platinum Catalyst Treatment of Outer Combustion Tube”.

CAUTION Disconnection of lower line from


combustion tube outlet
Before platinum catalyst treatment, be sure to remove the female ball joint.
When a new platinum catalyst or a platinum catalyst that has not been
used for a long time is used, the moisture contained in the platinum catalyst
may ooze out. Place a beaker under the outlet of the combustion tube.
Platinum catalyst treatment may generate acid gas.

NSX-5000V
1-8 Preparation

POINT Effects of platinum catalyst


treatment
Applying platinum catalyst treatment to the outer combustion tube
improves the linearity of calibration curves in a low-concentration range in
nitrogen measurement. However, it deteriorates area values in sulfur
measurement. Since the deterioration of area values in sulfur
measurement varies depending the condition of platinum treatment,
prepare calibration curves as needed. When measuring very trace sulfur,
the detector may not be able to detect the sulfur due to the deterioration of
area values. In this case, do not use the outer combustion tube to which
platinum catalyst treatment is applied.

(1) Ball 0.5 g of quartz wool and fill it into the outer combustion tube in such a way that
its height is about 25 mm.
(2) Fill about 30 g of the platinum catalyst into the outer combustion tube filled with the
quartz wool, in such a way that its height is about 85 mm.
(3) Ball 0.4 g of quartz wool and fill it into the outer combustion tube filled with the
platinum catalyst, in such a way that its height is about 30 mm.

0.4 g, about 30 mm

About 30 g, about 85 mm

0.5 g, about 25 mm

Fig. 1-8. Platinum Catalyst Treatment of Outer Combustion Tube

(4) Assemble the inner and outer combustion tubes by referring to “1-2-4. Assembly of
Inner and Outer Combustion Tubes”.
(5) Set the combustion tube to the electric furnace by referring to “1-3. Setting of
Combustion Tube to Vertical Furnace”.

NSX-5000V
Preparation 1-9

(6) While the female ball joint 18 is not set to the outlet of the combustion tube, keep
raising the temperature of VF-500 by setting the following conditions.
Inlet and outlet temperatures of the electric furnace are 900 degrees Celsius,
respectively.
Ar and O2 gas flows are 100 mL/min and 500 mL/min, respectively.
Set the SD-500 xenon lamp to “OFF”. For details on operations, refer to “Section 2:
Basic Operations”.
(6) After three hours have passed, set the electric furnace and gas of VF-500 to “OFF”
and wait until the temperature of the combustion tube drops sufficiently.
(7) After the temperature of the outer combustion tube drops sufficiently, remove the
platinum catalyst and fill combustion tube filler (alumina balls) into the outer
combustion tube by referring to “1-2-3. Preparation of Outer Combustion Tube”.
(8) Assemble the inner and outer combustion tubes by referring to “1-2-4. Assembly of
Inner and Outer Combustion Tubes” and set the combustion tube to the electric
furnace by referring to “1-3. Setting of Combustion Tube to Vertical Furnace”.

NSX-5000V
1-10 Preparation

NSX-5000V
Basic Operations 2-1

Section 2: Basic Operations


This section describes basic operations, such as start-up and measurement operations.
For details on maintenance, inspection, preparation before measurement, and
parameters, refer to the instruction manual of each unit. Measurement operations vary
depending on the injector. Also refer to the operations described in the instruction manual
of each injector.

2-1. Start Up

2-1-1. Maintenance, Inspection, and Preliminary Preparation for


Measurement

Perform daily and periodical inspections on each unit, and perform maintenance if needed.
In addition, make a preliminary preparation of each unit for measurement. Refer to the
instruction manual of each unit for details.

2-1-2. Power and Gas Supply

Supply power and gas by the following procedure.

(1) Supply power to the table outlet.


(2) Open the main valves of O2 and Ar cylinders to supply O2 and Ar gases. When using
N2 gas or dry Air as the dry gas of SD-500, open the main valve of the cylinder to
supply the dry gas.
(3) Adjust the secondary pressures of cylinders or stop valves to 0.3 ± 0.1 MPa with
regulators. Set the pressures of O2 and Ar gases to the same pressure at this time.
When using N2 gas or dry Air as the dry gas, set the same pressure.

2-1-3. Start

Start the system by the following procedure. If the nitrogen detector is connected, also
refer to the operation manual of TN-5000V.

(1) Turn on the power switches of VF-500, SD-500, and the injector.
(2) Turn on the power of the PC, monitor, and printer.
(3) Double-click the NSX-5000 shortcut on the desktop PC screen or select “Programs”-
“NSX-5000”-“NSX-5000” from the Windows start menu to start the NSX-5000
application.
When the NSX-5000 application starts, the splash screen is displayed. Then, the
logon window is displayed.

NSX-5000V
2-2 Basic Operations

2-1-4. Logon Window

This section describes the logon window. Fig. 2-1 shows the logon window and Table 2-
1 shows the items and functions of the logon window.

1
2
3
5
4

Fig. 2-1. Logon Window

Table 2-1. Items and Functions of the Logon Window

No. Item Function


1 User Name When the tab is opened, the user name set by user setting is
displayed.
2 Password Input the password of the user.
3 COM Port Set the COM port of the PC to communicate with the unit. Click
[Find Port] to display available COM ports in the tab. If a
connection is not established by clicking [Connect], change the
port using [Find Port] and click [Connect] again.
4 Exit This button shuts down the NSX-5000 application.
5 Logon Click [Offline] to display the mode selection window without
connecting with the unit. Click [Connect] to connect to the unit
and display the mode selection window.

NSX-5000V
Basic Operations 2-3

2-1-5. Mode Selection Window

This section describes the mode selection window. Fig. 2-2 shows the mode selection
window and Table 2-2 shows the items and functions of the mode selection window. The
NSX-5000 application software provides two modes: Simple and Advanced. The Simple
mode is a simplified measurement mode with limited functions. The Advanced mode is a
measurement mode that allows you to make advanced settings. For the functional
limitation in Simple mode, refer to “Table 2-3. Functional Limitation in Simple Mode”.

1 2

Fig. 2-2. Mode Selection Window

Table 2-2. Items and Functions of the Mode Selection Window

No. Item Function


1 Simple This button starts the application software in Simple mode.
2 Advanced This button starts the application software in Advanced mode.
3 The selected Check the checkbox to automatically start the application
mode is saved. software in the selected mode without displaying the mode
selection window from the next time.

Table 2-3. Functional Limitation in Simple Mode

Item Availability in
Simple mode
Schedule (Method) New Not available
Template registration Not available
Creation with template Available
Simultaneous expansion of multiple schedules (Measurement window) Not available
Status check (Measurement window) Not available
Check of registered calibration and blank (Result window) Not available
Audit trail check (Result window) Not available
User registration Available
Continuous schedule run Not available

NSX-5000V
2-4 Basic Operations

2-1-6. Logon and Connection

Log on to the software and connect the PC to the unit by the following procedure. For the
items and functions of the logon window, refer to “2-1-4. Logon Window”.

(1) Select the desired name in “User Name”, input the password in “Password”, and
click [Connect] in “Logon”. In the initial setting, select “NSX-5000” in “User Name”,
leave “Password” blank, and click [Connect] in “Logon”.
(2) Click [Connect] in “Logon” to connect to the unit and display the mode selection
window. For the mode selection window, refer to “2-1-5. Mode Selection Window”.
(3) Select a mode to display a setup window.

2-2. Initial Window Composition

This section describes the initial window composition. Fig. 2-3 shows the initial window
composition and Table 2-4 shows the items and functions of the initial window
composition. Table 2-5 shows the functions of icons.

1
2
3

Fig. 2-3. Initial Window Composition

Table 2-4. Items and Functions of the Initial Window Composition

No. Item Function


1 Application The application software and user names are displayed. When
software name the background color is blue, the Simple mode is selected.
When it is orange, the Advanced mode is selected.
2 Menus Click a menu to display a list.
3 Icons There are icons for printing and measurement start and stop
operations. Place the cursor over an icon to display the icon
name.
4 Window change These are icons for changing windows. Click an icon to change
icons the window. They represent the setup, system, measurement,
result, and shutdown windows, respectively.

NSX-5000V
Basic Operations 2-5

Table 2-5. Functions of Icons

Name Icon Function


Setup window Window where you make system configuration,
method, and schedule settings. The displayed window
varies between the Simple and Advanced modes.
System Window where you turn on/off the functions of each
window unit. Access maintenance information records from this
window.
Measurement Window where you mainly edit schedules and check
window results. A chart displays signals during measurement.

Result Window where results are displayed. You can view the
window results of calibration and reanalyze peaks. Also register
blank and calibration from this window.
Shutdown Window where you turn off the functions of each unit.
window Use this window when performing a shutdown
operation after measurement.
Print Clicking this icon displays the print settings window.
You can make print settings, display a preview, and run
printing.
Start Clicking this icon starts the steps of a measurement
schedule. The icon is enabled when the unit becomes
ready for measurement.
Step break Clicking this icon inserts “Step Break” step immediately
after the active step. When the active step finishes, the
continuous run stops.
Cancel Clicking this icon stops the active step. Use the icon for
emergent stop.

Clear effluent This icon is displayed when using ASC-550L. Clicking


volume this icon clears effluent volume information. As the
effluent volume increases, the color of effluent changes
from blue to yellow to red.
Mode change Clicking this icon displays the window where you
change the mode between Simple and Advanced. To
change the mode, temporarily close the schedule.

NSX-5000V
2-6 Basic Operations

2-3. Schedule and Method Preparation

The procedure for preparing a schedule varies between the Simple and Advanced modes.
Check the operation procedure corresponding to the selected mode.

2-3-1. Flow of Schedule Preparation in Advanced

This section describes the flow of schedule preparation in Advanced mode. Prepare a
schedule by referring to “Fig. 2-4. Flow Chart of Schedule Preparation in Advanced Mode”.
To prepare a new schedule, first prepare a method. For method preparation, refer to “2-
3-3. New Method Preparation”. If you have an existing method, prepare a new schedule
by referring to “2-3-4. New Schedule Preparation”. Register a prepared schedule as a
template so that you can prepare a schedule with the template. Refer to “2-3-5. Template
Registration” and “2-3-6. Schedule Preparation with Template (Advanced)”.

Fig. 2-4. Flow Chart of Schedule Preparation in Advanced Mode

NSX-5000V
Basic Operations 2-7

2-3-2. Setup Window (Advanced)

This section describes the setup window in Advanced mode. Fig. 2-5 shows the setup
window (Advanced) and Table 2-6 shows the items and functions of the setup window
(Advanced).

4
2 3
6 5

Fig. 2-5. Setup Window (Advanced)

Table 2-6. Items and Functions of the Setup Window (Advanced)

No. Item Function


1 System configuration The connected units are displayed. If multiple
units are connected, click the tab to display them
as choices.
2 Schedule Create This button creates a new schedule. For details,
refer to “2-3-4. New Schedule Preparation”.
Copy from This button creates a schedule by copying a
template schedule registered as a template. For details,
refer to “2-3-6. Schedule Preparation with
Template (Advanced)”.
Open This button opens a saved schedule.
3 Method Create This button creates a new method. For details,
refer to “2-3-3. New Method Preparation”.
Change This button changes the method used for the
selected schedule.
Edit This button edits the parameters of a saved
method.
4 Display Change This button changes the display to a schedule
directory display. Click the button again to change
the display to the regular setup window display.

NSX-5000V
2-8 Basic Operations

No. Item Function


5 Schedule and method names The schedule name is displayed to the left and
the method name is displayed to the right. Click
[Prepare] to set the schedule as a measurement
schedule and display a mark.
6 Prepare This button sets a schedule as a measurement
schedule.

2-3-3. New Method Preparation

This section describes the procedure for preparing a new method. Methods cannot be
prepared in Simple mode. Change the mode to Advanced before preparing one. Prepare
a new method by the following procedure. Refer to “Fig. 2-6. New Method Preparation
Window”.

(1) Check that the system consists of your intended units in the setup window in
Advanced mode. If it does not, click the tabs and select your intended units. If no
units are displayed as choices, select “Help” and “Equipment Composition” of the
menu to check the equipment composition. When measuring nitrogen and sulfur
simultaneously using a nitrogen detector, check that ND-500 and SD-500 are
selected as detectors.
(2) Click [Create] in “Method” to display the new method preparation window.
(3) Select a folder for save. To create a new folder, click [New Folder Create].
(4) Input a method name.
(5) Select injector conditions.
(6) Check “Protection” to make the method unable to be deleted in the method directory.
Methods created by the user ID “Administrator” become unable to be edited by the
user ID “NSX-5000”.
(7) Click [OK] to prepare a new method.

Fig. 2-6. New Method Preparation Window

NSX-5000V
Basic Operations 2-9

2-3-4. New Schedule Preparation

This section describes the procedure for preparing a new schedule. Schedules cannot be
prepared in Simple mode. Change the mode to Advanced before preparing one. Prepare
a new schedule by the following procedure. Refer to “Fig. 2-7. New Schedule Preparation
Window”.

POINT Method and schedule


If no methods are prepared, prepare a new one by referring to “2-3-3. New
Method Preparation”. If prepared methods are not displayed when you
select a method, check whether the equipment composition for the
methods matches the current system configuration and whether the
conditions of the injector match.

(1) Check that the system consists of your intended units in the setup window in
Advanced mode. If it does not, click the tabs and select your intended units. If no
units are displayed as choices, select “Help” and “Equipment Composition” of the
menu to check the equipment composition. When measuring nitrogen and sulfur
simultaneously using a nitrogen detector, check that ND-500 and SD-500 are
selected as detectors.
(2) Click [Create] in “Schedule” to display the new schedule preparation window.
(3) Select the same injector composition as for the method to be used.
(4) To use the automatic syringe dilution function, check the checkbox. For details on
the automatic syringe dilution function, refer to “3-8. Automatic Syringe Dilution”.
(5) Select a save destination. To create a new folder, click [New Folder Create].
(6) Input a schedule name and select a method.
(7) Check “Protection” to make the schedule unable to be deleted in the schedule
directory. Schedules created by the user ID “Administrator” become unable to be
edited or run by the user ID “NSX-5000”.
(8) Click [OK] to prepare a new schedule and display it in the setup window.
(9) Click [Prepare] for the schedule to set the schedule as a measurement schedule.

Fig. 2-7. New Schedule Preparation Window

NSX-5000V
2-10 Basic Operations

2-3-5. Template Registration

This section describes template registration. Templates cannot be registered in Simple


mode. Change the mode to Advanced before registering one. Fig. 2-8. shows the
“Template registration” window. Register a template by the following procedure.

(1) In Advanced mode, select the “Tool” in menu -“Template registration” to display the
“Template registration” window.

(2) Click in “Acquisition of existing schedule settings”, select the schedule to be


registered as a template, and check that the equipment composition (such as
electric furnace and injector) matches the composition for the schedule to be
registered.
(3) Click [Add], select your desired schedule, and register it as a template. Up to 10
schedules can be registered.
(4) If multiple schedules are registered as templates, you can set the order in which
they are displayed by selecting a schedule and clicking [Up] or [Down].
(5) Click [Close] to close the “Template registration” window.

Fig. 2-8. Template Registration Window

2-3-6. Schedule Preparation with Template (Advanced)

This section describes schedule preparation with a template in Advanced mode. Fig. 2-9.
Shows the “Schedule preparation with a template” window. Prepare a schedule by the
following procedure.

NSX-5000V
Basic Operations 2-11

POINT Template and system


configuration
If no templates are displayed as choices in the tab, check whether
templates are registered by referring to “2-3-5. Template Registration”.
Also check whether the equipment composition of the registered template
matches the displayed system configuration.

(1) Check that the system consists of your intended units in the setup window in
Advanced mode. If it does not, click the tabs and select your intended units. If no
units are displayed as choices, select “Help” and “Equipment Composition” of the
menu to check the equipment composition. When measuring nitrogen and sulfur
simultaneously using a nitrogen detector, check that ND-500 and SD-500 are
selected as detectors.
(2) Select “Template” for a schedule to display the “Schedule preparation with a
template” window.
(3) Select a folder for save.
(4) Open the template tab and select the schedule name of the template to be used.
(5) Input the name of the schedule to be prepared.
(6) Select whether to prepare the schedule using the template with or without results. If
“Without result” is selected, steps will be prepared without results even when the
template contains results. The steps can be run as new ones.
(7) Click [Create] to prepare the schedule and display it in the setup window.
(8) Click [Prepare] for the schedule to set the schedule as a measurement schedule.

Fig. 2-9. Schedule Preparation with a Template Window

NSX-5000V
2-12 Basic Operations

2-3-7. Setup Window (Simple)

This section describes the setup window in Simple mode. Fig. 2-10 shows the setup
window (Simple) and Table 2-7 shows the items and functions of the setup window
(Simple).
1

Fig. 2-10. Setup Window (Simple)

Table 2-7. Items and Functions of the Setup Window (Simple)

No. Item Function


1 System configuration The connected units are displayed. If
multiple units are connected, click the tab to
display them as choices.
2 Schedule Copy from This button creates a schedule by using a
template schedule registered as a template.
Open This button opens a saved schedule. Select
a schedule for measurement and click
[Apply] to set it as a measurement schedule.
Save folder Select a folder to save the schedule.
Template The tab displays the choices of schedules
registered as templates.
3 Create This button creates a schedule.

NSX-5000V
Basic Operations 2-13

2-3-8. Schedule Preparation (Simple)

This section describes schedule preparation in Simple mode. In Simple mode, create a
schedule by the following procedure using a schedule registered in Advance mode as a
template.

POINT Method and schedule


If no templates are displayed as choices in the tab, check whether
templates are registered by referring to “2-3-5. Template Registration”.
Also check whether the equipment composition of the registered template
matches the displayed system configuration.

(1) Check that the system consists of your intended units in the setup window in Simple
mode. If it does not, click the tabs and select your intended units. If no units are
displayed as choices, select “Help” and “Equipment Composition” of the menu to
check the equipment composition. When measuring nitrogen and sulfur
simultaneously using a nitrogen detector, check that ND-500 and SD-500 are
selected as detectors.
(2) Select “Copy from template”.
(3) Select a folder for save. The schedule will be prepared in this folder.
(4) Open the template tab and select the schedule name of the template to be used.
(5) Select whether to prepare the schedule using the template with or without results. If
“Without result” is selected, steps will be prepared without results even when the
template contains results. The steps can be run as new ones.
(6) Click [Create] to create the schedule. If any unit is connected, the window changes
to the system window.

NSX-5000V
2-14 Basic Operations

2-4. Measurement Preparation

2-4-1. System Window

This section describes the system window. The system window varies depending on the
connected units. Fig. 2-11 shows the system window and Table 2-8 shows the items and
functions of the system window.

4
2

1 5 6
3

Fig. 2-11. System Window

Table 2-8. Items and Functions of the System Window

No. Item Function


1 ON/OFF switch This switch sets “ON” or “OFF”. When “ON” is set, the color is
green. When “OFF” is set, the color is red.
2 Gas Leak Check This button displays the “Gas Leak Check” window. For details
on gas leak check, refer to “2-4-3. Gas Leak Check”.
3 Batch These buttons collectively turn ON/OFF all items.
processing
4 Status This area displays the statuses of the connected units.
5 Navigation This button displays the navigation window. Navigation enables
you to check the procedures for preparing units.
6 Maintenance This button displays the maintenance window. In the
maintenance window, you can record the serial number of each
unit and consumables change dates.

NSX-5000V
Basic Operations 2-15

2-4-2. Measurement Preparation

This section describes measurement preparation. Make preparations for measurement


by the following procedure. If the nitrogen detector is connected, also refer to the
operation manual of TN-5000V.

(1) In the system window, set the gas of VF-500 to “ON” to flow gas through the flow
path.
(2) Click [Gas Leak Check] to check for gas leak. For gas leak check, refer to “2-4-3.
Gas Leak Check”.
(3) Set the electric furnace of VF-500 to “ON” to raise the temperature of the electric
furnace.
(4) Set the SD-500 xenon lamp and dry gas to “ON”. The xenon lamp is turned on
automatically at the time of connection.

2-4-3. Gas Leak Check

This section describes gas leak check. Check for gas leak by the following procedure by
referring to “Fig. 2-12. Connection of Flow Meter for Gas Leak Check”.

WARNING Gas Leak Check


Never check for gas leak while the temperature of the electric furnace is
raised. Doing so may cause burns.
When gas flow is less than the preset value, gas may be leaking. If
measurement is performed in that state, a serious accident may result. Be
sure to check for gas leakage.

(1) Set Ar gas to 200 mL/min and O2 gas to 0 mL/min and click [Check start]. Check
that the display value of Ar gas is 200±20 mL/min and that of O2 gas is 0±10 mL/min.
(2) Set Ar gas to 0 mL/min and O2 gas to 200 mL/min and click [Check start]. Check
that the display value of Ar gas is 0±10 mL/min and that of O2 gas is 200±20 mL/min.
(3) Set Ar gas to 200 mL/min and O2 gas to 200 mL/min and click [Check start].
(4) Connect 2. flow meter for gas leak check and the outlet of the combustion tube with
1. clip 18 (long). Check that the flow rate is 400±40 mL/min on the O2 scale. If a
gas injector is connected, use a value obtained by adding the gas injector flow rate
as a reference value.
(5) If the flow rate is below the reference value, gas may be leaking. Check for gas
leakage and run gas leak check again.

NSX-5000V
2-16 Basic Operations

1.

2.

Fig. 2-12. Connection of Flow Meter for Gas Leak Check

Inspection When Gas is Leaking

If gas is leaking, identify the cause of gas leakage and take measures by referring to
“Table 2-9. Inspection When Gas Is Leaking”. If the gas flow rate does not meet the setting
value after inspection, contact our local distributor.

Table 2-9. Inspection When Gas Is Leaking

Inspection point Contents


Injection port Check that injection port is connected firmly. Also check that the
septum (flat) is set correctly.
Gas line to outer Check that the gas line (ball joints and connectors) to the outer
combustion tube combustion tube is connected firmly.
Top of combustion Check that the connection part of the combustion tube and flange
tube is not loose and that they are set firmly. Also check that the O-
ring is not twisted.
Outlet of pyrolysis Check that the combustion tube and the flow meter for gas leak
tube check are connected firmly.

NSX-5000V
Basic Operations 2-17

2-4-4. Measurement Window

This section describes the measurement window. Fig. 2-13 shows the measurement
window and Table 2-10 shows the items and functions of the measurement window. The
composition of the measurement window can be changed by selecting “Tool” in menu
-”Measurement window layout”. The display of the measurement window varies
depending on the system configuration.

11
1 2 3 4 6 7
9
5
8

10 12

13

Fig. 2-13. Measurement Window

Table 2-10. Items and Functions of the Measurement Window

No. Item Function


1 Blank read This button reads data corresponding to the registered blank ID
into the schedule.
2 Calibration This button reads data corresponding to the registered
curve read calibration ID into the schedule.
3 Parameter This button displays the parameter window.
4 Step Editor This button displays the Step Editor window.
5 Rule This button allows you to set the number of display digits and
the unit. For details, refer to “2-4-8. Rule Window”.
6 Fill This button displays the injection status check window.
7 ASC program This button displays the ASC program setting window.
8 Step Steps are run from top to bottom. One measurement is run per
measurement step row.
9 Schedule and The schedule name is displayed to the left and the method
method names name is displayed to the right. Click [Prepare] to set the
schedule as a measurement schedule and display a mark.
10 Chart You can switch between realtime and overlap charts.

NSX-5000V
2-18 Basic Operations

No. Item Function


11 Status You can check the statuses of the connected units. This tab is
not displayed in Simple mode.
12 Unit information This area displays unit information visually.
13 Temperature This area displays temperatures and flow rates. Gray indicates
and flow “not controlled”. Yellow indicates “controlled”. Green indicates
indications “controlled” and “ready”.

2-4-5. Parameter Check

This section describes the procedure for parameter check. Fig. 2-14. shows the
parameter window. Check the parameters by the following procedure. The parameter
window varies depending on the composition of connected units. For details on
parameters, refer to the instruction manual of each unit.

POINT Change of parameters


When parameter values are changed, the values of the method are
overwritten and saved. Since parameters reflect the latest method
information (overwritten values), you cannot check the original parameters
used for measurement by checking a schedule that used the same method
in the past.
To conduct measurement while changing parameters in order to consider
conditions or for other purposes, prepare a method with a different name
and apply it to a schedule by referring to “2-3-3. New Method Preparation”.

(1) Click [Parameter] in the measurement window.


(2) From the unit list to the left of the parameter indication, select a unit name to check
parameters.
(3) The parameter names, set values, and defaults are displayed. Change the set
values if necessary. When not using Ar gas but using N2/Air as the dry gas, make
settings in this window.

NSX-5000V
Basic Operations 2-19

Fig. 2-14. Parameter Window

2-4-6. Vertical Furnace Parameter Settings

Parameters for NSX-5000V vary depending on the measurement element (sulfur


measurement or simultaneous measurement of nitrogen and sulfur). Check that the
values of vertical furnace parameters are as shown in “Table 2-11. Vertical Furnace
Parameter Settings”. If conditions are set by standards or other specifications, change
the values properly. When using a gas injector, check parameters by referring to the
instruction manual of the gas injector.

(1) Click [Parameter] for the schedule.


(2) Select the vertical furnace (VF-500) from the unit list to the left of the parameter
indication.
(3) Check the setting value of each item. If there are different values, set ones again.

Table 2-11. Vertical Furnace Parameter Settings

Nitrogen
Sample type Sulfur
and sulfur
Electric furnace Inlet (C) 900 900
temperature
Outlet (C) 1000 900
Gas flow Ar (mL/min) 100 100
O2 (mL/min) 500 500

NSX-5000V
2-20 Basic Operations

2-4-7. Sulfur Detector Parameter Settings

The default dry gas for the sulfur detector is Ar gas. To use N2 gas or dry Air as the dry
gas, make dry gas settings in the parameter window.

(1) Click [Parameter] for the schedule.


(2) Select the sulfur detector (SD-500) from the unit list to the left of the parameter
indication.
(3) Select “N2/Air” for the gas type item.

2-4-8. Rule Window

Click [Rule] for the schedule to display the “Rule” window. In the “Rule” window, set the
number of display digits and the unit. Fig. 2-15 shows the “Rule” window and Table 2-12
shows the items and functions of the “Rule” window. The contents are different depending
on the system configuration. Set rules will be applied only to the schedule for which you
clicked [Rule].

2 3

Fig. 2-15. Rule Window

NSX-5000V
Basic Operations 2-21

Table 2-12. Items and Functions of Rule Window

No. Item Function


1 Continuous step Check the checkbox to move to and run the next step
run automatically after the completion of the current step. Check
the check box to conduct continuous measurement with the
ASC-550L unit.
2 Number of Set the number of digits to be displayed in the measurement
display digits and result windows.
3 Unit setting Select the classification of units and a unit.

2-4-9. Concentration Calculation

The NSX-5000V system prepares calibration curves using working solution and
calculates the concentration of samples. It uses absolute sulfur amounts for the X-axis of
calibration curves and area values for the Y-axis. It calculates the amount of detection
from a sample by applying area values obtained from sample measurement to a
calibration curve. It calculates the concentration of a sample by dividing the amount of
detection from a sample by the sample volume. This section describes absolute amount
calculation for calibration curves and sample concentration calculation.

Absolute Amount Calculation for Calibration Curves

Absolute amount calculation for calibration curves varies according to the concentration
unit of working solution. When the concentration unit is w/w, a density value is required
in addition to concentration and sample volume. Table 2-13 shows examples of absolute
amount calculation for calibration curves.

Table 2-13. Examples of Absolute Amount Calculation for Calibration Curves

No. State Classification Calculation example


of unit
1 Liquid w/v Concentration ሺµg/mLሻ × Sample volume ሺµLሻ
2 Liquid w/w Concentration (µg/g) × Sample volume (µL) × Density
(g/mL)

NSX-5000V
2-22 Basic Operations

Sample Concentration Calculation

Sample concentration calculation varies according to the concentration unit. When the
concentration unit is w/w, a density value is required. Table 2-14 shows examples of
sample concentration calculation.

Table 2-14. Examples of Sample Concentration Calculation

No. State Classification Calculation example


of unit
1 Liquid w/v Amout of detection ሺngሻ
Sample volume ሺµLሻ
2 Liquid w/w Amout of detection (ng)
Sample volume (µLሻ × Density ሺg/mLሻ

2-4-10. Step Editor Window

This section describes the “Step Editor” window. “Step Editor” is a window for inputting
measurement information for a step, so each step is handled as a single measurement
run. Select “Edit”-“Step Editor” of the menu to display the “Step Editor” window. Refer to
“Fig. 2-16. Step Editor Window”, “Table 2-15. Items and Functions of Step Editor Window”,
and “Table 2-16. Measurement Types and Functions”.
The contents displayed in the “Step Editor” vary depending on the component units and
conditions. This operation manual describes the “Step Editor” window when the ASC-
550L unit is connected. When using another injector, refer to the instruction manual of
the injector.

Fig. 2-16. Step Editor Window

NSX-5000V
Basic Operations 2-23

Table 2-15. Items and Functions of Step Editor Window

Item Function
Type Select “Blank”, “Standard”, “Sample”, or “Standby”. For details, refer to
“Table 2-16. Measurement Types and Functions”.
Sub Type The choices vary depending on the selected type. For details, refer to
“Table 2-16. Measurement Types and Functions”.
SD Select a PMT sensitivity and a measurement mode for SD-500.
Comment You can input a comment.
Blank ID Set the ID of blank measurement. Values such as average and RSD
are calculated for the same ID. When a blank ID is selected for sample
or standard measurement, values are calculated by subtracting blank
values.
Calib. ID Set the ID of calibration curve measurement. Results with the same ID
are adopted as a calibration curve and used for concentration
calculation in sample measurement.
Sample ID Set the ID of sample measurement. Values such as average and RSD
are calculated for the same ID.
Customer ID This ID can be set as a schedule search condition.
Site ID This ID can be set as a schedule search condition.
Sample Input sample information, such as sample volume and concentration.
information
Add This button adds a step at the bottom of the schedule.
Insert This button inserts a step above another step with a cursor.
Insert Below This button inserts a step below another step with a cursor.
Constant This button displays the constant window for inputting the same
contents repetitively.
Input the number of repeats and click [Add] or [Insert].
Overwrite The step with a cursor is overwritten.
Close This button closes the “Step Editor” window.

Table 2-16. Measurement Types and Functions

Type Sub Type Function


Blank Blank This setting specifies to perform blank measurement.
Conditioning This setting specifies to measure a sample as a
conditioning sample. Area values are displayed, but
concentration is not calculated. Report print is not
available.
Standard Calibration This setting specifies to measure calibration points for
a calibration curve.

NSX-5000V
2-24 Basic Operations

Type Sub Type Function


Sample Sample This setting specifies to measure a sample.
Spike Standard This setting specifies to perform measurement after
sample measurement by suctioning the sample and
another sample of known concentration
consecutively. Check whether there is interference
with measurement.
Standby Electric furnace This setting specifies to control the electric furnace
standby temperature to a temperature in stand-by status as
set by a VF-500 parameter.
Electric furnace This setting specifies to start electric furnace
ON temperature control and control the temperature to a
preset temperature.
Electric furnace This setting specifies to stop electric furnace
OFF temperature control.
Xenon Lamp This setting specifies to stop xenon lamp control.
OFF
Dry Gas ON This setting specifies to start gas flow control.
Dry Gas OFF This setting specifies to stop gas flow control.
Wait This setting specifies to maintain the step for the
specified time. Use this setting to set a wait time
before the next step.
Wait (date This setting specifies to maintain the step until the
designation) specified date and time. When the specified date and
time arrives, the next step starts.
Step Break This setting specifies to stop the progress of the step.
Click [Start] icon to run the step again.
Gas ON This setting specifies to start gas flow control and
control the gas flow to a preset flow rate.
Gas OFF This setting specifies to stop gas flow control.
Gas Standby This setting specifies to control the gas flow to a flow
rate in stand-by status as set by a VF-500 parameter.
Standby status This setting specifies to cancel the stand-by status of
cancel the electric furnace and gas flow that is set by a VF-
500 parameter.
Clearing of This setting specifies to clear effluent volume
Effluent information.

NSX-5000V
Basic Operations 2-25

2-4-11. ASC Program Setting Window

This section describes the ASC program setting window. To display the ASC program
setting window, click for ASC program in the schedule or Step Editor. The ASC
program is a set of parameters that can set conditions, such as absorption and injection,
for each step when the ASC-550L unit is used. Refer to “Fig. 2-17. ASC Program Setting
Window” and “Table 2-17. Items and Functions of ASC Program Setting Window”. For
details on the ASC program, refer to the instruction manual of ASC-550L.

1 2

3 4 5 6 8 10

7 9 11

Fig. 2-17. ASC Program Setting Window

Table 2-17. Items and Functions of ASC Program Setting Window

No. Item Function


1 Program number Number and name of the ASC program. This number is
and name displayed in the schedule and the Step Editor window.
2 ASC program Contents of the ASC program. For details on each item, refer
to the instruction manual of ASC-550L.
3 ASC-550L These fields display ASC-550L parameters. They are set in
parameter the method and schedule, so they cannot be set in this
window.
4 Add This button adds a new ASC program.
5 Edit This button edits the contents of the selected ASC program.
6 Delete This button deletes the selected ASC program.
7 Set as Default This button sets the selected ASC program as default. When
a new step is created, the set program number is
automatically input.
8 Import This button imports the exported ASC program.
9 Export This button exports the selected ASC program.
10 Select This button sets the selected ASC program as a program for
a step.

NSX-5000V
2-26 Basic Operations

No. Item Function


11 Cancel This button closes the window without setting the ASC
program. Programs set for steps are not changed.

2-4-12. Settings for Blank Measurement

To conduct blank measurement, make blank measurement settings for a schedule.


There are two methods: inputting settings directly into a step of the schedule and inputting
settings from the Step Editor window. The procedure for inputting settings from the Step
Editor window is described here.

(1) Select “Edit”-“Step Editor” of the menu to display the “Step Editor” window.
(2) Select “Blank” as type and sub type.
(3) Select sensitivity and measurement time conditions for SD-500.
(4) Input the blank ID.
(5) Select an ASC program and input B No. (bottle number).
(6) Input blank information (such as sample volume). Set the total of the sample volume
and solvent flush, etc. to 110% or less of the syringe capacity set when the schedule
or method was created.
(7) Click [Add] to add a step at the bottom of the schedule. Click [Insert] to insert a step
above another step with a cursor. Click [Insert Below] to insert a step below another
step with a cursor.
(8) To measure multiple blanks, repeat the operation of updating blank information and
clicking [Add], [Insert], or [Insert Below]. Click [Constant] to display the constant
window where you can input steps of the same contents collectively.

2-4-13. Standard Measurement Setting

To prepare a calibration curve, make standard measurement settings for a schedule.


There are two methods: inputting settings directly into a step of the schedule and inputting
settings from the “Step Editor” window. The procedure for inputting settings from the “Step
Editor” window is described here.

(1) Select “Edit”-“Step Editor” of the menu to display the “Step Editor” window.
(2) Select “Standard” as the type and “Calibration” as the sub type.
(3) Select sensitivity and measurement time conditions for SD-500.
(4) Input the calibration ID and, as needed, input or select other IDs.
(5) Select an ASC program and input B No. (bottle number).
(6) Input working solution information (such as sample volume and concentration). Set
the total of the sample volume and solvent flush, etc. to 110% or less of the syringe
capacity set when the schedule or method was created.

NSX-5000V
Basic Operations 2-27

(7) Click [Add] to add a step at the bottom of the schedule. Click [Insert] to insert a step
above another step with a cursor. Click [Insert Below] to insert a step below another
step with a cursor.
(8) To measure multiple calibration points, repeat the operation of updating working
solution information and clicking [Add], [Insert], or [Insert Below]. Click [Constant] to
display the constant window to input steps of the same contents collectively.

2-4-14. Sample Measurement Setting

To measure a sample, make sample measurement settings for a schedule.


There are two methods: inputting settings directly into a step of the schedule and inputting
settings from the “Step Editor” window. The procedure for inputting settings from the “Step
Editor” window is described here.

(1) Select “Edit”-“Step Editor” of the menu to display the “Step Editor” window.
(2) Select “Sample” as the type and as sub type.
(3) Select sensitivity and measurement time conditions for SD-500.
(4) Input the sample ID and select the calibration ID. Input or select other IDs, as
needed.
(5) Select an ASC program and input B No. (bottle number).
(6) Input liquid sample information (such as sample volume and density). Set the total
of the sample volume and solvent flush, etc. to 110 % or less of the syringe capacity
set when the schedule or method was created.
(7) Click [Add] to add a step at the bottom of the schedule. Click [Insert] to insert a step
above another step. Click [Insert Below] to insert a step below another step.
(8) To measure multiple samples, repeat the operation of updating sample information
and clicking [Add], [Insert], or [Insert Below]. Click [Constant] to display the constant
window to input steps of the same contents collectively.

NSX-5000V
2-28 Basic Operations

2-4-15. Injection Status Check

This section describes injection status check. You can check the injection status by
clicking in the column of the injection status of the step in the schedule. Fig. 2-18
shows an example of the injection status check window.

POINT Injectable volume


When the total injection volume, including the sample, Solvent Flush, and
others, exceeds 110% of the syringe capacity, the ASC injection status is
indicated by red text and automatic measurement cannot start.
Set the total injection volume to 110% or less of the syringe capacity.

Fig. 2-18. Injection Status Check Window

NSX-5000V
Basic Operations 2-29

2-5. Measurement Operations

This chapter describes measurement operations. Measurement operations vary


depending on the injector, so check the relevant operations in the instruction manual
before measurement. This section describes operations with the ASC-550L unit. When
using an injector other than ASC-550L, refer to the instruction manual of the injector.

WARNING “WARNING” indication


When “WARNING” is displayed in the PC monitor, this indicates risk of
serious accidents.
When these messages are displayed, deal with problems immediately.

WARNING Microsyringe to use


Always use our specified microsyringe to inject a sample.
Failure to do so may break the microsyringe or cause abnormal
combustion, resulting in a fire.

WARNING Measurement parameters and


unit condition
If the condition of the units is different from the measurement parameters
set by the application software, the units may be damaged and explosive
combustion may cause a fire.
Particularly, if the parameters of the injector are different, a serious
accident may result. Be sure to check measurement parameters and the
condition of the units before starting measurement.

CAUTION Problems during measurement


If any problems occur during measurement, click [Abort] icon in a PC
window to stop measurement and the unit. Suspended measurement
(step) can not be continued. Create a new step.
Resolve the cause of the problem and check that the unit is in proper
condition. Then, resume measurement.

NSX-5000V
2-30 Basic Operations

CAUTION Maximum injection volume


The maximum injection volume of a sample is 200 µL.
Never inject a volume exceeding the maximum injection value.

POINT Waste bottle


Before measurement, check that the waste bottle is empty and click the
“Clear effluent volume” icon.
If it is not empty, dispose of the waste solutions and set the empty waste
bottle on the tray.

POINT Vial cap


Do not tighten the vial cap too tightly.
Doing so causes the pressure inside the vial to be negative when a sample
is absorbed, which may result in poor sample absorption.

(1) In the status window of the measurement window, check that all the units are in
Ready status.
(2) From the schedule, select “Parameter”-“ASC-550L” and check that the preset
syringe capacity matches the capacity of the gastight microsyringe on the ASC-550L
unit.
(3) In the step in the schedule, check that “Fill” does not indicate over capacity.
(4) Check that the vial for the measurement contains a sample.
(5) Check that there is a sufficient amount of a solution used as washing solution or
solvent flush in each vial.
(6) Click [Start] icon to start measurement. The ASC-550L unit starts operating.
(7) When a sample is injected and sulfur compounds in the sample are combusted, SO2
is generated and a peak appears in the chart.
(8) When measurement finished, area value is displayed in the step in the schedule
and “Status” will indicate “Finished”.
(9) If “The next step is started automatically.” is checked in the rule window, the next
step starts automatically.

NSX-5000V
Basic Operations 2-31

2-6. Results

2-6-1. Result Window

This section describes the result window. Fig. 2-19 shows the result window and Table
2-18 shows the items and functions of the result window. The composition of the result
window can be changed by selecting “Tool” in menu -“Result window layout”. The display
of the result window varies depending on the system configuration. Table 2-19 shows the
functions of result icons.

4 5 6
10 11

2
1

7 3 9

Fig. 2-19. Result Window

Table 2-18. Items and Functions of Result Window

No. Item Function


1 Chart Displays peaks obtained from measurement. The display
mode can be changed between overlay and serial display.
2 Statistical Displays the results of statistical processing.
processing
3 Redisplay Select a step and click [Redisplay] to display only the peak of
the selected step.
4 Calibration curve Displays the calibration directory. You can edit data with a
registered calibration ID. This tab is not displayed in Simple
mode.
5 Blank Displays the blank directory. You can edit data with a
registered blank ID. This tab is not displayed in Simple mode.
6 Audit trail PC operations are logged. You can search for data by setting
criteria. This tab is not displayed in Simple mode.
7 Result icons Display blank, calibration curve, sample, and re-analysis
windows, respectively.

NSX-5000V
2-32 Basic Operations

No. Item Function


8 Step Displays steps for which measurement is finished.
9 Rule This button allows you to set the number of display digits and
the unit. For details, refer to “2-6-1. Result Window”.
10 Directory Displays schedule, calibration curve, and blank information.
11 Schedule search You can search for a schedule by setting criteria.

Table 2-19. Result Icons

Name Icon Function


Blank results window Displays the blank results window. You can
view blank results, register results, and add
data to registered data.
Calibration results window Displays the calibration results window. You
can view calibration results, register results,
and add data to registered data.
Sample results window Displays the sample results window. You can
display results by ID.

Re-analysis window The re-analysis window is displayed. You can


reanalyze the peak of the selected results
and change the start and end times.

NSX-5000V
Basic Operations 2-33

2-6-2. Blank Results Window

This section describes the blank results window. Fig. 2-20 shows the blank results window
and Table 2-20 shows the items and functions of blank results window.

1 3
2
4

Fig. 2-20. Blank Results Window

Table 2-20. Items and Functions of Blank Results Window

No. Item Function


1 PMT Sense Select a PMT sensitivity. If the PMT sensitivity does not
match, no blank ID is displayed.
2 Blank ID Select the blank ID whose results you want to display.
3 Data addition to Add the displayed blank data to the data of an already
the registered ID registered blank ID and register it with a different name.
4 Blank registration Register the data of the displayed blank ID.
5 Statistical This area displays the results of statistical processing.
processing
6 Step This area displays the data of the selected blank ID. Check
the “Not Used” box to prevent the step from being reflected
in the statistical results.

NSX-5000V
2-34 Basic Operations

2-6-3. Calibration Results Window

This section describes the calibration results window. Fig. 2-21 shows the calibration
results window and Table 2-21 shows the items and functions of calibration results
window. For calibration types, refer to “Calibration types”.

1
2
3

5 6

Fig. 2-21. Calibration Results Window

Table 2-21. Items and Functions of Calibration Results Window

No. Item Function


1 PMT Sense Select a PMT sensitivity. If the PMT sensitivity does not
match, no calibration ID is displayed.
2 Calibration ID Select the calibration ID whose results you want to display.
3 Factor Calculation Select “Automatic”, “1 Fixed”, or “Manual input”.
4 Appropriate curve Select the type of the calibration curve.
5 Data addition to Add the displayed calibration data to the data of an already
the registered ID registered calibration ID and register it with a different name.
6 Calibration curve Register the data of the displayed calibration ID.
registration
7 Step This area displays the data of the same calibration ID. Check
the “Not Used” box to prevent the step from being reflected
in calibration.

NSX-5000V
Basic Operations 2-35

Calibration Types

When “Automatic” is selected as factor calculation, the following four types of approximate
curves become available: calibration curve as a linear equation which passes through the
origin, calibration curve as a linear equation which does not pass through the origin,
calibration curve as a quadratic equation which passes through the origin, and calibration
curve as a quadratic equation which does not pass through the origin. X, Y, A, B, and C
are used to represent absolute amount, area value, quadratic coefficient, linear coefficient,
and intercept, respectively. The following describes the characteristics of each calibration
curve (approximate curve). Select the calibration curve type appropriate for measurement
results.

 Calibration curve as a linear equation which passes through the origin (Y=BX)
This is a calibration curve that has only a linear coefficient (slope) without an
intercept that a linear equation which does not pass through the origin. Since this is
a calibration curve from which blank is deducted, it is used when the absolute
amount of a sample is infinitesimal. At least one calibration point is required.

 Calibration curve as a linear equation which does not pass through the origin (Y=BX
+C)
A calibration curve approximated by a linear equation. At least two calibration points
with different absolute amounts are required.

 Calibration curve as a quadratic equation which passes through the origin (Y=AX2+
BX)
This is a calibration curve that has only a quadratic coefficient and a linear coefficient
without an intercept that a quadratic equation which does not pass through the origin.
This is not a calibration curve where the origin is added to calibration points. This is
used when the absolute amount of a sample is infinitesimal. At least three calibration
points with different absolute amounts are required.

 Calibration curve as a quadratic equation which does not pass through the origin (Y=
AX2+BX+C)
A calibration curve approximated by a quadratic equation. At least three calibration
points with different absolute amounts are required.

If the calibration point criterion is not satisfied, “0” is input as the quadratic coefficient or
intercept. In this case, even a calibration curve as a “linear equation which does not pass
through the origin” passes the origin and a “calibration curve as a quadratic equation”
becomes a calibration curve as a liner equation.

NSX-5000V
2-36 Basic Operations

When “Manual input” is selected as factor calculation and you select, for approximation
calculation, any of the four types: calibration curve as a linear equation which passes
through the origin, calibration curve as a linear equation which does not pass through the
origin, calibration curve as a quadratic equation which passes through the origin, and
calibration curve as a quadratic equation which does not pass through the origin, you can
input corresponding quadratic coefficient, liner coefficient, and intercept values.
When “1 Fixed” is selected as calculation curve factor calculation, a calculation curve
where Y = X is obtained.

2-6-4. Sample Results Window

This section describes the sample results window. Fig. 2-22 shows the sample results
window and Table 2-22 shows the items and functions of sample results window.

1 2

Fig. 2-22. Sample Results Window

Table 2-22. Items and Functions of Sample Results Window

No. Item Function


1 PMT Sense Select a PMT sensitivity. If the PMT sensitivity does not
match, no sample ID is displayed.
2 Sample ID Select the sample ID whose results you want to display.
3 Statistical This area displays the results of statistical processing.
processing
4 Step This area displays data with the same sample ID. Check the
“Not Used” box to prevent the step from being reflected in the
statistical results.

NSX-5000V
Basic Operations 2-37

2-6-5. Re-analysis Window

This section describes the re-analysis window. Fig. 2-23 shows the re-analysis window
and Table 2-23 shows the items and functions of re-analysis window. By displaying the
step peak selected in the result window at re-analysis and changing measurement start
and end times, area values can be recalculated. When several peaks are displayed, you
can analyze them while comparing them.

1 2 3
4
5
6

7
8
9
10

11

Fig 2-23. Re-analysis Window

Table 2-23. Items and Functions of Re-analysis Window

No. Item Function


1 Start bar Position at which peak read starts. You can change the point
by picking the bar.
2 End bar Position at which peak read ends. You can change the point
by picking the bar.
3 Step No. When only one peak is displayed, the step number of the
peak is displayed. When several peaks are displayed, step
numbers are not displayed.
4 Peak time The time from the start to the end is displayed. When the
peak time is changed, the area value changes.
5 Area value The area value after peak time change is displayed.

NSX-5000V
2-38 Basic Operations

No. Item Function


6 Apply to this data This button overwrites the area value of the selected step
with that obtained using the changed peak time. Unless this
button is clicked, data will not be updated.
7 Apply to This button changes a parameter (measurement time) of the
parameters same schedule.
8 Return to the This button returns the positions of the start and end bars to
original the original positions immediately after the measurement.
9 Link start with end Check this checkbox to change the positions of the start and
end bars while the width remains fixed.
10 Range unification Use this button when multiple steps are selected. The
positions of the start and end bars currently being edited will
be applied to the other selected steps.
11 Step This area displays data selected in the result window. Select
the step you want to reanalyze.

NSX-5000V
Basic Operations 2-39

2-7. Print

2-7-1. Report Settings Window

This section describes the report settings window. Fig. 2-24 shows the report settings
window and Table 2-24 shows the items and functions of report settings window. The
display of the report settings window varies depending on the system configuration.

1
2
3
4

5 7
8
6 9

10

11

12 13 14

Fig. 2-24. Report Settings Window

Table 2-24. Items and Functions of Report Settings Window

No. Item Function


1 Comment You can input comments in a summary report.
2 Edit Header This button displays the “Edit Header” window.
3 Summary Report Check this box to print results, including electric furnace
temperature, gas flow, calibration curve, and sample
average.
4 Measurement report of Check this box to print the measurement result of a
the selected step selected step.
5 Select All Click this button to check all the report preparation
condition checkboxes. Click it again to uncheck all the
checkboxes.
6 Parameter The parameters of each unit will be printed.

NSX-5000V
2-40 Basic Operations

No. Item Function


7 All data Area values, concentration, and other data will be
printed.
8 Chart Peaks will be printed.
9 Curve An approximate calibration curve will be printed.
10 No print of excluded Steps whose “Not Used” box is checked will not be
steps printed.
11 Chart Setting This button displays the chart setting window.
12 Preview This button displays the print preview window.
13 Print This button starts printing.
14 OK This button saves the report settings and closes the
“Report Settings” window.

2-7-2. Printing

You can run printing from the setup, measurement, or result window. The schedule
selected in each window will be printed. Select a schedule to print and run printing by the
following procedure.

POINT Printing of ASC program


When ASC-550L is selected as the parameter in the “Report Settings”
window, click [Preview] or [Print] to display the window where you select
the ASC program to print. Highlight the number of the ASC program to
print, and click [Select]. To print multiple ASC programs, highlight the
numbers of the ASC programs, and click [Select].

(1) Click [Print] icon or select “File”-“Print” from the menu to display the “Report
Settings” window.
(2) Make report settings. Refer to “2-7-1. Report Settings Window”. Click [OK] to save
the report settings. Click [Preview] to display a print preview.
(3) Click [Print] in the “Report Settings” window to start printing.

NSX-5000V
Basic Operations 2-41

2-8. Post-Measurement Operations

2-8-1. Shutdown Window

This section describes the shutdown window. Fig. 2-25 shows the shutdown window and
Table 2-25 shows its items and functions of the shutdown window. The display of the
shutdown window varies depending on the system configuration.

1
2

3 4

Fig. 2-25. Shutdown Window

Table 2-25. Items and Functions of the Shutdown Window

No. Item Function


1 OFF switch Click this switch to turn off the item.
2 Batch processing This button collectively turns off all items.
3 Disconnect This button disconnects the unit from the PC.
4 Navigation This button displays the navigation window. Navigation
enables you to check the procedures for shutting down units.

NSX-5000V
2-42 Basic Operations

2-8-2. Shutdown

This section describes NSX-5000V shutdown after measurement. If the nitrogen detector
is connected, also refer to the operation manual of TN-5000V.

WARNING Cooling of the electric furnace


Do not stop the power supply until the temperature of the electric furnace
drops to 300 degrees Celsius or lower because the electric furnace needs
to be cooled by the fan. Do not shut down the application software while
the electric furnace is hot. Doing so makes it impossible to check the
temperature of the electric furnace.

(1) In the shutdown window, set the SD-500 xenon lamp and dry gas to “OFF”.
(2) Set the electric furnace of VF-500 to “OFF”.
(3) Set the gas of VF-500 to “OFF”.
(4) Wait until the temperature of electric furnace becomes 300 degrees Celsius or lower.
(5) Select “File”-“Exit” from the menu or click [×] at the upper right of the window to exit
the application software. When you exit the application software, communication
with the units is disconnected and the injector starts initialization.
(6) Turn off the power of the PC, monitor, and printer.
(7) Turn off the power switches of VF-500, SD-500, and the injector.
(8) Close the main valves of oxygen and argon cylinders. When using N2 gas or dry Air
as the dry gas of SD-500, close the main valve of the cylinder.
(9) If a waste bottle is on the tray of the injector, dispose of the waste solutions in the
waste bottle and set the empty waste bottle again on the tray.

NSX-5000V
Advanced Operations 3-1

Section 3: Advanced Operations


This section describes advanced operations, such as functions and settings.

3-1. Disconnection and Connection

3-1-1. Communication Disconnection

This section describes communication disconnection. Click [Disconnect] in the shutdown


window or select “File”-“Disconnect” from the menu to disconnect communication with the
vertical furnace and communication of the whole system.
In Advanced mode, you can disconnect communication with individual units. However,
communication with the vertical furnace or units with which measurement is being taken
cannot be disconnected individually. Disconnect communication with each unit by the
following procedure. Refer to “Fig. 3-1. Status Window”.

(1) Click [Status] in the measurement window to display the status window.
(2) Click [Disconnect] to the right of a unit name in the status window to disconnect
communication with the unit.

Fig. 3-1. Status Window

3-1-2. Unit Connection

This section describes unit connection. When starting a unit after starting the application
software offline or when disconnecting and reconnecting communication with a unit,
connect the unit by the following procedure.

(1) Turn on the power switch of the unit to turn on the power.
(2) Select “File”-“Connect” from the menu to display the port search window. Select the
port to use with the tab, and click [Open Port] to connect the unit.
Units cannot be connected during initialization. After initialization finishes, connect
them.

NSX-5000V
3-2 Advanced Operations

3-2. User Settings

This section describes user settings. You can make user settings to set user information
and operation authority.

POINT User settings


User settings can be made by users whose user ID is “Administrator”.
Other user IDs cannot make user settings. Log in as “Administrator” to
make user settings.

3-2-1. User Management Window

Select “File”-“User management” from the menu to display “User management” window.
Refer to “Fig. 3-2. User Management Window” and “Table 3-1. Items and Functions of
User Management Window”.

2 3 4

Fig. 3-2. User Management Window

Table 3-1. Items and Functions of User Management Window

No. Item Function


1 User list Displays registered user information.
2 Add Adds a new user. Clicking this button displays the “Edit User
Account” window.
3 Edit Edits registered user settings. Clicking this button displays
the “Edit User Account” window.
4 Delete Deletes the selected user. “Administrator” cannot be deleted.

NSX-5000V
Advanced Operations 3-3

3-2-2. Edit User Account Window

Click “Add” or “Edit” in the “User management” window to display the “Edit User Account”
window. Fig. 3-3 shows the “Edit User Account” window and Table 3-2 shows the items
and functions of “Edit User Account” window.

1
2

5
6
7
8
9

Fig. 3-3. Edit User Account Window

Table 3-2. Items and Functions of Edit User Account Window

No. Item Function


1 User ID This ID is displayed at logon.
2 Password Set the password for logon.
3 Level Select “Administrator”, “Analyzers”, or “Operators”. Authority
depends on the selected level.
4 User information Input the company name and contact information.
5 Export This button exports user information and authority.
6 Import This button imports user information and authority.
7 Unit option Set operation authority for units and modes.
settings
8 Return to default This button returns the operation authority to the default.
9 This user ID is Check this checkbox to display the user ID as a choice in the
displayed in the logon window.
logon list.

NSX-5000V
3-4 Advanced Operations

3-3. Column Display Setting

This section describes column display setting for schedule column names. Select “File”-
“Column Setting” from the menu to display “Column Setting” window. Refer to “Fig. 3-4.
Column Setting Window” and “Table 3-3. Items and Functions of Column Setting Window”.

2
3
4

Fig. 3-4. Column Setting Window

Table 3-3. Items and Functions of Column Setting Window

No. Item Function


1 Column items This area shows the display order of columns and indicates
whether or not the columns are displayed. Check the
checkboxes of items to display them as columns. Uncheck
the checkboxes of items to hide them.
2 Column fixing line Columns set above this line are always fixed to the left. They
are not scrolled horizontally even when the schedule table is
scrolled horizontally.
3 Up This button moves the selected column up by one position in
the display order.
4 Down This button moves the selected column down by one position
in the display order.

NSX-5000V
Advanced Operations 3-5

3-4. Import and Export

This section describes the import and export functions. The NSX-5000 application
software enables you to export data saved in the database and import it in the NSX-5000
application software installed on another PC. Export calibration curve and blank data
registered in the database.

3-4-1. Import and Export of a Schedule

Importing and exporting a schedule enables you to conduct measurement with the same
measurement parameters and step information even on a different PC. When a schedule
is exported, the method used with the schedule is also exported. When a schedule is
imported, its method is also imported. Export and import a schedule by the following
procedure.

Export of a Schedule

(1) Select “File”-“Export/Import”-“Schedule”-“Export” from the menu to display the


schedule viewer window. Refer to “Fig. 3-5. Schedule Directory Window”.

Fig. 3-5. Schedule Directory Window

(2) Select the schedule to export and click [Selection].


(3) Select the destination of export, input the file name, and click [Save] to run the export.

NSX-5000V
3-6 Advanced Operations

Import of a Schedule

(1) Select “File”-“Export/Import”-“Schedule”-“Import” from the menu to display the


“Schedule folder selection” window. Refer to “Fig. 3-6. Schedule Folder Selection
Window”.

Fig. 3-6. Schedule Folder Selection Window

(2) Select the save destination of the schedule and click [OK] to display the “Method
folder selection” window. Refer to “Fig. 3-7. Method Folder Selection Window”.
However, when “Method import to the same folder” is checked, the method is saved
in the same folder and the “Method folder selection” window is not displayed.

Fig. 3-7. Method Folder Selection Window

(3) Select the save destination of the method and click [OK].
(4) Select the schedule file to import and click [Open] to run the import.

NSX-5000V
Advanced Operations 3-7

3-4-2. Import and Export of a Method

Importing and exporting a method enables you to conduct measurement with the same
measurement parameters even on a different PC. Export and import a method by the
following procedure.

Export of a Method

(1) Select “File”-“Export/Import”-”Method”-“Export” from the menu to display the method


directory window. Refer to “Fig. 3-8. Method Directory Window”.

Fig. 3-8. Method Directory Window

(2) Select the method to export and click [Selection].


(3) Select the destination of export, input the file name, and click [Save] to run the export.

Import of a Method

(1) Select “File”-“Export/Import”-“Method”-“Import” from the menu to display the


“Method folder selection” window. Refer to “Fig. 3-7. Method Folder Selection
Window”.
(2) Select the save destination of the method and click [OK].
(3) Select the method file to import and click [Open] to run the import.

NSX-5000V
3-8 Advanced Operations

3-5. Registration and Read

The NSX-5000 application software enables you to register measured blank and
calibration curve data in the database and read it into a different schedule.

POINT Use of registered data


Blank and calibration curve values change significantly depending on the
condition of units and other factors. Basically, measure the values on every
measurement day. Although the registration and read functions are
provided, use of them is not recommended. Before reading and using
registered data, be sure to run a system check to confirm that there are no
problems with the condition or sensitivity of units.

3-5-1. Blank Registration

This section describes blank registration. For blank registration, perform the following
procedure in the “Blank results” window from the result window.

(1) Click in the result window to display the “Blank results” window.
(2) Display the blank data to register in the “Blank results” window and click [Blank
registration]. Refer to “Fig. 3-9. Blank Results Window”.
By clicking [Data addition to the registered ID], you can add the displayed blank data
to already registered blank data and register it with a different name.

Fig. 3-9. Blank Results Window

NSX-5000V
Advanced Operations 3-9

(3) Input the blank name to register in the “Blank File Registration” window to register
blank. Refer to “Fig. 3-10. Blank File Registration Window”.

Fig. 3-10. Blank File Registration Window

By clicking the tab for blank files in the result window in Advanced mode, you can
check registered blank data.

3-5-2. Blank Read

This section describes blank read. Blank read is a function to read blank data registered
in the database into a schedule. Read blank data by the following procedure.

(1) In the setup or measurement window, click [Blank read] to display the blank data
selection window.
(2) In the blank data selection window, select blank data and read it into your desired
schedule. Refer to “Fig. 3-11. Blank Directory Window”.

Fig. 3-11. Blank Directory Window

NSX-5000V
3-10 Advanced Operations

The read blank data is inserted as the first and hidden step of the schedule. Check
“Display of hidden steps” in “Others” in the “Rule” window to display hidden steps.
Refer to “Fig. 3-12. Rule Window (Others)”.

Fig. 3-12. Rule Window (Others)

NSX-5000V
Advanced Operations 3-11

3-5-3. Calibration Curve Registration

This section describes calibration curve registration. For calibration curve registration,
perform the following procedure in the “Calibration results” window from the result window.

(1) Click in the result window to display the “Calibration results” window.
(2) Display the calibration curve data to register in the “Calibration results” window and
click [Calibration curve registration]. Refer to “Fig. 3-13. Calibration Results Window”.
By clicking [Data addition to the registered ID], you can add the displayed calibration
curve data to already registered calibration curve data and register it with a different
name.

Fig. 3-13. Calibration Results Window

(3) Input the calibration name to register in the “Calibration Curve File Registration”
window to register the calibration curve. Refer to “Fig. 3-14. Calibration Curve File
Registration Window”.

Fig. 3-14. Calibration Curve File Registration Window

NSX-5000V
3-12 Advanced Operations

By clicking the tab for calibration curve files in the result window in Advanced mode,
you can check registered calibration curve data.

3-5-4. Calibration Curve Read

This section describes calibration curve read. Calibration curve read is a function to read
calibration curve data registered in the database into a schedule. Read calibration curve
data by the following procedure.

(1) In the setup or measurement window, click [Calibration curve read] to display the
calibration curve data selection window.
(2) In the calibration curve data selection window, select calibration curve data and read
it into your desired schedule. Refer to “Fig. 3-15. Calibration Curve Directory
Window”.

Fig. 3-15. Calibration Curve Directory Window

The read calibration curve data is inserted as the first and hidden step of the
schedule. Check “Display of hidden steps” in “Others” in the “Rule” window to
display hidden steps. Refer to “Fig. 3-12. Rule Window (Others)”.

NSX-5000V
Advanced Operations 3-13

3-6. Continuous Schedule Run

This section describes continuous schedule run. This function starts preset schedule
steps automatically when all the steps of the schedule ends, if the schedule execution
order is set. You can start a schedule at any time by setting a start time. However, if
another schedule is running, the next schedule starts after the running schedule ends.
This function cannot be used in Simple mode. Change the mode to Advanced to use the
function.

3-6-1. Continuous Run Schedule Setting Window

Select “Measurement”-“Continuous run schedule setting” from the menu to display the
“Continuous run schedule setting” window. Refer to “Fig. 3-16. Continuous Run Schedule
Setting Window” and “Table 3-4. Items and Functions of Continuous Run Schedule
Setting Window”.

1
2 3
4
5
6
7
8
9
10

11

Fig. 3-16. Continuous Run Schedule Setting Window

Table 3-4. Items and Functions of Continuous Run Schedule Setting Window

No. Item Function


1 Status indication This field indicates whether continuous schedule run is
enabled or disabled.
2 Schedule list When a schedule is added, it is displayed in this list.
3 Add This button adds a schedule to be run continuously to the list.
4 Delete This button deletes the selected schedule from the
continuous run list.
5 Delete All This button deletes all schedules from the continuous run list.
6 Up This button moves the selected schedule up in the run order.

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3-14 Advanced Operations

No. Item Function


7 Down This button moves the selected schedule down in the run
order.
8 Edit This button is used to edit and set the start time.
9 Clear This button clears the set start time.
10 CSV This button exports the schedule list to a CSV file.
11 Enable/Disable This button enables/disables continuous schedule run.

3-6-2. Continuous Run Schedule Setting

This section describes continuous run schedule setting. Make continuous run schedule
settings by the following procedure.

CAUTION Error during continuous run


If an error occurs during continuous schedule run, the operation of the unit
stops, but the application software may not show that it is stopped.
If the application software is running the unit even when the unit is stopped
due to an error, click [Cancel] icon to stop it and properly deal with the
error. Then, click [Start] icon again.

POINT Conditions for continuous run


To run schedules continuously, the system configurations and contents
(syringe capacity, etc.) of the schedules must match.
Only schedules that match the schedule set at the top in terms of the
system configuration and the contents (syringe capacity) are displayed
when [Add] is clicked. Continuous schedule run can be performed even
when the electric furnace temperature and gas flow, which are set in a
method, do not match.

POINT Schedule setting


To run schedules continuously, do not set “Step break” for the final step of
the schedules.
When “Step break” is run, the next schedule cannot start.

(1) Prepare all the schedules to be used for continuous schedule run.

NSX-5000V
Advanced Operations 3-15

(2) Click [Add] in the “Continuous run schedule setting” window and select a schedule.
Click [Selection] to add it to the continuous run list.
(3) Add or delete schedules and set the run order by referring to “3-6-1. Continuous
Run Schedule Setting Window”.
(4) To set a start date and time, click [Edit] and set the date and time.
(5) To enable continuous run, click [Enable] and check that the status is indicated as
“Enabled”. (To disable continuous run, click [Disable] and check that the status is
indicated as “Disabled”.)
(6) Click [×] to exit the “Continuous run schedule setting” window.
(7) Open the schedule set at the top of the schedule list and click [Prepare] for the
schedule.
(8) To start the schedules immediately, check that units are ready for measurement and
click [Start] icon to start measurement.

NSX-5000V
3-16 Advanced Operations

3-7. Spike Standard

Spike Standard is a function to check whether there is interference with measurement by


absorbing and measuring a sample and another sample of known concentration
consecutively immediately after measuring the sample. To use this function, ASC-550L
needs to be used as the injector. This section describes the procedure using the Spike
Standard setting window shown in Fig. 3-17 as an example.

POINT Limitation on the function


When the automatic syringe dilution function is enabled for the schedule,
the Spike Standard function cannot be used.
To use the Spike Standard function, do not check the checkbox for the
automatic syringe dilution function when preparing a schedule.

(1) Set a sample to bottle No.1 and a solution of known concentration (for example, 1
µg/mL) to bottle No.2.
(2) Make sample measurement settings (bottle No.1) by referring to “2-4-14. Sample
Measurement Setting”.
(3) Select “Sample” as the type and “Spike Standard” as sub type for the next step and
input information on bottle No.2. The sample ID input here must be the same sample
ID as input for the immediately previous step.
(4) Check that units are ready for measurement and click [Start] icon to start
measurement. 20 µL of the sample in bottle No.1 is sampled and measured to
calculate concentration.
(5) When the measurement described in (4) ends, the system proceeds to the next step.
20 µL of the 1 µg/mL solution in bottle No.2 and then 20 µL of the sample in bottle
No.1 are sampled and measured.
(6) Concentration is calculated from the area value obtained by subtracting the area
value in (4) from the area value in (5) and the sample volume, and a recovery rate
is calculated. This concentration calculation uses the calibration curve used in (4).
In the result window, the area value column displays the measurement value and
the area value after subtraction and the concentration column displays the
concentration and recovery rate.

Fig. 3-17. Spike Standard Setting Window

NSX-5000V
Advanced Operations 3-17

3-8. Automatic Syringe Dilution

Automatic syringe dilution is a function that absorbs the liquid to be measured and the
solvent for dilution sequentially with a syringe to dilute the liquid in the syringe in a pseudo
manner and injects it into the unit. To use this function, the ASC-550L unit needs to be
used as the injector.

CAUTION Solvent for dilution


Select a solvent for dilution that easily dissolves the sample and has no
impact on measurement.
If a solvent that deposits or adheres as the result of mixing is selected, the
syringe or the ASC-550L unit may be damaged. In addition, if the solvent
has an impact on measurement, correct measurement results cannot be
shown.

POINT Use of automatic syringe


dilution
The automatic syringe dilution function does not effectively work for all
samples. Due to the property and homogeneity of the sample, the results
of measurement may be different from those when the liquid is manually
diluted. Be sure to check the effectiveness before using the function.

POINT Contamination of diluent solvent


Running automatic syringe dilution may cause the diluent solvent to be
contaminated by the sample and correct dilution may not be achieved.
Prepare multiple vials for the diluent solvent so as not to dilute the liquid
with the contaminated diluent solvent.

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3-18 Advanced Operations

3-8-1. Method and Schedule Setting

For the automatic syringe dilution function, a dedicated schedule needs to be set. Set a
method and schedule by the following procedure.

(1) Click [Create] in “Method” in the setup window in Advanced mode to display the
method preparation window.
(2) Set a syringe capacity and liquid type for ASC-550L in the method preparation
window. For details on the preparation procedure, refer to “2-3-3. New Method
Preparation”.
(3) Click [Create] in “Schedule” in the setup window in Advanced mode to display the
schedule preparation window.
(4) Check the checkbox for automatic syringe dilution for ASC-550L in the schedule
preparation window, select the method created for automatic syringe dilution, and
create a schedule. For details on the preparation procedure, refer to “2-3-4. New
Schedule Preparation”.
(5) Register a schedule, as a template, for which the automatic syringe dilution function
is enabled. This enables you to prepare a schedule with the template and use it
even in Simple mode. For details on the template registration procedure, refer to “2-
3-5. Template Registration”.

3-8-2. Step Editor Window (Automatic Syringe Dilution)

When the automatic syringe dilution function is used, setting items for B2 bottle No., which
is a solvent for dilution, and a sample volume are added, in addition to regular Step Editor
items. Besides, “B2→B1” checkbox is added. Check the checkbox to let the syringe
absorb samples in order from B2 to B1. Uncheck it to let the syringe absorb samples in
order from B1 to B2. Fig. 3-18 shows an example of the “Step Editor” window when
automatic syringe dilution is used. For details on other items in Step Editor, refer to “2-4-
10. Step Editor Window”.

Fig. 3-18. Example of Step Editor Window When Automatic Syringe Dilution Is Used

NSX-5000V
Advanced Operations 3-19

3-8-3. Calibration Measurement with Automatic Syringe Dilution

This section shows an example of preparing a calibration curve by diluting a high-


concentration working solution with the automatic syringe dilution function. In this
example, a 50 µL gastight microsyringe is used to prepare a calibration curve from a 100
µg/mL working solution.

(1) Set a vial with 100 µg/mL working solution in bottle No.1 and a measurement vial
with a diluent solvent in bottle No.2.
(2) Enter values in the Step Editor window or directly in a step by referring to “Table 3-
5. Example of Step Input (Calibration)” and “Table 3-6. Example of an ASC
Program”. Only the concentration of the bottle No. set in B1 can be input. The
absolute volume of the calibration curve is calculated from the concentration of B1
and the sample volume.

Table 3-5. Example of Step Input (Calibration)

B1 No. Sample B2 No. Sample Concentration after dilution


volume 1 volume 2 (dilution ratio)
(µL) (µL)
2 0 2 40 0 µg/mL (Diluent solvent only)
1 2 2 38 5 µg/mL (20 times)
1 4 2 36 10 µg/mL (10 times)
1 8 2 32 20 µg/mL (5 times)
1 20 2 20 50 µg/mL (2 times)
1 40 1 0 100 µg/mL (No dilution)

Table 3-6. Example of an ASC Program

Item Setting value


Solvent Air (µL) 0
Solvent Flush volume (µL) 10
Pre Air volume (µL) 3*
Post Air volume (µL) 0
Suction rate 1 (µL/s) 5
Wait time after suction 1 (s) 10
Injection rate (µL/s) 1.2
Wait time after injection (s) 2
Suction rate 2 (µL/s) 10
Wait time after suction 2 (s) 5

* If water is used as solvent flush for non-aqueous sample, you can set a value of
0 for operation.

NSX-5000V
3-20 Advanced Operations

(3) Check that units are ready for measurement and click [Start] icon to start
measurement.
(4) Check the operation during measurement and the results of measurement to
confirm that the calibration curve is prepared properly.

3-8-4. Sample Measurement with Automatic Syringe Dilution

This section shows an example of measurement by diluting a sample with automatic


syringe dilution. In this example, a 50 µL gastight microsyringe is used to measure a
sample by diluting it by 10 times.

POINT Cautions in sample


measurement
For sample measurement with automatic syringe dilution, pay attention to
the property of the sample.
High-viscosity samples cannot be absorbed by a gastight microsyringe,
and thus the preset dilution may not be achieved. Although making the fill
rate slower or the wait time after absorption longer may make it possible to
absorb a high-viscosity sample, these measures are not applicable to all
samples.
In addition, heterogeneous samples results in a poor repeatability and
accurate measurement may not be performed. When you find it difficult to
measure a sample with automatic syringe dilution, measure a manually
diluted solution.

(1) Set a sample in bottle No.11 and a measurement vial with a diluent solvent in bottle
No.12.
(2) Enter values in the Step Editor window or directly in a step by referring to “Table 3-
7. Example of Step Input (Sample)” and “Table 3-6. Example of an ASC Program”.
Since concentration is calculated from the sample volume in the bottle No. set in B1,
be sure to input the sample volume in B1.

Table 3-7. Example of Step Input (Sample)

B1 No. Sample volume 1 B2 No. Sample volume 2 Dilution ratio


(µL) (µL)
11 4 12 36 10 times

(3) Check that units are ready for measurement and click [Start] icon to start
measurement.
(4) Check the operation during measurement and the results of measurement to
confirm that the sample measurement is performed properly.

NSX-5000V

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