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Instruction Manual: Thermal Vaporization Mercury Analyzer MA-3

Solo

NIC-TD-0000090-15

142

Nippon Instruments Corporation

11.

Appendix

11.1.

Flow in Measurement Path

Using the on/off control of the valves V1 through V3, three patterns of a flow in the

measurement path are used during a measurement.

The V1 is turned on, the V2 and V3 are turned off and ordinary air flows through the path

indicated with the red lines.

Water produced in the thermolysis of sample is removed by the drain bottle, and gas is

discharged through the purge line.

Heater H3

(Mercury Collector Tube

Heating Furnace)

Mercury

Collector Tube

Heater H2

(Catalyst Furnace)

Heater H1

(Sample Heating Furnace)

Heater H4

Detector

Absorption

Cell

Lamp

Detector

Drain Bottle

Humidifica-

tion Bottle

Needle Valve

Air Pump Flow Sensor

Activated

Carbon Filter

Activated Carbon Filter

Nafion Tube

Exhaust

Air

Filter Unit

Summary of Contents for MA-3 Solo

Page 1: ...Thermal Vaporization Mercury Analyzer MA 3 Solo Instruction Manual NIC TD 0000090 15 Nippon Instruments Corporation ...

Page 2: ... 7 2 3 2 Right Side 9 2 4 Inside of Instrument 10 2 4 1 Top 10 2 4 2 Front 11 3 Installation and Connection 12 3 1 Installation of Instrument 12 3 2 Installation and uninstallation of PC Software 13 3 2 1 Installation Procedure for MA3SoloWin 13 3 2 2 Installation of COM_Class MA3 Solo USB SERIAL Driver 15 3 2 3 Setup of Communication Port 15 3 2 4 Uninstallation Procedure 18 3 3 Upgrade of PC Sof...

Page 3: ... 5 6 Creation of Calibration Curve 38 4 5 6 1 Registration of Calibration Curve Table 38 4 5 6 2 Setting of Sample 39 4 5 6 3 Measurement Start 40 4 5 6 4 Suspension of Measurement 41 4 5 6 5 Termination of Measurement 41 4 5 6 6 Checking of Calibration Curve 42 4 5 7 Unknown Sample Measurement 43 4 5 7 1 Measuring of Sample 43 4 5 7 2 Registration of Unknown Samples 44 4 5 7 3 Setting of Sample 4...

Page 4: ...2 6 4 Reset Window Size 69 5 2 6 5 Manufacturer Setup 69 5 2 7 About 69 5 2 8 Exit 69 5 3 Self Check Screen 70 5 3 1 Constitution of Screen 70 5 3 2 Sequence 72 5 4 Measurement Screen 76 5 4 1 Input Output Screen 77 5 4 2 Ribbon Menu 80 5 4 2 1 START 80 5 4 2 2 STOP 80 5 4 2 3 NEXT 81 5 4 2 4 PURGE 81 5 4 2 5 Method 82 5 4 2 6 Measure Cond 84 5 4 2 7 Table Cond 87 5 4 2 8 HEIGHT AREA 90 5 4 2 9 DR...

Page 5: ... 6 Maintenance 103 6 1 Daily Inspection 103 6 2 Yearly Inspection 104 6 3 Recommended Replacement Components 105 6 4 Errors and Warnings 106 6 5 Troubleshooting 109 6 5 1 Fall of Sensitivity 109 6 5 2 Abnormal Blank Value 110 6 6 Maintenance Work 111 6 6 1 Leak Check 111 6 6 2 Procedure for Opening Top Cover 114 6 6 3 Removal of Sample Heating Tube and Mercury Collector Tube 115 6 6 4 Fixing of Sa...

Page 6: ...ght 136 7 1 6 Power Supply 137 7 1 7 Standard Accessories 137 7 2 Options 138 7 2 1 Mercury Collector Tube Measurement Kit 138 7 2 2 AQUA kit for MA 3 Solo 138 7 2 3 Sample boat Large sized Metal 138 7 2 4 Recommended Spare Parts 138 8 Installation Requirements 139 8 1 Installation Environment 139 8 2 Power Requirements 139 8 2 1 Instrument Main Unit 139 8 2 2 PC and Optional Printer 139 8 3 Measu...

Page 7: ......

Page 8: ...perty Danger Do not put any inflammable or combustible around the instrument Otherwise a fire may result 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 Caution Be sure to use the supplied power cable If another cable is used it may cause a failure Observe installation requir...

Page 9: ...e instrument Take care not to get burned When touching the instrument for maintenance make sure that it has been cooled sufficiently When touching put on protectors such as heat resistant gloves Otherwise you may get burned When the instrument is turned off the surface temperature can be high due to the heat from the heater Be cautious about burn injuries and do not place anything on the instrumen...

Page 10: ...ass component take care not to suffer an injury such as cutting a hand Use neutral detergent to clean the holder exclusively for the collector tube that is used for the measurement of the mercury collector tube and put on heat resistant gloves or the like when touching it so that oil does not stick to it Otherwise it will rust and deteriorate sooner Caution After the termination of a measurement b...

Page 11: ...grade the firmware first and then the PC software If the sequence is reverse installation may not be carried out normally Never turn off the PC or instrument during the update of the firmware Never disconnect the USB cable Otherwise a failure may result Caution If the instrument is discarded inadequately environmental pollution or personal damage may result ...

Page 12: ... an instrument that measures mercury quantities contained in liquid samples such as wastewater and crude oil and solid samples such as coal and soil rapidly with high sensitivity and with high precision By using an option the measurement of metal mercury in gas is also possible It has a simple instrument configuration and user friendly software design and is optimum as an entry level instrument fo...

Page 13: ...oncentration is carried out selectively for the mercury gas as gold amalgam After the completion of the sample heating decomposition sequence the mercury collector tube is heated mercury is separated again as metal mercury gas and is led to the detection unit absorption cell and the absorbance at 253 7 nm which is the first absorption wavelength band of mercury is measured Heater H3 Mercury Collec...

Page 14: ...Instruction Manual Thermal Vaporization Mercury Analyzer MA 3 Solo NIC TD 0000090 15 Nippon Instruments Corporation 7 2 3 External Appearance of Instrument 1 2 3 4 7 6 8 9 5 11 10 ...

Page 15: ...ch Houses an earth leakage breaker 8 AC inlet Used to connect the supplied power cable 9 Rear fan Equipped with a mesh cover 10 Exhaust port A tube with an outside diameter of 6 mm is used 11 Inlet Port to let in carrier gas Status Status of Status Display Lamp Description Offline Blinks at intervals of 1 sec The PC and instrument are not communicating Maintenance Blinks at intervals of 1 sec Any ...

Page 16: ...w rate can be adjusted by turning the knob 2 Humidification bottle When pure water is poured into the bottle the carrier gas is made to contain saturated steam 3 Drain bottle Effluent produced during a measurement is stored 4 Inlet knob When this is turned clockwise the inlet is closed 5 Inlet This is where a sample is loaded 6 Solenoid lock Locked during a measurement so that the inlet is not ope...

Page 17: ...ng a boat the inside of the system is sealed 2 Heater H1 Heats sample The fan has been installed in the lower part for cooling after a measurement 3 Heater H2 Heats an oxidation catalyst and an acid gas remover 4 Thermostat Turns off the power to heaters H1 and H2 when H2 overheats 5 Heater H3 Controls the temperature of the mercury collector tube The fan has been installed in the lower part for c...

Page 18: ...or 2 Activated carbon filter Activated carbon column to remove mercury in exhaust gas 3 Valves V1 and V2 Valves to switch the decomposition path and measurement path 4 Flow sensor Sensor for flow control 5 Nafion tube Removes steam in exhaust gas 6 Air Pump Sucks in carrier gas 7 Filter unit Filter for protection of Flow sensor 8 Valve V3 Switches ordinary gas and humidification gas 9 Activated ca...

Page 19: ...he instrument Be sure to avoid a room for using an organic chlorine solvent or a halogen reagent such as potassium iodide Also avoid a room into which the gas of the above mentioned reagent may flow Such substances become the cause of trouble such as the sensitivity fall of the instrument 1 Put the MA 3 Solo and PC in the installation position For installation requirements and an installation layo...

Page 20: ...ccording to the procedures described below If the OS language setting is not English United States please set to English United States For the operational procedures for Windows and the PC main unit and the setup procedures for peripheral devices such as the printer refer to the manual of each apparatus 1 Push the power button of the PC to start Windows 2 Insert the setup CD ROM into the optical d...

Page 21: ...ck Next 5 When the Confirm Installation screen is displayed click Next Installation starts When the user account control screen is displayed click Yes 6 When the installation is completed the Installation Complete screen appears Click Close to close the window The folder MANUAL MA 3Solo is automatically created on the desktop The instruction manual and simplified manual are saved inside the folder...

Page 22: ...tup CD ROM into the optical drive of the PC 3 Select COM_class MA3 Solo USB SERIAL Driver dpinst_xxx exe in the CD ROM xxx shows the number of bits of the PC 4 When the installation screen for the driver is displayed select Next 5 When the installation is completed the following screen appears Click Finish to close the screen The communication port of the MA 3 Solo is set The screen of Windows 10 ...

Page 23: ...rts Driver 3 Click the icon on the Desktop to start MA 3 Solo Win 4 Click in the upper left part of the screen and click System Setting in Setting 5 For COM Port MA 3 Solo select the same number as the one checked in Step 2 and click OK If it is impossible to select the communication port check the power supply for the MA 3 Solo and the connection of the USB cable and restart from Step 1 ...

Page 24: ...n the center of the screen communication with the MA 3 Solo has been established If not because ports may not be in agreement make sure again whether or not the number of the USB serial port in Step 2 is identical to that of the communication port in Step 5 Communication port setting of the balance To use the automatic sample weight entry function by the balance set the communication port of the b...

Page 25: ...r updating carry out uninstallation The uninstallation procedure of COM_Class MA3 Solo USB SERIAL Driver is also the same 1 Display the Control Panel and click Uninstall a program 2 Double click MA3SoloWin 3 When a confirmation screen for uninstallation is displayed click Yes 4 After that carry out uninstallation according to instructions When the user account control screen is displayed click Yes...

Page 26: ...e is reverse installation may not be carried out normally When it is necessary to upgrade the PC software or firmware carry out upgrading in the following procedure Caution Never turn off the PC or instrument during the update of the firmware Never disconnect the USB cable Otherwise a failure may result 1 Click the Maintenance tab in the upper left part of the MA3SoloWin screen 2 Click 3 Click Ope...

Page 27: ...ayed click the Start button If an error is displayed repeat Step 3 If the problem persists even after repeating several times consult with the agency or us 5 When the following screen is displayed upgrading has been completed If an error is displayed repeat Step 4 If the problem persists even after repeating several times consult with the agency or us ...

Page 28: ... gloves Otherwise you may get burned Disconnect the power cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result If the update of the firmware failed and the instrument does not start rewrite the firmware according to the following procedure 1 Turn off the instrument and disconnect the power cable from it It is unnecessary to...

Page 29: ...ts in the boot mode the LED on the right side of the board blinks at intervals of 0 5 sec 5 Carry out writing according to 3 3 1 Upgrading Procedure for Firmware described above When the writing is completed the following screen appears Click OK 6 Turn off the instrument again disconnect the power cable from it and then set the SW2 on the control board and the front cover as before Normal Mode Boo...

Page 30: ...ation 23 7 Supply power and turn on the instrument again When the following startup menu is displayed the procedure is completed normally 1 Uninstall MA3SoloWin according to 3 2 4 Uninstallation Procedure 2 Carry out upgrading according to the procedure from Step 3 in 3 2 1 Installation Procedure for MA3SoloWin ...

Page 31: ...tion of mercury collector tube Cooling of H1 MEAS PURGE 20 sec 7 Cooling of H1 H3 COOL Set using a measurement condition Turning On Power Input of Measurement Condition Thermolysis of Sample and Mercury Collection Purge of Measurement Path and Cooling End of Measurement Turning Off Power Next Sample Exists Sample Unloading Sample Preparation and Sample Loading Instrument Check Approx 30 Min Heater...

Page 32: ...cous liquid sample such as crude oil 2 Additive B Highly volatile liquid sample or sample containing organic mercury plentifully For the specific operational procedure for the additive B refer to 4 5 7 1 Measuring of Sample and 4 5 7 2 Registration of Unknown Samples 3 Activated carbon Sample containing mercury species with high volatility plentifully For the specific operational procedure for the...

Page 33: ...ore in a cool dark place 2 Standard Mercury Solution 10 mg L Take 1 mL of standard mercury solution for the atomic absorption 1000 ppm and add L cysteine solution 100 mg L to make a total of 100 mL 3 Standard Mercury Solution 0 1 mg L Add L cysteine solution 100 mg L to 1 mL of the solution prepared in Step 2 to make a total of 100 mL The L cysteine solution and the standard mercury solutions prep...

Page 34: ...ng to 1 or 2 described below When the blank process is completed leave the sample boat to cool and retain it in an airtight container 1 Measure an empty boat using the MA 3 Solo main unit repeatedly to make sure that the blank value has been stabilized 2 Put a boat in a heat resistant ceramic container such as a crucible and heat it at 750 C for three hours or so using an electric furnace If possi...

Page 35: ...e like soaked with a little ethanol 2 Put mercury collector tubes on a heat resistant ceramic pan or the like and heat them at 700 C for 30 minutes or more using an electric furnace Take care because quartz tubes may break easily because of devitrification if sodium calcium or the like adheres to them 3 When the temperature in the electric furnace has lowered and it is possible to take out the tub...

Page 36: ...his the additive B may be used It is also used to suppress rapid combustion or bumping or to prevent fusion The additive B adsorbs mercury in environment during manufacture and storage If the additive B is used without the blank process higher mercury values may be detected Therefore carry out the blank process before use For the blank process put the additive in a heat resistant ceramic container...

Page 37: ...that the connector marked IN becomes the upstream side 2 Set the pump flow rate to 0 5L min 3 Set the operation time of the pump to 2 minutes 4 Start the pump operation 5 While the pump is in operation inject the standard gas from MB 1 into the septum 6 Create the calibration curve by changing the amount of standard gas injection for each collector tube Activated carbon case T joint with the septu...

Page 38: ...g from Tedlar Bag 1 Connect the Tedlar bag filled with the sample gas shown as below 2 Flow through the sample gas from the tedlar bag to the collection tube for the appropriate time 4 4 5 3 Ambient Air Start the pump without connecting anything to the collector tube Operate the pump for the appropriate time Collector tube Tedlar bag ...

Page 39: ...ument which is very dangerous When cleaning the filter in the rear make sure that the instrument has been cooled sufficiently Otherwise you may get burned Caution The inlet is locked while the instrument is turned off Do not open the inlet while it is locked The inlet can be damaged 1 Make sure that the supplied power cable has been connected to an outlet with the ground and turn on the power swit...

Page 40: ...e following window is displayed in the center of the screen Click one of the displayed items When the ordinary measurement is to be made we recommend that the instrument check be made Type Description Instrument Check Makes the instrument check Heat Up Start Makes the temperatures of the heaters H1 to H4 rise Cooling Carries out the cooling of the instrument for maintenance 4 When Start Heating is...

Page 41: ...eater temperature Warning Take care that there is no dust on the filter of the fan in the rear If the filter is clogged it will cause the abnormal temperature rise of the instrument which is very dangerous When cleaning the filter of the fan in the rear make sure that the instrument has been cooled sufficiently Otherwise you may get burned Caution The inlet is locked during the self check Do not o...

Page 42: ...3 Solo 3 Enter the peak height of the absorbance used as the threshold for the blank check of the instrument and click START 4 Some items in the instrument check must be carried out manually Carry out the procedure according to the instructions on the screen 5 If there is dust on the filter of backside fan turn off the instrument after the cooling Then clean the filter by using a vacuum cleaner Do...

Page 43: ...n pour pure water into the humidification bottle After pouring pure water attach the bottle in the procedure reverse to that for the removal When closing the lid make sure that the packing has not been deformed If the packing has been deformed a leak may occur 8 Pull up the knob of the flow adjustment valve to disable the lock While looking at the screen turn the knob to adjust the flow rate to 0 ...

Page 44: ... the function in 5 4 2 4 PURGE in the later part of this document Click the Measurement tab in the upper left part of the screen and then click Set information for the measurement range blank check and cooling time For details refer to 5 4 2 6 Measure Cond in the later part of this document Click the Measurement or Analysis tab in the upper left part of the screen and click Set information for the...

Page 45: ...reen is clicked and then is clicked it is possible to create and check a sample heating method For sample heating methods seven types of STD SOLID HEAVY OIL AQUEOUS LIQUID COLLECTOR TUBE AQUA kit LIGHT OIL PLASTIC PURGE and TEST have been prepared beforehand For the selection of a heating method for each sample refer to 4 5 7 2 Registration of Unknown Samples in the later part of this document Whe...

Page 46: ...ime of the creation of a calibration curve Usually select the COLLECTOR TUBE method Temperature Enter the temperature of standard mercury gas aerated through a mercury collector tube Sample volume Enter the volume of standard mercury gas aerated through a mercury collector tube Remark Enter contents you want to write if any The standard value is the assumed mercury quantity to be measured and auto...

Page 47: ...e Measurement or Analysis tab in the upper left part of the screen and click in the upper left part of the screen to start a measurement When operation is carried out on the Analysis tab make sure that check marks have been placed for samples to be measured and then click The same operation can be done by pressing F5 key 2 In the case of the first measurement the following screen appears Set a fol...

Page 48: ...mination of Measurement Warning The area near the inlet is hot Put on protectors such as heat resistant gloves and take care not to get burned When handling a sample boat or a mercury collector tube for a measurement or the like take care not to get burned When handling put on protectors such as heat resistant gloves and use boat tongs 1 When a measurement is completed the following screen appears...

Page 49: ...n curve on the Analysis screen If a calibration curve is abnormal the color of characters will turn red and WARNING will appear In that case make sure whether or not there is any abnormality in the setup of standard values standard mercury solutions or the instrument There is an individual difference in the instrument sensitivity and there is some gap in the value set when the software is installe...

Page 50: ...acid to 5 wt or less Put sample on a sample boat In the case of liquid sample measure it using a micropipette or the like In the case of solid sample measure it using a balance Example Measuring of Sample Weight 1 Put a sample boat on a boat mount using boat tongs 2 Put the boat mount with the sample boat on a balance 3 Eliminate a tare 4 While taking care not to spill sample put it in the sample ...

Page 51: ...so that its height becomes the same as or higher than that of the liquid surface If it is necessary to prevent fusion put an additive up to such a level that the bottom surface is covered When you want to suppress sudden combustion and bumping make an additive soaked with sample uniformly and cover the sample with the additive 4 5 7 2 Registration of Unknown Samples 1 Click the Measurement tab in ...

Page 52: ...layed when Gas is selected for Sample Type and the normal conversion is carried out for CONC in the table condition Moisture Content Enter the moisture content of sample This is displayed when Solid is selected for Sample Type and ON is selected for Moist Correction in the table condition Standard Addition When conducting the standard addition and collection test enter the volume of mercury added ...

Page 53: ... it may be recovered by measuring water repeatedly By measuring 200 L or so of standard mercury solution repeatedly sensitivity recovery and sensitivity checking can be carried out simultaneously For other sample measurements consult with the agency or us Sample Type Method Upper limit Volume of Sample Remark Standard Solution 1 STD 200 L Biotic Sample Solid Sample Such As Fish Meat or Plant 2 SOL...

Page 54: ...ected for Sample Type in Table Conditions 1 Click Analysis tab on the upper left of the window and click SAMPLE button Then click the cell you want to enter the sample weight Click Input of S Vol button in the ribbon menu 2 The following window appears The measured data is entered in the cell you clicked when the output button of the balance is pressed If the following window does not appear check...

Page 55: ...ling put on protectors such as heat resistant gloves and use boat tongs Caution Use neutral detergent to clean the holder exclusively for the collector tube that is used for the measurement of the mercury collector tube and put on heat resistant gloves or the like when touching it so that oil does not stick to it Otherwise it will rust and deteriorate sooner Liquid Sample 1 Turn the inlet knob cou...

Page 56: ...ng of sample refer to 4 5 7 1 Measuring of Sample described above 4 Push the inlet knob to set the sample in the sample cracking furnace To close the inlet check if the markings on the inlet cover and inlet knob are aligned and turn the inlet knob clockwise while pushing lightly 5 The inlet cover is closed completely if the marking on the inlet cover aligns with the marking on the inlet knob ...

Page 57: ...t knob to take out the boad in out rod 2 Put an appropriate quantity of sample on the sample boat For the measuring of sample refer to 4 5 7 1 Measuring of Sample described above 3 Put the boat on the boat in out rod using boat tongs 4 Push the inlet knob to set the sample in the sample cracking furnace To close the inlet check if the markings on the inlet cover and inlet knob are aligned and turn...

Page 58: ...with the marking on the inlet knob Gas in the case of a mercury collector tube 1 Turn the inlet knob counterclockwise to align the markings on the inlet cover and inlet knob Then pull the inlet knob to take out the boad in out rod 2 Attach the dedicated collector tube holder option to the mercury collector tube to be measured 3 Put the mercury collector tube on the boat in out rod using boat tongs...

Page 59: ...sh the inlet knob to set the sample in the sample cracking furnace To close the inlet check if the markings on the inlet cover and inlet knob are aligned and turn the inlet knob clockwise while pushing lightly 5 The inlet cover is closed completely if the marking on the inlet cover aligns with the marking on the inlet knob ...

Page 60: ...due to its volatility Samples that contain volatile material e g naphtha gasoline jet fuel are analyzed using this procedure 1 Prepare boat filled 80 with Additive B 2 Take the sample with a gas tight syringe Permitted sample volume per analysis is up to 200uL depending on its Hg conc Samples should be well hand shaken or lightly ultrasonic before sampling 3 Insert the syringe needle to the bottom...

Page 61: ... to its volatility 1 Prepare boat filled 80 with Additive B 2 Take the sample with a gas tight syringe Permitted sample volume per analysis is up to 200uL depending on its Hg conc Samples should be well hand shaken or lightly ultrasonic before sampling 3 Insert the syringe needle to the bottom of the boat before injecting the sample into it 4 Put the sample boat on the boat in out rod using boat t...

Page 62: ...vated charcoal 2 Due to its non homogenity the sample should be collected with a Pastuer Piptte Dropper or with a micro pipette not syringe 3 Tare the boat filled with the Charcoal pellets in an analytical balance 4 Carefully drip and spread the sample over the Charcoal pellets Record the sample amount indicated on the balance Recommend maximum amount per analysis is up to 200mg depending on the M...

Page 63: ...ve mentioned process and reuse a boat discard a residue on a boat after a solid sample measurement and rinse a boat using pure water and then remove moisture after a liquid sample measurement However a residual sticking to a sample boat may affect a measurement 4 5 7 8 Checking of Measurement Result After the termination of a measurement check the measurement result on the Analysis screen and dete...

Page 64: ...pon Instruments Corporation 57 1 Click in the upper left part of the screen 2 Click on the printing menu 3 Place check marks for items to be printed and click the Print Preview button to check the printing contents Set the printing direction header footer etc using Page Setup Step 1 Step 2 ...

Page 65: ...les for each of a standard sample and an unknown sample The width of each column is interlocked with the setup on the table screen When the column width at the time of printing is narrow make an adjustment on the table screen When the column width is set to zero that column is not printed To reset the column widths to the default settings refer to 5 5 3 2 Width Reset in the later part of this docu...

Page 66: ...ating tube and keep it in a desiccator or the like so that it does not absorb moisture The inlet is locked while the instrument is turned off Do not open the inlet while it is locked The inlet can be damaged 1 Click in the upper right part to terminate MA 3SoloWin When you carry out maintenance work or move the instrument after the termination of a measurement lower the temperature of the instrume...

Page 67: ...the screen is clicked the main menu appears Input of S Vol Drift Refer to 5 3 Self Check Screen Method Measuring Cond Statistical Calculation Reset Column Width Log Display Numbers of Displayed Profiles Leak Check GLP Counter Adjustment of Optical System Parameters Hardware Test Open Log Files Cooling Update of Firmware Exit New Open Save As Template Print Settings About Self Check Measurement Ana...

Page 68: ...truction Manual Thermal Vaporization Mercury Analyzer MA 3 Solo NIC TD 0000090 15 Nippon Instruments Corporation 61 5 2 Main Menu When in the upper left part of the screen is clicked the main menu appears ...

Page 69: ...samples are cleared Use this when the calibration curve creation and unknown sample measurement are carried out in fixed procedures Clear SAMPLE measurement data Of the measurement values of unknown samples table items only on the right of absorbances are cleared Use this when a calibration curve is reused and the unknown sample measurement is carried out in a fixed procedure When a check mark is ...

Page 70: ...ered When the calibration curve creation and unknown sample measurement are routine measurements they can be carried out easily by using a template file because the table registration can be omitted 5 2 4 1 Open Template File Click and open a template file Select a file to be opened and click Open 5 2 4 2 Save as Template File Click and save a template file Enter a file name and click Save ...

Page 71: ... printed Method A sample heating method used is printed Instrument Check The result of the instrument check is printed Table The contents written for the table is printed Setup is possible for each of standard samples and unknown samples Profile A peak profile of an absorbance is printed Setup is possible for each of standard samples and unknown samples Statistics The result of the statistical cal...

Page 72: ...ing direction Margins Set a margin in each direction Header Footer Specify items to be entered in the header and footer Items that can be entered in the header and footer are as follows Item Description Blank Select this when no item is entered Custom Select this when arbitrary characters are entered When this is selected a character input field appears File Name Select this when a file name is wr...

Page 73: ...er MA 3 Solo NIC TD 0000090 15 66 Nippon Instruments Corporation 5 2 5 3 Print Preview Click or click the Print Preview button on the screen in 5 2 5 1 Print and check the printing contents and layout 5 2 6 1 System Setup Click and set the following items ...

Page 74: ...start the software Communication Port Select a communication port Select a port from the COM ports displayed on the dropdown list Date Format Select a date format from the following HH mm yyyy MM dd HH mm MM dd yyyy HH mm The date of a table is displayed in this format Sound file to plat at the end of measurement Select the sound file to play by the PC at the end of measurement Click Browse button...

Page 75: ...dual difference in the instrument sensitivity and there is some gap in the value set when the software is installed While referring to data at the time of the shipment inspection in the factory and measurement values at the time of the delivery and after maintenance set information Deviation for Judgment of Calibration Curve If the deviation of a backward calculation value from a setting value is ...

Page 76: ... a registered sample name select a name displayed in 2 using the mouse and press the Delete key 5 2 6 4 Reset Window Size This returns the external appearance size of the software to the default setting 5 2 6 5 Manufacturer Setup Our agency or we use this at the time of the adjustment and maintenance of the instrument before a shipment from the factory Since the important setup is included the inf...

Page 77: ...ys the usage counts and times of consumables and the result of each item of the instrument check Screen 2 Displays a heating profile of the heater H1 Screen 3 Displays an absorbance profile of the background measurement Screen 4 Displays the current temperature of each heater flow rate and constant temperature cap lamp and photodiode voltages Screen 5 Displays a peak profile of the blank measureme...

Page 78: ...ECK During humidification bottle check FLOW ADJ FLOW ADJUST During flow rate adjustment V1 V2 CHK V1V2 CLOSE CHECK During V1 and V2 closing check V1 CHK V1 OPEN CHECK During V1 opening check V2 CHK V2 OPEN CHECK During V2 opening check V3 CHK V3 OPEN CHECK During V3 opening check WAIT WAIT Waiting temperature rising until turning off of WARNING of all heaters ATOMIZE ATOMIZE During heating of heat...

Page 79: ...ank check of the instrument and click START The threshold for the blank check of the instrument can be seen by clicking on the ribbon menu Reference values of the peak heights of the absorbance and the quantities of mercury are as follows Reference Values of Peak Heights of Absorbances and Quantities of Mercury Low Range High Range Peak Height of Absorbance Mercury Quantity ng Peak Height of Absor...

Page 80: ...he items of the GLP counter are as follows When a threshold is exceeded carry out component replacement Item Threshold Measures Combustion Tube Usage 2 000 times Replace the sample heating tube Adsorbed Hg mg 1 500 mg Replace the activated carbon filter Lamp ON Time H 5 000 hours Replace the lamp In the case of the lamp replacement consult with the agency or us Air Pump Usage H 2 000 hours Replace...

Page 81: ...s 0 18 to 0 22 L min 10 sec after the start of the flow rate check The flow rate check starts after 10 sec The V1 may be clogged Replace the valve V1 V2 Open The flow rate is 0 18 to 0 22 L min 10 sec after the start of the flow rate check The flow rate check starts after 10 sec The V2 may be clogged Replace the valve V2 V3 Open Is the humidification bottle bubbling Make sure whether the inlet has...

Page 82: ...mal Vaporization Mercury Analyzer MA 3 Solo NIC TD 0000090 15 Nippon Instruments Corporation 75 To suspend the instrument check click 5 When all items are OK the instrument check is completed and the following screen appears ...

Page 83: ...nu Input Screen Used to enter information on an object of a measurement Status Display Screen Displays the measurement flowchart each heater temperature and flow rate H1 Temperature Profile Displays a temperature profile of the H1 The real temperature and preset temperature are displayed in red and blue respectively Measurement Profile Displays a peak profile of an absorbance It is possible to cha...

Page 84: ...ry solution to be used STD AMOUNT Set the standard amount Gas METHOD Select the sample heating method at the time of the creation of a calibration curve Usually select the COLLECTOR TUBE method STD TEMP Enter the temperature of standard mercury gas aerated through a mercury collector tube STD AMOUNT Enter the volume of standard mercury gas aerated through a mercury collector tube Common to Liquid ...

Page 85: ...ter the moisture content of sample This is displayed when Solid is selected for Sample Unit and ON is selected for Moist Correction in the table condition ADD STD AMOUNT When conducting the standard addition and collection test enter the volume of mercury added to sample This is displayed only when ON is set for Add STD in the table condition ABS When the absorbance measurement is completed the ab...

Page 86: ...t be subtracted When Travel Blank or Operation Blank is selected for NAME the same calculation as in the case of above mentioned R Blank is made When both Travel Blank and Operation Blank exist the larger mercury quantity is adopted No Sample Name Sample Vol Detected Value Concentration mL ng mg L 1 Sample1 100 0 050 0 500 2 Sample2 100 0 051 0 510 With no correction 3 Sample3 100 0 052 0 520 4 R ...

Page 87: ...art and it will be possible to enter a mercury quantity directly 5 4 2 1 START Click to start a measurement After a measurement starts the solenoid lock operates as safety measures and it is impossible to open the inlet until the completion of the measurement During a measurement the status display lamp blinks at intervals of 0 1 sec Also the following window will pop up The same operation can be ...

Page 88: ... measurement is made to lower the blank Click set the purge measurement and then click START and a measurement will start 1 Set a method used for the purge measurement 2 Set the number of purge measurements Type Description Repeated until ABS Falls Below the Set Value Repeated until the peak height of the absorbance is equal to or less than the setting value Repeat N times The purge measurement is...

Page 89: ...clear the data and then execute PURGE Reference values of the peak heights of the absorbance and the quantities of mercury are as follows Reference Values of Peak Heights of Absorbances and Quantities of Mercury Low Range High Range Peak Height of Absorbance Mercury Quantity ng Peak Height of Absorbance Mercury Quantity ng 0 0001 0 05 0 0001 0 5 0 0006 0 3 0 0002 1 0 0021 1 0 002 10 5 4 2 5 Method...

Page 90: ...xport to CSV file A registered method is output as a CSV file 6 Save A newly created method is saved 7 Reset The method registration condition at the time of a shipment is restored It is impossible to change any of the 8 types of methods registered at the time of a shipment Parameters for each Atomize are as follows Type Description Temp degC Enter a temperature for the heating control Up to 600 C...

Page 91: ...time 1 Measurement Range The range is switched to LOW or HIGH according to a measured mercury quantity The measurement range of the LOW range is 0 to 1000 ng linear range 0 to 100 ng and that of the HIGH range is 0 to 10000 ng linear range 0 to 1000 ng 2 STD Method Select the method for calibration curve measurement Each method can be changed from the input of Measurement screen or table of Analys...

Page 92: ...the peak height of the absorbance ABS is the setting value or higher the blank check starts Return Level ABS The purge measurement is made repeatedly until the peak height of the absorbance of the purge measurement becomes the setting value or lower Max Repeation Time Set the maximum number of repetitions of the purge measurement The range allowed is 1 to 10 Supplement In the thermal vaporization ...

Page 93: ...ety the boat in out rod is locked and it is impossible to unload the sample boat until the preset cooling time passes Although it is possible to unload the sample boat after the completion of a measurement the cooling of the H1 continues Even when the cooling time is long enough a sample boat after cooling is hot as shown below and you may get burned When you touch a sample boat take sufficient ca...

Page 94: ...able 1 Memo Enter the contents written at the time of printing such as the data title date etc Item Description Title Enter the title of data Instrument Type The name of the instrument used and serial No MA3Solo SN XXXX are automatically entered Date It is possible to enter the date of a measurement When this is not entered the date and time of the first measurement are automatically entered Opera...

Page 95: ...rrection Make an analysis with OFF chosen for the drift correction only when the instrument condition is checked 3 STD Type Select samples used when preparing a calibration curve When standard mercury solutions are used select Liquid When mercury collector tubes aerated with standard mercury gases are used select Gas Conc When a calibration curve is prepared using standard mercury solutions set th...

Page 96: ...e 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 the curve calculated using the least square method and passing through zero 0 and their corresponding cubic equations 3 Unknown Sample Set the table condition for an unknown sample 1 2 ...

Page 97: ... display It is possible to select 0 to 6 digits Treatment of Negative Values Choose whether a calculated concentration or mercury quantity that is negative is displayed as it is or set to zero Add STD Choose whether or not the column of the standard addition is displayed Moist Correction Choose whether or not the column of the moisture content is displayed Normalization Temp Set the reference temp...

Page 98: ... Nippon Instruments Corporation 91 Analysis Screen 5 4 2 9 DRIFT ON OFF To choose whether or not the drift correction of a peak profile of an absorbance is used click Low Mode Drift Correction Off Low Mode Drift Correction On High Mode Drift Correction Off High Mode Drift Correction On ...

Page 99: ...g with the PC ATOMIZE1 ATOMIZE1 Status of the first step of the sample heating ATOMIZE2 ATOMIZE2 Status of the second step of the sample heating ATOMIZE3 ATOMIZE3 Status of the third step of the sample heating PURGE PURGE During the purge of the measurement path MEASURE MEASURE Status of the absorbance measurement MEASPURGE MEASPURGE During the purge after a measurement COOLING COOLING Cooling sta...

Page 100: ...bon Menu Profile Displays a peak profile of the absorbance of each measurement It is possible to change the peak profile number to be displayed and the scale using the scroll bars in the lower part and the right side respectively Calibration Curve Screen It is possible to check a calibration curve Table Screen Measurement information on each sample is entered and output The contents of each item a...

Page 101: ... such as a specified sample name Paste Pastes copied or cut characters to a specified input cell for a sample name or the like Remove Removes a specified line Insert Inserts a blank line above a specified line Move A line can be moved only by dragging and dropping a specified line Save as text file Used to save measurement data in a CSV file To save data enter a file name and click 保存 Add data Use...

Page 102: ...specified for the adoption or rejection is displayed SD The standard deviation of measurements for which is specified for the adoption or rejection is displayed C V The CV of measurements for which is specified for the adoption or rejection is displayed Using the menu button in the upper left part of the screen objects of statistics detected values or concentrations and the number of displayed dig...

Page 103: ... the flow rate using the flow adjustment valve Flow rate can t be adjusted with the flow adjustment valve please refer to 6 6 1 Leak Check V1 V2 Close The flow rate becomes 0 05 L min or less within 20 sec from the start of the flow rate check The flow rate check starts after 10 sec Make sure whether or not the cap of the drain bottle has been closed V1 Open The flow rate is 0 18 to 0 22 L min 10 ...

Page 104: ...evant component is replaced click the Clear button to reset the counter This is used to adjust voltages of the optical system For the operational procedure refer to 6 6 9 Adjustment Procedure for Optical System in the later part of this document Operating Condition Replacement Criterion Date of Replacement Date of Clearing Current Reference Voltage Current Signal Voltage Current Values of Digital ...

Page 105: ...this function This is used to check the instrument status The valves solenoid lock fans lamp and air pump can be turned on or off by clicking a button in a blue frame Green On Gray Off These are for control by temperature designation for the heaters Enter a numerical value and set it using ENTER These are for control by duty designation for the heaters Enter a numerical value and set it using ENTE...

Page 106: ... work or to move the instrument Click START and the fan s will start to operate and the instrument cooling will be carried out until and the preset temperature is attained This is used to upgrade firmware For details refer to 3 3 1 Upgrading Procedure for Firmware described above It is possible to check the instrument log stored on the PC We use this for the analysis of measurements ...

Page 107: ...2 𝑏 𝐵𝑙𝑎𝑛𝑘 𝒚 𝒂𝒙 𝟎 𝑎 𝑥𝑦 𝑥2 𝑏 0 5 7 1 2 Cubic Formula y ax3 bx2 cx d 𝒚 𝒂𝒙𝟑 𝒃𝒙𝟐 𝒄𝒙 𝒅 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 𝑡𝑥3𝑦𝑝 𝑥3 𝑦 𝑢1 𝑡𝑥3𝑦𝑝 𝑛 𝑡𝑦1𝑝 𝑡𝑥3𝑝 𝑠1 𝑢1 𝑢9 𝑢3 𝑢6 𝑡𝑥2𝑦𝑝 𝑥2𝑦 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 𝑢6 𝑢8 𝑡𝑥6𝑝 𝑎 𝑥6 𝑢5 𝑡𝑥5𝑝 𝑛 𝑡𝑥3𝑝 𝑡𝑥2𝑝 𝑠5 𝑢7 𝑢9 𝑢8 𝑢8 𝑡𝑥5...

Page 108: ... 𝑠2 𝑡𝑥2𝑦𝑝 𝑡𝑥2𝑝 𝑡𝑥1𝑦𝑝 𝑡𝑥3𝑝 𝑡𝑥1𝑦𝑝 𝑥𝑦 𝑠3 𝑡𝑥6𝑝 𝑡𝑥2𝑝 𝑡𝑥4𝑝 𝑡𝑥4𝑝 𝑡𝑦1𝑝 𝑦 𝑠4 𝑡𝑥5𝑝 𝑡𝑥2𝑝 𝑡𝑥4𝑝 𝑡𝑥3𝑝 𝑡𝑥6𝑝 𝑎 𝑥6 𝑠5 𝑡𝑥3𝑝 𝑡𝑥2𝑝 𝑡𝑥1𝑝 𝑡𝑥4𝑝 𝑡𝑥5𝑝 𝑎 𝑥5 𝑠6 𝑡𝑥4𝑝 𝑡𝑥2𝑝 𝑡𝑥3𝑝 𝑡𝑥3𝑝 𝑡𝑥4𝑝 𝑎 𝑥4 𝑠7 𝑡𝑥2𝑝 𝑡𝑥2𝑝 𝑡𝑥1𝑝 𝑡𝑥3𝑝 𝑡𝑥3𝑝 𝑎 𝑥3 𝑡𝑥2𝑝 𝑏 𝑥2 𝑡𝑥1𝑝 𝑐 𝑥 𝒚 𝒂𝒙𝟑 𝒃𝒙𝟐 𝒄𝒙 𝟎 𝑎 𝑠1 𝑠5 𝑠2 𝑠4 𝑠3 𝑠5 𝑠4 𝑠4 𝑏 𝑠1 𝑎 𝑠3 𝑠4 𝑐 𝑡𝑥3𝑦𝑝 𝑎 𝑡𝑥6𝑝 𝑏 𝑡𝑥5𝑝 𝑡𝑥4𝑝 𝑑 0 𝑡𝑥3𝑦𝑝 𝑥3 𝑦 𝑠1 𝑡𝑥3𝑦𝑝 𝑡𝑥2𝑝 𝑡𝑥1𝑦𝑝 𝑡𝑥4𝑝 𝑡𝑥2𝑦𝑝 𝑥2 𝑦 𝑠2 𝑡𝑥2𝑦𝑝 𝑡𝑥2𝑝 𝑡𝑥1𝑦𝑝 𝑡𝑥3𝑝 𝑡𝑥1𝑦𝑝 𝑥𝑦 𝑠3 𝑡𝑥6𝑝 𝑡𝑥2𝑝 𝑡𝑥4𝑝 ...

Page 109: ...04 10 693 10 783 10 873 10 964 11 056 18 0 11 148 11 242 11 337 11 433 11 529 11 626 11 724 11 823 11 922 12 022 19 0 12 123 12 225 12 328 12 432 12 536 12 641 12 747 12 854 12 961 13 070 20 0 13 179 13 289 13 400 13 511 13 623 13 737 13 851 13 965 14 081 14 198 21 0 14 315 14 434 14 553 14 674 14 795 14 917 15 040 15 164 15 289 15 415 22 0 15 542 15 670 15 800 15 930 16 061 16 193 16 326 16 461 1...

Page 110: ...or it could move smoothly last time Refer to 6 6 6 Greasing of Inlet Checking at Time of Measurement Calibration curve The correlation coefficient r shall be 0 999 or more Refer to 6 5 1 Fall of Sensitivity Sensitivity The gradient of the calibration curve shall be within 30 of the value at the time of the delivery History A blank value immediately after the measurement of 100 ng or so shall be 2 ...

Page 111: ...be no dirt after cleaning Replacement Cell There shall be no inside dirt after cleaning Replacement or cleaning Valves V1 and V2 No foreign matter shall stick to the inside of the valve Replacement Boat In Out Rod There shall be no deterioration that poses a problem for supporting a boat after cleaning using alcohol Apply grease to the screw s Refer to 6 6 6 Greasing of Inlet Replacement Inlet The...

Page 112: ...fer to 4 4 3 Blank Process of Mercury Collector Tube Gas Measurement Option Activated Carbon Filter 1 year or 1 500 mg of adsorbed mercury Inlet O Ring 1 year or when a leak occurs When a method with a high temperature and a long time is used deterioration is hastened Boat In Out Rod O Ring 1 year or when a leak occurs Measurement Piping 1 year or when a measurement value is abnormal Air Pump 1 5 ...

Page 113: ...d it is impossible to start a measurement Remove the cause of the error restart the instrument and then start a measurement If the error status is not canceled even after measures are taken an electric failure may be the cause Consult with the agency or us Warning Message Message Contents and Measures Standby display of measurement screen STAND BY xx xx After turning on the instrument wait for 20 ...

Page 114: ...CONNEECT ERROR The thermocouple has broken 6 H2 THERMOCOUPLE CONNEECT ERROR The thermocouple has broken 7 H3 THERMOCOUPLE CONNEECT ERROR The thermocouple has broken 8 H4 THERMOCOUPLE CONNEECT ERROR The thermocouple has broken 9 H1 BROKEN The temperature of the H1 does not rise to the preset temperature 10 H3 BROKEN The temperature of the H3 does not rise to the preset temperature 11 H1 OVER HEATIN...

Page 115: ...D 0000090 15 108 Nippon Instruments Corporation An error message is displayed on the red screen as shown below The status display lamp blinks at intervals of 0 3 sec The number of blinks is the same as the error code number The interval to the next series of blinks is 3 sec ...

Page 116: ...lution Has sensitivity recovered Consult with the agency or us End Yes Replace the mercury collector tube and other tubes or clean the joints Is the sample boat normal Conduct a test using a new boat Clean the cell Replace the sample heating tube Yes No No Check the method Is the replacement of the mercury collector tube and other tubes or the cleaning of joints completed No Is there any leak Find...

Page 117: ...ge measurement without a sample boat Does the peak height decrease to 0 0001 or less after repeated blank measurements Consult with the agency or us Start End Has the sample heating tube been replaced Clean the inlet and boat in out rod Yes No No No No Is the boat mount clean Is the boat new Repeat the measurement using a new boat Is the blank high even when a measurement is made using the heating...

Page 118: ...rement and leak check Do not open the inlet while it is locked The inlet can be damaged When touching a glass component take care not to suffer an injury such as cutting a hand Take care not to forget to fasten the screws fixing the top cover Since the screws are not only safety measures but also measures against noise etc the measurement performance may be affected if they are not fastened The in...

Page 119: ...e valve V1 may be clogged If the flow rate adjustment is impossible even in that case there may be a clogging of the filter unit a leak from the flow sensor to the air pump to the flow adjustment valve or some component may be faulty 4 Make the V1 and V2 closing check Close the valves V1 and V2 operate the pump in the closed condition and make sure that the flow rate decreases When the flow rate d...

Page 120: ...When there is no abnormality in the path valve replacement is necessary 6 Make the V3 opening check Switch the valve V3 to the humidification path and check the bubbling visually If the bubbling is not carried out there may be a leak from the humidification bottle to the inlet to the sample heating tube to the mercury collector tube to the cell to the inlet of the valve V1 or V2 Check the path and...

Page 121: ...ct the power cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result Caution Take care not to forget to fasten the screws fixing the top cover Since the screws are not only safety measures but also measures against noise etc the measurement performance may be affected if they are not fastened The top cover is fixed using the t...

Page 122: ...locked while the instrument is turned off Do not open the inlet while it is locked The inlet can be damaged When touching a glass component take care not to suffer an injury such as cutting a hand 1 Loosen the nut of the reducing joint connected to the mercury collector tube and remove the reducing joint 2 Loosen the screw of the sample heating tube retainer and remove it 3 Turn the inlet knob cou...

Page 123: ...rews fixing the inlet cover and inlet and remove the inlet cover 7 Pull out the sample heating tube Pull out the sample heating tube and mercury collector tube to the front while turning them slowly 8 Loosen the cap nut of the Teflon joint and remove the joint 9 Remove the three screws of the inlet and remove the inlet from the sample heating tube Step 6 Remove the PharMed tube Step 6 Step 7 ...

Page 124: ... using the three screws Retighten the three screws alternately little by little and fasten the components to the extent that the O ring can be fixed Take care because it will be impossible to insert the sample heating tube after this step if they are fastened fully 3 Place the inlet on a desk and insert the sample heating tube from the top It can be inserted easily by pushing it in while twisting ...

Page 125: ...easier Because the screw thread of the Teflon joint is damaged easily make sure that it turns lightly and smoothly If the cap nut is engaged with the screw thread aslant it will cause a leak 7 Wipe the outside of the sample heating tube and mercury collector tube using alcohol 8 Insert the sample heating tube and mercury collector tube while turning them lightly right and left If they are pushed i...

Page 126: ... of the mercury collector tube Adjust the position using the insertion depth of the Teflon joint Fix the Teflon joint firmly 12 Connect the reducing joint to the mercury collector tube and tighten the nut Tighten the reducing joint lightly by hand and then retighten it using a wrench by 1 6 to 1 4 turn If the joint is tightened too strongly it may be damaged 13 Attach the sample heating tube retai...

Page 127: ...ainst the sample heating tube tighten the two fixing screws to fix the thermocouple 16 Fix the boat in out rod using the screw 17 With the solenoid lock to lock the boat in out rod pushed up turn the boat in out rod clockwise while pushing it in lightly 18 When the sample heating tube has been replaced with a new one clear Combustion Tube Usage of the GLP counter For details refer to 5 6 2 GLP Cou...

Page 128: ...ut rod 2 Pull out the boat in out rod 3 Remove the screw fixing the boat in out rod and remove it 4 Remove the two screws fixing the boat in out rod and replace or clean it 5 To clean it cut and remove the O ring soak the metal part in nitric acid of 1 w v or less and carry out ultrasonic cleaning or leave it for 30 minutes After the cleaning rinse it using pure water dry it sufficiently and then ...

Page 129: ...n the boat in out rod clockwise while pushing it in lightly If the inlet cannot be closed loosen the screw that fixes the boat in out rod a little and jiggle the inlet knob After jiggling tighten the screw and turn the inlet clockwise Make sure the inlet can be closed Step 8 With the solenoid lock pushed up manually turn the boat in out rod clockwise while pushing it in lightly Step 7 ...

Page 130: ...1 to 2 in 6 6 5 Replacement and Cleaning of Boat In Out Rod described above remove the boat in out rod 2 Remove grease from the following two thread parts yellow parts If the type of grease is changed make sure to wipe off the old grease Mixing different types of grease can interfere the performance 3 Apply grease to the thread part of the boat in out side yellow part above Use a toothpick or the ...

Page 131: ...ed by a short circuit may result Caution When touching a glass component take care not to suffer an injury such as cutting a hand 1 Disconnect the Tygon tubes connected to the absorption cell Loosen the nuts and disconnect the L joints 2 Loosen the two knurled screws and remove the cover of the absorption cell 3 Take out the absorption cell and loosen the screws fixing the cell windows using a coi...

Page 132: ...ell and joints in the following procedure Finally wash the components using pure water and then put them in a drier to dry them 2 3 4 5 6 1 Put the absorption cell and joints in a plastic or glass beaker Pour neutral detergent and clean the components using an ultrasonic cleaner or by keeping them in the detergent for 30 minutes or so Take out and wash the components one by one Pour 1 10 dilute ni...

Page 133: ...djustment of the optical system will be automatically made Warning When touching the instrument for maintenance make sure that it has been cooled sufficiently When touching put on protectors such as heat resistant gloves Otherwise you may get burned Disconnect the power cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result W...

Page 134: ...FE tube 2 mm dia 4 320 2 Tygon tube 1 8 inch dia 1 4 20 3 PTFE tube 2 mm dia 4 15 4 PTFE tube 1 mm dia 2 110 5 Tygon tube 1 8 inch dia 1 4 130 6 Tygon tube 1 8 inch dia 1 4 70 7 Tygon tube 1 8 inch dia 1 4 50 8 PharMed tube 1 16 inch dia 1 8 170 9 PharMed tube 1 16 inch dia 1 8 170 10 Nafion Tube 11 Tygon tube 1 8 inch dia 1 4 50 12 PTFE tube 2 mm dia 4 30 1 2 6 8 5 3 4 9 10 11 12 7 ...

Page 135: ...Instruction Manual Thermal Vaporization Mercury Analyzer MA 3 Solo NIC TD 0000090 15 128 Nippon Instruments Corporation Piping Diagram Top View 2 14 15 13 ２ 16 9 18 1 19 0 20 1 21 22 23 17 1 ...

Page 136: ... dia 1 4 50 14 Tygon tube 1 8 inch dia 1 4 20 15 Tygon tube 1 16 inch dia 3 16 20 16 PTFE tube 0 5 mm dia 2 100 17 Tygon tube 1 8 inch dia 1 4 250 18 Tygon tube 1 8 inch dia 1 4 90 19 PTFE tube 2 mm dia 4 30 20 PharMed tube 1 16 inch dia 1 8 200 15 21 PharMed tube 1 16 inch dia 1 8 50 22 PharMed tube 1 16 inch dia 1 8 200 20 23 PharMed tube 1 16 inch dia 1 8 110 14 ２ 15 ２ 18 20 ２ 22 ２ 21 13 ２ 16 ２...

Page 137: ...wer cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result If NG is displayed for the V1 and V2 opening check in the leak check and valve clogging is possible replace the relevant valve 1 Disconnect the connectors of the valves V1 and V2 2 Loosen the four screws and remove the retainer of the valves V1 and V2 3 Loosen the scr...

Page 138: ...Disconnect the power cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result If NG is displayed for the V3 opening check in the leak check and the valve V3 may be clogged replace it 1 Remove the connector of the valve V3 2 Loosen the screws of the plate fixing the PharMed tubes and remove the plate and PharMed tubes from the v...

Page 139: ...e power cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result 1 Remove the connector of the air pump 2 Remove the three screws of the air pump retainer 3 Loosen the four screws fixing the air pump and remove and replace the air pump 4 Attach the components in the procedure reverse to that for the removal 5 When the air pump ...

Page 140: ...ce the activated carbon filter 1 Disconnect the connector of the air pump 2 Disconnect the tubes connected to the activated carbon filter When the tube is pulled while pushing the one touch joint by hand the tube is pulled out 3 Loosen the two screws of the fixtures of the activated carbon filter and remove the activated carbon filter 4 Replace the activated carbon filter and then attach the compo...

Page 141: ... been cooled sufficiently When touching put on protectors such as heat resistant gloves Otherwise you may get burned Disconnect the power cable from the instrument before maintenance work Otherwise an electric shock or a failure caused by a short circuit may result 1 Disconnect the tubes connected to the flow adjustment valve 2 Remove the screw shown below and replace the flow adjustment valve ...

Page 142: ... Precision Limit of detection 0 01 ng Precision RSD 3 0 1 ng or more 3 Measurement Range 0 1000 ng 0 10000 ng 2 step switching of measurement range Linear Range 0 100 ng 4 0 1000 ng 4 Measurement Time 30 300 sec Flow Rate During Measurement 0 2 L min Exhaust Treatment Activated carbon filter for mercury removal Sample Heating Temperature Up to 850 C Heating Control 3 step setup It is possible to s...

Page 143: ...n Control Self check calibration curve judgment blank check recovery calculation Printing Memo calibration curve formula and graph measurement value table statistical calculation peak waveform measurement date and time instrument check result PC Notebook PC Printer Option Ink jet printer The specifications of the PC and printer varies depending on the date of delivery Make inquiries separately USB...

Page 144: ... analysis software MA3_SoloWin instruction manual and simplified instruction manual 1 Dedicated Ceramic Boat Ceramic boat volume 1 5 mL 10 Boat Mount for Measuring For measuring and transferring boat 3 Boat Tongs Stainless steel tool to pick up boat 1 L Cysteine Used as stabilizer for standard solution 1 O ring For boat in out rod spare part 1 Filter Unit Used as protection of flow meter spare par...

Page 145: ...as spare parts because measurement precision may lower depending on the quality of sample or operational procedure Item Description Sample Heating Tube Should be replaced after approximately 2 000 measurements or every year in the case of ordinary samples Mercury Collector Tube Should be replaced when sensitivity has lowered Piping and Joint Set Set of joints O rings and tubes replaced frequently ...

Page 146: ...ecomes high 8 2 Power Requirements Voltage Single phase 100 240 VAC 10 There shall be no abrupt voltage change We recommend connection to a separate outlet with the ground in order to use the instrument stably Frequency 50 60 Hz Rating 1 1 kVA Quality of Power Supply There shall be no surge harmonic noise or the like An outlet with the ground shall be used Voltage Frequency Single phase 100 VAC 10...

Page 147: ...on the right of the instrument Secure space of 150 mm or more in the rear for hot exhaust general exhaust from the rear upper part of the instrument and for an operation to turn on or off the instrument In order to connect to the ventilation connect the OUTLET of backside to the inlet of ventilation by 6mm outer diameter hardened tube like PTFE tubes The length of tube needs to be less than 3m Set...

Page 148: ...mistake or intentional act Consumable that has been consumed or component the life of which has expired 10 Cautions Concerning Disposal of Analyzer Caution If the instrument is discarded inadequately environmental pollution or personal damage may result When discarding this instrument do so appropriately according to the regulations laws etc of each area Some parts of this instrument have hazardou...

Page 149: ...turned off and ordinary air flows through the path indicated with the red lines Water produced in the thermolysis of sample is removed by the drain bottle and gas is discharged through the purge line Heater H3 Mercury Collector Tube Heating Furnace Mercury Collector Tube Heater H2 Catalyst Furnace Heater H1 Sample Heating Furnace Heater H4 Detector Absorption Cell Lamp Detector Drain Bottle Humidi...

Page 150: ...lines Water produced in the thermolysis of sample is removed by the drain bottle and gas is discharged through the purge line Heater H3 Mercury Collector Tube Heating Furnace Mercury Collector Tube Heater H1 Sample Heating Furnace Heater H4 Detector Lamp Detector Drain Bottle Humidifica tion Bottle Needle Valve Air Pump Flow Sensor Activated Carbon Filter Activated Carbon Filter Nafion Tube Exhaus...

Page 151: ...s passes through the absorption cell mercury in it is removed by the activated carbon filter and the gas is discharged from the exhaust port Heater H3 Mercury Collector Tube Heating Furnace Mercury Collector Tube Heater H2 Catalyst Furnace Heater H1 Sample Heating Furnace Heater H4 Detector Absorption Cell Lamp Detector Drain Bottle Humidifica tion Bottle Needle Valve Air Pump Flow Sensor Activate...

Page 152: ...o NIC TD 0000090 15 Nippon Instruments Corporation 145 12 Contact Nippon Instruments Corporation 14 8 Akaoji cho Takatsuki shi Osaka 569 1146 Japan Please contact the distributor or the following Technical Service E mail info nic rigaku co jp URL https www hg nic com ...

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