Nippon MA-3000 User manual

Fully-automatic Thermal Vaporization
Mercury Analysis System
MA-3000
Instruction Manual
NIC-600-2231-14
Nippon Instruments Corporation

MA-3000 Instruction Manual NIC-600-2231-14
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

MA-3000 Instruction Manual NIC-600-2231-14
4.3.1. Installing MA3Win..........................................................................................14
4.3.2. Installing USB Serial Converter driver...........................................................15
4.3.3. Setting Communication port..........................................................................16
4.3.4. How to uninstall MA3Win ..............................................................................18
4.3.5. How to upgrade MA3Win ..............................................................................18
4.3.6. How to upgrade the version of ROM built into the MA-3000 .........................19
4.3.7. The case of fail in updating firmware.............................................................20
5.MEASUREMENT............................................................................................................21
5.1. Measurement Operation Flowchart ......................................................................21
5.2. Samples ...............................................................................................................22
5.3. Necessary supplies for measurements.................................................................23
5.4. Articles recommended for measurement..............................................................23
5.5. Preparation for measurement...............................................................................23
5.5.1. Preparing mercury standard solution.............................................................23
5.5.2. Blank treatment of sample boat.....................................................................24
5.5.3. Blank treatment of additives..........................................................................24
5.6. Starting up the system..........................................................................................25
5.6.1. Starting the control software..........................................................................25
5.6.2. Starting the MA-3000.....................................................................................25
5.6.3. Supplying carrier gas.....................................................................................26
5.6.4. Checking the tubes for leaks.........................................................................26
5.6.5. Conditioning ..................................................................................................28
5.6.6. Discharging liquid from the drain tank...........................................................28
5.7. Measurement .......................................................................................................29
5.7.1. Blank check...................................................................................................29
5.7.2. Setting the measurement condition...............................................................29
5.7.3. Setting the table conditions ...........................................................................31
5.7.4. Constructing the calibration curve.................................................................31
5.7.5. Measuring unknown samples........................................................................35
5.7.6. Termination....................................................................................................39
6.MAINTENANCE..............................................................................................................40
6.1. Inspection items ...................................................................................................40
6.1.1. Daily inspection.............................................................................................40
6.1.2. Annual inspection..........................................................................................41
6.2. Errors and warnings .............................................................................................42
6.3. Troubleshooting....................................................................................................48

MA-3000 Instruction Manual NIC-600-2231-14
6.3.1. Degradation of peak sensitivity......................................................................48
6.3.2. Outlying blank value......................................................................................49
6.4. Maintenance.........................................................................................................50
6.4.1. Leak check....................................................................................................50
6.4.2. Dismounting the sample heating tube...........................................................51
6.4.3. Mounting the sample heating tube ................................................................53
6.4.4. Installation of the boat handling poker...........................................................57
6.4.5. Removing the absorption cell........................................................................58
6.4.6. Cleaning the absorption cell and joints..........................................................60
6.4.7. Adjusting the sample changer.......................................................................61
6.4.8. Greasing the drive mechanism of the sample changer .................................65
6.4.9. Adjusting the optical system..........................................................................66
6.4.10. Adjusting the mass flow controller.................................................................67
6.4.11. Replacing the air pump tube (Option)............................................................68
7.MA3WIN..........................................................................................................................70
7.1. Basic screen.........................................................................................................70
7.1.1. Control screen...............................................................................................70
7.1.2. Analysis screen.............................................................................................71
7.1.3. Common controls..........................................................................................72
7.1.4. Table window.................................................................................................73
7.2. List of menu commands .......................................................................................77
7.2.1. File (f)............................................................................................................77
7.2.2. Edit (E)..........................................................................................................81
7.2.3. Run menu......................................................................................................83
7.2.4. Table (T) menu commands............................................................................99
7.2.5. System (S) ..................................................................................................103
7.2.6. Window (W).................................................................................................107
7.2.7. Help.............................................................................................................108
7.3. How to determine a calibration curve .................................................................109
7.3.1. 1Linear formula ...........................................................................................109
7.3.2. 3 Cubic formula...........................................................................................109
7.4. Calculation formula for mercury amount and concentration ............................... 111
7.5. Standard addition................................................................................................112
7.6. R.Blank Calculation method...............................................................................113
8.CONTACT.....................................................................................................................114

MA-3000 Instruction Manual NIC-600-2231-14
1
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
Danger
Indicates that incorrect handling could result immediately in death or
severe injury to the operator.
Warning
Indicates that incorrect handling could result in death or severe injury to
the operator.
Caution
Indicates that incorrect handling could result in moderate or minor injury to
the operator, or damage to property.
1.1.2. Installation precautions
Warning
Be sure to connect the protective grounding to prevent electric shock.
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.
Caution
Comply with the installation environment and power specification.
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.

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1.1.3. Handling precautions
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.
Caution
Do not disassemble or modify the product. This may cause a
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.
After washing the sample boat, first dry it at about 100C. Then, heat at a
high temperature to lower the blank. Heating a wet boat to high
temperatures can damage the sample boat.
1.1.4. Maintenance precautions
Warning
Maintenance of the heater must be carried out after the power has
been turned OFF and the heater has cooled down to close to normal
room temperature or it could result in burns.
Caution
Shut OFF the power supply before staring the maintenance work.
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.

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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.
MA-3000 System

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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.
Flow Diagram
Fan1
Fan3
Activated
carbon 1
Tray rack
Pressure regulator
Photoelectric
tube SIG1
Light absorption
cell SIG2
Light absorption cell 1
Light absorption
cell 2
Photoelectric
tube REF
Activated
carbon 2
Mercury
collecting tube
Lamp
Drain tank
Oxygen cylinder
Exhaust
Heating
vaporization
Exhaust
Air pump (P2)
Option unit
Silencer

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2.2. Part names and functions
2.2.1. Front
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
LED
“Green blinking”: Measurement in progress
“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.
④
⑤
②
③
①

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2.2.2. Inside front cover
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
rack
If there are any trays on the arm during an error
recovery, they are returned to this rack.
①
②
③
④
⑤
⑥
⑦
⑧

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2.2.3. Rear
No.
Name
Function

Pressure regulator
Adjusted to 0.05MPa, and connected to an oxygen
cylinder

Case fan
Exhausts heat

Activated charcoal for
exhaust gas
Used to remove mercury from exhaust gas

Activated charcoal for
carrier gas
Used to remove mercury from 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)
①
②
③
④
⑥
⑦
⑧
⑨
⑧
⑨
⑤
⑧
⑩
④
③
⑤
⑤
①

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2.2.4. Internal components seen from the top
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
board
Trimmer-less circuit

Pipe heater
Heats the connecting part to150˚C (Heater H4)

Mercury collecting
furnace
Heater H3 for heating the mercury collection tube,
Air-cooled by a fan from underneath.

Decomposing
furnace
Heaters for constant temperature control of
catalyst (H2A、H2B)

Sample heating
furnace
Used to heat sample boats (H1)

Case fan
Used to exhaust heat from the inside of the case

Infrared thermometer
for H1
Used to control the temperature of the sample
heating furnace
②
①
⑦
④
③
⑥
⑧
⑨
⑤

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2.2.5. Internal components seen from the right
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
rack
For cleaning purge air
①
②
③
⑤
⑥
⑦
⑧
⑨
④

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2.2.6. Internal components seen from the left
No.
Name
Function

Power switch
A safety circuit incorporated

Main circuit board
①


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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 : Windows 10 Pro, Window 8 Pro
(Internet Explorer 11 is necessary)
System control : Control of sample changer
Control of analysis conditions, Error indication
Data processing : Construction of calibration curve, Concentration
calculation, Statistical calculations

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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

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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.
RS-232C Cable
Power cable
Oxygen tube
Exhaust gas tube

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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.
(5) Once installation is complete, the "Installation
Complete" window will open. Click Close to close
the window.
The installation is completed

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4.3.2. 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.
Execute “USB60F_Setup.exe” located in “USB Driver (REX-USB60F VerXX)Windows10
Enterprise(Device guard)”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)