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6. Maintenance

AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER – MERCURY/PE-1000

No.600-2111-09

6.2. Errors and warnings

This section describes errors and warnings displayed on the system.

(1) Warning message

STAND-BY xx:xx

Appears for 20 minutes after the power is turned on.

LAMP LIFE EXCEEDED

Appears when the time for which the LAMP has been on

exceeds 5,000 hours.

CARBON FILTER FULL!!

Appears when 1 g or more of mercury has been

absorbed in the activated carbon of the measurement

gas disposal section.

SEPTUM COUNT EXCEEDED!!

Appears when the number of times measurement has

taken place exceeds 1,000 – as the expiration of service

life of the septum.

SYRING LIFE EXCEEDED!!

Appears when the number of times the syringe has been

used exceeds 10,000.

This value is not This value is not guarantee of the products.

(2) Error message

A/D HOLT

Appears when the A/D converter of PE-1 has stopped.

LAMP BROKEN

Appears when the REF voltage falls to the specified

value or less.

COMMUNICATION ERROR

Appears when a communication error has occurred with

the PC or the sample changer.

HEATER H1 BROKEN

Appears during possible disconnection on H1.

HEATER H5 BROKEN

Appears during possible disconnection on H5.

HEATER RH BROKEN

Appears during possible disconnection on RH.

Ar GAS ERROR

Appears when the flow rate of argon is abnormal.

Air GAS ERROR

Appears when the flow rate of air is abnormal.

(3) Heater overheating protection

Each of the heaters H1, H2, H3, and H5 contains a thermostat in order to protect against

overheating. When it is tripped, the front switch automatically turns off. If it is tripped, wait a

while, and then turn on the power again.

Summary of Contents for Mercury/PE-1

Page 1: ...AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER Mercury PE 1 Mercury PE 1000 Instruction manual NIC 600 2111 09 Nippon Instruments Corporation...

Page 2: ...overview 2 Principles 3 2 1 Operation 3 2 2 Description of each component 4 PE 1 4 HT 300A Option 7 Specifications 8 3 1 Standard configuration 8 3 2 Individual unit specifications 8 Installing the eq...

Page 3: ...in Windows 27 Startup 28 Set of Syringe Cleaning Liquid 28 5 5 Measurement 29 Purge 29 Setting samples 29 Setting the method 30 Selecting Measure Range 30 Setting the number of injections 30 STD valu...

Page 4: ...operation of the syringe 55 6 6 Replacing the backup battery 59 PE1000Win software 60 7 1 BASIC screen description 60 CONTROL screen 60 ANALYSIS screen 61 Common indications 62 Table window 63 7 2 Men...

Page 5: ...Condition C 91 Statistics S 94 Register sample name N 94 7 7 Details of System menu S 95 Communication port setting 95 System Setup 95 Color arrangement setting 96 Confirming the current parameters o...

Page 6: ...Warning Ensure the ground wire is connected so as to prevent electric shocks Servicing precautions Warning Before servicing disconnect the power supply or electric shock may occur Caution Before servi...

Page 7: ...ig 1 the system consists of the mercury measuring equipment PE 1 an auto sample changer HT 300A and a personal computer hereafter referred to as the PC Once samples are set in the HT 300A each sample...

Page 8: ...entrated in the form of gold amalgam in the mercury collection section The mercury is released and atomized again through the Mercury collection section being heated and then detected using the atomic...

Page 9: ...TIC PETRO PYROLYSIS MERCURY ANALYZER MERCURY PE 1000 4 No 600 2111 09 2 2 Description of each component PE 1 3 4 9 5 2 1 6 8 7 10 11 12 13 14 15 16 17 18 Fig 5 Rear view of PE 1 Fig 4 Inside the PE 1...

Page 10: ...Fluorescence cell made of quartz 8 Mercury lamp Mercury lamp 9 Phototube For measuring the amount of the lamp intensity 10 Gas liquid separation bottle Separates any liquid from the combustion gas 11...

Page 11: ...ated carbon for absorbing measured mercury 2 Solenoid valve V5 Valve for switching the path Only turned on when using the RH PE 3 Photomultiplier For measuring the intensity of the fluorescence 4 Sole...

Page 12: ...e HT 300A No Name Function Remarks 1 Syringe Syringe for dispensing samples 100 uL 2 Washing bottle Bottle containing liquid for washing the syringe 3 Waste bottle Bottle for the waste liquid used to...

Page 13: ...ds liquids and gases requires the RH PE Dimensions and weight 505 W x 380 D x 510 H mm 40 kg Detection method Atomic fluorescence spectroscopy Detection limit 0 003 ng Measuring range 0 to 100 ng 2 Au...

Page 14: ...A minimum area of 1 000 mm wide x 800 mm deep is necessary Ensure a firm foundation without any wobble capable of bearing approximately 60 kg Others Avoid direct exposure to sunlight and air from air...

Page 15: ...ange in a short period Maximum relative humidity 80 Main supply voltage fluctuations up to 10 of the nominal voltage Transient over voltages typically present on the main supply NOTE The normal level...

Page 16: ...Connect the RS232C cross cable between the PE 1 and the PC 3 Connect the power cable and connect with a power supply 4 Connect an Argon gas line and an Air line Please use the tube of 6mm OD 5 Connec...

Page 17: ...CURY ANALYZER MERCURY PE 1000 12 No 600 2111 09 HT 300A 1 Open the front cover of PE 1 remove two screws and open a panel 2 Remove two screws of the cover of a left side and open a cover 3 Place a HT...

Page 18: ...tion of the drain Pump Pass through the hole the line Remove the grommet and pass through the cable of the Pump Connect the cable with the line connector of the PE 1 inside Draw the cable from the ups...

Page 19: ...the tube from the Pump side and house the vial in the holder Put the vials on right and left side and check the height When the bottle has floated please roll and put in a little seal ring tapes Conne...

Page 20: ...over and shut the front panel 7 Turn on PE 1 and adjust the syringe position of a sample changer Refer 6 5 3 Replacing the syringe and 6 5 4 Adjusting the sample injection position 8 One the adjustmen...

Page 21: ...ows Terminate any other application running on Windows 2 Insert the CD ROM The installer will automatically launch 3 When the Welcome to the PE 1000Win Setup Wizard screen appears click the Next butto...

Page 22: ...nimations may not be displayed correctly In this case open the Macromedia Flash Player7 folder on the CD ROM with Windows Explorer and run install_flash_player_7 msi to install Flash Player7 1 Right c...

Page 23: ...ware wizard will automatically start Select No and click NEXT 2 Insert the CD ROM supplied with the converter select Install from a list or specific location Advanced and then click NEXT 3 Select Sear...

Page 24: ...t driver will automatically follow Select No and click NEXT 7 Select Install from a list or specific location Advanced and click NEXT 8 Select Search for the best driver in these locations and check I...

Page 25: ...ion of device drivers on Windows XP is now complete Setting Communication port The RS232C port needs to be set to enable the USB Serial Converter Follow the steps below to set the port 1 Find the port...

Page 26: ...ort Setting window 4 Select the communication port checked in Step 1 and click OK to apply the setting 5 Close PE1000Win and restart it for the setting to take effect The port number changes depending...

Page 27: ...t Setup Control Panel to display the control panel 2 Click Add or Remove Programs 3 Select PE1000win on the Add or Remove Program screen and click Remove 4 Delete confirmation screen appears Click YES...

Page 28: ...Ar substitution 4 PURGE4 30 seconds 7 Measurement MEASURE 50 seconds in LOW mode 60 seconds in HIGH mode 9 Cooling COOL 30 seconds POWER ON Loop Soft ware PE1000win Mercury PE 1 Temperature rises in...

Page 29: ...about the high concentration please dilute or lessen the amount of samples 5 3 Measurement necessities 1 Distilled water 2 Standard solution e g 5 ppm 0 5 ppm 0 05 ppm 0 01 ppm 3 Micropipette 50 L to...

Page 30: ...eigh 67 7 mg of HgCl2 and dissolve it in a 0 001 L cysteine solution to bring the volume to 500 mL A mercury solution with a concentration of 100 ppm will then be the result 3 Extract 1 mL of 1000 ppm...

Page 31: ...essure regulators of the PE 1 back to 0 2Mpa Open the main cock of supply of argon gas and air gas 0 3 0 5KPa 1 Cancel the lock of a pressure regulator The knob of that to the down side 2 Pull the kno...

Page 32: ...No 600 2111 09 Discharge of Liquid in Gas liquid separation bottle Open the frame front cover of PE 1 Turn the rollerclamp downward for Discharging liquid And then shut it off Starting the software i...

Page 33: ...ilize Set of Syringe Cleaning Liquid Put the liquid for syringe washing into washing bottles and set them to HT 300A And throw away the liquid of the waste bottle Press a button in order to turn the t...

Page 34: ...als to the tray of HT 300A The Vial Number is expressed as two digits The sample tray is divided into blocks numbered 0 to 9 with each block having 11 positions i e 0 to 9 and P Any location can be us...

Page 35: ...be made by selecting Run Methods set from the menu Refer to 7 5 1Method setting Selecting Measure Range Set the heating speed of the mercury collection section for measurement in accordance with the w...

Page 36: ...button 3 Input STD concentration and volume Input Gas Temperature and Volume for RH mode Sample Name Click the cell of NAME and Input a sample name SVOL is inputted automatically when HT 300A is used...

Page 37: ...mence measurement select Run Start from the menu or click the icon When you do not use a sample changer inject a sample after pressing the START button Inject sample from the sample inlet port by a sp...

Page 38: ...ed The measurement results register in the Table window Example of standard sample measurement Example of unknown sample measurement Data analysis is described in the next chapter PE1WIN software Meas...

Page 39: ...ment result Click on an icon and change from a CONTROL screen to an ANALYSIS screen A calibration curve window is displayed in a STD Check the correlation coefficient inclination and the deviation of...

Page 40: ...osal Washing bottle Are no soil and cleaning liquid being contained Syringe No soil No crack Replace the syringe PE 1 Gas liquid separation bottle It does not overflow Drain Status Not OFF LINE Check...

Page 41: ...e has been used exceeds 10 000 This value is not This value is not guarantee of the products 2 Error message A D HOLT Appears when the A D converter of PE 1 has stopped LAMP BROKEN Appears when the RE...

Page 42: ...he leak and repair it Replace the relevant heater Re prepare STD START Is any carrier gas leaking Are the all heaters working Were the joints and the collector replaced Contact our service center Is s...

Page 43: ...nd heat treat the collector tube Is standard sample measurement reproducible Are the Vials clean and is the DW pure Did the collector tube and the joint rinse Replace the sample heating tube Replace t...

Page 44: ...ow chart H1 H2 Atomic Fluorescence Detector H3 Lump Collector tube RH PE OPTION Exhaust filter Flow meter HT 300A MASS FLOW CONTROLLER V4 V2 V7 V6 V3 V1 V5 Pressure regulator Exhaust NC NO COM COM NO...

Page 45: ...ed the flow rate is not just 0 06L min But use this reading as the reference indicator of evaluations below CHECK 2 Argon gas is flowing in the measurement line same as above H5 is heated to maximize...

Page 46: ...on 3 Loosen the nut of the joint connected to the sample injection section and disconnect the Teflon tube 4 Loosen the lower screw of the sample injection section and remove the sample injection secti...

Page 47: ...of the HT 300A to display the following title screen 2 Press the SET key while the title screen is being displayed 3 Press the key to move to Vial Syringe Setup And then press the key for going into...

Page 48: ...operation of a plunger NDL Up and down operation of a syringe TUR Right and left revolution operation of a tower TRY Rotation operation of a sample tray 6 Loose Closing screw and then open the cover o...

Page 49: ...so that the tip of a needle is not out from a needle guide 10 Press the EXIT key in order to escape from Syringe Install menu 11 Press the key to move to Touch Plunger Zero And then press the key for...

Page 50: ...le and the No 01 vial will then both also automatically adjust 16 Press the STOP key to terminate adjustment Adjustment of the injection position is made in the next section 17 Press the SET key to re...

Page 51: ...oves to the preset injection position 6 While using the and keys to adjust the horizontal position use the key to lower the syringe to the sample injection section 7 Press the ENTER key to determine t...

Page 52: ...12 Loosen the nut of the joint connected to the sample injection section and disconnect the Teflon tube 13 Loosen the lower screw of the sample injection section and remove the sample injection sectio...

Page 53: ...ensure to let it cool down for approximately 30 minutes after turning off the power as it is very dangerous to work on during use 2 Open the front cover of the measuring section 3 Remove the jacket he...

Page 54: ...he reducing T joint 8 Loosen the nut of the T joint on the right side of the collection tube and pull the collection tube out to the left If it is difficult to hold and pull the collection tube out be...

Page 55: ...he left and then remove it Removing the collection agent from the collection tube Using the supplied bar for installing and removing the collection agent remove the collection agent and the quartz woo...

Page 56: ...ransparent field of a cell with the swab which attached ethanol 6 Place a fluorescence cell so that the side on which the film is stuck becomes front side and the bottom and insert packing over left h...

Page 57: ...them with an ultrasonic cleaning apparatus or leave them for approximately 30 minutes Add a neutral detergent and wash them with an ultrasonic cleaning apparatus or leave them for approximately 30 mi...

Page 58: ...es after turning off the power as it is very dangerous to work on during use 2 Open the front cover of the measuring section 3 Remove the jacket heater 4 Loosen the joint connected to the sample injec...

Page 59: ...sulators 9 Loosen the screws that secure the H1 H2 and H3 thermocouples in place and remove the thermocouples from the heater wires 10 Pull the sample heating tube upward and replace it 11 Assemble th...

Page 60: ...y while the title screen is being displayed 3 Press the key to move to Manual Operations and press the key to select Manual Operations 4 Use and keys to select the relevant item and use the and keys t...

Page 61: ...SET key to display the following screen 2 Press the MET and ENT key at the same time 3 Select BORDERS MARK OUT 4 Remove the syringe from the HT 300A and set the waste bottle and the vials to No 48 50...

Page 62: ...ate of turret is using key and the locate of the table is using MET and SEQ key Please check at the front and sides respectively Down the needle and press ENTER key Run the task at the 50th vial in th...

Page 63: ...commended to replace the 400 hours in luck or about one year Please note that the deterioration of the tube can cause failure of the pump 1 Turn off the power supply of the device and disconnect the t...

Page 64: ...a microcomputer in the equipment with a lithium button cell battery being used as the backup storage media battery The lifespan of that battery is about 5 years To replace it turn off power to the eq...

Page 65: ...e two BASIC screens and common indications are described in this section CONTROL screen Sequence window Animatedly displays the measurement sequence READY shows the state of the current measurement se...

Page 66: ...ttom left of the window is the number of data displayed in one window which can be set to any number Calibration curve window Displays the current calibration curve A prepared calibration curve is dis...

Page 67: ...software and the name of the file being currently edited Menu bar Displays a menu for the various functions Tool bar Displays button icons for the various functions Status bar Indicates measurement se...

Page 68: ...table click the relevant tab at the bottom of the window Data cannot be moved or copied between the standard sample table and the unknown sample table Displayed items slightly vary depending on stand...

Page 69: ...jection The count of injection is set up In un inputting it is 1 time Meas Range Specify the sample measurement mode LOW HIGH LOW 0 10ng HIGH 0 100ng 1 Click Meas Range cell And then Click of the cell...

Page 70: ...most effective when gas is specified as the type of sample It means data on a collection tube that has been transported to the field for sampling gas but that has yet to be used When Travel Blank is s...

Page 71: ...e PEAK INTEG The measurement result is entered Each measurement result is registered in the LOW or HIGH cell and values in the measurement mode specified in the current tabulation settings are display...

Page 72: ...TIME Comments can be added as additional information Or measuring times are inputted automatically Select item at Store date time to Remark in the Setup menu If the sample type is specified as gas or...

Page 73: ...ls Print Preview V Displays a print preview using the current printing conditions Print P Prints measurement data EXIT Terminates the software Edit menu Copy Copies cell data and images to the clipboa...

Page 74: ...eak Check Performs a leak check Maintenance Executes maintenance Syringe wash Washes the syringe Suspend Heating Suspend for heaters and a lamp Table T Memo Set M Sets a memo for printing Table Condit...

Page 75: ...YZER MERCURY PE 1000 70 No 600 2111 09 Window W DisplayChange CTL Switches to the CONTROL screen DisplayChange ANA Switches to the ANALYSIS screen Screen Layout Initialization Resets the screen size t...

Page 76: ...be read by selecting File Open from the menu or clicking the icon To save data select PE1000 Data File or PE1000 Template File from the File type items When PE1000 Data File is selected The measureme...

Page 77: ...7 PE1000Win software AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER MERCURY PE 1000 72 No 600 2111 09 Page Setup U Sets print details Print Preview V Displays a print preview...

Page 78: ...profile window in 7 1 2 ANALYSIS screen are used as profile tabulation settings Memo Prints the Memo item set at Memo Set in Table menu Condition Prints the Method detail Calibration Prints the calib...

Page 79: ...standard sample table and the unknown sample table Copy Copies data in the selected cell to the clipboard when the Table window is active and copies images to the clipboard when the profile window and...

Page 80: ...a standard sample make the STD tab active before execution To save an unknown sample make the SMP tab active before execution Only the data with a circle in the X cell can be saved Save as Jpeg File S...

Page 81: ...ly changed Select the method number to be changed After changing it save the setting using the Save button at the upper right corner of the window If the method is measured even once the conditions of...

Page 82: ...size cannot be specified Post Wash2 Solvent Specify the place of the liquid that secondarily washes the syringe after injecting a sample Post wash2 count Specify the number of times to wash secondaril...

Page 83: ...dle into the septum Post injection dwell time s Specify the waiting time before removing the syringe needle from the septum and after injecting a sample Sampling time s Specify the sampling time follo...

Page 84: ...0 79 No 600 2111 09 WASH process Washing solution should be changed for water samples and oil samples isopropyl alcohol IPA is effective for switching water Oil Water Recommended example A Toluene C I...

Page 85: ...easurement Set it in accordance with the mercury weight A guide for that is as follows LOW 0 to 10 ng Low concentration The heater H5 of the mercury collection is heated at full power and mercury gas...

Page 86: ...ically measuring a standard sample when an unknown sample is measured The blank check function allows measurement after a high concentration is measured and then the blank is reduced Standard check To...

Page 87: ...ndard sample is to be measured and specify CHECK STD in the corresponding NAME cell Set the standard sample in the sample position specified as CHECK STD Setting is now complete In the above example t...

Page 88: ...nt Return Level Specify a concentration value for determining that blank reduction has completed Blank Sol Position Specify the number of the vial to be measured during blank measurement If you do not...

Page 89: ...fied as BLANK CHECK and BLANK respectively and then blank measurement starts The sample with the specified vial number is measured during blank measurement If you do not use any solutions use an empty...

Page 90: ...ts of standard solutions are found Refer 6 4 1 in details Maintenance Maintenance can be performed from the PC by selecting Run Maintenance from the menu Operation and the condition of each part of th...

Page 91: ...r with the needle penetrates though the septum Sample Injection Count Number of times that the syringe has been operated The figures in parentheses are threshold warning values with a warning being is...

Page 92: ...scence Ref V Voltage value converted from the intensity of light of the mercury lamp H1 C Current temperature of sample heating furnace H1 H2 C Current temperature of decomposing furnace H2 H5 C Curre...

Page 93: ...f the cooling fan for sample heating furnace H5 FAN RH Turns on off the PH PE cooling fan FLOW Specifies the flow rate H1 Controls the temperature of sample heating furnace H1 The left field is used t...

Page 94: ...7 PE1000Win software AUTOMATIC PETRO PYROLYSIS MERCURY ANALYZER MERCURY PE 1000 89 No 600 2111 09 Parameters This tab is used for adjustments made by the manufacturer...

Page 95: ...ATIC PETRO PYROLYSIS MERCURY ANALYZER MERCURY PE 1000 90 No 600 2111 09 Washing the syringe The syringe can be automatically washed Before pressing the START button be sure to check that the waste bot...

Page 96: ...asurement can be entered if necessary The other fields can also be freely used The memo is output when printing takes place but has no effect on tabulation settings Table Condition C To specify tabula...

Page 97: ...and cubic Each type of calibration curve formula is divided into three calibration curves a calibration curve b determined by the ordinary least squares method a calibration curve Blank intersecting...

Page 98: ...m3 ppt ppt ng Nm3 ppb ppb g Nm3 ppm ppm mg Nm3 ng kg g kg mg kg Decimal Places Specify the number of decimal places displayed for concentrations Drift Correction Select whether drift correction is ap...

Page 99: ...collected and calculated For unknown samples data with the same sample name are collected and calculated The results can be saved in a text file or copied to the clipboard Click Table Table Condition...

Page 100: ...p from the menu Receipt Holder for Measurement Data Specify the folder for storing measurement data Language Select Japanese or English for the language to be displayed on the screen Auto sample chang...

Page 101: ...11 09 Color arrangement setting Click System Color from the menu to specify the color arrangement if necessary Confirming the current parameters of the HT300 Click System HT300 Actual parameter from t...

Page 102: ...x x 2 b Blank y ax 0 a yx x 2 b 0 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...

Page 103: ...4p tx4p a x 4 s6 tx4p tx2p tx3p tx3p tx3p a x 3 s7 tx2p tx2p tx1p 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 Bla...

Page 104: ...ent Concentration of diluting solvent x Amount of sample x Ratio of diluting solvent x Specific gravity of mixed solution Ratio of diluting fluid Total Sample Total Mercury weight of diluting solution...

Page 105: ...ringe has been used exceeds 10 000 This value is not this value is not guarantee of the products 2 Error message A D HOLT Appears when the A D converter of PE 1 has stopped LAMP BROKEN Appears when th...

Page 106: ...Gas tight syringe 100uL ILS for HT 300A S1085 9200 00 Injection port septa S1085 0851 00 Condensate Bottle N 1085 9414 403 Mercury collector tube S1085 0820 00 Sample heating tube S1085 0810 00 Teflo...

Page 107: ...ll branch S1085 6102 11 AFS Detector Cell S1100 9901 00 20mL vial Waste bottle 10pcs set S1085 6104 11 10mL vial Rinse bottle 10pcs set S1085 6103 11 Septa for Rinse Waste Bottle 10pce set S1085 6106...

Page 108: ...i 569 1146 Japan Phone 81 72 693 6820 Fax 81 72 694 0663 Singapore Office 41 SCIENCE PARR ROAD 04 01A SINGAPORE SLENCE PARK SINGAPORE 117610 Phone 65 6873 7068 Fax 65 6873 6372 Osaka Sales Office 14 8...

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