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Endress+Hauser analytikjena PlasmaQuant 9100 Operating Manual Download Page 33

PlasmaQuant 9100 (Elite)

Installation and commissioning

33

4.3

Putting the ASPQ 3300 into operation

Connections

Figure 17ASPQ 3300 sampler

1 Sampler arm

2 Sampler head with cannula holder

3 Cannula

4 Rack for special samples

5 Rack for special samples

6 Base plate for racks

7 Sample racks

8 Purging vessel

9 Purging vessel pump

10 Controller for purging vessel pump

11 Power LED

12 Sample intake hose

Summary of Contents for analytikjena PlasmaQuant 9100

Page 1: ...Operating Manual PlasmaQuant 9100 Elite High Resolution Array ICP OES...

Page 2: ...se Stra e 1 07745 Jena Germany Phone 49 3641 77 7407 Fax 49 3641 77 9279 Email service analytik jena com General Information http www analytik jena com Documentation Number 13 5851 002 23 Edition 01 2...

Page 3: ...on cleaning and decontamination measures 12 2 5 Safety instructions for maintenance and repair 12 2 6 Behavior during emergencies 12 3 Function and design 13 3 1 Function and measuring principle 13 3...

Page 4: ...6 Checking the gas system for leaks 67 7 2 7 Replacing the argon hose 68 7 2 8 Changing the plasma compartment windows 68 7 2 9 Replacing fuses 71 7 2 10 Replacing the water filter 71 7 2 11 Replacin...

Page 5: ...c tions and their repair Conventions Instructions for actions which occur in chronological order are numbered and combined in action units Warnings are indicated by a warning triangle and a signal wor...

Page 6: ...yses listed in the user man ual Only this specified use is regarded as the intended use ensuring the safety of the user and the device This device is not suitable for solutions containing hydrofluoric...

Page 7: ...m bol Meaning Comment Warning of a haz ardous location At the exhaust vent Warning against optical radiation If no ex haust air hose is connected looking indirectly by mirror into the radia tion of th...

Page 8: ...afety and accident prevention regulations of the respective country the device is op erated in must be observed and adhered to The operator must ensure the latest ver sion of these regulations The use...

Page 9: ...l safety and may lead to limitations regarding the war ranty and access to customer service During operation free access to the connections the power switch and the man ual plasma deactivation switch...

Page 10: ...tances causing fatal injuries electrical shock and skin injuries Observe the following To ensure safe plasma torch torch operation the plasma must not be ignited unless the following conditions are me...

Page 11: ...of the compressed gas containers or system the device must be checked for proper operation prior to recommissioning Unauthorized assembly and installation are not permitted 2 4 8 Handling of samples...

Page 12: ...ed 2 5 Safety instructions for maintenance and repair The device is generally maintained by the customer service department of Analytik Jena AG or specialist personnel trained and authorized by them U...

Page 13: ...ay cham ber in which larger droplets are separated The exhaust heat of the plasma is dissipated partly by the recirculating chiller and partly by the exhaust unit 3 2 Design Essentially the optical em...

Page 14: ...plasma ignition period a high voltage spark is passed from the ignition spark generator to the discharge spring in the high frequency field in the torch The dis charge spring is located near the induc...

Page 15: ...torch has to be completely replaced when worn Figure 3 Demountable torch Figure 4 One piece torch A special design V Shuttle Torch is used in the emission spectrometer The upright po sitioning of the...

Page 16: ...optimized sample supply systems for special applications Sample supply system Application Standard Kit Standard applications Environmental sam ples foodstuffs pharmaceuticals HF Kit Digestions contai...

Page 17: ...ed plasma deactivation switch are located on the left hand side of the device Also on the left side under a cover plate there are the connec tions for PC and accessories as well as the media connectio...

Page 18: ...onnection via USB 2 PC for serial PC connection op tional 3 RS 232 service only 4 Autosampler for serial autosampler connection 12 V 5 Service 6 Chiller remote 7 Device fuses S1 S2 S3 The Chiller remo...

Page 19: ...optionally connected as an auxiliary gas Plug in connectors are used for the gas connections Hoses are pushed into the connec tor as far as possible and are thus securely fastened To release the conn...

Page 20: ...ent The type plate contains the following information Figure 10Type plate 1 Manufacturer address 2 Trade name 3 Electrical connection data 4 CE marking 5 WEEE device identification 6 Serial number 7 N...

Page 21: ...charge spring 4 Type plate 5 Photodetector for plasma monitoring 6 Induction coil with bonnet torch The serial number of the HF generator is located in the plasma compartment 1 2 3 4 5 6 7 8 9 10 Figu...

Page 22: ...0 ml 21 50 ml 24 30 ml 40 20 ml 60 14 ml 7 ml 7 ml The purging vessel is installed on the sampler The hose pump at the sampler pumps the purging liquid from the storage bottle into the purging vessel...

Page 23: ...ASXPress Plus oil accessory Both accessories for aqueous samples or oils shorten sample intake time and also the purging times Higher sample throughput can be achieved The accessories consist of a swi...

Page 24: ...responding accessory user man ual This user manual only describes the installation of a temperature controlled spray chamber argon humidifier and inline filter The operator is also instructed in coupl...

Page 25: ...sible altitude 2000 m Storage Temperature 40 C to 70 C Use dessicant 4 1 2 Power supply WARNING Danger due to electrical voltage Only connect the device to a properly grounded socket which complies wi...

Page 26: ...5 ppm 600 kPa 6 bar 13 to 21 l min Oxygen 4 5 as optional auxiliary gas 600 kPa 6 bar 0 04 l min 4 1 4 Exhaust unit The exhaust unit must be switched on during operation of the emission spectrometer W...

Page 27: ...the cooling water circuit Aside from the corrosion risk base metals can increase the conductivity of the cooling water When selecting the recirculating chiller make sure that no base metals are used i...

Page 28: ...resistant and must not absorb moisture Component Width x Height x Depth mm Mass kg On the workbench Basic device 990 mm x 940 mm x 855 mm 170 kg ASPQ 3300 sampler 285 mm x 510 mm x 490 mm 15 kg Teled...

Page 29: ...king and setting up the device The device will be delivered directly to the final device location by a transportation com pany The delivery by this company requires the presence of a person responsibl...

Page 30: ...le supply system The systems for sample supply the torch and the nebulizer with spray chamber and the sampler must be installed by the customer during maintenance CAUTION Risk of injury A risk of inju...

Page 31: ...induction coil The outer tube must be removed to adjust the ceramic torch HF kit Adjust the torch with the manual height adjustment 2 so that the outer edge of the inner tube is situated approx 1 2 m...

Page 32: ...terial from being pumped into the nebulizer system in case of faulty pump hose connection Notes on the pump hoses Different materials can be selected for the pump hoses depending on the sample The inn...

Page 33: ...nnections Figure 17ASPQ 3300 sampler 1 Sampler arm 2 Sampler head with cannula holder 3 Cannula 4 Rack for special samples 5 Rack for special samples 6 Base plate for racks 7 Sample racks 8 Purging ve...

Page 34: ...ed for the use of the sampler together with the basic device All other connections and displays are for service purposes or not in use Figure 19Purging vessel and pump on the sampler 1a Intake connect...

Page 35: ...s correctly mounted if it fails to move after light shaking Installing the purge vessel Insert the purging vessel into the rear left re cess and turn it clockwise by 90 Fit the racks for special sampl...

Page 36: ...lamping lever Insert the cannula into the holder on the sampler head Move the holder along the Z axis down and up and check whether the cannula fits through the guide at the lower end of the head Fast...

Page 37: ...cessories were ordered and supplied individually Details descriptions for installing the accessories can be found in the corresponding user manuals Connecting the sampler and the dilution system Conne...

Page 38: ...r and the emission spec trometer via the following hoses 1 2 3 4 5 6 7 8 Figure 22Hose connections on the dilution system 1 Diluent storage bottle connection 2 Syringe pump 3 Waste bottle connection 4...

Page 39: ...ing on the switching valve control unit 1 2 3 4 5 Figure 23Connecting the switching valve control unit Connections on the rear of the sampler 1 RS 232 interface COM 1 to the control unit Connections o...

Page 40: ...ice area Time Measure Software command Installation of the di lution system During syringe re placement Inserting the syringe in the syringe pump of the dilution system Move syringe plunger to positio...

Page 41: ...o not usually require changes during operation Loop Rinse Delay and Extra Loop Rinse Loop Evacuation Delay and Loop Load Time Equalization Delay Time To Evacuate Probe and Probe Wash Rinse Station Fil...

Page 42: ...er 5 Clamp the waste and sample pump hoses in the hose pump between two stoppers Note the pump direction for this see arrows Insert the sample hose in the sample or connect it to the sampler Insert th...

Page 43: ...accompanying datasheet Ensure that the membrane coil is not damaged Fill the glass vessel with the membrane coil 4 with deionized water up to the mark ing Connect the hose on the gas outlet of the arg...

Page 44: ...emble the inline filter as described in the accompanying datasheet To do so insert the nebulizer hose in the banjo bolt via a ferrule The conical side of the ferrule must point toward the banjo bolt S...

Page 45: ...e of the axial observation window for dirt and wear Check the cone for proper fit with the supplied C wrench NOTICE If the cone is loose it will not be cooled sufficiently and will corrode Close the d...

Page 46: ...toward the top If a ring plasma plasma only forms within the induction coil forms or a rattling noise is heard Press the red plasma deactivation switch on the left side of the device Check that the s...

Page 47: ...ng off the device via the plasma deactivation switch in an emergency Immediately switch off the plasma using the plasma deactivation switch on the left hand side of the device if one of the following...

Page 48: ...ample ID table Starting the measurement Start the measurement routine by clicking on or selecting the Routine Start sequence menu item In the Start sequence window select or enter a file name for the...

Page 49: ...e fault message 3762 Wavelength correction error 3765 No neon correction peak found 3766 Correction range exceeded 3782 No neon peaks found 3783 Too many neon peaks found 3783 No prim peak available C...

Page 50: ...nstable plasma due to the sample matrix Before ignition close the clamping brackets of the pump hoses insert the hoses in water purge the spray ing chamber with Ar via nebulizer gas Dilute the sample...

Page 51: ...ut down gas flow control error MFC 4015 Argon inlet pressure too low Cause Remedy No Ar gas flow present Open Ar gas cylinder Set Ar inlet pressure to 600 kPa 6 bar 4023 Ignition failed RF generator C...

Page 52: ...No Ar gas flow If the plasma is burning activate the CCD cooling option in the Spectrom eter window and click on Set 6 2 Device faults and analytical problems This section describes a number of devic...

Page 53: ...dies as the No signal fault screen Measured value too low Cause Remedy Incorrect calibration Check calibration solutions and re peat calibration Low solubility substances lead to low concentrations Lo...

Page 54: ...ault when using an internal stan dard Wrong standard dosage Insufficient reaction adjustment to plasma temperature change Matrix adjustment and better fit between the analytical line behavior and the...

Page 55: ...ture change in the spray chamber A change of 1 C causes a drift of ap prox 1 Use temperature controlled spray chamber or ensure air conditioning in the laboratory Insufficient transparency in the UV v...

Page 56: ...e power plug before performing maintenance work Power to the device is only disconnected by disconnecting the power plug After the device is switched off some parts are still live Only leave the devic...

Page 57: ...ter indicates a significant pressure loss If the plasma fails to ignite or is accompanied by loud noise Replace argon hose if hose is discolored Sample supply system Maintenance interval Maintenance t...

Page 58: ...all instructions and specifications in the safety data sheets for the basic ma terials CAUTION Risk of burns from the hot torch Plasma is extremely hot The torch is still very hot after the plasma has...

Page 59: ...motion CAUTION The quartz tubes are very fragile and are firmly mounted in the ground glass connector of the holder Wear protective gloves for working with glass when disassembling the torch Unscrew t...

Page 60: ...tube The injector tip must not protrude beyond the outer edge of the inner tube The tip can however be a maximum of 1 mm below the outer edge If the injector tip could not be properly aligned Remove...

Page 61: ...gs out of the holder Clean the holder of dust and deposits Insert a new glass body into the holder Align the glass body to ensure that the individual bore is visible centered in the front opening of t...

Page 62: ...NOTICE The gas connections are of different lengths and must not be confused Only screw in the gas connections until they are flush with the surface of the holder Otherwise the glass body can break wh...

Page 63: ...Risk of chemical burns from aqua regia Aqua regia is a 3 1 mixture of concentrated hydrochloric acid and nitric acid Aqua regia is highly corrosive and has an oxidizing effect Wear protective glasses...

Page 64: ...Wear glass han dling gloves to grip the torch safely When pulling out the torch ensure it does not become jammed Remove the quartz bonnet from the induction coil Place the glass components in aqua re...

Page 65: ...en O ring spacer ring green O ring flat retaining ring clamping screw The spacer ring must be turned so that one of the two bore holes in the ring is aligned with the small gas inlet opening see arrow...

Page 66: ...zer 2 Nebulizer holder 3 1st red O ring 4 Syringe WARNING Risk of methanol poisoning Methanol is poisonous if inhaled swallowed or on skin contact The liquid and its vapors are highly flammable Wear p...

Page 67: ...ove stubborn contamination Remove spots drops or larger reagent spillages and clean them using an absorbent ma terial such as cotton wool laboratory wipes or cellulose 7 2 6 Checking the gas system fo...

Page 68: ...sion has greatly deteriorated especially in the UV range Cleaning the windows does not usually completely restore UV transmission The cleaning effect varies depending on the wavelength Average losses...

Page 69: ...ate the quick purge of the optics in the via the ASpect PQ software in the Spectrometer window in the Parameters tab via the On button Purging prevents contamination of the spectrometer with laborator...

Page 70: ...cautions prevent the glass parts from becoming damaged dur ing installation of the cone Clean the cone with a damp cloth and dry it Unscrew the cone with the supplied hook wrench If the window is stuc...

Page 71: ...the fuse holder Reattach the cover Reattach the cover plate Switch on the device via the power switch Inform customer service if the fault repeats itself 7 2 10 Replacing the water filter The water fi...

Page 72: ...evice Carefully pull the sample hose from the hose guides on the automatic sampler Unscrew the cannula from the holder on the automatic sampler Remove the cannula with the sample hose and the connecti...

Page 73: ...the hose guides on the automatic sampler Unscrew the cannula from the holder on the automatic sampler Unscrew the banjo bolt on both the cannula and the sample hose from the connec tion piece Only use...

Page 74: ...nd pull them out of the purging vessel connections Pull the connection hoses for purging solution and waste from the pump hoses Connect the pump hose for the purging solution to the lower intake conne...

Page 75: ...e screw on the clamping lever so that the clamping brackets no longer press on the hoses Place the intake hose in purging solution Insert the waste hose in the waste bottle Switch on the basic device...

Page 76: ...Risk to health due to cooling water additives The biocide used is corrosive and can cause an allergic reaction on skin contact When handling the cooling water additive wear protective glasses clothing...

Page 77: ...ooling water return flow connection and hold the hose in the collection vessel bucket Switch the recirculating chiller back on and allow it to run until the flow of cooling water ends and only mist co...

Page 78: ...side of the device press the blue ring inwards and pull out the hose Unplug the interface cables of the electrical components sampler PC from the con nections on the connection panel on the left rear...

Page 79: ...tic conditions of the storage location can be found in the specifications 8 5 Recommissioning the device Unscrew the handles and keep them in a safe place Connect the exhaust hose to the smokestack of...

Page 80: ...chiller with the In con nection on the device Cooling water outlet flow connection on the recirculating chiller with the Out connection on the device Connect the recirculating chiller to power and swi...

Page 81: ...all solutions must be neutralized with an alkaline so lution such as a diluted sodium hydroxide solution The neutralized waste must be disposed of correctly in accordance with statutory regulations O...

Page 82: ...optic design on a compact cast baseplate for stability and durability Protection against moisture exhaust and chemical environ mental influences Detector Two dimensional FFT backside illuminated CCD w...

Page 83: ...tion 4500 VA Maximum current consump tion 32 A Fuse protection grid side 32 A Device fuses Fuse Type Protected circuit S1 10 A NFC 10x38 gG AC 400 V Spectrometer S2 6 A NFC 10x38 gG AC 400 V Tube heat...

Page 84: ...0 32 64 Bit Graphics resolution 1280 x 1024 1024 x 768 possible with restrictions Direct X 9 WDDM 2 0 Processor 1 6 GHz Dual Core CPU RAM 2 GB RAM 32 Bit 4 GB RAM 64 Bit Hard drive space 4 GB SSD reco...

Page 85: ...on the outlet side and p 40 kPa 10 1 4 ASPQ 3300 sampler technical data Dimensions W x H x D 285 mm x 510 mm x 490 mm Mass 15 kg Supply voltage frequency 100 to 240 V 50 60 Hz Fuse T 5 A H 250 V 5 x...

Page 86: ...and meets the requirements according to ISO 9022 2 ISO 9022 3 ISO 9022 32 03 0 EU directives The device meets the requirements of the directive 2011 65 EU The device is designed and tested in accorda...

Page 87: ...the sampler 34 Figure 19 Purging vessel and pump on the sampler 34 Figure 20 Connecting the sampler and the dilution system 37 Figure 21 Control PC connection via hub 38 Figure 22 Hose connections on...

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