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ZN5SQVE-00_TS-5000V
ZN5SQVE-00_TS-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
(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 Composition
About Indications
About Terms
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.
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
Cautions
Read the following cautions carefully to use the unit correctly and safely.
NSX-5000V
SAFETY PRECAUTIONS 3
NSX-5000V
4 SAFETY PRECAUTIONS
NSX-5000V
SAFETY PRECAUTIONS 5
NSX-5000V
6 SAFETY PRECAUTIONS
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
NSX-5000V
Table of Contents 3
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.
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
NSX-5000V
1-2 Preparation
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”.
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.
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.
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.
(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
NSX-5000V
1-4 Preparation
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.
(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
NSX-5000V
Preparation 1-5
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.
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”.
NSX-5000V
1-6 Preparation
(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
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.
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”.
NSX-5000V
1-8 Preparation
(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
(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
2-1. Start Up
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.
2-1-3. 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
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
NSX-5000V
Basic Operations 2-3
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
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
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.
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
NSX-5000V
Basic Operations 2-5
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.
NSX-5000V
2-6 Basic Operations
The procedure for preparing a schedule varies between the Simple and Advanced modes.
Check the operation procedure corresponding to the selected mode.
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)”.
NSX-5000V
Basic Operations 2-7
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
NSX-5000V
2-8 Basic Operations
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.
NSX-5000V
Basic Operations 2-9
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”.
(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.
NSX-5000V
2-10 Basic Operations
(1) In Advanced mode, select the “Tool” in menu -“Template registration” to display the
“Template registration” window.
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
(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.
NSX-5000V
2-12 Basic Operations
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
NSX-5000V
Basic Operations 2-13
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.
(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
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
NSX-5000V
Basic Operations 2-15
(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.
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”.
(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.
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.
NSX-5000V
Basic Operations 2-17
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
NSX-5000V
2-18 Basic Operations
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.
NSX-5000V
Basic Operations 2-19
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
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.
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
NSX-5000V
Basic Operations 2-21
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 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.
NSX-5000V
2-22 Basic Operations
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.
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.
NSX-5000V
Basic Operations 2-23
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.
NSX-5000V
2-24 Basic Operations
NSX-5000V
Basic Operations 2-25
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
NSX-5000V
2-26 Basic Operations
(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.
(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.
(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
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.
NSX-5000V
Basic Operations 2-29
NSX-5000V
2-30 Basic Operations
(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
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
NSX-5000V
2-32 Basic Operations
NSX-5000V
Basic Operations 2-33
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
NSX-5000V
2-34 Basic Operations
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
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.
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
NSX-5000V
Basic Operations 2-37
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
NSX-5000V
2-38 Basic Operations
NSX-5000V
Basic Operations 2-39
2-7. Print
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
NSX-5000V
2-40 Basic Operations
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.
(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
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
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.
(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
(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.
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
This section describes user settings. You can make user settings to set user information
and operation authority.
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
NSX-5000V
Advanced Operations 3-3
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
NSX-5000V
3-4 Advanced Operations
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
NSX-5000V
Advanced Operations 3-5
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.
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
NSX-5000V
3-6 Advanced Operations
Import of a Schedule
(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.
(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
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
Import of a Method
NSX-5000V
3-8 Advanced Operations
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.
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.
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”.
By clicking the tab for blank files in the result window in Advanced mode, you can
check registered blank data.
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”.
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)”.
NSX-5000V
Advanced Operations 3-11
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.
(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”.
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.
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”.
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
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.
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
Table 3-4. Items and Functions of Continuous Run Schedule Setting Window
NSX-5000V
3-14 Advanced Operations
This section describes continuous run schedule setting. Make continuous run schedule
settings by the following procedure.
(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
(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.
NSX-5000V
Advanced Operations 3-17
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.
NSX-5000V
3-18 Advanced Operations
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”.
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
(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.
* 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.
(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.
(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