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4 Operation

4-12

Note

After recalibration analysis, check the intensity of the internal

standard element and also recalibration coefficients

α, β and k to

make sure that they have not changed considerably from the values

before recalibration.

Note

After recalibration, carry out check analysis using the sample for

checking (see page 4-14).

When master curve correction is used, carry out master curve

correction (see page 4-13) after recalibration and then carry out check

analysis using the sample for checking.

Содержание PDA-7000

Страница 1: ...re you use the product Keep this instruction manual for future reference Refer to the following document for detailed operation of software Data Processing Software PDA for Windows Operatioin Manual P...

Страница 2: ...This page is intentionally left blank...

Страница 3: ...alyses of multi elements in metal with a high precision The photoelectric photometric emission spectrometer which is adopted in a wide range of fields is an essential instrument for quality control Th...

Страница 4: ...ce and does not represent a commitment on the part of the vendor Any errors or omissions which may have occurred in this manual despite the utmost care taken in its production will be corrected as soo...

Страница 5: ...the following conventions Warning Indicates a potentially hazardous situation which if not avoided could result in serious injury or possibly death Caution Indicates a potentially hazardous situation...

Страница 6: ...Warning Labels Warning Electric Shock Before removing the excitation unit front panel be sure to turn OFF the power of the excitation source unit Never remove other panels Front Panel of Excitation Un...

Страница 7: ...ation Site Warning Do not operate PDA 7000 under explosive and or corrosive atmosphere Note When installing PDA 7000 near apparatus generating a ferromagnetic field such as an electric arc furnace con...

Страница 8: ...kers should be especially careful during discharge Caution Electric Shock Never start the discharge without correctly setting and holding the sample on the spark stand Caution Thoroughly read the inst...

Страница 9: ...ot disassemble or modify the instrument without permission as it may compromise the safety of the instrument Caution Use of the instrument is allowed only to personnel who have understood the safety p...

Страница 10: ...temperature and turn ON the AIRCON switch again If the buzzer gives a warning sound even after that turn OFF the AIRCON switch and contact your Shimadzu representative Safety measure for other emergen...

Страница 11: ...w for the safe use of high pressure gas Warning Install the gas cylinder in a well ventilated outdoor location that is not exposed to direct sunlight and convey the gas indoors via a pipe Regarding li...

Страница 12: ...Note Do not use the argon gas cylinder until it is empty Otherwise the inside of the cylinder will be contaminated For the exchange procedures of the cylinder refer to 5 13 Replacing argon gas cylinde...

Страница 13: ...warranty period 1 Improper product handling 2 Repairs or modifications performed by parties other than Shimadzu or Shimadzu designated companies 3 Product use in combination with hardware or software...

Страница 14: ...er such parts may cease to be available Note however that the availability of parts not manufactured by Shimadzu shall be determined by the relevant manufacturers If Shimadzu receives notice of the di...

Страница 15: ...xiii Disposal Precautions Dispose of this product using a qualified industrial waste management company in compliance with the applicable laws in the country where it is used...

Страница 16: ...rvice and Availability of Replacement Parts xii Disposal Precautions xiii Definition of Terminology xviii Parts List xix Checking of parts xix Consumables and maintenance parts xx Repair parts xxi How...

Страница 17: ...ment Daily use 3 3 3 3 Starting the instrument after it has not been used for a long time 3 4 3 4 Shutting down the instrument Daily use 3 5 3 5 Shutting down the instrument for a long time 3 6 3 6 Em...

Страница 18: ...ntrol gap 5 23 5 7 Replacing pump oil 5 26 5 8 Manual scanning 5 27 5 9 Lamp test 5 29 5 10 Waste discharge 5 30 5 11 File utility 5 31 1 Saving Backup 5 31 2 Loading Restoration 5 32 5 12 Replacing r...

Страница 19: ...xvii 7 Troubleshooting 7 2 7 1 Basic items to be checked 7 2 7 2 Troubleshooting 7 3 7 3 Installing the software 7 4...

Страница 20: ...instruction manual it means counter electrode unless specially noted Pre burn time Time set as non measurement time from discharge start until emission intensity is stabilized Integral time Measuremen...

Страница 21: ...Manual 1 pc 7 Standard accessories No P N Part name Q ty 1 211 74363 02 Gap gauge 4mm 1 pc 2 202 41917 Electrode extraction tool 1 pc 3 211 74362 Electrode D6 x 100 1 pc 4 036 11204 O ring 4D P6 10 pc...

Страница 22: ...239 07003 08 Molecular sieves 13 x 4 x 8M 1 year 1 bottle 15 017 30813 01 Silicon grease HIVAC G 1 can 1 5000 emissions is a typical value Electrode can be used until its length reduces to 65 mm in th...

Страница 23: ...gF2 Condenser lens MgF2 16 211 74649 91 Ignition coil assembly 17 211 50467 01 Control gap electrode 2mm 18 042 60424 23 Fan 4710PS 20T B30 B00 19 042 60934 13 Filter set 9450 M Filter set used for fa...

Страница 24: ...F Spectrometer exhaust line 46 018 31550 09 Super sun spring hose 1 7MT 1 There are two types of condenser lenses and which one to use depends on the specification of the instrument See below for more...

Страница 25: ...Chapter 1 Configuration and Function of the Instrument...

Страница 26: ...nd then measuring the intensity of the bright line spectra peculiar to those elements using the spectrometer The quantitative analysis for emission analysis is carried out by utilizing a proportional...

Страница 27: ...control system CONSOLE Read out unit power switch Supplies power to the read out and data processor system TEMP Temperature control display Displays temperature of the spectrometer system and set temp...

Страница 28: ...system this may cause deterioration of analysis precision The set temperature is 40 C Before turning off the main power be sure to turn off the SOURCE AIRCON and CONSOLE switches If the temperature of...

Страница 29: ...t consists of a spark stand which generates spark discharge between a metal sample and electrode and an excitation unit which controls high voltage for discharge Spark stand Condenser lens inside the...

Страница 30: ...switch prevents emission from being started by mistake at the time of maintenance and inspection of the spark stand Opening the spark stand door activates the safety circuit cutting off the emission...

Страница 31: ...ne could be aligned correctly on the exit slit 1 Condenser lens The condenser lens leads the light generated by the light source to the spectrometer At the same time it serves as a partition between t...

Страница 32: ...of 2Pa or less by the evacuation system Vacuum pump Power On switch Starts the vacuum pump Power Off switch Stops the vacuum pump Oil gauge Indicates the oil level Pump Leak Valve Used to prevent the...

Страница 33: ...into the current and measures it On an emission analysis the intensity of the light emitted from a sample generates large fluctuation at a short time Therefore the method of integrating the output cu...

Страница 34: ...trument 1 10 1 5 Data processor system Data processor system rear side CPU Cont UNIT Communications connectors Power cable for CPU Cont UNIT SCSI card SCSI cable Display cable Keyboard cable Mouse cab...

Страница 35: ...e to print switch to enable printing is OFF or there is no printing paper etc causes the print data to accumulate in the printer buffer resulting in abnormal printing when print operation is restarted...

Страница 36: ...1 Configuration and Function of the Instrument 1 12 This page is intentionally left blank...

Страница 37: ...Chapter 2 Specification...

Страница 38: ...er of photomultipliers 64 maximum 2 2 Excitation unit 1 Spark stand Gas type Argon gas Gas consumption During analysis Approximately 3L n 2 Standby 1L min Sleep 0 1L min 2 Excitatiion source unit Main...

Страница 39: ...4 Data processor system 1 Hardware Specifications required for the data processing PC CPU Core i3 3 00GHz or more Memory 2GB or more Storage devices HDD with 100MB or more free space CD R Drive x 1 Op...

Страница 40: ...can be shared Number of internal standard elements 2 maximum for each channel Recalibration 1point 2 points recalibration Working curve calculation 1st to 3rd order formulas Channel skip Number of sta...

Страница 41: ...play and print out orders Number of digits Display and print out items Ave R SD CV Display and print out layouts and fonts Result transmission Serial single host transmission Serial multi host transmi...

Страница 42: ...o CSV format Database support Microsoft Access Maintenance Instrument check Internal pressure of spectrometer Temperature of spectrometer Maintenance Management Spark stand cleaning Electrode change S...

Страница 43: ...Chapter 3 Starting and Stopping the Instrument...

Страница 44: ...he switch on the distribution board which supplies power to the instrument is ON Check that the grounding cable is correctly connected to the switch panel Check that the vacuum pump is working correct...

Страница 45: ...onfirm that the vacuum pump is operating 4 Check the water level in the argon gas bubbler See 4 1 Argon gas bubbler 5 Adjust the argon gas flow rate to 1L min using the BYPASS valve See 4 2 Checking g...

Страница 46: ...rate during analysis to 10L min See 4 2 Checking gas flow rate 7 Confirm that the pump leak valve is closed and then turn on the vacuum pump Note When the vacuum pump is OFF confirm that the vacuum st...

Страница 47: ...CE switch on the switch panel Keep the MAIN AIRCON and CONSOLE switches ON 2 Place an analysis sample for blank analysis on the sample plate of the spark stand and prevent air or debris from entering...

Страница 48: ...he pump leak valve slowly to allow the air into the suction hose to prevent the contamination of the hose by the pump oil After the sound of the air flowing into the hose disappears close the pump lea...

Страница 49: ...top and recovering Caution If any problem should occur on the instrument stop the instrument by emergency stop and immediately remove the cause of the problem 1 Emergency stop To stop the instrument i...

Страница 50: ...rgency stop 1 Turn OFF the AIRCON CONSOLE SOURCE and then MAIN switches on the switch panel 2 Turn on the MAIN switch on the switch panel and then turn on the AIRCON CONSOLE and SOURCE switches 3 Turn...

Страница 51: ...Chapter 4 Operation...

Страница 52: ...tion in the spark stand Keep the water level in the argon gas bubbler at 8 to 10cm Replace the water if it is heavily contaminated After adding or changing water in the argon gas bubbler recalibration...

Страница 53: ...Fine powder of evaporated samples iron aluminum copper etc is accumulated in the bubbler Evaporated samples accumulated in the vinyl hose that connects the spark stand and bubbler may cause analytical...

Страница 54: ...en the argon gas supply pressure which is set to 140kPa to 200kPa 1 4kg cm2 to 2 0kg cm2 changes the argon gas flow rate changes accordingly In this case set the flow rate to an appropriate value agai...

Страница 55: ...n source SW is turned off argon gas flow rate can be set to this flow rate The BYPASS valve can also be closed with the main cock of the argon gas cylinder open Return the argon gas flow rate during s...

Страница 56: ...FF the detector 1 Select Instrument Check on Maintenance menu Instrument Check window appears Screen 4 1 Instrument check 2 Check the photo detector status by the indicator in Photo Detector Voltage a...

Страница 57: ...of the belt sander and the dust collector filter and also replace the filter Dust accumulated in the dust collector may become a fire hazard There is a high risk of fire when aluminum or magnesium sa...

Страница 58: ...ished sample surface becomes poor which may result in argon gas leakage and unstable discharge Note When using a lathe for sample pretreatment follow the instructions below Regularly clean the lathe R...

Страница 59: ...tly hold the sample using the sample holder Tightly hold the sample over the hole of the sample plate with the sample holder Insufficient holding creates a clearance between the sample and the sample...

Страница 60: ...alytical group in the Group textbox or select it by pressing S4 Group key Screen 4 2 Content analysis 3 Set the sample on the spark stand and hold it by the sample holder 4 Start the discharge by pres...

Страница 61: ...hold it by the sample holder 5 Start the discharge by pressing 1 Start key or the start button on the spark stand 6 Take out the sample and change the position of the sample to be analyzed Then repea...

Страница 62: ...make sure that they have not changed considerably from the values before recalibration Note After recalibration carry out check analysis using the sample for checking see page 4 14 When master curve c...

Страница 63: ...combo box Screen 4 4 Master curve recalibration analysis 4 Set the sample on the spark stand and hold it by the sample holder 5 Start the discharge by pressing 1 Start key or the start button on the...

Страница 64: ...he menu bar 2 Input the name of the analytical group in the Group textbox or select it by pressing S4 Group key Screen 4 5 Content analysis 3 Set the sample on the spark stand and hold it by the sampl...

Страница 65: ...Chapter 5 Maintenance...

Страница 66: ...ing the spark stand Using manual brushing Every 3 000 discharges Electrode O ring Monthly 5 4 Exchanging the electrode O ring Condenser lens When MgF2 lens is used Every 10 000 discharges 5 5 Cleaning...

Страница 67: ...tion only when necessary 4 9 Master curve correction Check analysis using the Sample for checking 4 10 Check analysis 4 Maintenance service by Shimadzu service engineer Maintenance Item Cycle Referenc...

Страница 68: ...Spark stand maintenance O O O Exchanging electrode O ring O O O Cleaning the condenser lens O O O Control gap adjustment X O O Exchanging pump oil X O O Entrance slit adjustment O O O Lamp test X X X...

Страница 69: ...lysis gap distance and in turn fluctuates analytical values To prevent this and keep appropriate conditions for correct analysis perform maintenance service on the spark stand regularly Spark stand Cr...

Страница 70: ...ctrode opposite to automatically remove evaporant If the reverse discharge time is too short evaporant may not be removed completely On the contrary if the reverse discharge time is too long the tip o...

Страница 71: ...rode using the brush remove the evaporant from the entire circumference of the electrode Brush the electrode from the lower section blackish area to the top Although the maintenance cycle for recondit...

Страница 72: ...d 5L min to 10L min of argon gas Warning Electric Shock Never carry out maintenance operations on the spark stand unless the SOURCE switch on the switch panel is turned OFF 3 Press out the end of the...

Страница 73: ...used without removing the hose water in the gas bubbler may rise into the stand and thus could damage the instrument 7 Detach the dust cup remove evaporant under the cup using a vacuum cleaner and dr...

Страница 74: ...attach the vinyl hose Apply a small amount of grease on the outer surface of the exhaust pipe and insert the hose Note Improper or loose fitting of the exhaust outlet pipe and vinyl hose may result i...

Страница 75: ...the emission chamber following steps 1 through 9 Attaching or detaching the electrode when the emission chamber is dirty may damage the electrode O ring Oil has been applied to the electrode removal t...

Страница 76: ...til its bottom contacts the electrode holder Note Electrode tip contamination may cause analytical value fluctuations Handle the electrode with care Touching the tip with your hand may cause contamina...

Страница 77: ...s on the spectrometer side Note If the dust cup is mounted in the incorrect direction spectral light cannot go into the spectrometer inhibiting analysis 18 Apply a small amount of silicone grease to t...

Страница 78: ...s surface is scratched or damaged Reverse the top and bottom faces of the sample plate every time the stand is cleaned Be careful with the amount of silicone grease applied to the joint surfaces of th...

Страница 79: ...gap gauge to prevent rust generation Be sure to wipe the oil off before use 23 With the gap gauge placed on the spark stand tighten the adjusting bolt gradually until the tip of the electrode contacts...

Страница 80: ...ectrode position 26 Place an analytical sample on the spark stand and tighten the BYPASS needle valve to return the argon gas flow rate to the original BYPASS rate 27 Turn on the SOURCE switch on the...

Страница 81: ...ion below on Condition 2 tab No of emission 1 time Purge time 3 sec Discharge condition SEQ1 Cleaning SEQ2 Cleaning SEQ3 Cleaning cleaning Cleaning Discharge time SEQ1 9999 SEQ2 9999 SEQ3 9999 cleanin...

Страница 82: ...h 10 described in 5 3 Maintaining the spark stand 2 Detach the O ring using a toothpick or plastic screwdriver Do not use a metal screwdriver for watches because it may damage the sealing surface of t...

Страница 83: ...lts 1 Disconnect the vinyl hose for exhausting argon gas from the spark stand following step 3 described in 5 3 Maintaining the spark stand Caution Be sure to disconnect the vinyl hose prior to cleani...

Страница 84: ...rub the lens with gauze with toothpaste Then remove the toothpaste with gauze soaked in ethanol Caution Do not soak the lens in organic solvents such as benzene or paint thinner for a long time or pol...

Страница 85: ...d place it on the lens holder Note Be sure that silicone grease does not stick to the condenser lens since it is difficult to remove Be sure your hands are not dirty when cleaning the lens 10 Return t...

Страница 86: ...ithout the O ring 1A P34 It may break the vacuum inside the spectrometer and contaminated water in the spark stand or bubbler may enter the spectrometer As a result the optical units may be contaminat...

Страница 87: ...ribed below 1 Turn OFF the SOURCE switch on the switch panel for safety Warning Electric Shock Never carry out maintenance operations unless the SOURCE switch on the switch panel is turned OFF 2 Detac...

Страница 88: ...xcitation unit to remove the electrode Upper Part of Excitation Unit Control Gap The used electrode should be polished with sandpaper 240 or machined in a lathe It is also possible to use a special el...

Страница 89: ...astening screw How to Adjust Control Gap 6 Take off the gap gauge 7 Mount the front panel of the excitation unit 8 Turn ON the SOURCE switch on the switch panel Caution If the gap gauge is used upside...

Страница 90: ...il While doing this rotate the vacuum pump for a short time as described above to let the new oil go over entire inside of the pump Fill the new oil until the oil surface reaches within the red circle...

Страница 91: ...er 3 Start the discharge by pressing 1 Start or the start button on the spark stand The discharge begins and the intensity profile starts being displayed 4 Change the sensitivity value using arrow key...

Страница 92: ...below Removing backlash When turning the dial largely first turn it to a value 20 30 lower than the target value Then turn the dial clockwise slowly to adjust at the intended position Note For elemen...

Страница 93: ...f every element is equal to or less than 0 1 after the test 1 Select Maintenance Lamp Test on the menu bar Screen 5 2 Lamp Test 2 Start the measurement by pressing 1 Start or the start button on the s...

Страница 94: ...tart or the start button on the spark stand 4 After repeating the discharge specified times Content Analysis screen is displayed automatically Note Below are the recommended conditions for waste disch...

Страница 95: ...mation and data report files onto removable media regularly using File Maintenance window 1 Saving Backup The procedure of how to backup analysis information files is described here Data report files...

Страница 96: ...File Maintenance Restore is selected 2 Select Restore in the upper left area on the screen 3 Select the restoration target items in the lower left area Press 5 All if you would like to backup all the...

Страница 97: ...new recalibration sample are the same as those of the sample currently used carry out intensity reference value analysis for the recalibration on Int for target window The reference value is automati...

Страница 98: ...piping of cylinder No 1 to be replaced 2 Replace cylinder No 1 with a new one and open the valve of the pressure regulator 1 3 Open and close the purge valve 3 two or three times to release contamina...

Страница 99: ...is 5 40m set the secondary pressure to 500kPa 5kgf cm 2 and place a regulator inside analysis room to set the pressure at PDA 7000 gas inlet 140 200kPa 1 4 2 0kgf cm 2 as described with in the figure...

Страница 100: ...5 Maintenance 5 36 This page is intentionally left blank...

Страница 101: ...Chapter 6 Installation...

Страница 102: ...0 8cm sec 6 3 Dust PDA 7000 uses high voltages and tiny electrical currents Therefore dust can cause it to malfunction The installation site should be as free as possible of dust To prevent dust impl...

Страница 103: ...as inlet If the argon gas is provided from a gas cylinder a pressure regulator is needed Ex Ar gas regulator P N 200 33871 Secondary pressure 150kPa 1 5kgf cm2 Plumbing pipes for high purity gases sho...

Страница 104: ...Electrode grinder MT 11M P N 085 50802 01 AC100V type Grinding wheel CBN75 100 P N 085 50802 51 Electrode grinder for control gap electrode 2mm Ex Electrode grinder MT 10M P N 085 50801 01 AC100V type...

Страница 105: ...Chapter 7 Troubleshooting...

Страница 106: ...pectrometer reaches the sufficient level on Instrument Check screen Is the temperature of the spectrometer ok Check if the temperature display on the indicator on the switch panel stands within the ra...

Страница 107: ...is suspected that the room temperature is not normal or the fan which supplies the hot air has a problem Check that the room temperature is within 10 28 C and reset the AIRCON switch on the switch pa...

Страница 108: ...211 78114 Data Processing software PDA for Windows Installation Manual By the procedure above the data processing software will be recovered However at this point the analysis information and results...

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