MA-3000 NIC-600-2231-11 Instruction Manual PDF

Fully-automatic Thermal Vaporization
Mercury Analysis System

MA-3000
Instruction Manual
NIC-600-2231-11
Nippon Instruments Corporation

NIC-600-2231-11
Fully-automatic Thermal Vaporization

Mercury Analysis System
MA-3000
Instruction Manual
Table of Contents
1. INTRODUCTION ................................................................................................................ 1
1.1. Safety precautions ................................................................................................... 1

1.1.1. Meaning of safety alert symbols ....................................................................... 1
1.1.2. Installation precautions ..................................................................................... 1
1.1.3. Handling precautions ........................................................................................ 2
1.1.4. Maintenance precautions ................................................................................. 2
1.2. System Outline ......................................................................................................... 3
2. OPERATING PRINCIPLE .................................................................................................. 4
2.1. Operation ................................................................................................................. 4

2.2. Part names and functions ........................................................................................ 5
2.2.1. Front.................................................................................................................. 5
2.2.2. Inside front cover .............................................................................................. 6
2.2.3. Rear .................................................................................................................. 7
2.2.4. Internal components seen from the top ............................................................ 8
2.2.5. Internal components seen from the right .......................................................... 9
2.2.6. Internal components seen from the left .......................................................... 10
3. SPECIFICATIONS .............................................................................................................11
3.1. Standard configuration ............................................................................................ 11

3.2. Component specifications ....................................................................................... 11
4. SYSTEM INSTALLATION................................................................................................ 12
4.1. Conditions for installation ....................................................................................... 12

4.1.1. Environment for installation ............................................................................ 12
4.1.2. Power supply .................................................................................................. 12
4.2. Installation and connections .................................................................................. 13
4.2.1. MA-3000 ......................................................................................................... 13
4.3. Installing software .................................................................................................. 14
NIC-600-2231-11
4.3.1. Installing MA3Win ........................................................................................... 14

4.3.2. Installing animation display controller............................................................. 16
4.3.3. Installing USB Serial Converter driver ............................................................ 17
4.3.4. Setting Communication port ........................................................................... 18
4.3.5. How to uninstall MA3Win................................................................................ 20
4.3.6. How to upgrade MA3Win................................................................................ 20
4.3.7. How to upgrade the version of ROM built into the MA-3000 ......................... 21
4.3.8. The case of fail in updating firmware.............................................................. 22
5. MEASUREMENT .............................................................................................................. 23
5.1. Measurement Operation Flowchart ....................................................................... 23

5.2. Samples ................................................................................................................. 24
5.3. Necessary supplies for measurements ................................................................. 25
5.4. Articles recommended for measurement............................................................... 25
5.5. Preparation for measurement ................................................................................ 25
5.5.1. Preparing mercury standard solution ............................................................. 25
5.5.2. Blank treatment of sample boat...................................................................... 26
5.5.3. Blank treatment of additives ........................................................................... 26
5.6. Starting up the system ........................................................................................... 27
5.6.1. Starting the control software ........................................................................... 27
5.6.2. Starting the MA-3000 ...................................................................................... 27
5.6.3. Supplying carrier gas ...................................................................................... 28
5.6.4. Checking the tubes for leaks .......................................................................... 28
5.6.5. Conditioning .................................................................................................... 30
5.6.6. Discharging liquid from the drain tank ............................................................ 30
5.7. Measurement ......................................................................................................... 31
5.7.1. Blank check .................................................................................................... 31
5.7.2. Setting the measurement condition ................................................................ 31
5.7.3. Setting the table conditions ............................................................................ 33
5.7.4. Constructing the calibration curve .................................................................. 33
5.7.5. Measuring unknown samples ......................................................................... 37
5.7.6. Termination ..................................................................................................... 41
6. MAINTENANCE ............................................................................................................... 42
6.1. Inspection items ..................................................................................................... 42

6.1.1. Daily inspection............................................................................................... 42
6.1.2. Annual inspection ........................................................................................... 43
6.2. Errors and warnings ............................................................................................... 44
NIC-600-2231-11
6.3. Troubleshooting ..................................................................................................... 50

6.3.1. Degradation of peak sensitivity ...................................................................... 50
6.3.2. Outlying blank value ....................................................................................... 51
6.4. Maintenance........................................................................................................... 52
6.4.1. Leak check ...................................................................................................... 52
6.4.2. Dismounting the sample heating tube ............................................................ 53
6.4.3. Mounting the sample heating tube ................................................................. 55
6.4.4. Installation of the boat handling poker............................................................ 59
6.4.5. Removing the absorption cell ......................................................................... 60
6.4.6. Cleaning the absorption cell and joints........................................................... 62
6.4.7. Adjusting the sample changer ........................................................................ 63
6.4.8. Greasing the drive mechanism of the sample changer.................................. 67
6.4.9. Adjusting the optical system ........................................................................... 68
6.4.10. Adjusting the mass flow controller .................................................................. 69
6.4.11. Replacing the air pump tube (Option) ............................................................ 70
7. MA3WIN............................................................................................................................ 72
7.1. Basic screen........................................................................................................... 72

7.1.1. Control screen ................................................................................................ 72
7.1.2. Analysis screen............................................................................................... 73
7.1.3. Common controls............................................................................................ 74
7.1.4. Table window .................................................................................................. 75
7.2. List of menu commands ......................................................................................... 79
7.2.1. File (f) .............................................................................................................. 79
7.2.2. Edit (E) ............................................................................................................ 83
7.2.3. Run menu ....................................................................................................... 85
7.2.4. Table (T) menu commands ........................................................................... 101
7.2.5. Window (W) ................................................................................................... 110
7.2.6. Help................................................................................................................ 112
7.3. How to determine a calibration curve ................................................................... 113
7.3.1. 1Linear formula .............................................................................................. 113
7.3.2. 3 Cubic formula.............................................................................................. 113
7.4. Calculation formula for mercury amount and concentration................................. 115
7.5. Standard addition .................................................................................................. 116
7.6. R.Blank Calculation method ................................................................................. 117
8. CONTACT ........................................................................................................................118
NIC-600-2231-11 1. Introduction
1. Introduction
1.1. Safety precautions
For the safe use of this product, please observe the following precaution.
In no event shall Nippon Instruments Corporation, Inc. be liable for any direct,
indirect, punitive, incidental, special consequential damages, to property or life,
whatsoever arising out of or connected with the use or misuse of our products.
Please refer to the attached documents for the optional reagent dispenser and sample
changer.
1.1.1. Meaning of safety alert symbols
Indicates that incorrect handling could result immediately in death or

Danger
severe injury to the operator.
Indicates that incorrect handling could result in death or severe injury to
Warning
the operator.
Indicates that incorrect handling could result in moderate or minor injury to
Caution
the operator, or damage to property.
1.1.2. Installation precautions
 Be sure to connect the protective grounding to prevent electric shock.

Warning  If there is any risk of generation of any harmful gasses such as
halogen, sulfur and selenium during decomposition by heating, please
be sure to vent the exhaust gas.
 Comply with the installation environment and power specification.
Caution
Electric shock may occur.
 Install on flat, level, and stable workbench with surface parallel to floor.
 Never install the system anywhere volatile halide reagents such as
organic chlorine solvents are handled. Also avoid installation
anywhere those gases could enter.
1
1.1.3. Handling precautions
 Do not directly measure the sample decomposed with nitric acid. The
Warning
activated carbon in the exhaust gas filter may generate heat. Dilute the
sample until the concentration of nitric acid falls to 5wt% or less before
the measurement.
 Do not disassemble or modify the product. This may cause a
Caution
malfunction.
 Use the product after consulting the manual. Improper operation
may cause malfunction or bodily injury.
 Comply with the range of specifications. Failure may occur with
misuse.
 Do not operate with wet hands.
 Be careful when touching or handling any of the glass components or

they could be broken.
 Be sure to discharge any liquid from the drain tank once the work has
been completed. It is very important to confirm that the power has
been turned OFF before starting the discharge.
 If you don’t turn-on MA-3000 for a long time, the sample heating tube
might be obstructed or break by moisture absorption. If you don’t
turn-on MA-3000 more than 2 weeks, please turn on the MA-3000
power switch and do conditioning, or dismount the sample heating
tube and store it in a desiccator to prevent moisture absorption.
1.1.4. Maintenance precautions
 Maintenance of the heater must be carried out after the power has
Warning
been turned OFF and the heater has cooled down to close to normal
room temperature or it could result in burns.
 Shut OFF the power supply before staring the maintenance work.
Caution
Otherwise electric shock may occur.
 Be sure to do degreasing cleaning the O-ring before use. If degreasing
cleaning is not carried out, there is a possibility that the sample heating
tube will come off during measurement.
2
1.2. System Outline

The Mercury/MA-3000 is a mercury analysis system that realizes the quick,
highly-sensitive and precise quantitative measurement of mercury contained in liquids,
solids, and gases (requires optional unit) with very easy operation.
The system has a built-in auto sample changer as a standard feature that is operated
using a personal computer (hereafter “PC”).
After a sample has been set in place, the system automatically transfers it to the
measurement unit and performs the measurement, with the output data then being
analyzable in various ways such as through statistical calculations on a PC.
An optional unit being connected also allows reducing vaporization measurements as well
as the measurement of gas collection tubes.
It is strongly recommended to carefully read this manual before using the system in order
to ensure that its full performance can be utilized.
Mercury/MA-3000 System
3
NIC-600-2231-11 2. Operating principle
2. Operating Principle
2.1. Operation
The sample heating furnace (H-1) heats samples to evaporate any mercury compounds
contained in them. The decomposing furnace (H-2A, H-2B) then decomposes the mercury
compounds in the gases generated in H-1 to remove any interfering ingredients from
them.
The mercury collector (H-3) collects the atomized mercury gas in the form of gold
amalgam, removes any interfering ingredients, and condenses and purifies the mercury.
After the heat decomposition sequence has completed, the mercury collection tube is
heated to liberate the mercury again as mercury gas, and the absorbance is then
measured.
Cold-vapor atomic absorption at a wavelength of 253.7nm is used in the detection.
Pressure regulator
Mercury Activated
collecting tube carbon 1
Fan3 Oxygen cylinder
Light absorption cell 1

Fan1
Lamp Photoelectric
tube SIG1 Exhaust Heating
Light absorption vaporization
cell 2 Exhaust
Tray rack Light absorption
cell SIG2
Photoelectric
tube REF
Activated
carbon 2
Air pump (P2)

Option unit
Drain tank
Silencer
Flow Diagram
4
2.2. Part names and functions
2.2.1. Front
⑤
④
②
No. Name Function

 Top cover Locked whenever the power is ON.
* To remove the top cover, turn OFF the power and flip up
the ring latches.
 Front cover Locked whenever the power is turned ON to prevent any
accident which may occur while the sample changer is
activated.
* Cannot be opened/closed unless the top cover is
removed.
 Operation status “Green blinking”: Measurement in progress
LED “Green lights ON”: Stand by
“Red lights ON”: During maintenance, error
 Tray racks Ten racks from the top are used to hold boat trays and the
bottom rack is used as a place for a tray to evacuate when
an abnormal stop occurs.
A sensor is installed on each rack, and the measurement is
skipped if the sensor does not detect any tray on the rack.
Error alarming function is equipped and it generates an
alarm if a tray is inserted onto a rack where the
measurement is being performed.
A purge is performed in the rack with clean air to suppress
the increase of blank.
 Tray rack door Prevents trays from sliding out. Prevents the malfunction of
the tray detection sensor.
Equipped with a sensor which triggers an error alarm if the
door is open when a tray is transferred.
5
2.2.2. Inside front cover
③ ①
②
⑤
⑥
④
No. Name Function

 Z axis Inserts a boat into the sample heating tube
 Sample inlet Seals and secures the sample heating tube
 X axis For horizontal movement
 Y axis Motor for vertical movement, with trapezoidal
thread
 Arm Transfers a tray
Equipped with a tray detection sensor and detects
abnormal transfer of a tray
 Lift Lifts the sample boats
 Tray racks Holds 10 racks of trays
 Tray evacuation If there are any trays on the arm during an error
rack recovery, they are returned to this rack.
6
2.2.3. Rear
②
①
⑤
③ ④ ⑥
⑦
⑧
⑨
No. Name Function

 Pressure regulator Adjusted to 0.05MPa, and connected to an oxygen
cylinder
 Case fan Exhausts heat
 Activated charcoal for Used to remove mercury from exhaust gas
exhaust gas
 Activated charcoal for Used to remove mercury from carrier gas
carrier gas
 RH-MA3 connection port Port for connection to mercury collection tube
measurement unit (Option)
 PC connection port Port for communication with PC
 SC-5 connection port Port for communication with sample changer for reducing
vaporization (Option)
 RD-5 connection port Port for connection with reagent dispenser for reducing
vaporization (Option)
 Power cable connection
port
 Exhaust port Outlet port of measurement exhaust gas (activated
carbon outlet)
7
2.2.4. Internal components seen from the top
④
③
⑤ ①
⑨ ⑦
No. Name Function

 Cell box 1mm cell, 200cell, maintained at a temperature of
150°C with Heater H5
 Lamp box Low-pressure mercury lamp with a built-in
reference detector
 Optical system circuit Trimmer-less circuit
board
 Pipe heater Heats the connecting part to150˚C (Heater H4)
 Mercury collecting Heater H3 for heating the mercury collection tube,
furnace Air-cooled by a fan from underneath.
 Decomposing Heaters for constant temperature control of
furnace catalyst (H2A、H2B)
 Sample heating Used to heat sample boats (H1)
furnace
 Case fan Used to exhaust heat from the inside of the case
 Infrared thermometer Used to control the temperature of the sample
for H1 heating furnace
8
2.2.5. Internal components seen from the right
③
① ②
⑤ ⑦
⑥
⑧ ⑨
No. Name Function

 V3 Valve Opens/closes the flow channel (Water removal
circuit)
 V2 Valve Opens/closes the flow channel (Measurement
circuit)
 V1 Valve Opens/closes the flow channel (Decomposition
circuit)
 H3 cooling fan Cools the mercury collection tube
 H1 cooling fan Cools the sample heating furnace
 Drain tank Removes any moisture in the exhaust gas
 Mass-flow controller For flow control of carrier gas
 Air pump for tray rack Perform a purge in the tray racks with clean air to
suppress the increase of blank
 Activated carbon for tray For cleaning purge air
rack
9
2.2.6. Internal components seen from the left
No. Name Function

 Power switch A safety circuit incorporated
 Main circuit board
10
NIC-600-2231-11 3．Specifications
3. Specifications
3.1. Standard configuration

(1) Mercury analysis system MA-3000
(2) Data analysis/System control software MA3Win
(3) Standard accessories

(4) Personal computer
3.2. Component specifications

(1) Mercury analysis system MA-3000
Analysis method: Thermal vaporization atomic absorption

Carrier gas: Oxygen gas (Purity: at least 90%; Pressure: 0.1MPa
to 0.5 MPa)
Samples: Solid, Liquid, Gas (RH-MA3 required)

Size/Weight: 430W x 770D x 470H, 45kg
Measurement principle Non-dispersion triple-beam cold atomic absorption

Detection limit: 0.001ng
Measurement range: 0.001 to 70,000ng
(2) Auto sample changer

Number of samples: up to 100
Sample boat: Ceramic boat specified for the system
(3) Data analysis/System control software MA3Win
OS: Windows7, Window8, Windouws10

System control: Control of sample changer
Control of analysis conditions, Error indication
Data processing: Construction of calibration curve, Concentration

calculation, Statistical calculations
11
NIC-600-2231-11 4. System installation
4. System installation
4.1. Conditions for installation
4.1.1. Environment for installation
Room temperature: 15 to 35°C

Relative humidity: 35 to 80%RH (with no condensation)
Vibration: No vibrations strong enough to be felt by the human
body.
Dust, Fume: Environment with clean atmosphere free of fumes,
dust, and others which could affect the measurement.
(No smoking)
Installation space: 1000W x 700D (mm) or larger with a rigid foundation
and capable of supporting a weight of about 60kg.
Others: Install the unit somewhere not in direct sunlight or
exposed to air from an air conditioners or blower.
Special note: Never install the system anywhere volatile halide
reagents such as organic chlorine solvents are
handled. Also avoid installation anywhere those gases
could enter.
4.1.2. Power supply
Power voltage: Single phase 100,110,120,220,230,240VAC, 50/60Hz

(Should be selected before delivery)
Voltage fluctuation: Within ±5%
Capacity: 1.5kVA (3 pole plug)
Power quality: No surges, harmonics, or noise.
Distance from power outlet to the system: Closer than 2 m
12
4.2. Installation and connections

4.2.1. MA-3000
(1) Place the MA-3000 where it will be operated.

(2) Connect the system and a PC with an RS232C null modem cable.
(3) Plug in the power cable and connect it to the power source.
(4) Connect the tube with outside diameter of 4mm from an oxygen cylinder to the
system.
* If there is any risk of generation of any harmful gasses such as halogen, sulfur and
selenium during decomposition by heating, please be sure to vent the exhaust gas.
* Use a >4mm tube to connect the exhaust gas tube. Be noted that accurate
measurements will be impossible if the tube is too thin or bended.
Exhaust gas tube RS-232C Cable
Power cable
Oxygen tube
13
4.3. Installing software

Install the control/analysis software of MA3Win on a PC before running the MA-3000.
* The operation of the PC itself and Windows, and the setup of peripheral devices
such as a printer are not explained in this manual. Refer to the manuals supplied
with any of those devices.
4.3.1. Installing MA3Win
*IF the OS language setting is not English (United States), please set as follows.
Control Panel – Clock, Language, and Region – Change date, time, or number formats
Format: English (United States)
(1) Insert the supplied CD-ROM. (The installer will start automatically.)
* If any other application programs are running on Windows, close them.
(2) The “Welcome to the MA3Win Setup Wizard”
window will open. Click Next.
(3) The “Select Installation Folder” window will appear.

Usually click Next if you wish to install the software
in the default folder. If you wish to change the
installation folder, click Browse... and select the
folder.
(4) When the “Confirm Installation” window opens, click

Next. Installation will start.
14
(5) Once installation is complete, the "Installation

Complete" window will open. Click Close to close
the window.
The installation is completed
15
4.3.2. Installing animation display controller
If MACROMEDIA FLASH PLAYER is not installed on PC, install it from the supplied
CD-ROM.
In Explorer, open the folder “Macromedia Flash Player” and execute ”install_flash_player_
_active_x.msi” from the CD-ROM.
(1) Click Install when “Adobe Flash Player

ActiveX Install Wizard” screen appears.
(2) Installation is completed when “Install

Shield Wizard Completed” screen appears.
16
4.3.3. Installing USB Serial Converter driver
Use the supplied USB-Serial converter REX-USB60F to control the MA-3000 from a PC
without a serial port.
* Operation is guaranteed only when REX-USB60F USB-Serial Converter is used.
Windows7
Execute “USB60F_Setup(Windows7).exe” located in
“USBDriver(REX-USB60FverXX)Windows7” of the supplied CD-ROM.
* Complete the following setup procedures before connecting the
REX-USB60F to the PC.
(1) Click “Next” on the setup start screen.
(2) Click Install on the “ready to install”

screen.
(3) When asked “Would you like to install

this device software?” click Install .
(Installation of USB-Serial Converter)
(4) When asked “Would you like to install

this device software?” click Install.
(Installation of USB-Serial Port)
17
(5) This concludes the installation

process.
The device driver is automatically

installed when REX-USB60F is
connected to the USB port of the PC.
4.3.4. Setting Communication port
The RS232C port needs to be set to enable the communication. Follow the steps below to
set the port.
(1) Find the port No. on the device manager.

Windows7
Open “Control Panel” from

“Start Menu” and click “Device
Manager”.
* Set “View by" to “Small

icons”.
18
Click + on the left side of “Ports (COM &

LPT) on “Device Manager.” Check the
number of the USB Serial Port.
(2) Double click the icon on the desktop to start MA3Win.

(3) Select [System (S)] – [Comm Port Set (C) on the MA3Win Menu bar, and open the
Communication Port Setting window.
(4) Select the communication port checked in Step (1) and click OK to apply the setting.
(5) Close MA3Win and restart it for the setting to take effect.
* The port number changes depending on the port to which the USB-Serial
Converter is connected. Note that the setting needs be made again if the
converter is connected to another port.
19
4.3.5. How to uninstall MA3Win
Windows7
(1) Click “Uninstall a program” on the

control panel.
(2) When a list of installed programs is

displayed, double click “MA3Win”.
Then proceed according to the

instructions displayed on the screen.
4.3.6. How to upgrade MA3Win
To upgrade MA3Win, first uninstall it and then install the upgraded version.
20
4.3.7. How to upgrade the version of ROM built into the MA-3000
Follow the steps below to upgrade the version of the ROM built into the MA-3000.
Select [Run]-[System]-[Firmware Update] from the menu. The following Firmware Update
window will appear.
Click “Open”. Then the file is started to be

downloaded. New firmware name is
“MA3_VerXXX.mot”.
After “File load success.”is displayed, click

“Program”.
Firmware update will start.

※ Do not turn the power off while writing.
After update is complete, verify will start.
21
The left message will appear when the

verification has completed. Click “OK”.
Turn off MA-3, and turn on again.
4.3.8. The case of fail in updating firmware
If the update fails, re-update by the following producer.
(1) Close the oxygen cylinder.

(2) Turn off the power of the main unit, and
terminate MA3Win.
(3) Flip up the ring latches on the top cover and
remove the cover.
(4) Unfasten the thumb screw on the rear side of

the left side cover and the screw on the front
side, and then remove the cover.
(5) Turn on the No.2 DIP switch 3 located in the

center of the circuit board.
(6) Turn on the power of the MA-3000.
(7) Open MA3Win, and start re-upgrade in the
same procedure as the “4.3.7How to upgrade
the version of ROM built into the MA-3000”.
(8) After update is complete, close MA3Win and
turn off the power of the MA-3000.
(9) Switch the setting of DIP switch to restore.
O N only No.1
OFF others
(10) Install the left side cover and top cover back
onto the unit.
22
NIC-600-2231-11 5. Measurement
5. Measurement
5.1. Measurement Operation Flowchart
POWER ON MA3Win, MA-3000
First turn OFF the power if any problem

Check of flow path occurs and correct it and then turn ON the
power again.
Warming-up operation starts. Flow carrier

Conditioning gas to purge moisture and other
impurities from the system.
Calibration curve Check the blank value, gradient and

construction correlation coefficient of the calibration
curve.
Enter measurement
conditions
Start measurement
Operation Status name Time

Insert a boat 1 Transfer the boat SAMPLE
2 ATOMIZE 1
3 ATOMIZE 2
Heating Heat the sample Set by method
4 ATOMIZE 3
decomposition and
mercury collection 5 ATOMIZE 4
6 Clean the heating
PURGE1 5 sec
Loop
circuit
Heating collection tube / 7 Clean the
PURGE2 15sec.
Measuring absorbance measurement circuit
8 Measurement MEASURE 30sec.+7sec.
9 Clean the mercury
collection tube MEAS PURGE 30sec.
Cooling Cool H1
10 Cool H1 and H3 COOL 20 sec.
Boat unloading
End
23
5.2. Samples
Type of sample Method Typical sample amount

Standard solution, water Standard solution ,
Up to 200μL
(rivers) Liquid samples
Urine; Blood Urine; Blood Up to 200μL
Organism (Solid)
SOLID sample Up to 200mg
Fish meat / Plant
Soil Up to 200mg,
SOIL&SLUDGE
Sludge Up to 100μL
Mineral
MINERAL Up to 200mg
Coal / Metal / Ore
Plastic PLASTIC Up to 100mg
Waste water Waste water Up to 200μL
* If the measurement is expected to result in a high concentration, dilute the sample

or reduce the sample amount.
* As for some samples that contain a lot of halogens (percent order) or are
easy-flammable, measurements by the default methods are impossible. If the
recovery of the measured standard solution or standard additive is low, reduce the
sample amount.
* When a liquid sample containing organic mercury species is measured, use
Additive B.
* When a liquid sample containing hydrochloric acid is measured, dilute the sample
until the concentration of hydrochloric acid falls to 1wt% or less before the
measurement. In particular, when the hydrochloric solution of high concentration
is measured using Additive B, the result may be lower than the actual value.
* Please contact us as for measurements of oily sample, such as cooking oil, fat
and butter. These samples may damage the sample heating tube. It is
recommended to try sample amount of ≤50mg (50μL).
Warning
· Do not directly measure the sample decomposed with nitric acid. The activated
carbon in the exhaust gas filter may generate heat. Dilute the sample until the
concentration of nitric acid falls to 5wt% or less before the measurement.
24
5.3. Necessary supplies for measurements
(1) Oxygen (purity:≥ 90%: Pressure: 0.1 MPa to 0.5 MPa)

(2) Diluted water
(3) Mercury standard solution (examples: 5ppm, 0.5ppm, 0.05ppm, 0.01ppm)
(4) Micropipette (up to 200 μL) (For quantitation of liquid samples including standard
solution)
(5) Electronic balance (Measurable down to 0.1mg)
5.4. Articles recommended for measurement

(1) Additive B * For liquid samples with high volatility or those containing a large
amount of organic mercury.
(2) Quartz sand * For measurement of samples that deposit onto a boat such as silver
granule.
5.5. Preparation for measurement
5.5.1. Preparing mercury standard solution
The concentration of a mercury standard solution tends to change significantly after being
prepared, which can cause variations in the calibration curve or low reproducibility of a
measurement. L-cysteine should therefore be added to the dilution water of a mercury
standard solution to control the change in concentration.
(Preparation procedure)
(1) L-cysteine solution (100mg/L)

100mg of L-cysteine HSCH2CH(NH2)COOH (not Cystine) is added to a 1000mL
flask with water and 2mL of nitric acid is then added to make a total of 1000mL of
solution. Shake the flask to stir the solution.
Store in a cool dark place.
(2) Mercury standard solution 10mg/L
Take 1mL of mercury standard solution for atomic absorption (1000ppm) and add
L-cysteine solution (100mg/L) to make a total of 100mL.
(3) Mercury standard solution 0.1mg/L
Add L-cysteine solution (100mg/L) to 1mL of the solution prepared in Step (2) to
make a total of 100mL.
* The L-cysteine solution and the mercury standard solutions prepared can be
used for 6 months if they are stored in a cool dark place.
* The stability of the solutions will deteriorate as they age or if kept anywhere
warm. Store in a cool dark place and quality control by, for example, labeling
it with the date prepared.
* Use the same measuring flask if possible when re-preparing the standard
solutions again. If a new flask is used, ensure to thoroughly clean it with
(1+10) nitric acid. Particularly when preparing a standard solution of 1ppm or
less, care should be taken to avoid contamination from the flask by
thoroughly cleaning with acid the flask itself along with the plug.
* When constructing the calibration curve of 20000ng or greater, put about
100μL of L-cysteine solution into the sample boat and directly add drops of
the mercury standard solution of 1000ppm (mercury chloride).
25
5.5.2. Blank treatment of sample boat
<At first use>

Please use the sample boats after heat treatment.
Heat treatment can run purge measurement by MA-3000. Or please put into oven at 750
degrees for 1 hour.
* Don’t wash the sample boats before heat treatment. Performance may be
impaired.
<Daily Work>
Accurate measurement is achieved by the sample boats being heat-treated before
measurement to remove any trace quantities of mercury. To heat-treat the sample boats,
repeat measurements on the MA-3000, or heat them in an electric furnace at 750°C for
around 3 hours.
Sample boats must be cooled down after the blank treatment and stored in a hermetically
sealed container.
* Use different boats for high and low concentration samples. When a liquid sample
is measured, in particular, mercury penetrating in a boat seeps out and the
outputted measurement value becomes higher than the actual value.
* If there is any contamination on the sample boats, immerse them in a solution of

neutral detergent to soak and clean with ultrasonic vibrations for at least 30
minutes. Then, scrub away any grime with a brush etc. and immerse the boats in
an approximately 1% nitric acid solution. Thoroughly rinse in distilled water, and
then dry at a temperature of around 100°C for 2 hours.
* If a liquid splashes over a boat tray when it is dropped from a micro-pipette or

powder sample spills, the tray can be contaminated and the next measurement will
be affected. Trays should be used in clean condition and should be washed with
water if contaminated.
5.5.3. Blank treatment of additives
With measurements for some types of samples such as highly volatile substances, the
mercury contained in them can evaporate during the interval of the sample being placed
on the sample changer to starting measurement. Additive B is sometimes added to
prevent this phenomenon.
Additive B absorbs any mercury in the environment during the manufacturing process and
storage. Use of any additive B that has not undergone blanking treatment can lead to
falsely high mercury content in the measurement, thus making blank treatment of the
additive necessary before being used.
Heat the additive in a crucible at 750°C for about 3 hours as the blank treatment. Any
additive that has undergone the blank treatment must be stored in a hermetically sealed
container or used immediately after having cooled down or it will absorb mercury from the
atmosphere, thereby increasing its blank value.
26
5.6. Starting up the system
5.6.1. Starting the control software
Click the shortcut icon on the desktop, or click [Start] and select [NIC] – [MA3Win] –
[MA3Win] from [All programs].
The icons are indicated in gray if RS-232C port does not exist.
Connect the USB serial converter REX-USB60F to the USB
port, and set the port number again.
5.6.2. Starting the MA-3000
Turn ON the main power switch on the left side.
27
5.6.3. Supplying carrier gas
Open the main cock of the oxygen gas cylinder and adjust the pressure regulator on the
rear panel of the MA-3000 to 0.05 through 0.07 MPa.
(1) Turn the knob fully counter-clockwise.

(2) Open the main cock of the oxygen gas
supply. (0.2 to 0.5MPa)
(3) Turn the knob to adjust the pressure to
0.05MPa.
The pressure rises when the knob is turned
clockwise and drops when turned
counter-clockwise
5.6.4. Checking the tubes for leaks
Gas supply, leak, and operation of the valves from V1 through V3 are checked. The check
proceeds automatically but the diagnostic software automatically closes if any problem is
detected. In that case, turn OFF the power once, correct the problem and then turn ON
the power again.
When the MA-3000 is powered ON and the start-up operation of the sample changer is
completed, “Check of flow path” window opens. Select Yes and the check of flow path
starts.
(Refer to details of the flow of the flow path check in the next section.)
If you do not wish to execute the check of flow path, select No and then the following
dialog box appears.
If you wish to heat the heaters, click OK to start heating.
* Once you cancel the check of flow path, the "Check of flow path” window is not
displayed until theMA-3000 main unit is powered ON again.
28
Details of the flow of the flow path check

The flow rate of oxygen, the leak, and the operation of V1, V2, and V3 valves are
examined by this check program.
(1) Checking the flow rate.

If the carrier gas flow rate is less than 0.4 L/min, it is considered that failure has
occurred. This is considered to be due to insufficient supply pressure or the failure of
mass flow controller. First check the supply pressure.
(2) Executing the leak check.

If the flow rate does not fall to 0.0 L/m within 30 seconds after all the valves are closed,
it is considered that failure has occurred. Check the piping to make sure that any
connected parts are not loosened.
* If the mass flow controller's zero point is displaced due to insufficient adjustment, a
failure may be caused. If the MFC does not indicate zero when the flow rate is zero,
adjust zero point using a zero point adjustment trimmer of the MFC.
(3) Checking the blockade in V1 circuit

Opens only V1 valve and checks that the flow rate of combustion circuit does not fall
below 0.38L/min. If the check fails, it is considered to be caused by the blockade of the
sample heating tube or the mercury collection tube, insufficient supply pressure, or a
failure of V1 valve. Increase the supply pressure and, if the problem persists, replace
the sample heating tube.
(4) Checking the blockade in V2 circuit.

Opens only V2 valve and checks that the flow rate of measurement circuit does not fall
below 0.38L/min. If the check fails, it is considered to be caused by the blockade of the
cell or the failure of V2 valve.
(5) Checking V3 circuit.

Opens only V3 valve and checks that the flow rate of water removal circuit does not fall
below 0.38L/min. If the check fails, check the piping of the boat handling poker, Teflon
tube, and V3 valve.
(6) When all the checks are successfully completed, the heaters automatically start the
heating.
29
5.6.5. Conditioning
If the check of flow path is successfully completed, the conditioning process starts. The
temperature of each heater is increased with oxygen so that the system is purged to
remove moisture and other impurities adhering on the sample heating tube.
* Each heater is heated up to the temperature set for measurement. The set
temperature of the heater H1 is 150˚C and that of H3 is 500˚C. Click Stop if you wish
to stop the conditioning.
* If there is no abnormality, be sure to perform conditioning. Otherwise, the sample
heating tube absorbs moisture, it may be obstructed or break.
5.6.6. Discharging liquid from the drain tank
Discharge any liquid that has accumulated in the drain tank.
(1) The liquid in the drain tank can be discharged by turning the roller of
the roller clamp downward. Collect the waste water in an appropriate
container and dispose of it in the correct manner.
(2) Close the roller clamp.
* Do not apply any excessive force or you may break the indentations on
the clamp.
30
5.7. Measurement
5.7.1. Blank check
The blank of the system is checked. Perform the blank measurement until the values are
stabilized because mercury adhering to the flow path is released when the measurement
is started.
Click the icon to perform the purge measurement or register the blank check on the
table as in the normal measurement. If the boat number is set to 0, it is possible to check
only the system blank.
Pretreatment of sample boat

A sample boat absorbs mercury in the air, which raises the blank value. Therefore to
achieve accurate measurement, the sample boat should be heat-treated to remove
mercury before the measurement.
As a method of the heat-treatment, before measurement, the sample boat is repeatedly
measured with the MA-3000 until it is confirmed that the blank value is stable, or it is
heated at 750˚C for more than 3 hours in a heat-resistant ceramic container such as
crucible and cooled down.
After the measurement, if the sample boat is contaminated, it should be cleaned with
neutral detergent, dried, and then heat-treated in the same manner as above.
5.7.2. Setting the measurement condition
Click the icon to open “Measurement Condition” screen and set the flow rate for
measurement, the standard heating mode (method), the standard check and the blank
check.
 When the calibration curve is

constructed with a standard
substance instead of a
① standard solution, select a
heating mode suitable for it.
②
 The default value of flow rate
for measurement is 0.2L/min.
③ 0.1L/min: For high
sensitivity measurement
0.2L/min: For normal
measurement
0.5L/min: For high
concentration measurement
 Set them only when STD
check is used.
31
 Set the measurement condition when the

blank value is automatically lowered after
④ the measurement of a high concentration
sample.
About 1% of the value of the immediately

previous measurement is detected as
historic record in the case of thermal
vaporization measurement. When a sample
of which concentration is significantly
different from that of the previous sample is
measured, the sample with lower
concentration indicates a value higher than
the actual value due to the influence of
historic record.
When the blank check is set, the influence
of historic record can be reduced by
lowering the blank value automatically even
if a sample of unexpectedly high
concentration is measured.
* However, if there is a large difference in
concentration of two or more samples, it is
recommended to measure the sample with a
lower concentration first.
Mode: Select the range for the measurement.

Threshold Level: Blank check starts when the peak height is higher than the set
value.
Return Level: Purge measurement is repeatedly executed until the peak height
of the purge measurement falls below the set value.
ABS reference values (when measurement

flow rate is 0.2L/min)
ABS(LOW) ABS(HIGH)
0.1ng 0.002 10ng 0.001
1ng 0.02 100ng 0.01
5ng 0.1 1,000ng 0.1
10ng 0.2 5,000ng 0.4
20ng 0.3 10,000ng 0.6
When the blank check functions, a line of BlankCheck is inserted below the corresponding
sample line.
32
5.7.3. Setting the table conditions
Click the icon to open “Table Condition.” Select the type of sample, unit and other
conditions. The settings can be changed after the measurement. (For details, refer to
7.2.4.2 Table condition)
Analysis mode：
Select either PEAK (Peak
height) or AREA (Peak area).
Usually AREA is selected and
PEAK should be selected in the
case the peak is so small that
the variation becomes large if
AREA is used.
Type of sample：
Select either Solid or Liquid,
which changes only the
displayed unit and items but not
affect the method.
Type of calibration curve：

Respective calibration curves
can be set for LOW range and
HIGH range. Usually, please
select “y=ax+blank”.
5.7.4. Constructing the calibration curve
5.7.4.1. Registering standard values
Entering standard values in the fields of standard samples

 Click “STD” to open the “STD
INPUT” box.
 Enter the concentration of the

standard solution and the
amount of sample.
* The measurement method is set as “STD” initially. When using other CRM (especially
solid CRM), select proper measurement method from measurement condition.
33
5.7.4.2. Setting the samples
Place the standard samples in the special sample boats side by side on a boat tray and
then set on a rack.
* The boat tray has 10 partitions and

can seat 10 boats per tray.
Check the “Measurement” box to add a check mark to it.
34
5.7.4.3. Starting a measurement
Select [Run]-[Measurement start] from the menu or click the icon to start a
measurement.
As the measurement starts, the system
asks you the name of the file in which
the measurement data should be stored.
Set the file name.
Click Save and then the measurement
starts.
5.7.4.4. Finishing a measurement
The following message will appear when the system has completed measurement of all the
samples whose boxes were checked.
5.7.4.5. Stopping a measurement
To stop a measurement, select [Run] – [Stop] from the menu or click icon.
This will result in measurement ceasing after the current measurement has completed.
In this state, if [Run] – [Emergency] from the menu or the icon is clicked, the system will
immediately switch to the cooling sequence, and then returns to READY mode on completion
of the cooling process.
35
5.7.4.6. Reviewing a calibration curve
Click the icon and check the calibration curve using the “Calibration curve” window
on the analysis screen.
Check respective calibration curves for
LOW and HIGH.
It is possible to ignore erroneous data and

exclude it from calculation and printing by
clicking the X column on TABLE window
and selecting “X”.
* Letters are shown in red and “WARNING"

is displayed when the calibration curve
has a problem. In this case, check if there
is a problem with the set standard values,
the standard solution or the equipment.
The sensitivity of each system is different and the “WARNING” may be displayed
depending on the values set during the software installation. Set the values with reference
to the data of the shipping inspection and the measured values at the time of delivery or
after the maintenance.
Open System (S) - Environment

setup (S) - Calibration curve setup
and set the standard values.
Input the peak height and area of

the 1ng measurement into Low
range and those of 100ng
measurement into High range.
* The standard value should be set

for each flow rate in the case of
thermal vaporization.
* X (employ or ignore the data) is automatically entered according to the height of PEAK.
Change the X as necessary.
(LOW is adopted when ABS is 0.3 or less, while HIGH is adopted when ABS is 0.3 more.)
* Calculation is done with an AREA value (area value).In low-concentration measurement

(Area of 0.05 or less), PEAK analysis may give better results.
* If the gradient of the calibration curve has changed ±30% or more since the system was
first delivered, or the blank value is extremely high, there could be something wrong with
the standard solution or the system itself. In this case, refer to “6.3 Troubleshooting. “
36
5.7.5. Measuring unknown samples
5.7.5.1. Measuring samples
Place the sample in a sample boat. If the sample is liquid, measure it with a micropipette
or if it is a solid, with a balance.
* When measuring the weight of a sample

(Example)
 Place a weighing fixture on the balance.
 Place a sample boat on the weighing
fixture.
 Subtract the tare weight.
 Place a sample in the boat with care not to

spill any of it.
 Record the weight.
 Remove the boat and lay it on the boat

tray.
* Contamination can result in outlying values in the measurement of trace quantities of

mercury. When handling the boats, be careful to avoid any contamination by using
disposable gloves or clean tweezers.
* When an additive is used, put it into a boat before weighing the sample.
● In the case of a liquid sample, put an additive up to the

level same as or higher than the liquid level.
● If it is necessary to prevent fusion, put an additive to such a

level that the bottom surface is covered.
● When rapid combustion needs to be suppressed, disperse
a sample over a boat and cover it with an additive.
37
5.7.5.2. Registering unknown samples
Register sample numbers, sample names and sample amounts.
 Click the box of “Measurement” and put a check on it.

 Enter the sample number of the boat tray on which the sample boat is placed.
 Enter the sample name.
 Enter the sample amount.
* Perform purge measurement several times before measuring an unknown sample.

Historic records of standard solution measurements may affect the measurement of a low
concentration sample.
5.7.5.3. Selecting method
Select the method to be used for the measurement.

The setting is made by selecting a method suitable for the sample from the pull-down
menu.
* The method can freely be modified or set by

selecting [Run] – [Methods set] from the
menu.
38
Selecting the method

Select the condition of the H1 for heat-decomposition of a sample. The following 8
types are registered in default state, and up to 12 types of methods can be registered in
one measurement.
Method Standard
Type Method amount of
Number sample
Standard Relatively clean water such as river or

Standard solution,
solution / lake water. Additive B should be used
0 Liquid sample 200μL for organic mercury and samples that
liquid
(Including w/ additive) are easily reduced and vaporize.
solution
Organism (Solid)
1 Solid sample 200mg Ordinary solid samples.
Fish meat/Plant
2 Soil/Sludge Soil 200mg Samples containing halogen/water.
Liquid sample containing a large

3 Urine/Blood Urine/blood 200μL
amount of organic matter.
Polymeric plastic material. The amount

of a sample should be decreased to
4 Plastic Plastic 100mg several mg if the sample contains a
large amount of halogen
Mineral Used for samples that require high

5 Mineral 200mg
Coal/Metal/Metal/Ore temperature treatment.
Used for difficult-to-measure liquid

samples containing halogen.
6 Waste water Waste water 200μL Additive B should be used for
difficult-to-measure samples.
Used to reduce the blank of the system
7 Purge Purge -
or heat-treatment of a boat.
5.7.5.4. Starting a measurement
Select [Run] – [Measurement start] from the menu or click the icon to start a
measurement.
39
5.7.5.5. Reviewing measurement data
Review the measurement results and determine whether to use the data or not.
* As for the analysis range, the data less than 10ng are automatically applied for LOW
range and the data greater than 10ng are applied for HIGH range. An analysis range
can be changed and is performed in the Range column.
* If the recovery of the standard solution after the measurement is 90% or less (≤ 90%),
the sensitivity might decrease due to poor decomposition of the sample. Try to reduce
the amount of sample or reconsider the method.
* When the sensitivity decreases, repeated measurements of water may recover the
sensitivity. The sensitivity can be recovered and checked at the same time by
repeating the measurements of the standard solution of around 200μL.
5.7.5.6. Printing a report
To print the measurement results, select [File (F)] – [Print] from the menu, or click the
icon. (For details, refer to 7.2.1.6 Print)
● Select an item and confirm it by preview.

● The title and the name of a measurer can be entered by selecting Table - Memo
setting (M).
● The scale of print profile synchronizes with the profile scale of the analysis screen. Set
the HIGH/LOW range scale and the number of profiles for both the standard solution
and unknown solution.
Low range High range
scale scale
adjustment adjustment
Number of
profiles per
line
● The width of each column synchronizes with the setting in the table screen. Adjust the
width of column on the table screen if the column seems too narrow when printed. A
column is not printed if its width is set to 0.
40
5.7.6. Termination
(1) Press the upper right button of MA3win.

Please follow the message displayed at the end.
Caution
*If you don’t turn-on MA-3000 for a long time, the sample heating tube might be
obstructed by moisture absorption.
・If you don’t turn-on MA-3000 more than 2 weeks, please turn on the MA-3000 power
switch and do conditioning. (Conditioning process start automatically after checking the
flow path)
・Otherwise, please dismount the sample heating tube and store it in a desiccator to
prevent moisture absorption. (Refer to 6.4.2 Dismounting the sample heating tube and
6.4.3 Mounting the sample heating tube)
(2) Close the Windows and turn off the power of PC and Printer.
(3) Power off MA-3000.
(4) Discharge liquid of a drain tank.
(5) Close the main cock of the Oxygen gas cylinder.
41
NIC-600-2231-11 6. Maintenance
6. Maintenance
6.1. Inspection items
6.1.1. Daily inspection
Inspection before start-up

Inspection items Criteria Corrective actions
Oxygen pressure Secondary supply pressure must be between Replace the gas
0.05MPa and 0.07MPa. cylinder.
Sufficient gas must be in the cylinder.
Drain tank No water must be accumulated. Dispose of waste
The cock must be closed. liquid.
Status Must not be in OFF-LINE mode. Check cable

connection and port
setting.
Check of flow path Must be completed without any failure. Refer to 5.6.4Checking
the tubes for leaks
Measurement The system must be set to the method to be Change the setting by
method used. selecting Environment
settings (S)-System
settings
Error/Warning No error or warning message must be
displayed when the countdown is completed.
Inspection during measurement operation

Inspection items Criteria Corrective actions
Sample changer All boats must be retained without falling out. Contact our service
when the problem is
not solved by the
adjustment.
Unusual noise No noise is generated while the sample Grease the drive
changer is running. mechanism.
Blank value Repeat purge measurements, and the peak 6.3.2 Outlying blank
value at Low range must be at most 0.001. value
Calibration curve When the calibration curve is drawn for the 6.3.1 Degradation of
standard solution, the correlation coefficient peak sensitivity
must be at least 0.999.
Sensitivity Gradient of the calibration curve must be within 6.3.1 Degradation of
±30% of the inclination at delivery. peak sensitivity
Carry over The blank value immediately after Replace the sample
measurement of a standard solution must be at heating tube/mercury
most 2% of the mercury amount measured just collection tube.
before it.
Accuracy The value of a standard solution measured Review the method and
after an actual sample measurement must be the amount of sample
within ±5%.
42
6.1.2. Annual inspection
Annual inspection
Inspection criteria Criteria Corrective action
O-rings at sample inlet No cracks on the O-rings Replace the O-ring with a
new one.
Sample inlet fork No cracks on the fork Replace the sample inlet.
Drive unit linear guide No rust on the operating shafts Grease the shafts.
Sample heating tube Catalyst retained in its place without Replace the sample heating
displacement tube.
Mercury collection tube No contamination on the quartz tube, Replace the mercury
and no discoloration of quartz wool. collection tube.
Absorption cell No contamination Tear-down and clean or
replace the cell
Pressure regulator No variation in pressure Replace the pressure
regulator.
Flow rate No flow variation exceeding 0.02 Replace the mass flow
L/min. controller.
Detector output Must be 4±0.5V in the maintenance Wipe off any dirt on the
(Ref) window of MA3Win. lamp/lens etc.,
Adjust optical systems.
Detector output Must be 4±0.5V in the maintenance Clean the cell unit or replace
(SIG1, SIG2) window of MA3Win. it. Wipe off any dirt on the
cell window and
photoelectric tube
Air pump tube (Option) Needs to be replaced every year. Replace.
43
6.2. Errors and warnings

Measurement can continue even if a warning message is displayed. However, if an error
message is displayed, measurement will be disabled until the cause of the error has been
solved.
(1) Warning messages

Message Description and corrective action
STAND-BY xx:xx Appears for 20 minutes after turning the power ON.
The measurement data are not reliable during the count
down because the heaters and optical systems are not
stable.
The heater (%) interlock has occurred and Displayed when the heater interlock has occurred. Contact
the heater (%) turned OFF. our service if there is any odor. When no deficiency is
Turn ON the power again if there is no observed in the appearance, turn OFF the power and then
problem found. turn it ON again, and check if the error continues.
THERE IS A TRAY IN This warning is generated when there is any boat tray left
There is a tray in the tray evacuation rack. on the tray evacuation rack. Remove the tray and confirm
Remove the tray. that there are all the boats on the tray. If not, the sample
boats are left on the inlet shaft. Turn OFF the power of the
system and open the front cover to remove the sample
boats.
A tray is loaded into a tray rack which is under Do not load a tray into a tray rack which is under
measurement. Remove the tray. measurement. If the warning message is displayed when
the tray is not loaded, it is considered to be caused by the
influence of outer light or a failure of the sensor.
The number of measurements has exceeded Displayed when the number of measurements has
2000. It is recommended to replace the exceeded 2000.
sample heating tube. It is recommended to replace the sample heating tube
because its performance may be degraded. Be sure to
reset the counter after the replacement. (Maintenance
=>GLP=>MEAS CNT CLEAR)
There is a problem with the case fan. The rotation of heat exhaust fan is not detected. If the fan
If the case fan is not rotating, stop the use of is not rotating, the temperature in the unit will rise and the
the system. system may be damaged.
The heater (%) does not reach the pre-heat The heater does not reach the set temperature. When the
temperature. set temperature is reached, the message automatically
disappears.
The heater wire may be broken if the temperature does not

rise at all. The displacement of the temperature sensor
may be also considered when the set temperature is not
reached. Contact our service.
Cell dark (%): The cell is contaminated. The amount of light transmitting through the cell has
Check the blank value by performing the decreased. Perform the purge measurement, and, if the
purge measurement. base line is faulty, clean the cell with nitric acid.
No response has returned from MA3!! Poor electrical contact at the cable or improper PC setting
is considered. Check the electric connection.
Constant read error!! Contact our service.
Please re-enter the constants!!
44
(2) Error messages 1
If any of the following errors occurs during a measurement, the system will cease
measurement and switch to the cooling sequence. Once the temperatures of heaters H1
and H3 has cooled, the system will stop.
01 A/D FULL The increase in the amount of light of lamp, the

The voltage of the optical system exceeds the increase in the sensitivity of photoelectric tube, or a
preset value. failure of the circuit is considered.
Execute "Adjust the optical system". Adjust the optical system (Refer to 6.4.9 Adjusting
the optical system) and, if not improved, contact our
service.
02 LAMP BROKEN Deterioration of the lamp, a failure of the
REF voltage (light volume) is below than photoelectric tube for compensation of light amount,
regulated value. or a failure of the circuit is considered.
Turn off the power and Check the connection Adjust the optical system (refer to 6.4.9 Adjusting the
of the optical system. optical system) and, if not improved, contact our
service.
03 COMMUNICATION ERROR(PC) A problem with the PC setting, the influence of other
Communication error occurs with PC software, or a failure of the cable or USB conversion
connection. Check the connection between adapter is considered.
the system and PC, and then restart them. If a software program other than MA3Win is using
the resource, terminate the software.
04 COMMUNICATION ERROR(SC-5) Check the connection of the SC5 communication
Communication error occurs with SC-5. Check cable or the power cable. If the error frequently
the connection and power, and then restart the occurs, a problem on hardware such as a circuit
software. board or power supply is considered. Contact our
service.
05 FLOW ERROR If the error repeats even after the pressure is correct
Flow rate decreased lower than 1/2 of and the sample heating tube is replaced, the choking
regulated rate. Replace the sample heating in activated carbon or a failure of the mass flow
tube, if the O2 pressure is normal. controller is considered. Contact our service.
06 HEATER (H1) BROKEN The error message is issued when the temperature
The temperature of H1 does not rise to of H1 does not reach the specified temperature
required pre-heating temperature. within 5 minutes after the measurement is started.
Turn OFF the power once and turn it ON again and,
if the error repeats, contact our service.
07 HEATER (H2A) BROKEN The error is issued when the temperature of H2A
The temperature of H1 does not rise to does not reach 90% of the pre-heating temperature
required pre-heating temperature 30 minutes after turning on the instrument.
08 HEATER (H2B) BROKEN The error is issued when the temperature of H2B
The temperature of H1 does not rise to does not reach 90% of the pre-heating temperature
required pre-heating temperature 30 minutes after turning on the instrument.
09 HEATER (H3) BROKEN The error message is issued when the temperature
The temperature of H3 does not rise. of H3 does not reach 400˚C at the end of thermal
vaporization measurement.
Turn OFF the power once and then turn it ON again
and, if the error repeats, contact our service.
10 HEATER (H4) BROKEN The error is issued when the temperature of H4 does
The temperature of H1 does not rise to not reach 90% of the pre-heating temperature 30
required pre-heating temperature minutes after turning on the instrument.
45
11 HEATER (H5) BROKEN The error is issued when the temperature of H5 does
The temperature of H1 does not rise to not reach 90% of the pre-heating temperature 30
required pre-heating temperature minutes after turning on the instrument.
12 HEATER (RH1) BROKEN The error message is issued when the temperature
The temperature of the 1st mercury collector of the heater does not reach 400˚C at the end of
tube of RH-MA3 does not rise. Check the ATOMIZE process.
connection and power of RH-MA3. Check the power cable and the switch of RH-MA3,
and, if no problem is observed with them, contact our
service.
13 HEATER (RH2) BROKEN The error message is issued when the temperature
The temperature of the 2nd mercury collector of the heater does reach 400˚C at the end of
tube of RH-MA3 does not rise. Check the ATOMIZE process.
connection and power of RH-MA3. Check the power cable and the switch of RH-MA3,
and, if no problem is observed with them contact our
service.
46
If any of the following errors occurs during a measurement, the system will immediately
cease measurement and stop.
14 BC MOTOR-X TIME OUT ERROR An error has occurred when the home position
The movement of X axis motor does not sensor of the horizontal shaft moved.
complete. Turn off the system, and remove Turn OFF the power and open the front cover to
the tray on the X axis. check it.
If the system cannot be recovered, contact our
service.
15 BC MOTOR-Y TIME OUT ERROR] An error has occurred when the home position
The movement of Y axis motor does not sensor of the vertical shaft moved.
complete. Turn off the system, and remove Turn OFF the power and open the front cover to
the tray on the Y axis. grease the linear guide and the trapezoidal screw
thread.
service.
16 BC MOTOR-Z TIME OUT ERROR An error has occurred when the home position
Turn off the system, and remove the boat on sensor of the inlet shat moved.
the boat handling poker. Turn OFF the power and open the front cover to
grease the linear guide and the trapezoidal screw
thread.
service.
17 BC LIFT TIME OUT ERROR An error occurred when the lift went up/down.
The movement of lift motor does not Turn OFF the power, open the front door, and adjust
complete. Turn off the system, and remove the sample changer with BC ADJUST. (Refer to
the boat on the lift. 6.4.7Adjusting the sample changer.)
service.
18 NO TRAY!! Open the front cover to check. If a tray is not placed
The try is not placed on the arm correctly. Turn on the arm correctly due to displacement of the
off the system, and check the tray sensor of sample changer, adjust the sample changer. (Refer
the arm. to 6.4.7 Adjusting the sample changer)
service.
19 BC MOTOR-Z ERROR!! The error message is displayed when stepping out
The movement of the inlet shaft motor does of the motor is detected.
not complete. Turn off the system, and Contact our service.
remove the boat on the boat handling poker.
20 THE RETURNING OF TRAY FAILED!! A tray may be stopped on the way. Turn OFF the
The sample boat tray cannot be correctly set power, open the front cover and remove the tray. If
in the rack. Turn off the system, and remove the error repeats, adjust the sample changer.
the tray on the arm.
21 LIFT SENSOR ERROR Contact our service.
An error has occurred in the lift sensor.
22 HEATER(H1) TEMP ABNORMAL] A failure of the fan or infrared temperature sensor.
The temperature of H1 does not decrease to Contact our service.
pre-heat temperature.
23 HEATER(H2A) The error is issued when the temperature is above
H2A Overheating Detected. 660 deg C
Contact our service.
24 HEATER(H2B) The error is issued when the temperature is above
H2B Overheating Detected. 390 deg C
25 HEATER(H3) The error is issued when the temperature is above
H3 Overheating Detected. 800 deg C
47

28 EEPROM ERROR Failed to write the constants. Contact our service.
91 SC-5 TABLE DRIVE ERROR An error occurred in SC-5.
Malfunction of the SC-5 turntable. Contact our service
92 SC-5 ARM DRIVE ERROR An error occurred in SC-5.
Malfunction of the SC-5 arm. Contact our service.
93 SC-5 LIFT DRIVE ERROR An error occurred in SC-5.
Malfunction of the SC-5 lift. Contact our service.
48
When any of the following messages is displayed, the measurement sequence stops
temporarily and, if the problem is corrected, the sequence restarts.
Close the door of tray rack. If the door of tray rack is opened during the transfer
of a tray, the tray cannot be transferred correctly.
Close the door during the transfer of a tray.
There is a tray in the return position. A tray is detected on the rack to which a tray is to be
Remove the tray. returned. Remove a tray if any.
The sensor on the tray rack may malfunction due to
the influence of an intensive light. Ensure that the
rack is not directly exposed to outer light.
There is a tray on the tray evacuation rack. A tray is detected on the tray evacuation rack when a
Remove the tray. tray is returned there. Remove a tray if any.
The sensor on the tray rack may malfunction due to
the influence of an intensive light. Ensure that the
rack is not directly exposed to outer light.
(5) Heater overheating protection
The heater H-2 has a thermostat to protect it from overheating. A thermostat being
activated will result in the heater not working. In this case, press the central button on the
thermostat to reset it.
49
6.3. Troubleshooting
6.3.1. Degradation of peak sensitivity
When the sensitivity does not recover by repeated measurements with a standard solution,
check the flow chart as below.
START
NO
Check for leak Find any leak and repair.
YES
NO
Does the method work Check the method.
without any problem?
YES
NO Prepare the STD solution

Is the STD solution good?
again.
YES
Does the sample boat NO

work OK? Try with a new boat.
YES
NO
Have collection tube and joints been Replace the sample heating
cleaned or replaced? tube. Clean the collection
tube/joint
YES
NO
Has the heating tube been replaced Replace the sample
with a new one? heating tube.
YES
Has the absorption cell

NO
Clean the cell.
been cleaned?
YES NO
Has the peak
sensitivity been
restored?
Contact our YES

service.
50 END
6.3.2. Outlying blank value
When the blank value does not decrease from an extremely large value (for example
several nanograms) even if the sample boats are washed or the blank measurements are
repeated, check the flow chart as below.
* Use a sample boat suitable for high/low concentration depending on the purpose.
START NO
Is the blank value high in purge

measurement without a boat?
NO
YES
Are the boat tray and boat NO
Clean the boat fixture with
fixture (for weighing) clean?
ethanol.
YES
NO
Is the boat new? Repeat measurement with
a new boat.
YES
NO
Is the blank value high even if measured
with “TEST” method?
Clean the sample inlet.
YES
Have the collection tube/joints NO Clean or replace the

been cleaned or replaced? collection tube/joints.
YES
Has 捕集管・ジョイントは

the sample heating tube NO Replace the sample
洗浄又は交換済みか？
been replaced? heating tube.
YES
NO
Does the peak value decrease to 0.001 or
less when the blank measurement is
repeated?
YES
Contact our
service.
END
51
6.4. Maintenance
6.4.1. Leak check
Check the tubes for any loose joints or leaks.

Click [Run] – [Leak check] to open the Leak check window.
The following screen is displayed. Then click Start.
Sequence of leak check

1. The flow rate is checked as the check is started.
Unless the flow rate is 0.4L/min or more, an error is generated.
2. The sample inlet closes and then the leak check starts.
The check has been successfully completed if the flow rate decreases from around
0.4L/min to 0.00L/min within 30 seconds.
If the check fails, turn OFF the power and check for loosened joints, insufficient
tightening of the sample inlet screw, or damage on flow path.
Check the tubes only after the power switch has been turned
Warning OFF and the heater has cooled down to room temperature or it
could result in burns.
52
6.4.2. Dismounting the sample heating tube
Carry out maintenance of the heated sections only after the power
Warning switch has been turned OFF and the heater has cooled down to
room temperature or it could result in burns.
 Remove the top cover and open the front

cover. (Locked when the power is ON)
 Open the front cover and turn ON the power of

the MA-3000.
Turn OFF the MA-3000 after the sample
changer operates, and the Z axis moves
toward you and stopped.
 Loosen the Teflon joint at the sample inlet.
 Unscrew 4 knurled screws holding the sample

heating tube retainer and the pipe heater
cover, and remove the retainer and the cover.
 Loosen the joint connecting the mercury

collection tube and the cell.
Loosen 2 box nuts of the reducing T joint on
the side of the mercury collection tube and on
the side of the detector to remove the joint.
* The joint would be a cross joint in the case an

optional unit is supplied.
53
 Loosen the 4 panel fasteners on the inlet shaft

on both the left and right sides with a Phillips
screw driver (No.2) and open the door to the
right.
 Remove the 3 screws that fix the sample inlet.
 Remove the sample heating tube.

Remove the 3 flat head screw on the sample
inlet and slowly turn sample heating tube and
mercury collecting tube to pull them out.
 Unscrew 3 screws with a hex wrench and pull

out the sample heating tube. Also remove the
box nuts of the Teflon joint.
54
6.4.3. Mounting the sample heating tube
Be sure to do degreasing cleaning the O-ring before use. If

Caution degreasing cleaning is not carried out, there is a possibility that
the sample heating tube will come off during measurement.
① For degreasing, wash the O-ring with neutral

detergent well.
*Please wash for both new and used O-rings.
② Final rinse with distilled water.
③ Dry off the O-ring moisture. After that, wipe

with alcohol.
*Inspect the O-ring for any damaged

*Don’t touch it directly with your hand.
④ Place the O-ring in the center of the sample

inlet retainer and pass the branch tube
through the sample inlet ring.
Sample inlet ring *Do not confuse the head and tail of the ring.
Position the inlet ring in the direction shown below.
For screw (big)
O-ring
For branch tube
Sample inlet retainer
For screw (small)
⑤ As shown on the left, please lightly tighten the

three points of the sample inlet retainer
bracket with screws.
Tighten the screw to the extent that the
sample inlet ring can be fixed.
*When the screw is completely tightened, the

sample heating tube will not enter. Be careful.
55
⑥ Wipe outside the inlet of the sample heating

tube well with alcohol.
⑦ Put the sample inlet retainer on the desk. Put

in the sample heating tube from above.
If you press the sample heating tube twisting,

it will be easier to put in.
*Be careful not to break the sample heating
tube.
⑧ Check there is no space between the sample

No space heating tube and the sample inlet retainer.
⑨ Retighten the screws until there is no space

between the sample I let retainer and sample
inlet ring.
No space
56
⑩ Install the Teflon joint and the mercury

collection tube to the sample heating tube.
Disassemble the Teflon joint, pass the sample
heating tube through the box nut, washer,
O-ring and joint in this order and tighten the
nut.
Here, do not insert the joint too deep so that
the position can be easily adjusted later.
* The thread on the Teflon joint is easily

damaged. Ensure to verify that the nut turns
smoothly. If the box nut does not correctly
engage the thread, it could result in leaking.
⑪ Wipe the outside of the sample heating tube

and the mercury collection tube with alcohol.
*If hand sweat is attaching, there is a
possibility that the sample heating tube will be
broken during heating.
⑫ Insert the sample heating tube.
Slowly insert the sample heating tube into the
sample inlet while twisting it gently to the left
and right.
* Pushing it too forcefully could result in the

heater being deformed or disconnection.
⑬ Pass the mercury collection tube through the

H3 heater and push it until the sample inlet
touches the reducing joint.
⑭ Fix the sample inlet retainer in place.

Tighten the screws with the supplied hex
wrench.
57
⑮ Adjust the position of the mercury collection

dent tube. Align the end of the heater and the dent
of the mercury collection tube. Adjust the
position by adjusting the insertion depth of the
Teflon joint.
Tighten the Teflon joint securely. In particular,
the reducing joint must be tightened lightly
with a hand at first and then re-tightened with
a wrench by about ½ turn.
* The joint may be broken if excessively
tightened.
⑯ Close the door of the sample inlet shaft.

Gradually tighten the panel fasteners with a
Phillips driver (No.2). Tighten all of the 4
screws lightly and then the re-tighten them
little by little.
⑰ Connect the elbow joint to the branch pipe on

the sample inlet.
⑱ Install the pipe heater cover and sample

heater tube retainer. Close the front cover and
install the top cover.
⑲ Turn ON the power of the MA-3000 and

perform the check of flow path to make sure
that there is no leak.
58
6.4.4. Installation of the boat handling poker
The boat handling poker is heated to high temperature. Carry out

Warning the maintenance work after it has cooled down to room
temperature, or it could result in burns.
 Turn OFF the power and open the top cover and
then the front cover.
 Start the MA-3000 and open the maintenance

screen.
 Remove the Teflon joint facing you on the side of the

boat handling poker, and remove 3 screws holding
the handling poker.
 When washing the boat handling poker, please

remove the O-ring with tweezers etc.
The boat handling poker and O-ring put in 1wt%
nitric acid apply ultrasonic vibrations or leave them
for about 30 minutes.
Next, wash them with distilled water and dry well.
After that, reattach O-ring to the boat handling
poker.
*If there are scratches or cracks in the O-ring,
please replace with a new one.
 Install a new handling poker.
Put a spring at the center and spacers onto the
surrounding 3 screws and tighten them.
 Loosen the 4 screws that hold the handling poker on

to the linear guide shown in the left picture.
 Enter the password to open BC-ADJUST, and then

advance the sequence to the step where the inlet
moves. (Refer to 6.4.7Adjusting the sample
changer)
 Fix the handling poker at such an angle that it does

not touch the lift and attach the Teflon joint to it.
59
6.4.5. Removing the absorption cell
Carry out maintenance on the optical box only after having turned
the power switch OFF and allowing it to cool down to normal room
Caution
temperature or it could result in burns as the box keeps the
constant temperature of approx. 150°C during operation.
 Remove the top cover and then the right side

cover.
The covers are fastened with 2 screws at the
front and back.
 Remove the lid of the cell case. Loosen 6

screws with a driver and remove the lid.
 Remove the Teflon joint (FLW-30-4UE) from

the cell.
60
 Remove the pipe heater cover by unscrewing 2

screws.
 Loosen the box nut of the reducing T-joint on

the side of the mercury collection tube.
 Take out the cell and loosen the screw holding

the cell window with a coin. Also loosen the box
nut of the cell body.
 Disassemble the 1mm cell in the same manner

and wash it but exclude the metal parts.
 Dry the washed parts at a temperature of

around 100°C and then reassemble the cell.
Reverse the disassembly process to
reassemble it.
61
6.4.6. Cleaning the absorption cell and joints
Clean the removed tubes using the following procedure.
Remove the cell and joints, and put them in a plastic

or glass beaker.

Pour neutral detergent in the beaker

and apply ultrasonic vibrations to or
leave the tubes and joints for about
30 minutes.

Take them out of the

beaker and clean one by
one.
Pour diluted nitric acid (1+10) again

and apply ultrasonic vibrations to or
leave them for about 30 minutes.



As the final step, clean them with distilled

water and dry them in a dryer.
62
6.4.7. Adjusting the sample changer
If the transfer error occurs in the sample changer, adjust the position.
Open Maintenance screen, select “BC” tab and click BC Adjust.
63
① Initial screen BC ADJUST window opens.

Designate the Tray No. and advance the movement.
Tray No.: Enter the number of the tray onto which the
boat is loaded.
Boat No.: Enter the boat number.
►: Advances by 1 movement
◄: Returns by 1 movement
►►: Advances to the next step.
◄◄: Returns to the previous step.
① Axis-Y Down Move the arm to the designated
tray.
Adjust the height with

OFFSET Y.
③Axis-X In Insert the arm into the rack.

Return to  and change
OFFSET-Y so that a
clearance of 1.5mm is
present between the arm
and the frame of the
rack.
Move the tray to the right

end, and also change
TABLE POS OFFSET so
that a clearance of
0.5mm is present
between the arm and the
tray.
④Axis-Y Up Lift up the tray.

Make sure that the
projction of the arm fits
into the hole of the tray
and the tray and the rack
are in parallel.
If they are not in paralle,
loosen the screw of the
arm and adjust the
parallelism.
64
⑤Axis-X Out Pull out the tray.

Make sure that the tray
detection sensor
responds to the tray.
Adjust the angle and
position of the sensor if
the tray is not detected.
* The side of the sensor

lights up in red when
the tray is detected,
⑥Axis-Y Origin The tray moves to the Y-axis home

position. Designate the boat
No.10.
⑦Axis-X Sample The tray is moved onto the lift.

Make sure that the lift is
located at the center of
the hole. Adjust the
location with the
parameters of
OFFSET-X if it is
misaligned to the right or
left.
⑧Lift Up The lift moves up and the boat is

lifted up. Check the clearance
between the tray and the
lift again while the lift
moves up.
Also make sure that the
boat handling poker and
the lift do not touch each
other.
Loosen the 4 screws and
adjust the angle of the
boat handling poker so
that it does not touch the
lift.
65
⑨Axis-Z Boat Insert the boat handling poker into

the lift. Check the left and right
clearances of the
handling poker. Adjust
the mounting angle of
the handling poker if the
1.5mm clearance is too small.
Adjust OFFSET-Z so that
a clearance of about
1.5mm is present
between the lift and the
center of the handling
poker.
⑩Lift Down Move down the lift and place the
boat on the handling poker. Adjust the OFFSET-Z if
the boat is placed on the
claw of the handling
poker.
⑪Axis-Y Down Move down the tray.
⑫Axis-Z Measure Seal the inlet.

Adjust the
pre-compression of the
spring. Set the
MEASURE POS
OFFSET so that the
distance shown left is
1.5mm shorter than the
distance when the spring
is not compressed.
66
6.4.8. Greasing the drive mechanism of the sample changer
If any unusual noise is heard when the sample changer is running, apply grease to where
the noise is generated.
Apply grease to the horizontal shaft, vertical shaft, sample inlet shaft, slide guides of the
lift, and trapezoid screw threads.
* Use only the grease specified for the system. Any other type of grease may not adhere
very well and thus cause failure of the equipment.
67
6.4.9. Adjusting the optical system
Re-adjust the optical system if A/D FULL or LAMP BROKEN error occurs.
Open “Run"－“Maintenance” and click Optical Adjust button.
Optical Adjust screen opens, where the gain SIG1, SIG2, and REF can be adjusted.
(Adjust to ZERO＝0V, SPAN＝4V)
Maintenance
Exit
Click AUTO, and the span and zero of each detector are automatically adjusted.
The power of the lamp is turned OFF when the zero adjustment is performed. Wait at least
20 minutes before carrying out the measurement of a sample after the zero adjustment.
68
6.4.10. Adjusting the mass flow controller
Carry out the zero adjustment of the mass flow controller if the flow rate is not zero even
when the carrier gas is not flowing.
Maintenance
Open “Run”-“Maintenance”, and click the button.
Check the value of FLOW [L/min] and, if it is not 0

through 4, adjust the value with the ZERO trimmer
of the mass flow controller.
● Turn OFF the power of the MA-3000

and remove the top cover and then the
right side cover.
● Start the MA-3000 and open

Maintenance screen.
● Press 2 seconds the ZERO calibration

button.
● Adjust the ZERO trimmer of the mass

flow controller to a value of 1 through 4
using a blade precision screw driver
while watching the value in FLOW
ZERO [L/min] on the maintenance screen.
Adjustment
69
6.4.11. Replacing the air pump tube (Option)
(1) Remove the Teflon tube connected to the Pharmed tube of the air pump.
(2) Grip the cover (blue) of the air pump and turn it about 30 degrees
counterclockwise. The hook fixing the cover will be released and the cover will
come off. Pull the cover out toward you.
(3) Turn over the cover, remove the internal rotor, and then the Pharmed tube.
70
(4) Push a new Pharmed tube into the cover while turning the rotor.
* Engage the INSULOKs at both ends of the tube using the hooks inside the cover.
Ensure to engage the INSULOKs with
the hooks inside the cover when
inserting the tube.
(5) Put the hooks of the cover in the hole of the air pump, and install the cover by
turning it slightly clockwise.
(6) Install the Teflon tube to the right-side Pharmed tube of the air pump.
Insert the Teflon tube, and fix it in place

using two INSULOCKS.
71
NIC-600-2231-11 7. MA3Win
7. MA3Win
This software has two functions; controlling the MA-3000 and processing the
measurement data.
All the operations of the MA-3000 can be controlled using the software.
7.1. Basic screen

MA3Win can be used by switching between two main screens: the control screen for the
setting of measurement conditions and display of current status, and the analysis screen
for checking and reviewing the measurement data.
To switch between the screens, select [File] – [Window] – Screen select (Control screen)]
or [Screen select (Analysis screen)] from the menu, or click the icon.
7.1.1. Control screen
 Control window
Displays measurement sequence in animation.
 On line profile window

The temperature curve of H1 and absorbance during a measurement can be viewed
as a profile.
Instantaneous values are shown using graphs during a measurement. After a
measurement has completed, they then indicate the results.
The scale can be changed using the scroll bar on the left side of the window.
 Table window
The measurement conditions including the Method are set in this window. Standard
samples and unknown samples have their own individual tables. The results are
shown after a measurement has been completed.
72
NIC-600-2231-11 7. MA3Win
7.1.2. Analysis screen
 
 Profile window
The profiles of the measurement results can be viewed.
(1) The profile can be magnified or shrunk with respect to the vertical axis.
(2) Different data can be viewed by shifting the screen to the left or right.
(3) The number of data items to be displayed can be specified. The profile can
also be magnified or shrunk with respect to the time axis.
*The scale of the profiles set on this screen applies to the scale used in printing.
 Calibration curve window
The window displays the current calibration curve.
The “CALIB” tab displays the constructed calibration curve.
The “Result” tab displays the verification results of the calibration curve.
* The verification result of the calibration curve is used to evaluate the accuracy of
the constructed cubic calibration curve. The standard value is plotted on the
horizontal axis while the amount of mercury obtained by the constructed cubic
calibration curve is plotted on the vertical axis, and the correlation coefficient
between them is taken as an index of the accuracy.
 Table window
The measurement results can be viewed in this window.
73
NIC-600-2231-11 7. MA3Win
7.1.3. Common controls
Title bar: The title of the software and the file being currently edited can be viewed.：
Menu bar: Functions shown are displayed. (Refer to 7.2 List of menu commands)
Tool bar: The functions you often use are listed in the form of icons.
          
11 
12 
13 
14 
15
① "Display Change" Refer to 7.2.5.1 Display change (CTL), 7.2.5.2 Display change
(ANA)”
② “Start" Refer to “7.2.3.1Measurement start”
③ “Stop" Refer to “7.2.3.2Stop”
④ "Purge" Refer to “7.2.3.4 Purge”
⑤ "Emergency" Refer to “7.2.3.3 Emergency”
⑥ "Method Set" Refer to 7.2.3.8 Measurement condition”
⑦ "New" Refer to 7.2.1.1 New project (N)”
⑧ "Open" Refer to 7.2.1.2 Open (D)”
⑨ "Save as." Refer to 7.2.1.3 Save as (A)”
⑩ "Print Preview" Refer to 7.2.1.5 Print Preview (V)”
⑪ "Print" Refer to 7.2.1.6 Print (P)”
⑫ "Statistics" Refer to 7.2.4.3 Statistics (S)”
⑬ "Table Condition" Refer to 7.2.4.2 Table condition”
⑭ "PEAK/INTE" Refer to 7.2.4.2 Table condition”
⑮ "Drift Correction" Refer to 7.2.4.2 Table condition”
Status bar: The measurement sequence status can be viewed.

Refer to the section “5.1Measurement Operation Flowchart” for more details on the
measurement sequence.
If “OFF LINE” is displayed, communication with the MA-3000 is not established.
* In this case, confirm that the MA-3000 is powered ON, the communication cable is
connected correctly, and that multiple applications are not being simultaneously executed.
74
NIC-600-2231-11 7. MA3Win
7.1.4. Table window
Samples are registered and the results of measurement can be viewed in the Table
window.
The Table window includes a standard sample table and an unknown sample table.
Calibration curves are created in the standard sample table, and unknown samples are
analyzed in the unknown sample table. 50 standard samples and 200 unknown samples
can be registered in respective tables.
The two tables can be switched by clicking the tabs at the bottom of the window.
* The items to be displayed change according to the settings made in table conditions.
* The width of column can be arbitrarily changed. (When the width of a column has
been set to zero, select the columns on both sides of it and widen it so that it can be
re-displayed.)
7.1.4.1. Common items
   
 Measurement
Check the samples to be measured.
Click the box to enter a checkmark and click again to clear it.
Only samples with checkmarks will be measured
 Sample Number
Enter the tray number of the sample changer.
The sample changer allows random access and hence any number you want can be
entered.
If “0” is entered, the system will carry out a purge measurement without inserting a
boat.
 Date
The time when the measurement is completed is registered after the measurement.
 Remarks
Any comment can be entered.
75
NIC-600-2231-11 7. MA3Win
7.1.4.2. Standard sample
 
     
 Sample name
Select STD when using the measurement data to construct a calibration
curve, or CV when calculating a quantitative lower limit or checking system
operation
 Standard value
Enter the standard sample (mercury) amount.
“STD INPUT” window appears when the “Standard”
cell is clicked. Enter the standard concentration
(temperature in the case of the standard gas), the
injection volume, and then the calculated value of the
amount of mercury.
The unit of the standard concentration can be
changed by clicking the unit button. When you want to input the standard value
(amount of mercury) directly, press ESC and the “STD INPUT” window disappears.
 LOW
Indicates the measurement result of LOW range.
 HIGH
Indicates the measurement result of HIGH range.
 PEAK or AREA
The cell indicates a measured PEAK value (peak height) or AREA value (area).
[ON/OFF] indicates whether or not drift correction has been activated.
 MEAS[ng], Measured value

The PEAK value or AREA value displayed by a calibration curve is converted into an
amount of mercury.
The unit synchronizes with the unit of “Standard value”.
 Dev[%], Deviation
The deviation between the measured value and standard value is displayed as a
percentage.
 ‫ס‬Χ, Employ or ignore the data

You can select whether to employ the data or not.
Clicking it will toggle between “○” and “×.” If you do not wish to use it, select “×.”
When set to “×,” the data will be excluded from the construction along with the
printing of a calibration curve, and also from the statistical calculations.
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7.1.4.3. Unknown sample
         
 Method
The heating conditions can be individually set for each
sample with the measurement of unknown samples. Select
an option from the pull-down menu* Detailed settings of
the method can be made from “Run“ –“Method setting”
 Name
Enter any sample name.
Click the arrow on the right of a cell to open the pull-down
menu on which special names and names added by
executing “Table” – “Registration of names” are displayed.
* The number of characters is not limited, but some

characters may not be printable if the name is too long.
Special names
CHECK STD
Used to check the condition (sensitivity) of the unit when measuring unknown
sample.
When a measurement is performed using the sample name of “CHECK STD,” it can
be discontinued if the result is out of the range. (Refer to 7.2.3.8Measurement
condition.)
For measurements under “CHECK STD,” use a standard solution in a sample boat.
R Blank
If an additive reagent is used in the measurement of unknown samples, the amount
of mercury contained in it may affect the measurement results. To compensate for
that, the mercury amount contained in the reagent is measured as R.Blank and used
to make adjustments for it.
Select “R.Blank” in the Name column, and perform the measurement of the reagent
in the same way as an unknown sample. The value of R.Blank is then automatically
subtracted from the measured value (mercury amount and concentration) of an
unknown sample. (For the details, refer to 7.6 R.Blank Calculation method.)
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 SVOL
Enter the sample volume or weight into this cell.
 ADDSTD
Used to determine the addition recovery of an unknown sample. Enter the amount of
mercury added to the sample.
 MOIST
Enter the moisture content in the cell to compensate for moisture. If the cell was blank,
the calculation will be made with assumption that the value is zero. It is displayed
when “Moisture Content” is “ON.”
 PEAK or AREA
Peak or Area and HIGH range and LOW range is outputted after measurement.
 MEAS
The amount of mercury calculated by the calibration curve from PEAK or AREA value
is outputted.
 CONC
Concentration is outputted.
Concentrat ion  (Measured mercury value - R.BLANK ） 
Sample amount x (100 - Moisture content ratio)  100
 Recovery
Recovery rate is outputted
Recovery  Measured value - Sample amount x Average concentration of sample 
Standard addition
Measurement results with the same sample name are used in the calculation.
The recovery rate is calculated from the concentration obtained from the results
whose standard addition cells are blank.
 X (Employ or ignore the data)

Selects whether the data should be employed or ignored after the measurement.
Clicking it will toggle between ○ and ×. Set to × if you do not employ the data. When
this cell is set to ×, the data are excluded from printing and statistic calculation.
⑪ Range
Selects whether the LOW data or the HIGH data should be employed.
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7.2. List of menu commands

The followings are descriptions of functions of each menu.
7.2.1. File (f)
7.2.1.1. New project (N)
Executed to clear all the data displayed and start new measurement.
Standard and Sample Clear All

Clear all the data both in STD and SMP tables.
Only Sample is clear
Clear data only in SMP table. Any data in STD table remain.
All Abs is clear
Clear only the data such as Peak values and Measured values without changing the
STD values, sample names and method.
Sample Abs is clear
Clear only the data such as Peak values and Measured values in SMP table.
Clear MEMO
If “Clear MEMO” is checked, the content in “MEMO” will also be cleared when the data
are cleared.
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7.2.1.2. Open (D)
Executed to open and display files saved in the past.
“Files of Type” has the following two options

MA3 Data File: The file in which the measured results are registered.
MA3 Template File: Template file in which items excluding the measured results are
registered
7.2.1.3. Save as (A)
Saves the measurement data in a file.
“Files of Type” has the following two options。

MA3 Data File： The file in which the measured results are saved.
MA3 Template File： Template file in which the items excluding the measured results
(such as sample names and methods) are saved.
Used as a template for the mercury amount for calibration curves or
routine measurements.
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7.2.1.4. Page Setup (U)
Set page details for printing.

Header
Set text which is printed as the
header.
Page
Set whether to print page numbers.
Start page No.
Set the start page number.
7.2.1.5. Print Preview (V)
Displays print preview image.
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7.2.1.6. Print (P)
Print measurement data.

Only items with a checkmark are printed.
Table and Profile are printed only when they have a  mark in the X column on the
table screen.
The table conditions for Profile are determined using the profile window settings described
on the Analysis screen described in 7.1.2.
Memo Set ： Print the items in “Memo” that were set in the measurement
conditions.
Calibration ： Print the calibration curve as a graph.
Standard
Table ： Print the table of standard samples.
Statistics ： Print the statistical results of standard samples.
Profile ： Print the profiles of standard samples.
The settings of the scale and the number of profiles printed in one
line are the same as those for the table of the standard sample.
Set the respective scales for HIGH and LOW ranges.
Sample
Table ： Print the table of unknown samples.
Statistics ： Print the statistical results of unknown samples.
Profile ： Print the profiles of unknown samples.
The setting is the same as that for the table of unknown sample.
Method ： Print the measurement condition.
Measure comp ： Print the measurement completion time for each sample.
time
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7.2.2. Edit (E)
Data can be copied, moved or deleted using the Edit menu
* Right-clicking also displays the pull-down menu.
7.2.2.1. Copy (C)
Copies selected data to the clipboard. Any data in the selected cells are copied to the
clipboard when the table window is active. When the profile window is active, any image
data are copied to the clipboard
7.2.2.2. Cut (T)
Cuts the data in selected cells. PEAK/AREA, HG and CONC cannot be cut.
* The values of SVOL, CVOL, and DVOL turn to “1” when cut
7.2.2.3. Paste (P)
Pastes data copied to the clipboard to cells. Click cells in which the data are to be pasted,
and then execute the command.
* No data can be pasted in the PEAK / AREA, HG or CONC columns.
7.2.2.4. Remove (R)
Removes a line(s). Click the line number to select the entire line and execute the
command.
7.2.2.5. Insert (I)
Inserts a blank line. Click the line number to select the entire line and execute the
command. When multiple lines are selected, blank lines in the same number are inserted.
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7.2.2.6. Move (M)
Use when the data sequence is rearranged.

The pointer changes to a shape when Move mode is enabled. Click the number of the
line you wish to move and drag it to the target place, and then release the mouse button.
* A line can not be moved from the STD table to an SMP table and vice versa.
7.2.2.7. Save as Text File (T)
Saves data as a text file (CSV).

To save any standard data, click the “STD” tab. To save any unknown sample data, click
the “SMP” tab.
* Only data with a circle () marked in the X cell will be saved.
7.2.2.8. Save as Jpeg File (J)
Saves image data as a file.
7.2.2.9. Add Data (A)
Imports past data into a current table.

Click the line number below which you wish to insert the data and then execute the Add
Data command.
* The data below the clicked line will all be deleted.
7.2.2.10. Reading Sample Amount from the balance
Receives sample amount data from an electronic balance and writes it into the sample
amount cell.
1. Click the first cell into which the

data are to be entered and then
execute the “Reading Sample
Amount from the balance”
command.
2. Press the data output key on the

balance to output the data.
* The function is effective only when the type of sample is set to “Solid” in the table.
* Balances available include the MS series, ML series and ME series of Mettler-Toledo.
The balance can be set by selecting System Menu - Balance Port Set.(Refer to
7.2.4.9 Balance communication settings (B))
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7.2.3. Run menu
7.2.3.1. Measurement start
Start the measurement. (Short cut key F5)

The system displays a screen for setting the name of a file in which the data are saved
first. Set a file name.
File name Save

File name Cancel
The default file name is “Date + Time”. (Example：2013-03-12 09-59-12.MA3)

The template file is read, the measurement is started, and the file is named “Template file
name + Date + Time”.
(Example：TEST.MA3TMP→TEST(2013-03-12 09-59-12).MA3)
The measurement starts when the Save is pressed.
Then the measurement result is saved automatically in the designated file every time the
measurement is completed.
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*Backup file
Every time the file is automatically saved, a backup file with the same name and the
extension “MA3DEPOSIT” is created. (Example: TEST.MA3  TEST.
MA3DEPOSIT)
If a file has been erroneously edited and saved, it is possible to restore the data by
reading the backup file after changing its extension to “MA3.”
* However, if the measurement is continued with the same file name, the file is saved
based on the erroneously edited content.
The backup files continue to increase if not deleted intentionally. Periodically delete
those that are not necessary.
7.2.3.2. Stop
The measurement stops once the current measurement has been completed (the shortcut
key: F8).
7.2.3.3. Emergency
The measurement is immediately terminated and the cooling cycle starts.
7.2.3.4. Purge
Any mercury content remaining in the system is purged before measurement starts. The
result of the purge measurement is not recorded in the Table.
7.2.3.5. Reset
The system terminates all the sequences and return to READY Status.
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7.2.3.6. Method Setting
Sets the heating conditions (Atomize1 through 4) of the sample heating furnace H1.
Several conditions have been preset as factory defaults, but it is also possible to change
them or create new conditions.
A heating sequence consists of 4 stages, i.e. the moisture removal stage and 3
temperature raising stages.
Atomize1: Remove any moisture and interfering substances with low boiling points.
Atomize2 through 4： Decompose mercury compound in the sample.
* If a sample containing a large amount of halogen is rapidly heated, a gas containing

interrupting components is quickly generated, so that the throughput capability of the
catalyst is exceeded and the normal measurement becomes impossible. In this case,
the temperature is raised stepwise to disperse the load on the catalyst, by which the
measurement may continue.
Heat temp:
Set the highest heating
temperature.
Heat time:
Set the heating time.
Flow:
Set the flow during heating.
Start duty:
Set the duty cycle when heating
starts.
Max duty:
Set the maximum duty cycle.
* The temperature control will only
work if the temperature exceeds the
set Heat temp.
Slope time:
Set the time interval from Start duty to
Max duty.
Method Number: Select the method number to display the details of the method settings.
Save to: Save the settings as a specified number.
Method name: The method name can be freely changed here.
Save : Save the settings of the method after having been edited.
* The settings are saved for each method instead of all at once.
* Ensure to save settings every time changes are made.
Reset: The settings are returned to the factory default.

* The method name will not change.
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7.2.3.7. Starting the measurement and turning OFF the heater after the
measurement
Start the measurement and turn OFF the heater after the measurement.
The heater can be automatically turned on again after it is turned OFF.
When “A heater automatic return is not carried out” is selected.

(1) The measurement starts when
Execute is clicked.
(2) The heater turns OFF when the

measurement is completed. The
turned OFF heater does not turn ON
until Cancel is clicked.
When “It heater-automatic-returns" is selected.

(1) Set the time when the heater turns
ON again.
(2) The measurement starts when

Execute is clicked.
(3) The heater turns OFF when the

measurement is completed.
(4) The heater automatically turns ON

when the set time comes.
* The stand-by mode is cancelled and the
heater immediately turns ON when
Cancel is clicked.
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7.2.3.8. Measurement condition
The measurement condition is set on this screen.
7.2.3.8.1 General
STD Method
Sets the method used for the measurement of standard solution.
Flow rate
Sets the flow rate during the measurement. (Selected from 0.1L/min, 0.2L/min, or
0.5L/min.)
* There is a limitation in the change of the flow rate because the condition must be the
same to maintain the consistency of the date in the same table.
● Once the measurement is carried out, the flow rate cannot be changed. (It can
be changed when a new measurement is carried out.)
● It cannot be changed even in a new measurement if ABS remains in it.
STD check
Sets the condition of standard check.
STD [ng] Enter the amount of mercury of the standard sample to be measured.
Recovery Rate Set the deviation of recovery rate, which should be determined to be
[100%±] abnormal for measurements under CHECK STD.
Abnormal Select to “Discontinue” or “Continue” the subsequent measurement in
condition the case the recovery rate falls below the set value.
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7.2.3.8.2 Blank check
Sets the condition of blank check.
OFF/ON Check “ON” to enable the blank check function.

Mode The detection mode is selected from “LOW” or “HIGH.”
“LOW” is for the low conc. cell, and “HIGH” for high conc.
cell.
Threshold Level Set the PEAK height as the threshold value for high
concentration.
Default: 0.2ABS (about 10 ng)
Return Level Set the PEAK height at which the purge measurement will
return to normal measurement.
Default: 0.001ABS (about 0.05ng)
Repeat Times Set the number of times the purge is repeated.
Default: 5 times
Abnormal Select “Continue” or “Discontinue” for the process for the
Condition case the value does not fall below the Return level even if the
purge is repeated the maximum number of times:
Default/ Continue
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* When the blank value is measured after the measurement of a sample, about 1% of
the immediately previous detection value is detected as historic record.
* Using the default setting, Blank check may be frequently carried out and the
measurement may take a long time to complete when only samples of which
concentration is high are measured. In such a case, change the threshold level and
recovery level.
ABS value (0.2L/min)
ABS(LOW) ABS(HIGH)*
0.1ng 0.004 10ng 0.001
1ng 0.02 100ng 0.01
5ng 0.1 1,000ng 0.1
10ng 0.2 5,000ng 0.4
20ng 0.4 10,000ng 0.6
50ng 1.0 20,000ng 0.9
7.2.3.9. To Heater suspension
Suspends the heater and automatically turns it ON at the designated time.
1. Set the return time and click Execute,

and then the heater turns OFF.
2. The heater turns ON when the set time

comes.
The stand-by mode is cancelled and
the heater immediately turns ON when
Cancel is clicked.
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7.2.3.10. Leak check
Confirms that there are no loose joints or damage to the tubes.

Click “Leak Check” in “Run” menu to open "Leak Check” window.
(1) The flow rate is checked first when

“START” is clicked. The leak check
displays “FLOW ERROR” and
terminates when the flow rate does
not reach 0.4L/min. In this case,
check the oxygen supply pressure.
(2) The sample inlet is closed and the

leak check starts if the flow rate
reaches 0.4L/min.
When the flow rate decreases from
around 0.4L/min to 0.00L/min within
30 seconds, the check has been
completed successfully. If the flow
rate does not fall to 0.00L/min, check
the flow path.
(3) Click EXIT to cease the leak check.
Check the tubes only after the power switch has been
Warning turned OFF and the heater has cooled down to room
temperature or it could result in burns.
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7.2.3.11. Maintenance
The movement and status of the hardware components get monitored on the screen.
Used for maintenance or when a system failure has occurred.
7.2.3.11.1 MA
A/D
H1[degC] H1 temperature
H2A [degC] H2A temperature
H2B [degC] H2B temperature
H3 [degC] H3 temperature
H4 (PIPE)[degC] Temperature of piping heater
H5 (OPT)[degC] Temperature of optical system heater.
H6 (RH1)[degC] Temperature of heating furnace (Optional)
H7 (RH2) Temperature of heating furnace RH2 (Optional)
H8 (RSV) Not used
FLOW1[L/min] Flow of mass flow controller
LAMP [V] Lamp voltage
CAP [V] Lamp heater voltage
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I/O
V1 Turns ON/OFF the solenoid valve 1.
V4 Turns ON/OFF the three directional solenoid valve 4.
V5 Turns ON/OFF the three directional solenoid valve 5.
FAN1 Turns ON/OFF the cooling fan of sample heating furnace H1.
FAN3 Turns ON/OFF the cooling fan of mercury collecting furnace H3.
BUZZER Turns OFF/ON the buzzer.
LED Turns ON/OFF the LEDs on the board.
P2 Turns ON/OFF pump P2 for reducing vaporization (Optional)
FAN6 (RH1) Turns ON/OFF cooling fan 1 for RH-MA (Optional)
FAN7 (RH2) Turns ON/OFF cooling fan 2 for RH-MA (Optional)
FAN8 (YOBI) Not used
FLOW [L/min] Flow test of mass flow controller
HEATER
For the test of H1 (Enter temperature). Limited up to 10% of
H1 the capability for protection purpose.
For the test of H2A (Enter temperature). *Do not set any
H2A value higher than the default.
For the test of H2B (Enter temperature). *Do not set any
H2B value higher than the default.
For the test of H3 (Enter temperature). *Do not set any value
H3 higher than the default.
H4 (PIPE) higher than the default.
H5 (OPT) higher than the default.
H6 (RH1) Controls the H1 temperature of the collection tube heating
furnace PH-MA. (Optional)
H7 (RH2) Controls the H2 temperature of the collection tube heating
furnace PH-MA. (Optional)
H8 (YOBI) Not used
The heaters are tested using the temperature entered in the left column and the duty
entered in the right column.
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Sig/Ref
Sig1 [V] Output voltage of the signal from “LOW” side detector
Ref [V] Output voltage of the signal from the Ref. lamp detector
Sig2 [V] Output voltage of the signal from “HIGH” side detector
Lamp OFF Optical lamp OFF
Lamp ON Optical lamp ON
Optical Adjust Adjustment of voltage of Sig1, Ref, Sig2
Optical Adjust (Adjustment of the optical system)

The optical system adjustment screen opens when “Optical Adjust” button is clicked.
Voltages SIG1, SIG2, and REF of the optical system are adjusted here. (Adjusted to
ZERO=0V, SPAN＝4V)
There are the following 3 types of adjustment methods.

① Individual automatic adjustment for each channel
② Adjustment of voltage by entering the gain value directly. (Allowable input range：
0-255)
③ All channel automatic adjustment
 
Exit
Click a button to execute automatic adjustment.

The lamp turns OFF temporarily when automatic adjustment such as ZERO adjustment is
executed.
Therefore you need to wait for the lamp voltage to be stabilized when executing SPAN
after ZERO is executed.
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7.2.3.11.2 BC
SENSOR
LIFT-UP Status of the upper limit sensor of the lift
LIFT-DOWN Status of the lower limit sensor of the lift
TRAY Status of the tray detection sensor on the arm
BOAT Status of the boat detection sensor
DOOR OPEN Status of the door open sensor
REFUGE TRAY BOX Status of the refuge tray box sensor
AXIS=Z IN0 Z axis sensor
SPARE1 Not used
TRAY SENSOR
TRAY01 to 10 Status of the tray detection sensors in the rack
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BC ADJUST
For any sample boat, the action of the sample changer can be tested.
Run an action
Return before an action
Run a step
Return before a step
7.2.3.11.3 ETC
OVER HEATING Turns ON when the safety device for accident

prevention is triggered to stop the heater.
LIGHT Not used
LED Tests LEDs on the front panel. (4 through 7 are not
used)
DIP-SW Indicates the status of the DIP-switches on the board
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7.2.3.11.4 SC5
Used for testing the SC-5 sample changer for reducing vaporization
TABLE Turns the turntable to the entered position.

ARM Moves the arm to the entered position.
LIFT Moves the arm to the entered height.
SAMPLE No. Lowers the cap of the entered unknown sample number.
Item Function
RD Turns ON/OFF each pump.
Get the SC-5 information (VERSION, SERIAL). Click
INFORMATION “REQUEST”.
Click “READ”. Turns ON/OFF H2SO4 pump. Get the location
OFFSET information (TABLE, ARM, LIFT).
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7.2.3.11.5 GLP
Item Function
LAMP ACTIVE TIME Indicates the accumulated active period of the lamp.
ABS Hg Indicates the accumulated amount of mercury
measured.
MEAS CNT Indicates the accumulated number of measurement.
The values can be cleared by clicking the respective “CLEAR” buttons.

* After exchanging a sample heating tube, clear “MEAS CNT”.
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7.2.3.11.6 Parameter
Only used in inspections made by the manufacturer.

Maintenance
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7.2.4. Table (T) menu commands
7.2.4.1. Memo set (M)
Attaches a memo to the measurement data.

Items to be recorded include Title, Date, Name, Etc (other information) and Memo.
These items can also be printed out.
－Print example－
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7.2.4.2. Table condition
Sets the table conditions.
The calibration curve, mercury amount, and concentration are calculated based on the
conditions set in this window. The conditions can be changed even after a measurement
has taken place.
PEAK/INTE
Selects Analysis mode from PEAK (peak analysis) or AREA (area analysis).
Sample
Selects the type of Sample from “Liquid” or “Solid”
Calibration Curve
Selects the type of calibration curve for each of the Low and High measurement ranges.
Three options are available for use as the type of calibration curve: the normal curve
calculated using the least square method (+b), the curve calculated using the least
square method and passing through the blank (+Blank), and the curve calculated using
the least square method and passing through zero (+0).
Selecting the normal curve (+b) with normal measurements and the curve passing
through the blank (+Blank) with measurements of trace quantities of mercury close to
the blank value enable the best measurement results.
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Unit
Sets the units of standard mercury amount, sample amount, mercury amount, and
concentration.
The selectable unit varies depending on the type of sample.
Others
Decimal Places
Sets the decimal places of the concentration to be displayed.
Drift Correction
Selects whether or not to apply drift correction to the base line
In normal use, “Yes” should be selected. Cancel the drift correction for analysis only
when checking the condition of the system.
Minus Display
When a calculated concentration/amount of mercury is a negative, selects to display
whether the value with minus sign or zero instead.
Moisture Content
Selects whether to display moisture correction or not.
* Can only be selected when the type of sample is set to “Solid”.
Statistic
Selects Mercury amount or Concentration as the object of the statistical calculations.
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7.2.4.3. Statistics (S)
Used to perform statistical calculations.

For standard samples, data from the same standard samples, and, for unknown samples,
data from unknown samples with the same name are used in the statistical calculations.
The results of the calculations can be saved in a file in text format or copied to the
clipboard from the menu.
7.2.4.4. Registration of sample name (N)
Often used sample names can be registered in the system.

The registered names are listed on the pull-down menu when the sample name cell in the
unknown table is clicked.
Enter the sample name

and press “Enter key” or
click “Add” button.
The sample names

currently registered are
displayed here.
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7.2.4.5. System (S)
7.2.4.6. Communication port setting (C)
Sets the RS232C port used for communication with the MA-300
7.2.4.7. Environment settings (S)
7.2.4.7.1 System settings
Folder in which the measurement data are saved

Sets the folder in which the measurement data are saved.
Click the Browse button and select the folder.
It can be set for each measurement method.
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Language
Selects Japanese or English as the display language.
Measurement method
Selects the measurement method from the options listed below.
If REDUCTION-AMALGAM or REDUCTION-DIRECT is selected, also select an
optional unit.
 HEATING VAPORIZE
 RH
 REDUCTION-AMALGAM
 REDUCTION-DIRECT
Optional Unit
1. IMPINGER UNIT ····················· Impinger unit

2. IMPINGER UNIT + RD·············· Impinger unit + reagent injection unit
3. SC3 + RD3 ····························· Sample changer + reagent injection unit
4. SC5 + RD5 ····························· Sample changer + reagent injection unit
Format of the date

Selects the format of the measurement completion time displayed in the table from the
following 3 types.
 hh:mm： Only time is memorized.
 yyyy/mm/dd hh:mm： Date (Year/Month/Day) and time
 mm/dd/ yyyy hh:mm： Date (Month/Day) and time
* Any new settings with “Language” and “Measurement method” only take effect after
the software has been restarted. The software automatically restarts after any
changes to the settings.
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7.2.4.7.2 Setup of calibration curve
Sets the criteria for good/no-good evaluation of the calibration curve.

A deviation between the ABS for 1ng or 100ng and the set value is back-calculated from
the constructed calibration curve, from which the calibration curve is determined whether
it is good or no-good.
Calibration Test ABS Value

Sets the PEAK and AREA standard values for each measurement method. Enter the
median for 1ng in LOW range and that for 100ng in High range.
Limit (%)
The equation of the calibration curve changes to red and WARNING is displayed when
the deviation between the back-calculated value and the set value is out of this range.
* The ABS value changes depending on the

measurement method and the condition of the system.
* Carefully change the set values.
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7.2.4.8. Color arrangement settings (W)
Sets the color arrangement of the screen.
If the “Reset” button is clicked, the color

arrangement is returned to the factory
default settings.
7.2.4.9. Balance communication settings (B)
Sets the communication parameters according to the balance to be used.

The system supports the following balances: Mettler’s MS series, ML series, and ME
series.
* The baud-rate must match the baud rate of the balance to be connected.
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NIC-600-2231-11 7. MA3Win
7.2.4.10. Firmware Update
Upgrade the version of the ROM built into the MA-3000. (Refer to 4.3.7
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NIC-600-2231-11 7. MA3Win
How to upgrade the version of ROM built into the MA-3000)
7.2.5. Window (W)
7.2.5.1. Display change (CTL)
Switches the screen to Control.
7.2.5.2. Display change (ANA)
Switches the screen to Analysis.
7.2.5.3. Display Initialize
Resets the screen size to the factory default.
7.2.5.4. Sequence Log and Error History Labeling
Displays the contents of sequence log files and error history files.
File name Open

Save as type Cancel
Sequence log files and error history files

The sequence log files, in which the system’s operation history is recorded, and the
error history files, in which the contents of error are recorded, are created as a means to
analyze system troubles.
The files are created in “LOGDATA” folder in the application program folder.
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NIC-600-2231-11 7. MA3Win
The sequence log file is named as “SEQUENCELOG(XXXX-XX-XX).txt” and the error

log is named as “ERRORLOG(XXXX-XX-XX).txt”.
(Where XXXX-XX-XX is a date.)
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NIC-600-2231-11 7. MA3Win
7.2.6. Help
7.2.6.1. About…
Displays the version of the software.
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NIC-600-2231-11 7. MA3Win
7.3. How to determine a calibration curve

The calibration curve is calculated using the least square method as follows.
7.3.1. 1Linear formula
《ｙ＝ａｘ＋ｂ》
a = ( ∑yx ＊ n - ∑y ＊ ∑x ) ／ ( ∑x^2 ＊ n - ∑x^2 )
b = ( ∑y - a ＊ ∑x ) ／ n
《ｙ＝ａｘ＋Ｂｌａｎｋ》
a = ( ∑yx - (Blank ＊ ∑x) ) ／ ∑x^2
b = Blank
《ｙ＝ａｘ＋0》
a = ∑yx ／ ∑x^2
b=0
7.3.2. 3 Cubic formula
《ｙ＝ａｘ＾３＋ｂｘ＾２＋ｃｘ＋ｄ》
tx3yp= ∑x^3y u1= (tx3yp＊n - ty1p＊tx3p) s1= (u1＊u9 - u3＊u6)
tx2yp= ∑x^2y u2= (tx2yp＊n - ty1p＊tx2p) s2= (u2＊u9 - u3＊u8)
tx1yp= ∑xy u3= (tx1yp＊n - ty1p＊tx1p) s3= (u4＊u9 - u6＊u6)
ty1p = ∑y u4= (tx6p ＊n - tx3p＊tx3p) s4= (u5＊u9 - u8＊u6)
tx6p = a∑x^6 u5= (tx5p ＊n - tx3p＊tx2p) s5= (u7＊u9 - u8＊u8)
tx5p = a∑x^5 u6= (tx4p ＊n - tx3p＊tx1p)
tx2p = b∑x^2 u9= (tx2p ＊n - tx1p＊tx1p)
tx1p = c∑x
a= ( s1＊s5 - s2＊s4 ) ／ ( s3＊s5 - s4＊s4 )
b= ( s1 - a ＊ s3 ) ／ s4
c= ( u1 - a ＊ u4 - b ＊ u5 ) ／ u6
d= ( tx3yp - a ＊ tx6p - b ＊ tx5p - c ＊ tx4p ) ／ tx3p
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NIC-600-2231-11 7. MA3Win
《ｙ＝ａｘ＾３＋ｂｘ＾２＋ｃｘ＋Ｂｌａｎｋ》
tx3yp= ∑x^3y s1= (tx3yp ＊ tx2p) - (tx1yp ＊ tx4p)
tx2yp= ∑x^2y s2= (tx2yp ＊ tx2p) - (tx1yp ＊ tx3p)
tx1yp= ∑xy s3= (tx6p ＊ tx2p) - (tx4p ＊ tx4p)
tx6p = a∑x^6 s4= (tx5p ＊ tx2p) - (tx4p ＊ tx3p)
tx2p = b∑x^2
tx1p = c∑x
a= ( (s1＊s6- s2＊s4) - Blank(s5＊s6 - s7＊s4) ) ／ ( s3＊s6 - s4＊s4 )
b= ( s1 - Blank＊s5 - a＊s3 ) ／ s4
c= ( tx3yp - (a ＊ tx6p) - (b ＊ tx5p) - (Blank ＊ tx3p) ) ／ tx4p
d= Blank
《ｙ＝ａｘ＾３＋ｂｘ＾２＋ｃｘ＋０》
tx3y1p= ∑x^3y s1= (tx3yp ＊ tx2p) - (tx1yp ＊ tx4p)
tx2y1p= ∑x^2y s2= (tx2yp ＊ tx2p) - (tx1yp ＊ tx3p)
tx1y1p= ∑xy s3= (tx6p ＊ tx2p) - (tx4p ＊ tx4p)
tx6p = ∑x^6 s4= (tx5p ＊ tx2p) - (tx3p ＊ tx4p)
tx5p = ∑x^5 s5= (tx4p ＊ tx2p) - (tx3p ＊ tx3p)
Tx4p = ∑x^4
Tx3p = ∑x^3
Tx2p = ∑x^2
a= ( s1＊s5 - s2＊s4 ) ／ ( s3＊s5 - s4＊s4 )
b= ( s1 - a＊s3 ) ／ s4
c= ( tx3yp - (a ＊ tx6p) - (b ＊ tx5p) ) ／ tx4p
d= 0
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NIC-600-2231-11 7. MA3Win
7.4. Calculation formula for mercury amount and concentration

The measured value is obtained through calculations using the selected calibration curve,
with the concentration and mercury amount then being calculated as follows.
 Mercury amount
Thermal vaporization
Mercury amount = Measured value
* If R.BLANK is specified,
Mercury amount = Measured value – Measured value of R.BLANK
Reducing vaporization
If the unit of sample amount is “none”,
Mercury = None
If the unit of sample amount is not “none”,
Mercury amount = Measured value x (Constant volume / Dispensed
volume)
 Concentration
Thermal vaporization
Concentration = Mercury amount / Sample amount
Reducing vaporization
If the sample amount is “none”,
Concentration = Measured value
If the sample amount is not “none”,
Concentration = Mercury amount / Sample amount
If the moisture correction is valid (i.e. the type of Sample is set to “Solid” and
Moisture Content is set to “Yes”),
Concentration = Concentration x 100 / (100 – Moisture content [%])
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NIC-600-2231-11 7. MA3Win
7.5. Standard addition

A recovery rate is calculated by adding a known amount of mercury and measuring it
together with a sample.
The recovery rates of some samples are not more than 90% and therefore are used to
determine whether the measurement method is good or no-good.
(1) Measure a sample and obtain the concentration of the sample.

(2) Weigh the sample on a sample boat and add the standard solution.
* It is also possible to add a sample of a known concentration such as standard
substance to calculate the recovery rate.
(3) The name of the standard solution-added sample should be the same as the name
of the sample.
Example
Name SVOL ADDSTD PEAK MEAS CONC RECOVE
[mg] [ng] [ng] [ppm] RY[%]
Sample1 40 0.004005 48.7061 1.218 -
Sample1 30 0.003719 45.2043  1.507 -
Sample1 35 0.003927 47.7510 1.364 -
Sample1  30  40.000 0.006713  81.2528 2.708  100.9
MEAS [ng] – Averaged CONC (ppm) x SVOL )

Recovery [%] = x 100
ADDSTD [ng]
* In measuring a sample with large variation, the variation of the recovery of the added
standard solution/substance becomes larger as the added amount is smaller. Take
the variation of the sample into consideration when determining the amount of
standard solution/substance to be added.
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NIC-600-2231-11 7. MA3Win
7.6. R.Blank Calculation method

If an additive reagent is used in the measurement of unknown samples, the amount of
mercury contained in it may affect the measurement results. To compensate for that, the
mercury amount contained in the additive is measured as R.Blank and used to make
adjustments for it.
When “R.Blank" is selected for a name of a sample, the R.Blank value is automatically
subtracted from the measurement results of an unknown sample (the amount and
concentration of mercury).
It is possible to set two or more R.Blank values by adding a letter after the character string
of R.Blank when changing the type of the additive or reset the R.Blank value at a certain
interval.
The R.Blank values with the same name obtained from a sample are averaged, which is
used for the compensation for the measurement value of the sample.
Sample Measured
Concentration
No. Sample Name Volume Value
[μg/L]
[μL] [ng]
1 Sample1 100 0.050 0.500
2 Sample2 100 0.051 0.510 No compensation
3 Sample3 100 0.052 0.520
4 RBlank1 0.001
5 RBlank1 0.000
6 Sample4 100 0.005 0.043 Concentration calculated
by subtracting the
7 Sample5 100 0.051 0.503 average of RBlank1 from
the measured value.
8 Sample6 100 0.052 0.513
9 Sample7 100 0.050 0.493
10 RBlank2 0.006
11 RBlank2 0.005
by subtracting the
the measured value.
14 RBlank3 0.010
by subtracting RBlank3
16 Sample11 100 0.012 0.020 from the measured value.
17 RBlank1 0.001
18 Sample12 100 0.051 0.503
by subtracting the
the measured value.
21 Sample15 100 0.054 0.533
Average of RBlank1 0.0007 =(0.001+0.000+0.001)/3

Average of RBlank2 0.0055 =(0.006+0.005)/2
Average of RBlank3 0.0100
117
NIC-600-2231-11 8. Contact
8. Contact
Nippon Instruments Corporation

URL http://www.hg-nic.com
E-mail [email protected]
For technical inquiries and maintenance parts
Technical Center
14-8 Akaoji-cho, Takatsuki-shi, Osaka 569-1146, Japan
Phone: +81-72-693-6820
Fax: +81-72-694-0663
118

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Fully-automatic Thermal Vaporization

Mercury Analysis System

Nippon Instruments Corporation

Fully-automatic Thermal Vaporization

1.1. Safety precautions ................................................................................................... 1

2. OPERATING PRINCIPLE .................................................................................................. 4

2.1. Operation ................................................................................................................. 4

3.1. Standard configuration ............................................................................................ 11

4.1. Conditions for installation ....................................................................................... 12

4.3.1. Installing MA3Win ........................................................................................... 14

5.1. Measurement Operation Flowchart ....................................................................... 23

6.1. Inspection items ..................................................................................................... 42

6.3. Troubleshooting ..................................................................................................... 50

7.1. Basic screen........................................................................................................... 72

1.1. Safety precautions

1.1.1. Meaning of safety alert symbols

Indicates that incorrect handling could result immediately in death or

1.1.2. Installation precautions

 Be sure to connect the protective grounding to prevent electric shock.

1.1.3. Handling precautions

 Be careful when touching or handling any of the glass components or

1.1.4. Maintenance precautions

1.2. System Outline

Fan3 Oxygen cylinder

Light absorption cell 1

Air pump (P2)

2.2. Part names and functions

No. Name Function

2.2.2. Inside front cover

No. Name Function

No. Name Function

2.2.4. Internal components seen from the top

No. Name Function

2.2.5. Internal components seen from the right

No. Name Function

2.2.6. Internal components seen from the left

No. Name Function

3.1. Standard configuration

(3) Standard accessories

3.2. Component specifications

Analysis method: Thermal vaporization atomic absorption

Samples: Solid, Liquid, Gas (RH-MA3 required)

Measurement principle Non-dispersion triple-beam cold atomic absorption

Measurement range: 0.001 to 70,000ng

(2) Auto sample changer

Sample boat: Ceramic boat specified for the system

(3) Data analysis/System control software MA3Win

OS: Windows7, Window8, Windouws10

Data processing: Construction of calibration curve, Concentration

Room temperature: 15 to 35°C

4.1.2. Power supply

Power voltage: Single phase 100,110,120,220,230,240VAC, 50/60Hz

4.2. Installation and connections

(1) Place the MA-3000 where it will be operated.

Exhaust gas tube RS-232C Cable

4.3. Installing software

4.3.1. Installing MA3Win

(3) The “Select Installation Folder” window will appear.

(4) When the “Confirm Installation” window opens, click