Analytik Jena PlasmaQuant PQ 9000 Скачать руководство пользователя страница 70

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Fault removal

Edition 05/2014

PlasmaQuant PQ 9000

The measured value is too high
Cause

Remedy

−

Calibration

−

Check the calibration solutions

−

The peak position has slightly

shifted or measurement takes

place on a peak shoulder

−

The spectral interference was overlooked



use another

analysis line or activate an interference correction

−

Contamination/carry-over

−

Find and remedy the cause for contamination/carry-over

−

Concentrations appear higher

due to volatile substances

−

Optimize sample preparation

−

The analyte is an alkali metal (or

an easily excitable atomic line)

−

Alkali effect



optimize the plasma temperature (nebulizer

gas flow and/or performance) and plasma observation

−

When using an internal standard

−

The standard dosage is wrong

−

The adjustment of the response to changes in the plasma

temperature is inadequate



1. Adjust the matrix

2. Find a better adjustment between the behavior of the

analysis line and the internal standard

−

The warm-up phase is not

observed

−

Wait for the warm-up phase to complete before commencing

calibration

−

The sample foams when shaken

−

There are surface-active substances in the measurement

solutions



1. Optimize sample preparation

2. Also add the surface-active substances to the calibration

solutions

Precision is poor
Cause

Remedy

−

The pump fast mode was

activated up to shortly before the

measurement

−

Limit the fast mode to the time that is required to pass the

measurement solution up to the nebulizer

−

The prewash time is too short

−

Extend the prewash time

−

The nebulizer or injector is

clogged

If necessary, check with Na solution (1 g/L) – if no plasma coloring

(orange) is observed:

−

Check the nebulizer nozzles for obstructions and clean them

(see "Cleaning the nebulizer" p. 50)

−

If the sample nozzle is clogged



filter the solutions

−

If the argon nozzle is clogged



dilute the measurement

solutions or use an argon humidifier

−

The nebulizer gas flow is not

optimal

−

Optimize the nebulizer gas flow

−

There are leaks in the argon

supply

−

Seal the leaks

Содержание PlasmaQuant PQ 9000

Страница 1: ...PlasmaQuant PQ 9000 High Resolution Array ICP OES Operating manual...

Страница 2: ...AG on the internet http www analytik jena de Copyrights and trademarks PlasmaQuant is a registered trademark of Analytik Jena AG Microsoft Windows 7 MS Excel are registered trademarks of Microsoft Cor...

Страница 3: ...mas 13 2 6 6 Safety instructions relating to the formation of ozone and toxic vapors 13 2 6 7 Safety instructions relating to compressed gas containers and systems 13 2 6 8 Handling of samples auxilia...

Страница 4: ...a deactivation switch in the event of faults 42 7 4 Starting a measurement routine 42 8 Maintenance and care 44 8 1 Maintenance intervals 45 8 2 Base device maintenance 46 8 2 1 Cleaning the demountab...

Страница 5: ...Equipment faults and analytical problems 66 10 Transport and storage 70 10 1 Preparing the PlasmaQuant PQ 9000 for transport 70 10 2 Ambient conditions for transport and storage 71 10 3 Recommissioni...

Страница 6: ...11 Connections for cooling water and gases 31 Figure 12 Plug in connectors for gas connections 31 Figure 13 Ventilation openings and air filter on the rear of the PlasmaQuant PQ 9000 32 Figure 14 Data...

Страница 7: ...t PQ 9000 Edition 05 2014 5 Summaries Summary 1 Environmental conditions for operation 20 Summary 2 Power supply 21 Summary 3 Gas supply 21 Summary 4 Exhaust unit requirements 22 Summary 5 Cooling cir...

Страница 8: ...Summaries 6 Edition 05 2014 PlasmaQuant PQ 9000...

Страница 9: ...Safety notes The elements of the control and analysis program are indicated as follows Program terms are identified with SMALL CAPS e g Menu FILE Buttons are shown by square brackets e g OK button Men...

Страница 10: ...y Warranty and liability claims are excluded for personal injury and property damage if resulting from one or several of the following causes use of the PlasmaQuant PQ 9000 other than intended imprope...

Страница 11: ...2 2 Symbols and signal words used The user manual uses the following symbols and signal words to indicate hazards or instructions The safety instructions are always placed before an action WARNING In...

Страница 12: ...ng burnt Notice symbol Meaning Remark Observe the operating manual At the power switch Before starting work read the operating manual Before opening the device always disconnect the mains plug On the...

Страница 13: ...e sound condition of the protection and safety equipment must be checked regularly Any defects must be corrected as soon as they occur Protective and safety equipment must never be removed modified or...

Страница 14: ...ith 1500 V RMS and 40 68 MHz High frequency radiation and UV radiation can cause serious injuries to skin and eyes Contact with the torch plasma torch shortly after operation will cause skin burns An...

Страница 15: ...plasma 2 6 7 Safety instructions relating to compressed gas containers and systems Observe the following notes Argon is taken from compressed gas containers or local liquid gas systems The required p...

Страница 16: ...residue liquid from the waste bottle are disposed of in an environmentally responsible manner and according to local regulations Examples of dangerous organic solvents Methyl isobutyl ketone MIBK Flam...

Страница 17: ...ed commercial surfactants For cleaning the sampling compartment and transport channels hose system of the PlasmaQuant PQ 9000 the operator is responsible for establishing appropriate safety precaution...

Страница 18: ...cast base plate for stability and endurance protection against moisture exhaust fumes and chemical environmental impacts Detector Two dimensional FFT backside illuminated CCD with high quantum efficie...

Страница 19: ...rmitted components Oxygen 3 ppm Nitrogen 10 ppm Hydrocarbons 0 5 ppm Humidity 5 ppm 6 bar 5 7 bar 13 L min Additive gas optional Oxygen 4 5 or superior 6 bar 5 7 bar 0 02 L min Environmental condition...

Страница 20: ...than 3 m Mouse Operating system Windows 7 Professional or later 3 1 3 Cooling system data Tank capacity 4 2 L Dimensions height x width x depth 576 mm x 368 mm x 702 mm Supply voltage Frequency 100 2...

Страница 21: ...atibility The PlasmaQuant PQ 9000 has been tested for environmental compatibility and fulfills the requirements stipulated by DIN ISO 9022 3 2000 DIN ISO 9022 32 03 0 DIN ISO 9022 2 2003 01 EC directi...

Страница 22: ...possible during measuring Max humidity 90 at 20 Air pressure 0 7 bar to 1 06 bar Max permissible altitude 2000 m Summary 1 Environmental conditions for operation 4 2 Energy supply WARNING Observe the...

Страница 23: ...orrected immediately If the gas is supplied by pressure cylinders these must be secured to the wall in an upright position with cylinder mounts outside the laboratory space The following gases are use...

Страница 24: ...utput Min 3 5 m3 min max 5 5 m3 min at best 4 5 to 5 m3 min Adapter using flexible aluminum pipe Internal pipe diameter 125 mm Length approx 1000 mm Summary 4 Exhaust unit requirements 4 5 Recirculati...

Страница 25: ...pe scrape and corrosion resistant and must not absorb moisture It must be freely accessible from all sides A bottle for receiving non nebulized sample liquids and automatic sampler wash liquid is plac...

Страница 26: ...Installation conditions 24 Edition 05 2014 PlasmaQuant PQ 9000 Figure 1 Dimensions of the PlasmaQuant PQ 9000 front view Figure 2 Dimensions of the PlasmaQuant PQ 9000 top view...

Страница 27: ...centric pipes The plasma gas also called cooling gas flows at a rate of approx 12 L min on the outside to cool the external torch pipe The sample aerosol is injected in the plasma in the internal pipe...

Страница 28: ...ignition period a high voltage spark is passed from the conducting spring located in the vicinity of the induction coil through the high frequency field in the torch Pump nebulizer and spray chamber A...

Страница 29: ...s in the intermediate space between the inner tube and the injector It pushes the aerosol of the sample solution away from the injector The injector has the task of injecting the sample aerosol into t...

Страница 30: ...coupled via the transfer optics from one of the two directions to the monochromator The working range is increased by attenuating both directions of observation The selectivity of analysis is impleme...

Страница 31: ...es Cup volume mL 6 special samples 50 21 50 24 30 40 20 60 14 90 7 The purging vessel is installed at the automatic sampler A hose pump at the automatic sampler delivers the wash liquid from the dilue...

Страница 32: ...the left hand side of the PlasmaQuant PQ 9000 Also on the left side under a cover plate there are the connections for PC and accessories as well as the media connections for gas and the cooling water...

Страница 33: ...The purge gas is then directed via the cone for axial observation as a counter gas to avoid a heavy load being placed on the cone and plasma window by the plasma torch Oxygen can be optionally connec...

Страница 34: ...3 Ventilation openings and air filter on the rear of the PlasmaQuant PQ 9000 The electrical connection data can be found on the type plate on the terminal strip 1 Device type 2 Voltage 3 Frequency 4 T...

Страница 35: ...or optical plasma monitoring 6 Information plate containing device serial number 7 Induction coil with bonnet and torch Figure 16 Plasma compartment 1 Torch 2 Mechanical height adjustment 3 Fork clamp...

Страница 36: ...AG Sample supply systems the torch the nebulizer with spray chamber and the automatic sampler have to be installed by the customer during maintenance operations Descriptions of these installation proc...

Страница 37: ...upply is connected leak proof 6 Fit together the spherical joint connection of the torch and the spray chamber and secure the connection with the fork clamp 7 Push the torch on the adjusting rail upwa...

Страница 38: ...sure the pump hoses are in the groove of the hose guides Fasten the guides with the clamping levers the clamping levers must snap in audibly 13 Connect the sample pump hose to the hose of the automati...

Страница 39: ...12 Sample aspiration hose Figure 18 Automatic sampler overview 1 Connection to the PlasmaQuant PQ 9000 HOST 2 Power switch 3 Fuse holder 4 Mains connection Note DIP switch 5 is set to ON Figure 19 Co...

Страница 40: ...sitions are coded with a three digit number e g 108 The first number indicates the sample rack the following numbers the position on the rack The first sample rack is located in front of the wash cup...

Страница 41: ...ad the hose from the left side through the eyelet 2 at the lower end of the head 11 Place the hose at the rear in the eyelets at the rear of the automatic sampler arm 12 Connect the hose to the sample...

Страница 42: ...he wash solution should have the same acid content as the samples and standards Use a 2 nitric acid solution unless specified differently 11 Empty the waste bottle 12 Dip the sample aspiration hose in...

Страница 43: ...ystem for approx 3 min followed by water for 1 min Allow the device to run dry after this until there is no more liquid in the hoses If any hoses need to be replaced they will be drained of acid as a...

Страница 44: ...rting a measurement routine A method must be developed before a measurement can be made The Analytik Jena AG application team is on hand to offer support Please observe the information provided in the...

Страница 45: ...nt routine will start according to the settings made in the method and the sequence 6 If you use an automatic sampler the measurement runs automatically In the case of manual sample feed without an au...

Страница 46: ...suring environment Always observe all warnings and instructions which are displayed on the device itself or which are displayed by the control program of the PlasmaQuant PQ 9000 CAUTION Electric shock...

Страница 47: ...a distinct pressure loss If the plasma fails to ignite or is accompanied by loud noise Torch and nebulizer Torch Remove and clean If visible soiling can be seen particularly a metallic film or if the...

Страница 48: ...dismantling and assembling the torch You will have a better grip on the glass parts and minimize the risk of injury due in case of breakage of glass CAUTION Risk of burns Plasma is extremely hot Wait...

Страница 49: ...ng gloves to dismantle the torch 5 Unscrew the connecting piece from the holder and pull out the injector 6 Take the quartz bonnet out of the induction coil 7 Place all glass components for approx 12...

Страница 50: ...hat the injector is seated correctly 12 Insert the outer tube into the torch body Make sure that the ground joint seal is tight 13 Install the torch and bonnet according to the section Installation of...

Страница 51: ...on inlet are located in the openings at the rear of the holder 6 Check the O rings and renew any worn rings Place O rings in all three screw holes and carefully press onto the torch body 7 Screw the w...

Страница 52: ...you pull the quartz torch from the white holder You will have a better grip on the quartz torch and minimize the risk of injury due in case of breakage of glass CAUTION Risk of burns Plasma is extreme...

Страница 53: ...he holder and if necessary clean with water and a commercial surfactant 8 Take the quartz bonnet out of the induction coil 9 Place the glass components for approx 12 h in aqua regia 10 Rinse the glass...

Страница 54: ...ed it up An indicator that the nebulizer has clogged up is increased carrier gas pressure 1 Use to open the PLASMA CONTROL window 2 Compare the current percentage pressure of the CARRIER GAS parameter...

Страница 55: ...contamination a commercial surfactant may be used Spots drops or larger spillages should be removed and cleaned using an absorbent material such as cotton wool laboratory wipes or cellulose 8 2 6 Repl...

Страница 56: ...nse with water and dry in the gas flow argon or compressed air 4 Check the sealing rings for wear and replace if necessary 5 Insert a new or cleaned window into the holder See the note on the seating...

Страница 57: ...sticks in the frame it must be pushed out from the top This requires the deflection mirror of the transfer optics to be dismantled see below 5 Clean the window if necessary 6 Insert a new or cleaned...

Страница 58: ...ly safety check or before placing the PlasmaQuant PQ 9000 into operation if the device has been previously disconnected from the gas supply system For this purpose close the shut off valve of the gas...

Страница 59: ...enerator The fuse holders are located on the terminal strip on the left hand side of the device 1 Switch off the PlasmaQuant PQ 9000 at the power switch 2 Pull the cover in front of the side connectio...

Страница 60: ...Quant PQ 9000 8 2 10 Replacing the air filter of the PQ 9000 The air inlet filter of the PlasmaQuant PQ 9000 is located at the rear of the device Replace the filter if it is very dirty Pull the dirty...

Страница 61: ...hose end for the connection when replacing the sample hose First push the banjo bolts and then one sealing cone with the conical side onto the hose and the cannula The sealing cone and the hose or ca...

Страница 62: ...vice 1 Stop the workflow immediately 2 Take up the liquid with cellulose wadding or a cloth Wipe the surface dry 3 Ensure that the outlet can be drained i e remove any sharp bends in the draining hose...

Страница 63: ...ng and close the sealing cap by screwing hand tight 8 4 3 Changing the cooling water CAUTION Biocide Observe the safety data sheet of the biocide used Required equipment 10 L of distilled deionized wa...

Страница 64: ...bserve the level indicator The level drops when the pump is operating Continue to slowly fill the tank with the coolant until the level stabilizes slightly below the MAX mark Remove the funnel and sea...

Страница 65: ...of individual faults Error code Error message 3762 3765 3766 3782 3783 3783 Wavelength correction error No neon correction peak found Correction range exceeded No neon peaks found Too many neon peaks...

Страница 66: ...TER window activate the CCD COOLING option and then click on SET 5208 Status CCD cooling error Please check purge gas flow Cause Remedy No Ar gas flow is present If the plasma is burning in the SPECTR...

Страница 67: ...rature of max 18 C 4010 Plasma shut down because cooling water temperature too high out Cause Remedy The cooling water flow is too low The cooling temperature setting at the recirculating chiller is t...

Страница 68: ...problems Other problems that are not detected by system monitoring can also occur Starting a measurement is possible Such errors are usually detected on the basis of implausible measuring results anal...

Страница 69: ...imize sample preparation Volatile substances escape during sample preparation Optimize sample preparation There is a spectral interference in the calibration standard Use another analytical line Error...

Страница 70: ...of the analysis line and the internal standard The warm up phase is not observed Wait for the warm up phase to complete before commencing calibration The sample foams when shaken There are surface ac...

Страница 71: ...e spray chamber A change of 1 C causes a drift of approx 1 Thermostatically control the spray chamber or ensure air conditioning in the laboratory The transparency in the UV vacuum is not sufficient C...

Страница 72: ...evice Pull the cover plate from the upper mounting and lift it up from the bolts on the floor plate of the device 6 Disconnect the mains power connection of the PlasmaQuant PQ 9000 PC and automatic sa...

Страница 73: ...m moisture 10 3 Recommissioning after transport or storage ATTENTION Check that all requirements are met at the installation location see the section Installation conditions p 20 Observe the safety in...

Страница 74: ...unit Inlet PlasmaQuant PQ 9000 Out Note For better allocation of the connections one of the hoses is marked with hose clips at both ends 2 Electrically connect the recirculating chiller and switch it...

Страница 75: ...Nebulizer 25 Pump 25 Spray chamber 25 Torch 26 Transfer optics 27 Fuse Change 56 G Gas connection 30 Gas flows 26 Gas supply 20 Gas system Maintain 56 Guidelines 18 H High Frequency Generator 25 High...

Страница 76: ...partment 24 Clean 52 Connections 33 Serial number 31 Space requirement 22 Spray chamber 25 Symbols Device 8 Manual 8 T Technical data Automatic sampler 17 Computer 17 Cooling system 17 Environmental c...

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