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Shimadzu ICPE-9000, Инструкция по эксплуатации

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5 Configuration and Operating Principle of the ICPE-9000 

 

5-15

(1)  Switching Observation Direction 

The observation direction is switched using the software. When igniting the plasma, perform the 

switching operation from the software's [Instrument Control] window and check that the observation 
direction has been switched properly. The mark shown below is displayed in the observation 
direction indicator. 

 Axial-view 

observation: 

z

 

 Radial-view 

observation: 

{

 

 

(2)  Switching Radial-View Observation Height 

The observation height is switched using the software. The measurement position is indicated by the 

observation height indicator. 

The observation height for radial-view observation (i.e., the position above the RF coil) is indicated 

by the observation height indicator. 

 

(3)  Changing Radial-View Observation Height 

The observation height is changed using the upper and lower observation position setting knobs. 
To adjust the upper observation position, loosen the locking knob with [Up] set in the software's 

[Instrument Control] window, and turn the upper observation position setting knob while viewing 
the observation height indicator scale. Tighten the locking knob when the position on the scale is 
aligned with the desired setting. 

To adjust the lower observation position, loosen the locking knob with [Down] set in the software's 

[Instrument Control] window, and turn the lower observation position setting knob while viewing 
the observation height indicator scale. Tighten the locking knob when the position on the scale is 
aligned with the desired setting. 

 

NOTE 

Tighten the locking knob securely after adjusting the observation position. If the 
locking knob is loose, the reproducibility of analytical values may be adversely 
affected. 

 
 

(4)  Attaching Entrance Window Cover 

 

NOTE 

Remove the cooling jacket when analyzing organic solvent samples or hydrofluoric 
acid samples. Otherwise, the cooling jacket may be damaged. 

 

Attach the entrance window cover (provided) when performing radial-view observation with the 

cooling jacket removed. 
 

Содержание ICPE-9000

Страница 1: ...the instruction manual thoroughly before you use the product Keep this instruction manual for future reference Shimadzu Multitype ICP Emission Spectrometer ICPE 9000 Hardware INSTRUCTION MANUAL 305 34...

Страница 2: ......

Страница 3: ...the next user If this manual or the warning labels on the product are lost or damaged promptly contact your Shimadzu representative To ensure safe operation be sure to read Safety Precautions before u...

Страница 4: ...ces wars riots and criminal activity 6 moving or transporting the product after its initial installation 7 items or parts that can be regarded as consumable e g parts for which the service life depend...

Страница 5: ...available for this product for a period of seven 7 years after its discontinuation Thereafter replacement parts may cease to be available Note however that the availability of parts not manufactured b...

Страница 6: ...iv...

Страница 7: ...ty In this manual precautionary information is indicated using the following conventions WARNING Indicates a potentially hazardous situation which if not avoided could result in death or serious injur...

Страница 8: ...near the product If solvent gets into your eyes or you come in contact with toxic solvent you must wash away the solvent immediately Provide a sink as near the product as possible CAUTION Consider the...

Страница 9: ...ons may not be attained Provide a power supply that complies with the power supply capacity required by the entire system Ground the product If the product is not grounded electric shock may occur whe...

Страница 10: ...Otherwise the sample may catch fire and cause a serious accident involving fire or explosions Wear protective glasses and gloves when handling solvents and samples If solvent gets into your eyes your...

Страница 11: ...th those of the type specified in this instruction manual Using a different type of fuse may result or fire Contact your Shimadzu representative to inquire about fuses not specified in this instructio...

Страница 12: ...Warning Labels on the Equipment in this instruction manual for details on the positions where the labels are attached See page Warning Label Positions The warning labels shown below are attached to t...

Страница 13: ...xi 3 Plasma Stand Door 037 72122 00 LABEL WARN SA40 122P Japanese 037 72125 00 LABEL WARN SA40 125P English...

Страница 14: ...xii 1 3 2 Warning Labels...

Страница 15: ...uipment is for industrial professional use only WEEE Mark Contact Shimadzu service representative when the equipment has reached the end of its life They will advise you regarding the equipment take b...

Страница 16: ...xiv...

Страница 17: ...e Processing With this product most samples generate waste that requires processing Be sure to process the waste properly 5 Ventilation This product uses argon gas and so if the installation location...

Страница 18: ...manual without consent 11 The contents of this manual are subject to change without prior notice 12 Contact your Shimadzu representative if you find any errors in this manual 13 Shimadzu accepts no re...

Страница 19: ...rol and fire defense Handling Precautions 1 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 liquef...

Страница 20: ...xviii...

Страница 21: ...ation BEC and Limit of Detection LOD 4 2 4 2 FUNDAMENTALS PRINCIPLES AND CHARACTERISTICS OF INDUCTIVELY COUPLED PLASMA 4 3 4 2 1 Definition of Plasma 4 3 4 2 2 Principles of ICP 4 3 4 2 3 Features of...

Страница 22: ...H AND ORIFICE ASSEMBLY 5 25 6 SPECIFICATIONS 6 1 6 1 PLASMA LIGHT SOURCE 6 1 6 2 RF POWER SUPPLY 6 1 6 3 SPECTROMETER 6 1 6 4 MEASURING UNIT 6 1 6 5 DATA PROCESSING UNIT SOFTWARE ICPESOLUTION 6 2 6 5...

Страница 23: ...7 8 3 2 Attaching the Leveler 8 10 8 3 3 Attaching the Nebulizer 8 11 8 3 4 Attaching the Nebulizer to the Chamber 8 11 8 3 5 Attaching the Chamber 8 12 8 4 REPLACING THE SAMPLE INTRODUCTION TUBE 8 13...

Страница 24: ...AND COOLANT PIPING 8 30 8 18 CLEANING THE FILTER FOR THE MAINS WATER SUPPLY CONNECTION KIT OPTION 8 30 9 MAINTENANCE PARTS AND CONSUMABLE ITEMS 9 1 9 1 MAINTENANCE PARTS LIST 9 1 9 2 CONSUMABLE ITEMS...

Страница 25: ...gs many advantages For example the simultaneous analysis of multiple elements reduces analysis time the use of a mini torch reduces running costs and axial view plasma observation increases sensitivit...

Страница 26: ...1 Introduction 1 2...

Страница 27: ...f torch 2 211 86533 EXTENSION PIPE L 1 Connects torch and chamber glass 2 046 00092 02 NEBULIZER AR30 1 FC1S 1 Nebulizer glass 2 046 00093 02 SPRAY CHAMBER 808 8881 1 Chamber glass 2 046 00093 01 DRAI...

Страница 28: ...G 2 For securing back of leveler exhaust tube 2 022 27045 BOLT SUS WITH HOLE M4X12 2 For securing CLAMP KCA 64 2 072 60342 04 CLAMP KCA 64 2 For securing leveler exhaust tube duct 2 016 31428 VINYL T...

Страница 29: ...400 mm min normally 600 mm min during maintenance Left side of equipment 200 mm min normally 600 mm min during maintenance 7 There must be no high capacity heat generating sources near the equipment 8...

Страница 30: ...he unit in a location subject to shocks or vibrations 5 Do not install the unit on a slope 3 2 2 Maintenance 1 If the main unit becomes dirty wipe it with a soft dry cloth If the dirt is particularly...

Страница 31: ...he frequency of the light is the energy difference can be expressed as follows E E2 E1 h h Planck s constant The frequency and the wavelength of the light satisfy the following relationship c c Speed...

Страница 32: ...rform thorough preparatory experiments 4 1 4 Self Absorption In general the light source used for the emission spectral analysis has temperature distribution higher in the center and lower in the peri...

Страница 33: ...d is generated The electric field accelerates electrons and ions and as a result of collisions between high speed electrons and argon atoms the argon atoms are ionized The rate at which electrons are...

Страница 34: ...temperature and a doughnut shaped hole where a sample is placed for a comparatively long time 4 Less self absorption and extremely wide dynamic range with the linear range of the calibration curve ex...

Страница 35: ...perpendicular d is the grating constant and is the wavelength then the following equation holds sin sin d n 1 n Order of diffraction Here n is the order of diffraction n 0 corresponds to the direct im...

Страница 36: ...ion by increasing the order of diffraction as shown in equation 5 in 4 3 1 Basic Equations for Diffraction Gratings and to improve the angular dispersion by increasing the diffraction angle i e reduci...

Страница 37: ...r Approximately one million 1 024 1 024 independent elements pixels with vertical and horizontal dimensions of a few tens of microns are arranged within an area of one square inch After accumulation t...

Страница 38: ...ough to excite the PA power amplifier 3 3 Power Amplifier This unit amplifies the power from the exciter to the output of kW order enough to ignite and maintain the ICP 4 Matching Box The power amplif...

Страница 39: ...e ICPE 9000 5 1 Block Diagram Peristaltic pump Autosampler Ultrasonic nebulizer Data processing unit Computer CPU for hardware control Controller Spectrometer temperature adjustment CCD detector RF po...

Страница 40: ...pectrometer case the echelle spectrometer is contained in a temperature controlled bath The controller incorporates the gas controller and the control power supply Controller RF power supply Plasma st...

Страница 41: ...the RF coil is provided from the same system Either mains water or a cooling water circulation system is used The coolant for the CCD is provided separately from a cooling water circulation system See...

Страница 42: ...r cable Ground cable Argon gas inlet Coolant outlet for RF coil and cooling jacket CCD coolant inlet CCD coolant outlet CCD coolant pumping signal connector Coolant inlet for RF coil and cooling jacke...

Страница 43: ...coolant pumping signal connector See Fig 5 4 Connect to CCD outlet Fig 5 5 Piping and Wiring for CCD Cooling water circulation system Option 5 4 Connecting the Data Processing Unit to the ICPE 9000 C...

Страница 44: ...th 79 grooves mm and a blaze angle of 63 4 Light that passes through the pinhole rectangular entrance slit is converted to parallel light by the collimator mirror parabolic mirror and is divided in a...

Страница 45: ...easured with the shutter closed This is also controlled with signals from the computer 5 8 Temperature Control The spectrometer is housed in a thermally insulated case The temperature of the spectrome...

Страница 46: ...er circulation system RF coil Outlet Cooling jacket Coolant circulation system option CCD Mains water Coolant circulation system 5 11 Argon Gas System The argon gas passes through an in line filter be...

Страница 47: ...ury There is a risk of burn injury When checking the plasma stand do NOT touch the plasma stand interior for 3 minutes after the plasma is extinguished Temperature stickers Fig 5 7 Plasma Light Source...

Страница 48: ...as depends on the nebulizer 5 Purge gas For the purge gas argon gas is circulated in the area between the light focusing lens and the plasma to prevent dirt from the plasma or the sample adhering to t...

Страница 49: ...uction System Argon Gas System and Cooling Jacket Plasma Stand Interior 10 RF Coil A 27 MHz RF current is applied to the RF coil the argon gas is heated and ionized by the induced current generated be...

Страница 50: ...ple in the leveler to the exhaust duct Sample Sample introduction tube Leveler drain tube leads to waste tank Condensation drain tube To condensation collector Condensation outlet Leveler exhaust tube...

Страница 51: ...um ultraviolet region the area between the plasma and the spectrometer septum is purged Light passes through the center of the orifice it is reflected off the back surface mirror it passes through the...

Страница 52: ...lation the points 9 and 15 mm for the optional plasma torch above the RF coil are set but these can be changed with the observation position setting knobs Setting range 7 to 22 mm Radial view observat...

Страница 53: ...the upper observation position loosen the locking knob with Up set in the software s Instrument Control window and turn the upper observation position setting knob while viewing the observation heigh...

Страница 54: ...16 Entrance window cover Entrance window cover locking screw Fig 5 12 Entrance Window Cover Back surface mirror inside cooling jacket Entrance window Spectrometer vacuum Fig 5 13 Cooling Jacket Optic...

Страница 55: ...ng Principle of the ICPE 9000 5 17 Reflective mirrors for radial view observation Entrance window Spectrometer Interior vacuum Fig 5 14 Optical System for Radial View Observation with Radial View Obse...

Страница 56: ...be for purge in radial direction 211 88158 91 CYLINDER 4KA1 ASSY 14 Cylinder drive valve for upper mirror 211 88158 92 CYLINDER 4KA1 ASSY 15 Cylinder drive valve for lower mirror 211 86128 91 TUBE ASS...

Страница 57: ...onfiguration and Operating Principle of the ICPE 9000 5 19 Consumable Items List P N Part name Notes 211 86218 91 PURGE PIPE ADHESIVE Quartz tube for purge in radial direction 211 84356 BONNET STD TOR...

Страница 58: ...signed specifically for use with plasma and improved for the use of digital control instead of analog control Matching box RF coil Phase detector RFG CONT PCB RF unit Fig 5 15 Names of RF Power Supply...

Страница 59: ...plasma stand If the plasma stand door is opened a safety circuit operates and interrupts RF output 3 Coolant Flow Switch Monitors the coolant If no coolant is flowing a safety circuit operates and int...

Страница 60: ...mperature is too low or if the humidity level of the installation location is too high condensation may occur on the internal radiator plate and possibly result in damage to the CCD If the humidity le...

Страница 61: ...nel The connector panel is used to connect to optional units PUMP Terminal used to connect to a peristaltic pump option ASC Terminal used to connect to the ASC 6100F autosampler option Connector panel...

Страница 62: ...3 Connect the autosampler s power cable to the extension cable 4 Turn ON the autosampler s power switch Refer to the instruction manual provided with the ASC 6100F autosampler for further details 5 1...

Страница 63: ...ched to the cooling jacket with the orifice assembly P N 211 43740 Cleaning of the orifice assembly P N 211 43740 is the same as for cleaning of the axial view observation orifice assembly L in sectio...

Страница 64: ...5 Configuration and Operating Principle of the ICPE 9000 5 26...

Страница 65: ...output 1 6 kW max 4 Output stability Within 0 3 5 RF circuit element Transistor 6 Control system CPU control 7 Ignition method Completely automated 8 Loading matching function Automatic matching suppo...

Страница 66: ...omatic printing of analysis results after measurement Batch printing analysis conditions calibration curves analysis results etc x Saving data Echelle mode all data saved Analysis wavelength save mode...

Страница 67: ...Flow rate 1 L min min CCD cooling water Temperature setting range 0 C to room temperature Temperature control precision 0 1 C Cooling capacity 200 W min Liquid temperature 10 C Pumping capacity maxim...

Страница 68: ...000 must satisfy the following specifications 1 CPU Intel Celeron D300 2 66 GHz min or equivalent 2 RAM 768 MB min 3 HDD 80 GB min 4 FDD 3 5 1 min 5 CD ROM 1 min 6 Display Resolution of 1 280 1 024 do...

Страница 69: ...er power switch 7 Perform the operations described below under 7 1 2 Starting the ICPE 9000 in Daily Use 7 1 2 Starting the ICPE 9000 in Daily Use 1 Supply coolant to the ICPE 9000 If mains water is u...

Страница 70: ...ur Shimadzu representative NOTE During vacuum pump operation exhaust from the exhaust outlet contains oil mist Use the following oil mist trap to trap this mist purchased separately P N 042 00125 25 O...

Страница 71: ...h is turned OFF the spectrometer temperature control circuit stops operating The time required for the spectrometer to stabilize varies with the external temperature but if it has been OFF for 24 hour...

Страница 72: ...rom above turn the valve counter clockwise 2 complete turns 2 After the air leak sound disappears close the leak valve Leak Valve Fig 7 1 Molecular Sieve Case NOTE Do NOT turn OFF the power switch bef...

Страница 73: ...supply of argon gas to the ICPE 9000 by closing the main valve of the argon gas supply Stop the supply of coolant to the ICPE 9000 NOTE If there is enough time stop the ICPE 9000 as described in 7 1 3...

Страница 74: ...7 Operation 7 6...

Страница 75: ...are is fragile Handle it with care 8 1 1 Replacing the Torch Replace the torch in the following cases If the torch melts periphery If samples adhere to the torch s center orifice If after analyzing hi...

Страница 76: ...ce significantly and sample suction may even stop In this case the nebulizer must be replaced or cleaned 8 1 3 Replacing the Chamber Replace the chamber in the following cases If a conspicuous amount...

Страница 77: ...is a risk of burn injury Do NOT touch the plasma stand interior for 3 minutes after the plasma is extinguished CAUTION Glass parts break easily and may cause injury if they are damaged Handle them wit...

Страница 78: ...emove the ball joint clip that connects the chamber and the extension pipe and remove the chamber Remove the ball joint clip that connects the extension pipe and the torch and remove the extension pip...

Страница 79: ...h the other hand pull and turn the carrier gas tube to remove it 4 Remove the sample introduction tube Hold the part connecting the nebulizer s sample introduction tube with one hand and with the othe...

Страница 80: ...rom the drain tube 8 2 4 Removing the Torch 1 Remove the torch from the torch mount Turn the torch clamp to loosen it and remove the torch If the chamber is set remove the chamber first 2 Remove the p...

Страница 81: ...t of the torch 2 Push the igniter cable through the hole shown in Fig 8 6 Igniter Cable Installation until there is no slack NOTE Check that the igniter cable is securely connected to the auxiliary ga...

Страница 82: ...sma torch Plasma gas tube ASSY Auxiliary gas tube 130mm Teflon ring Igniter cable 46mm Free orientation Fig 8 7 Attaching Gas Tubes Igniter Cable and Teflon Ring 4 Secure the torch to the torch mount...

Страница 83: ...pull the chain protruding from the torch position adjustment jig outside the plasma stand door NOTE Do NOT tighten the clamp with a driver or some other tool Tightening the clamp forcefully with a to...

Страница 84: ...drain tube into the bottom end of the leveler Secure the drain tube with the clamp 2 Attach the leveler to the chamber Insert the leveler into the bottom end of the chamber Attach the clip for TS 15 3...

Страница 85: ...tube insertion port Sample introduction tube insertion port Sample introduction tube Clamp Carrier gas tube 350mm Carrier gas inlet Fig 8 10 Attaching the Nebulizer Sample Introduction Tube and Carrie...

Страница 86: ...ction with the ball joint clip 2 Join the ball joint of the extension pipe and the chamber and secure the connection with the ball joint clip 3 Set the torch extension pipe and chamber so that they fo...

Страница 87: ...uction tube up to the end of the nebulizer s sample introduction tube insertion port Sample introduction tube insertion port Fig 8 13 Replacing the Sample Introduction Tube 8 5 Replacing the Drain Tub...

Страница 88: ...ere is no slack in the drain tube between the leveler and the tube hook 6 Secure the drain tube and the leveler exhaust tube with the tube holding block Ensure that there is no slack in the drain tube...

Страница 89: ...holding bands on the duct Ensure that the end of the leveler exhaust tube does not protrude above the top end of the plasma stand exhaust guide 6 Secure the leveler exhaust tube with the holding band...

Страница 90: ...urn Injury There is a risk of burn injury Do NOT touch the plasma stand interior for 3 minutes after the plasma is extinguished Set screws Do not touch these four screws Fig 8 16 Removing the Mirror H...

Страница 91: ...oved replace the mirror with a new one Loosen the leaf springs to replace the mirror Position the mirror so that the reflecting side is facing downward After cleaning or replacing the mirror insert th...

Страница 92: ...f cleaning will differ depending on the samples being analyzed and the period of use 1 Remove the orifice assembly L 1 Turn the orifice assembly L with a spanner 2 When the orifice assembly L becomes...

Страница 93: ...deterioration of the orifice assembly L surface In this case replace with a new orifice assembly L 8 9 Attaching and Removing the Cooling Jacket There is a possibility that the mirror inside the cool...

Страница 94: ...8 Maintenance 8 20 Remove the water cooled tubes Fig 8 21 Removing the Water Cooled Tubes Remove the argon gas purge tube Fig 8 22 Removing the Argon Gas Purge Tube...

Страница 95: ...ole and turn the jacket slightly in a clockwise direction until the lower positioning pin makes contact with the bottom of the cooling jacket Secure the cooling jacket in this position using the two a...

Страница 96: ...ometer side of the entrance window is maintained in a vacuum state Do NOT remove the entrance window NOTE Touching the glass part of the entrance window may cause the transmittance to decrease due to...

Страница 97: ...3 Purge tube screws 2 places Radial axis purge tube Fig 8 25 Cleaning the Entrance Window NOTE The area on the spectrometer side of the entrance window is maintained in a vacuum state Do NOT remove th...

Страница 98: ...ng procedure 1 Push the vacuum pump stop switch to stop the vacuum pump 2 Loosen the leak valve 4 to allow leakage 3 Remove the filter lid 3 and take out the absorbent container 2 4 Replace the absorb...

Страница 99: ...ing the pump for a short while The rotary pump weighs approx 16kg Do NOT perform maintenance work with an inappropriate posture 1 Remove the drain plug to let the oil out Collect the oil in a containe...

Страница 100: ...t be cleaned on a regular basis Clean the filters once every three months The cleaning methods are described below 8 15 1 Cleaning the Side Filter Filter Filter cover Fig 8 28 Cleaning the Side Filter...

Страница 101: ...ctrometer temperature control circuit stops operating The time required for the spectrometer to stabilize varies with the external temperature but if it has been OFF for 1 to 2 hours 6 hours is requir...

Страница 102: ...computer power supply and the power switch 2 Slide the filter restraining bar at the bottom of the right side of the ICPE 9000 to the left The bar is in the pouch at the bottom of the ICPE 9000 Hook a...

Страница 103: ...power interruption 8 16 Checking Operation of Safety Devices The operation of the safety devices used with the ICPE 9000 can be checked as described below Check the operation of the safety devices on...

Страница 104: ...t is opened while the main valve for the mains water supply is open mains water will spurt out Be sure to close the main valve for the mains water supply before performing maintenance work When the fi...

Страница 105: ...Open the main valve for the mains water supply 6 In the Instrument Control window set the Coolant Water Valve to OFF and click Apply 7 Check that there are no water leaks 8 Close the main valve for th...

Страница 106: ...8 Maintenance 8 32...

Страница 107: ...ory plasma stand Ar gas piping outside of main body and coil coolant 1 035 65503 HALF UNION C1N1 4XPT1 4 Accessory Ar gas piping outside of main body 206 52224 03 LABEL VOLTAGE 200V Accessory Sticker...

Страница 108: ...AS CONTROL ASSY Gas controller Gas controller with PCB 211 84516 91 PCB GASCON ASSY Gas controller Gas controller PCB 016 46027 12 POLYURETHANE TUBE TIUB05G X4 Gas controller For carrier gas 1 016 460...

Страница 109: ...FOR SLOW LEAK Gas controller Sensor and capillary for slow leak 211 86125 91 MAINTENANCE PART ECHELLE COIL Plasma stand RF coil 016 31425 TYGON TUBE 3 32X5 32 1M Plasma stand For protection of photoel...

Страница 110: ...system part Vacuum hose for 3MT need 1 037 61028 HOSE BAND WIRE 36 Vacuum system part For vacuum hose 211 86074 91 SLOW LEAK VALVE ASSY Vacuum system part Slow leak valve 036 10217 O RING 1A P16 Vacu...

Страница 111: ...l part 30A breaker power switch 074 80624 32 POWER SUPPLY EWS1500 48 Electrical part 48V 32A RF unit 074 80654 51 POWER SUPPLY VS50B 24 Electrical part 24V 2 5A Matching box 074 80654 77 POWER SUPPLY...

Страница 112: ...l part Connector ASSY for condensation sensor 211 88166 91 CABLE CCD POWER CCD power cable CCD peripheral part Power cable 078 29152 HEATER STF1002 Temperature control batch Heater at rear side of spe...

Страница 113: ...85118 91 PLASMA GAS TUBE ASSY 1 month Plasma stand plasma gas tube 200 30864 24 DRAIN TUBE TYGON T 7 16X1 16 3 months 2 Plasma stand 3 211 84352 91 ORIFICE ASSY L 1 month 2 Plasma stand 211 43740 ORIF...

Страница 114: ...9 Maintenance Parts and Consumable Items 9 8...

Страница 115: ...orch s center orifice changed x The reflective mirror inside the cooling jacket is dirty in axial view observation x The entrance window is dirty x Foreign matter adhered to the center of the orifice...

Страница 116: ...ty for elements is high even with a blank x The blank liquid is dirty x The torch is dirty x The chamber is dirty x The rinse time is short If the problem is not resolved by performing the appropriate...

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