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Troubleshooting

Poor Signal Stability

Thermo Fisher Scientific

iCAP Q Operating Manual (P/N 1288090, Revision B)

7-9

Poor Signal Stability

Stability is interpreted as the ability of the instrument to produce good
% RSD values on repeats of the same sample (sometimes defined as
internal precision). Poor stability is often the reason behind a set of data
being discarded. Sample matrix can affect stability, especially if the
nebulizer cannot form a stable aerosol. System-related stability problems
will occur, if short term stability test % RSD’s worse than 2 to 3% are
obtained when running a standard tune solution.

The log view in the Experiment Editor is most useful. It is
recommended to check the previous days log and to make sure that
none of the instrument parameters has significantly changed.

❖

To solve stability issues

1. Ensure that the total dissolved solids level of the solution being

aspirated is below the recommended levels.

2. Check that the laboratory temperature is stable.

3. Check that the temperature of the cooling water supplied to the

instrument is stable.

4. Make sure that the gas lines are securely connected, free from kinks,

and not trapped.

5. Make sure the gas flow readback values in the Dashboard are stable.

6. Make sure that the tubings of the peristaltic pump are not damaged

or clogged and that the tubings are secured with the collars and
brackets.

7. Make sure that the nebulizer is not damaged or blocked.

8. Make sure that the nebulizer tubing is not damaged or clogged.

9. Make sure that the spray chamber is not damaged.

10. Make sure that the plasma torch is in good condition with no

cracked or melted areas.

11. Make sure the torch body is aligned correctly inside the torch

holder, see

“Maintaining the Torch”

.

12. Make sure that the waste tubing is inserted in the vessel and the

vessel is empty.

13. Make sure that the pump speed of the Peristaltic pump is stable.

14. Make sure that the vacuum system is stable.

If none of the above shows any improvements on the signal, contact
the Qtegra Administrator for further troubleshooting.

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Содержание iCAP Q

Страница 1: ...Part of Thermo Fisher Scientiﬁc Revision B 1288090 Thermo Fisher Scientific iCAP Q Operating Manual ...

Страница 2: ...her trademarks are the property of Thermo Fisher Scientific Inc and its subsidiaries Thermo Fisher Scientific Inc provides this document to its customers with a product purchase to use in the product operation This document is copyright protected and any reproduction of the whole or any part of this document is strictly prohibited except with the written authorization of Thermo Fisher Scientific I...

Страница 3: ...to latest software updates and manuals application reports and brochures Thermo Fisher Scientific recommends that you register with the site as early as possible To register visit register thermo bremen com form cis and fill in the registration form Once your registration has been finalized you will receive confirmation by e mail Suggestions to the Manual To suggest changes to this manual Please s...

Страница 4: ...Contacting Us Suggestions to the Manual ii iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific ...

Страница 5: ... Components 2 2 Chapter 3 System Description 3 1 General Description 3 2 Instrument Layout 3 3 Sample Introduction System 3 4 Peristaltic Pump 3 4 Nebulizer 3 5 Spray Chamber 3 5 Injector 3 6 Torch 3 6 Interface 3 7 Sample Cone and Skimmer Cone 3 7 Extraction Lens 3 8 Ion Optics 3 9 RAPID Lens 3 9 QCell 3 9 DA Assembly 3 10 Mass Analyzer 3 10 Quadrupole 3 10 Detector 3 10 Vacuum System 3 11 Forepu...

Страница 6: ...l 4 7 Permitted Materials 4 7 Electrical Safety Precautions 4 8 Residual Hazards 4 9 Personal Protective Equipment 4 10 EMC Information 4 11 In Case of Emergency 4 12 Chapter 5 System Setup 5 1 Safety Guidelines for Installation 5 2 Placing the System 5 3 Instrument Dimensions 5 3 Moving the Instrument 5 4 Workbench for Instrument 5 5 Laboratory Conditions 5 7 Power Supply 5 7 Gas Supply 5 7 Labor...

Страница 7: ...apter 7 Troubleshooting 7 1 General Remarks 7 2 Administrator User 7 2 Safety Guidelines for Troubleshooting 7 2 Error Messages 7 4 Plasma not Lit 7 5 Sensitivity Problems No Signal 7 7 Signal Drifts with Time 7 8 Poor Signal Stability 7 9 Interlocks 7 10 Door Lock 7 10 Interface Temperature 7 10 Low Water Flow 7 10 Hardware Lock Open 7 11 Water Valve Closed 7 11 Low Argon Pressure 7 11 Low Cool G...

Страница 8: ...ch 8 15 Cleaning the Glassware 8 16 Maintaining the Interface 8 17 Tools 8 17 Maintaining the Sample Cone 8 17 Maintaining the Skimmer Cone 8 20 Maintaining the Extraction Lens 8 23 Thermo Fisher Scientific Service 8 26 Health and Safety Form 8 26 Services to be Performed by Thermo Fisher Scientific Service Only 8 26 Chapter 9 Additional Safety Information 9 1 Fore Vacuum Pump 9 2 Recirculating Ch...

Страница 9: ...Typographical Conventions on page 1 2 Reference Documentation on page 1 4 About this Manual This iCAP Q Operating Manual contains precautionary statements that can prevent personal injury instrument damage and loss of data if properly followed It describes the modes of operation and principle hardware components of your iCAP Q mass spectrometer and provides step by step instructions for cleaning a...

Страница 10: ...is manual the following conventions indicate data input and output via the computer Messages displayed on the screen are represented by capitalizing the initial letter of each word and by italicizing each word Input that you enter by keyboard is identified by quotation marks single quotes for single characters double quotes for strings For brevity expressions such as choose File Directories are us...

Страница 11: ...o Fisher Scientific iCAP Q Operating Manual P N 1288090 Revision B 1 3 Topic Headings The following headings are used to show the organization of topics within a chapter Chapter 1 Chapter Name Second Level Topics Third Level Topics Fourth Level Topics ...

Страница 12: ... software also provides Help A printed version of the iCAP Q Operating Manual is shipped with the instrument A printed version of the iCAP Q Preinstallation Requirements Guide is part of the Preinstallation Kit This kit is sent to your laboratory before the arrival of the iCAP Q mass spectrometer NOTICE If this manual is in another language than English Translations of the above are shown with the...

Страница 13: ...ard system comprises the following components iCAP Q mass spectrometer Fore vacuum pump Data system computer and monitor CCT gas module for iCAP Qc and iCAP Qs only Additional gas kit for iCAP Qs only Installation Kit including Tools for installation and maintenance Spare parts Equipment for connecting the basic instrument Printed manuals iCAP Q Operating Manual For a list of the manuals delivered...

Страница 14: ...tific Optional System Components The following optional components are frequently shipped with the standard iCAP Q MS system Autosampler ESI ESI FAST or CETAC Autosampler housing NESLAB ThermoFlex 2500 Recirculating Chiller Dionex ICS Ion Chromatography System Noise reduction cover and drip pan for fore vacuum pump ...

Страница 15: ...elements of the iCAP Q instrument It contains the following topics General Description on page 3 2 Sample Introduction System on page 3 4 Ion Optics on page 3 9 QCell on page 3 9 Mass Analyzer on page 3 10 Detector on page 3 10 Vacuum System on page 3 11 Gas Supply on page 3 13 Cooling System on page 3 19 Exhaust System on page 3 21 Connections on page 3 22 ...

Страница 16: ...AP Q mass spectrometer is designed for direct analyses of liquid samples and can be coupled to further devices for analyses of gases or solid aerosols Three models are available iCAP Qa iCAP Qc and iCAP Qs Differences in the systems will be noted where applicable Figure 3 1 shows a front view of the instrument Figure 3 1 iCAP Q MS front view ...

Страница 17: ...yout The iCAP Q instrument can be divided into four main components which are described in the following topics Sample introduction Interface ion generation Ion Optics ion focussing Mass Analyzer Labeled Components 1 sample introduction 2 interface 3 ion optics 4 mass analyzer Figure 3 2 Instrument schematics front view 1 2 3 4 ...

Страница 18: ...he injector Figure 3 3 shows a schematic view of the sample introduction system Peristaltic Pump A peristaltic pump passes the liquid sample to the nebulizer Figure 3 4 shows the peristaltic pump with sample and drain tubing Labeled Components 1 ICP torch with injector 2 spray chamber 3 nebulizer 4 drain to waste peristaltic pump 5 to waste 6 sample to nebulizer peristaltic pump 7 nebulizer gas Fi...

Страница 19: ...Spray Chamber The spray chamber filters out larger aerosol droplets for improved signal stability and low oxide rates Depending on the model ordered the spray chamber is made of either quartz or PFA see Table 3 1 Table 3 1 Material used in different iCAP Q models Model Item Material iCAP Qa nebulizer PP spray chamber quartz injector quartz 2 5 mm ID iCAP Qc nebulizer PFA spray chamber quartz injec...

Страница 20: ...ferent types of analysis Injectors with smaller inner diameters are for example employed with organic based solutions see Table 3 1 Due to the semi demountable design of the torch the injectors can easily be replaced see Figure 3 6 Torch The torch consists of two concentric quartz tubes each with variable flow rates The gas stream through the outer tube of the torch shapes the plasma and shields t...

Страница 21: ...s and the extraction lens are held in the interface block which is mounted to the plasma door The interface region is water cooled because of the intense heat of the plasma Sample Cone and Skimmer Cone The sample cone and the skimmer cone are located at the right side of the interface The sample cone introduces ions from the plasma into the first vacuum stage interface vacuum and the skimmer cone ...

Страница 22: ...or analysis of organics or reactive acids like HF hydrofluoric acid Extraction Lens The extraction lens is located at the left side of the interface in Figure 3 9 The extraction lens focusses and accelerates the ions from the back of the skimmer cone into the intermediate vacuum region of the analyzer Labeled Components 1 extraction lens holder 2 extraction lens 3 extraction lens adapter Figure 3 ...

Страница 23: ...ctly out of the lens without interacting with an active lens surface for improved reliability and reduced maintenance QCell Leaving the deflection device the ions are focused onto the entry of the collision cell QCell It consists of a quadrupole with flat rods fpole in a semi contained region which keeps the ions close to the beam axis by a RF guide field The QCell can be pressurized few 10 2 mbar...

Страница 24: ...Directly behind the DA plate the beam is deflected again by the DA lens to remove residual collision gas particles from the ion beam Mass Analyzer Quadrupole The ions are then introduced into the quadrupole mass analyzer which filters out ions of a specific mass to charge ratio depending on the RF voltage and DC voltage applied to the quadrupole rods Detector Ions transmitted through the quadrupol...

Страница 25: ...ass analyzer and detector requires a high vacuum for optimum performance The iCAP Q instrument has a three stage pumping system realized by a rotary pump and split flow turbomolecular pump Figure 3 11 shows a schematic view of the vacuum stage in the instrument Labeled Components 1 interface vacuum 2 intermediate vacuum 3 high vacuum Figure 3 11 Vacuum stages in the instrument 1 3 2 ...

Страница 26: ...ular Pump The split flow turbomolecular pump backed by the forepump pumps the intermediate stage and the high vacuum analyzer stage The turbomolecular pump is located inside the instrument Pressure Measurement The pressure in the instrument is controlled by an Active Pirani Gauge APG and an Active Inverted Magnetron Gauge AIM The APG monitors the pressure in the interface region The AIM monitors t...

Страница 27: ...left side see Figure 3 13 For the CCT gases 1 and 2 in Figure 3 13 stainless steel capillaries are installed inside the iCAP Q MS from the connector to the optional CCT mass flow controller Two stainless steel capillaries of 3 m length for the connection to 1 and 2 in Figure 3 13 are supplied with the models iCAP Qc and iCAP Qs Argon gas is connected at 3 inFigure 3 13 A rigid plastic tubing polyu...

Страница 28: ...and 5 in Figure 3 13 Figure 3 14 shows the gas outlets at the inlet system Plasma and Cooling Gas Table 3 2 details the argon gas requirements The argon supply to the iCAP Q system must be stable A high quality 2 stage regulator at the source is recommended See Table 3 4 for suppliers Labeled Components 1 additional gas 2 2 additional gas 1 3 nebulizer gas Figure 3 14 Gas ports at the inlet system...

Страница 29: ...s not specified for pressure above approximately 0 8 MPa 8 bar CCT Gas Collision Cell Technology CCT allows the selective removal of polyatomic interferences If an iCAP Q model including CCT is ordered iCAP Qc or iCAP Qs CCT operation at the system is possible NOTICE The CCT gas outlet should be located within 2 to 3 meters to the left of the iCAP Q instrument The following services must be suppli...

Страница 30: ...fferent regulator Examples for regulators are given by region in Table 3 4 1 If your region is not listed contact your local Thermo Fisher Scientific service office for advice Thermo Fisher Scientific supplies the 1 16 inch to 1 4 inch adapter for the iCAP Qc and the iCAP Qs instruments to connect the CCT gas tubing to the gas bottle regulator If the outlet from your regulator is not 1 4 inch you ...

Страница 31: ...TICE Temperature down to 10 C will be required for the analysis of organic solvents This is controlled via the Peltier cooler Helium For laser ablation analysis helium gas may be needed The gas requirements are detailed in Table 3 6 Table 3 5 Additional gas requirements for oxygen Gas Requirements Specification Purity 99 996 Maximum water content 5 ppmv Supply rate max 1 L min Pressure regulator o...

Страница 32: ... Argon For some applications the use of additional argon gas is beneficial The gas requirements are detailed in Table 3 7 Table 3 7 Additional gas requirements for argon Gas Requirements Specification Purity 99 996 Maximum water content 5 ppmv Supply rate max 1 L min Pressure regulator output 0 6 MPa 6 bar ...

Страница 33: ...ater quality Connections for Water Supply The iCAP Q system can be supplied with cooling water either from a central system or from the optionally shipped recirculation water chiller NESLAB ThermoFlex 2500 The connections for the cooling water are shown in Figure 3 16 Table 3 8 Cooling water specification Item Specification Supply rate 5 5 L min Temperature 15 to 25 C optimum at 21 C Pressure 0 25...

Страница 34: ...ecirculating Chiller Optionally the iCAP Q mass spectrometer is delivered with the recirculating chiller NESLAB ThermoFlex 2500 with closed circuit cooled by a refrigerating device NOTICE For more information refer to the manufacturer s manual supplied with the instrument and see Recirculating Chiller on page 9 4 ...

Страница 35: ...e plasma exhaust duct should be equipped with a throttle valve Other peripheral devices might need additional exhaust connections Refer to the manual of these peripheral devices NOTICE Do not switch off the exhaust system when plasma is running Plasma will be shut off automatically when the air removal capacity drops below 36 m h Labeled Components 1 plasma exhaust 2 heat exhaust Figure 3 17 Exhau...

Страница 36: ...e located at the left side of the instrument see Figure 3 18 The connections for peripherals such as the computer or an autosampler are located at the right side of the instrument see Figure 3 19 Labeled Components 1 main power switch 2 main power supply 3 water connections 4 pumping connections 5 gas connection Figure 3 18 Schematic view left side Labeled Components 1 connectors to peripherals co...

Страница 37: ...cuum pumps In the On position power is supplied to the mass spectrometer In the standard operational mode the circuit breaker is kept in the On position Power Connections The main power supply connection and the power connection for the fore vacuum pump are located at the left side of the iCAP Q mass spectrometer see Figure 3 21 Figure 3 20 Main power switch of iCAP Q MS Labeled Components 1 main ...

Страница 38: ...een sample and skimmer cone The power connection the vacuum connection and the exhaust connection of the fore vacuum pump to iCAP Q MS are located at the left side of the instrument see Figure 3 22 Labeled Components 1 power connection to fore vacuum pump 2 pumping hose to fore vacuum pump 3 exhaust fore vacuum pump Figure 3 22 Fore vacuum pump connection detail of left view of iCAP Q MS 1 2 3 ...

Страница 39: ...I O 2 Digital I O 3 USB connector to computer 4 USB connector for example to autosampler 5 power connector for autosampler housing Figure 3 23 Detail connections right view of iCAP Q MS base Table 3 11 Connections at right side of the instrument Item Description Digital I O 1 Phoenix Contact connector series MC 1 5 4 G 3 81 4 pole Digital I O 2 Phoenix Contact connector series MC 1 5 6 G 3 81 6 po...

Страница 40: ...System Description Connections 3 26 iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific ...

Страница 41: ...contains the following topics Safety Symbols and Signal Words in this Manual on page 4 2 Safety Symbols on the Instrument on page 4 3 Rating Plate on page 4 5 Intended Use on page 4 6 Permitted Materials on page 4 7 Electrical Safety Precautions on page 4 8 Residual Hazards on page 4 9 Personal Protective Equipment on page 4 10 EMC Information on page 4 11 In Case of Emergency on page 4 12 ...

Страница 42: ...ept near the instrument to be available for quick reference System configuration and specifications in this manual supersede all previous information received by the purchaser Indicates the use and effect of safety instructions CAUTION Indicates unsafe situations that can cause mild injury or bodily harm WARNING Indicates unsafe situations that can cause moderately severe injury or bodily harm DAN...

Страница 43: ... damage If present read and follow the instructions on the labels Table 4 1 Safety labels on the instrument Label Label description Label position The label indicates the presence of UV radiation category 2 in the plasma The total averaged and weighted UV irradiance in 100 mm measuring distance is 1 53 x 10 3 W m The label indicates an in running nip point hazard at the peristaltic pump The label ...

Страница 44: ...ide the instrument The total averaged and weighted UV irradiance in 100 mm measuring distance is 0 27 x 10 3 W m The label indicates the presence of noxious gases at the plasma exhaust The label marks the gas connections Only permitted gases may be connected here see Permitted Materials on page 4 7 Table 4 1 Safety labels on the instrument Label Label description Label position ...

Страница 45: ...de of the iCAP Q MS SERVICE BY QUALIFIED PERSONNEL ONLY FREQUENCY RANGE 50 60Hz AC VOLTAGE 200 240 V CURRENT MAX 3x16A year of manufacture 2012 Mass Spectrometer MODEL iCAP Q SERIAL No 61 5 Made in Germany Hanna Kunath Str 11 28199 Bremen Germany This device complies with Part 18 of the FCC Rules SERVICE BY QUALIFIED PERSONNEL ONLY FREQUENCY RANGE 50 60Hz AC VOLTAGE 200 240 V CURRENT MAX 30A year ...

Страница 46: ...ench in the laboratory It is not designed for the use outdoors The instrument is designed for laboratory research use only It is not designed for use in diagnostic or medical therapeutic procedures If the iCAP Q mass spectrometer is used in a manner not specified by Thermo Fisher Scientific the protection provided by the instrument could be impaired Thermo Fisher Scientific assumes no responsibili...

Страница 47: ...pure hydrogen with the iCAP Q instrument Only employees of Thermo Fisher Scientific or personnel acting on behalf of Thermo Fisher Scientific are permitted to install the iCAP Q mass spectrometer Personnel that installs or operates iCAP Q mass spectrometer must have the following qualifications Electrical Connections The electrical installation must be carried out by qualified and trained personne...

Страница 48: ...e system without the housing on Permanent damage can occur When leaving the system make sure that all protective covers and doors are properly connected and closed and that heated areas are separated and marked to protect unqualified personnel Do not turn the instrument on if you suspect that it has incurred any kind of electrical damage Instead disconnect the power cords of mass spectrometer and ...

Страница 49: ...spray chamber is disassembled Do not disassemble the spray chamber when the plasma is still on CAUTION Hazardous Chemical Samples and solvents might contain toxic carcinogenic mutagenic or corrosive irritant chemicals Avoid exposure to potentially harmful materials Always wear protective clothing gloves and safety glasses when you handle solvents or samples Also contain waste streams and use prope...

Страница 50: ...ical hazards should be worn over street clothes Lab coats are appropriate for minor chemical splashes and solids contamination while plastic or rubber aprons are best for protection from corrosive or irritating liquids Gloves For handling chemical compounds and organic solvents Thermo Fisher Scientific recommends the following gloves white nitrile clean room gloves Fisher Scientific P N 19 120 294...

Страница 51: ...001 registered facility this instrument has been shipped to you from our manufacturing facility in a safe condition This instrument must be used as described in this manual Any use of this instrument in a manner other than described here may result in instrument damage and or operator injury Notice on the Susceptibility to Electromagnetic Transmissions Your instrument is designed to work in a cont...

Страница 52: ...ise for 180 degrees 2 Open the plasma door 2 in Figure 4 2 After 1 second the plasma switches off To shut off the system in case of emergency 1 Switch off the system at the main switch see Figure 3 20 on page 3 23 All power to the mass spectrometer is shut off 2 To separately turn off the computer use the On Off switch on the computer Labeled Components 1 plasma door closed 2 plasma door open Figu...

Страница 53: ...s the following sections Safety Guidelines for Installation on page 5 2 Placing the System on page 5 3 Laboratory Conditions on page 5 7 Only employees of Thermo Fisher Scientific or personnel acting on behalf of Thermo Fisher Scientific are allowed to install the iCAP Q mass spectrometer Only employees of Thermo Fisher Scientific or personnel acting on behalf of Thermo Fisher Scientific are allow...

Страница 54: ...uidelines for the installation of the iCAP Q mass spectrometer WARNING Noxious Gases Danger to health Hazardous materials might be present in the effluent of the fore vacuum pump Be sure to connect to an adequate exhaust system CAUTION Hazardous Gases Danger to health When operating the instrument with hazardous gas an external warning sensor must be installed in the vicinity of the instrument ...

Страница 55: ...d on top of a table with its rear panel against a wall Instrument Dimensions Figure 5 1 shows the typical required floor space for the system without autosampler All values are given in mm Labeled Components 1 monitor 2 mouse 3 keyboard 4 iCAP Q MS 5 wall 6 standard workbench Figure 5 1 Required floor space for iCAP Q MS without autosampler 700 1000 1200 748 772 767 15 1000 4 5 6 1 2 3 ...

Страница 56: ...ches prevent the handles from inadvertently being retracted after they have been pulled out Inspect the handles to verify that their safety catches are engaged before you start lifting the instrument Once the instrument is in place push down the safety catch on a handle to slide it into the instrument Labeled Components 1 monitor 2 mouse 3 keyboard 4 iCAP Q MS 5 wall 6 autosampler housing 7 comput...

Страница 57: ...e pump stator 1 person stands on the right side one hand under the oil casing and one hand under the motor fan cover Attention to your hands when setting down the pump into the drip pan to avoid squashing NOTICE Do not lift the pump at the frequency converter or the cables Workbench for Instrument The workbench for the MS system must be capable of supporting the weight of the mass spectrometer 148...

Страница 58: ...vacuum hose of the fore vacuum pump On the left side panel free access to the mains switch and circuit breaker is needed to allow shutting off the instrument in case of an emergency at all times It is recommended to leave sufficient space on the right side of the iCAP Q system for the connections to the computer and peripheral devices NOTICE Avoid blocking the ventilation slots at the side of the ...

Страница 59: ...s with the aid of pneumatics Additional gases might be required depending on the type of analysis planned For details see Gas Supply on page 3 13 Table 5 1 Basic power requirements for iCAP Q instruments Specification Value Power Apparent power 3750 VA Effective power 3500 W Single phase instrumentsa Nominal voltage 230 V AC 10 50 60 Hz AC single phase Wire Single phase 3 wire system neutral wire ...

Страница 60: ...non corrosive atmosphere It is recommended that your laboratory be equipped with a temperature and humidity monitor to insure that your laboratory is always within the required temperature and humidity specifications NOTICE Operating an iCAP Q system at very low humidity might cause the accumulation and discharge of static electricity which can shorten the life of electronic components Operating t...

Страница 61: ...um hose during operation The vibration of the fore vacuum pump might impede the performance of the instrument Install the fore vacuum pump on the floor beneath the mass spectrometer Do not install the fore vacuum pump near the system on the workbench Airborne Noise Emission The mean value for the emission sound pressure level of the iCAP Q instrument is below 70 dB CAUTION Hazardous Chemical Sampl...

Страница 62: ...System Setup Laboratory Conditions 5 10 iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific ...

Страница 63: ...e basic system operations and checks before operation It contains the following sections Safety Guidelines for Operation on page 6 2 System Controls on page 6 4 Starting Up the System on page 6 6 Shutting Down the System on page 6 7 Getting Ready on page 6 9 Working with LabBooks on page 6 14 After Operation on page 6 16 ...

Страница 64: ...Hazard Fore vacuum pump in operation is hot and some surfaces could reach a temperature higher than 80 C 176 F Switch off the pump and let it cool down before any intervention or take appropriate precautions All work on a pump that is still warm from operation should be done only while wearing heat protective gloves CAUTION Hot Surface Danger of burns Switch off the plasma two minutes before handl...

Страница 65: ...n the Peltier chiller may be cold Do not touch the Peltier chiller in normal operation and directly after operation CAUTION Pinch Point Hazard Danger of injuries Keep hands clear from the peristaltic pump during operation CAUTION Rotating Parts Hazard Danger of injuries The peristaltic pump rollers can pull in hair clothing ties and other loose objects Stay clear from the peristaltic pump during o...

Страница 66: ...le 6 1 lists their meaning MS Labeled Components 1 system LEDs Figure 6 1 ICP MS front with system control LEDs 1 Table 6 1 System Status LEDs of the iCAP Q MS LED Status Information Power Green Main power switch on Off Main power switch off Vacuum Green The high vacuum in the analyzer is reached Red Malfunction of the turbo pump Orange The turbo pump is 800 Hz Orange flashing The turbo pump is 80...

Страница 67: ...n the OFF position and that the power cords of mass spectrometer and forepump are disconnected It is not sufficient that the Power LED is off because it might be defective Power Panel Figure 6 2 shows the location of the main power switch at the left side of the instrument In the OFF position the power to the instrument and the forepump is switched off In the ON position power is supplied to the i...

Страница 68: ...e instrument 1 Switch the main power switch to position On see Figure 6 2 2 Start the vacuum system in the Instrument Control window a Click in the Vacuum submenu b Wait for the turbomolecular pump to reach at least a frequency of 800 Hz 3 Check the vacuum The vacuum pressure is correct when the vacuum LED is green see Figure 6 1 4 If the system was vented the detector should be calibrated regardl...

Страница 69: ...as flushed To set the instrument to standby 1 Click inside the Experiment Editor window The plasma is switched off Data that have not been saved before are saved now If installed the autosampler moves to the home position The vacuum is still intact The instrument is in standby mode 2 Release the tubings from the peristaltic pump to maintain their flexibility Shutting Down the Complete System Instr...

Страница 70: ...em is fully vented 3 Switch the main power switch to position Off see Figure 6 2 Shutting Down the Instrument only Instrument not Vented Initial position The experiments are finished The plasma is still lit The system was flushed NOTICE If the plasma is not lit start with step 2 To shut down the instrument 1 Click inside the Experiment Editor window The plasma is switched off 2 Switch the main pow...

Страница 71: ...for samples containing matrix load are provided by Thermo Fisher Scientific Additionally the modes STDS KEDS and CCTS are provided for optimized sensitivity for samples without matrix load The Lab Manager may create company specific measurement modes Before Operating the System Before operating the system it is recommended to check the tubings of the peristaltic pump To check the pump tubings 1 Ma...

Страница 72: ...d configuration is marked with a green check mark b Select a new configuration with a mouse click c Click OK to load the new configuration 3 Click to start the instrument A dialog will open in which all modes to be used during the measurements can be selected 4 If required configure a delay for warmup of the instrument Figure 6 3 Experiment Editor Dashboard Figure 6 4 Experiment Editor Example of ...

Страница 73: ...g steps can be observed in the Get Ready panel The STD mode is always the first mode to be checked in the procedure If an autosampler is installed after rinsing of the probe the autosampler moves automatically to the vial containing the solution for running the performance report Within the performance report several criteria are defined for example mass calibration sensitivity oxide rate that hav...

Страница 74: ...any case the real time display shown on the Dashboard page shows the observed signal intensities during all steps of the procedure If all tests were passed the newly generated settings are saved and the Get Ready procedure indicates its successful completion If other modes have been selected in the Get Ready procedure they will be tested once the STD mode performance report has been passed success...

Страница 75: ...ilure and to clean or exchange the sample skimmer cone In any case although the Get Ready procedure was not completed successfully the instrument can be used for analysis 5 Click to return to the principal Dashboard screen or go to the Analysis tab to prepare LabBooks for measurement Going to Operation Status with Instrument Control As an alternative to the Get Ready procedure the instrument can a...

Страница 76: ...LabBook or an existing LabBook To load a recent LabBook click a LabBook in the Recent LabBooks section To load an existing LabBook do the following a Click Open in the Open LabBook section b In the Browse for LabBook dialog box select a LabBook c Click OK to open the LabBook 3 The LabBook opens in a new tab of the Experiment Editor Table 6 2 Evaluation methods in Qtegra Method Description aQuant D...

Страница 77: ...data acquisition queue for measurement To submit the LabBook to the data acquisition 1 Click in the panel in the upper side of the LabBook The LabBook is now sent to the acquisition queue for measurement 2 Open the Scheduler panel to start and revise the current status of the data acquisition process The Scheduler lists all LabBooks sent to the queue and shows their current status sample actually ...

Страница 78: ...pectrometer 1 Move the probe to a vial containing an appropriate blank solution 2 Let the system flush with the blank solution for about 5 to 10 minutes Release Peristaltic Pump Tubing To maintain their flexibility it is also important to release the tubings from the peristaltic pump To release the tubing 1 Open the brackets at the peristaltic pump 2 Remove the collar from the tube 3 Take out the ...

Страница 79: ...remedial action Many problems in high performance instrumentation are the result of trivial concerns usually after some routine maintenance or if another operator has left the instrument in a non standard configuration It contains the following topics General Remarks on page 7 2 Safety Guidelines for Troubleshooting on page 7 2 Error Messages on page 7 4 Sensitivity Problems No Signal on page 7 7 ...

Страница 80: ...described in the following assume that you are logged in as a Qtegra User For advanced troubleshooting procedures access rights to the Instrument Control window are required Safety Guidelines for Troubleshooting When performing troubleshooting on the iCAP Q system please pay attention to the following general safety guidelines CAUTION Service by the customer must be performed by trained qualified ...

Страница 81: ... causing personal injury are used in the instrument Do not remove protective covers from PCBs Opening the instrument housing is only allowed for maintenance purposes by Thermo Fisher Scientific personnel To ensure that the instrument is free from all electric current always disconnect the power cords of mass spectrometer and fore vacuum pump before attempting any type of maintenance ...

Страница 82: ...itor Table 7 1 Troubleshooting Problem Remedy Plasma not lit page 7 7 No signal page 7 8 Signal drifts with time page 7 9 Poor signal stability page 7 9 Door Lock Interlock not satisfied page 7 10 Interface Temperature not satisfied page 7 10 Low Water Flow not satisfied page 7 10 Hardware Lock Open not satisfied page 7 11 Water Valve Closed not satisfied page 7 11 Low Argon Pressure not satisfied...

Страница 83: ...nnected and free from kinks 3 Make sure that the gas flow readback values in the Dashboard are ok 4 Make sure that the tubings of the peristaltic pump are not damaged or clogged 5 Make sure that the nebulizer is not damaged or blocked 6 Make sure that the nebulizer tubing is not damaged or clogged 7 Make sure that the nebulizer tubing is securely fastened 8 Make sure that the spray chamber is not ...

Страница 84: ...ndition with no burns or damages 16 Make sure that the waste tubing is inserted in the waste container and the waste container is empty 17 Make sure that the sample cone is in good condition 18 Make sure the Forward Power during ignition is 900 W or greater 19 Make sure that the cooling water meets the conductivity requirements If the problem remains contact the Qtegra Administrator for further tr...

Страница 85: ...ignal is found a Make sure that the instrument is ready for operation b Make sure that all cables between instrument and computer are securely connected If none of the above shows any improvements on the signal contact the Qtegra Administrator for further troubleshooting If a signal is found a Check the solution concentration b Check that the aspirated sample is visible in the spray chamber c Make...

Страница 86: ...emperature of the cooling water supplied to the instrument is stable 4 Make sure that the cooling water lines at the Peltier cooler are securely connected 5 Make sure that the pump speed of the Peristaltic pump is stable 6 Make sure that the vacuum system is stable 7 Make sure that the tubings of the peristaltic pump are not damaged or clogged 8 Make sure that the nebulizer is not damaged or block...

Страница 87: ...s 2 Check that the laboratory temperature is stable 3 Check that the temperature of the cooling water supplied to the instrument is stable 4 Make sure that the gas lines are securely connected free from kinks and not trapped 5 Make sure the gas flow readback values in the Dashboard are stable 6 Make sure that the tubings of the peristaltic pump are not damaged or clogged and that the tubings are s...

Страница 88: ... that the temperature of the interface exceeds 50 C or has not been below 40 C after exceeding 50 C Also see the readback value of the interface temperature in the Plasma pane see Figure 7 1 The interlock may also be set when the temperature sensor is not connected or damaged To reset the Interface Temperature interlock 1 Check the interlocks Low Water Flow and Water Valve Closed 2 Make sure that ...

Страница 89: ...es that the argon gas flow is not sufficient Also see the readback value of the gas flow in the Gas Flow pane see Figure 7 1 To reset the Low Argon Pressure interlock 1 Check that the argon supply is switched on and can supply 6 bar 2 Make sure that the gas lines are securely connected free from kinks and not trapped Low Cool Gas Flow The Low Cool Gas Flow interlock indicates that the cool gas flo...

Страница 90: ...et the Low Exhaust Gas Flow interlock 1 Check the plasma exhaust ducts at the top of the instrument 2 Check that the exhaust system on site is working properly Plasma Lit Sensor The Plasma Lit Sensor interlock indicates that the plasma is lit although is has not been started Also see the readback values in the Plasma pane see Figure 7 1 on page 7 4 See Plasma not Lit on page 7 5 for more informati...

Страница 91: ...nsure optimum performance of the iCAP Q mass spectrometer Safety Guidelines for Maintenance on page 8 2 General Advice for Maintenance on page 8 4 Servicing Plan on page 8 5 General Maintenance Routines on page 8 7 Maintaining the Air Filter on page 8 9 Maintaining the Inlet System on page 8 11 Maintaining the Interface on page 8 17 Thermo Fisher Scientific Service on page 8 26 ...

Страница 92: ...ids When handling the corrosive acids required to perform the cleaning procedures described below take the following precautions Wear protective clothing Use acid resistant laboratory gloves and glasses Make yourself aware of all safety procedures in case of spillage or exposure to skin or eyes before commencing the cleaning The acid cleaning should take place in a fume hood CAUTION Hot Surface Da...

Страница 93: ...in waste streams and use proper ventilation Refer to your supplier s Material Safety Data Sheet MSDS for proper handling of a particular solvent It is the responsibility of the operator to maintain the system properly by performing the system maintenance procedures on a regular basis Service by the operator must be performed by trained qualified personnel only and is restricted to servicing mechan...

Страница 94: ...ached Therefore a Thermo Fisher Scientific field service engineer must be called if removal of the instrument housing is required To successfully carry out the procedures listed in this chapter observe the following rules Proceed methodically Always wear clean talc free and lint free gloves when handling the components of the iCAP Q mass spectrometer Thermo Fisher Scientific recommends white nitri...

Страница 95: ...mber Clean the spray chamber If necessary page 8 13 Replace the spray chamber If necessary page 8 13 Injector Clean the injector If necessary page 8 14 Replace the injector If necessary page 8 14 Torch Clean the torch If necessary page 8 15 Replace the torch If necessary page 8 15 Interface Cones Cleaning the cones Depending on operation condition page 8 19 Replacing the skimmer cone insert Depend...

Страница 96: ...ck anti suck back valve Annually Clean fan cover Annually 1st oil change Depending on operation condition Replace PFPE oil Annually or depending on operation condition Chiller Replace fluid bag Depending on operation condition see manufacturer s manual Replace condenser filter Depending on operation condition Clean reservoir Depending on operation condition Table 8 1 Maintenance procedures Item Pr...

Страница 97: ... solvent like isopropanol in accordance with your local safety practices Several liters of distilled water Aqua regia Nitric acid Checking Warning Labels The safety warnings on the machine must always be complete clearly visible and legible In addition to the safety instructions that can be found throughout this manual various warning labels on the instrument inform the user about possible hazards...

Страница 98: ...ignificantly for example the argon pressure falls by more than 10 psi 690 mbar within two minutes you should search for leaks in the gas line 3 Search for leaks in the gas line for example by using a conventional thermal conductivity based leak detector such as is widely used to check leaks in gas chromatography equipment 4 If you detect a leak which is usually at a connection verify the tightness...

Страница 99: ...at regular intervals Before performing any checks or routine maintenance procedures at the fan filter the instrument must be switched off To check the air filter 1 The air filter cover is held by magnetic forces Open the filter cover at the left side of the instrument a Slightly lift up the cover b Pull off the cover 2 Visual inspect the filter for dirt or damage 3 Close the cover again Figure 8 1...

Страница 100: ...288090 Revision B Thermo Fisher Scientific To clean the filter 1 Open the fan cover at the left side of the instrument see Figure 8 2 2 Carefully pull out the filter 3 Clean the filter with a vacuum cleaner 4 Insert the filter again 5 Close the cover Figure 8 3 Remove filter ...

Страница 101: ...rticulate matter that is present in either the supply gas or the sample Solids might deposit in the nozzle thus restricting the nebulizer and causing a loss in performance To prevent nebulizer blockage 1 Rinse the nebulizer 2 Allow the nebulizer to dry before turning off the gas supply 3 Make sure that the sample uptake is disconnected or arranged so that it prevents siphoning into the nebulizer w...

Страница 102: ...staltic pump tubing can affect the stability of the ion beam Therefore the peristaltic pump tubing should be replaced regularly To maintain the peristaltic pump 1 Make sure the peristaltic pump is not running 2 Wipe the surface of the peristaltic pump rollers and tension arms with a dry cloth to remove any dust CAUTION Corrosive Acid When handling corrosive acids such as aqua regia take the follow...

Страница 103: ...ICE You must be logged in as Qtegra Administrator to access the Instrument Control window 9 Check that the sample is being taken up into the instrument and being drained efficiently 10 If needed adjust the tension of the tubing using the thumbscrews on the peristaltic pump NOTICE If an autosampler is being used it is recommended to renew the wash station tubing whenever the sample uptake and drain...

Страница 104: ...l the spray chamber 1 Mount the elbow tube to the spray chamber 2 Attach the drain tubing 3 Insert the spray chamber with the elbow connector 4 Mount the Peltier cooling lid 5 Fit the thumb screw and secure the lid 6 Insert the nebulizer Maintaining the Injector Removing the Injector To remove the injector 1 Remove the nebulizer see Removing the Nebulizer on page 8 11 2 Remove the spray chamber se...

Страница 105: ... nebulizer see Inserting the Nebulizer on page 8 12 Maintaining the Torch Removing the Torch To remove the injector 1 Remove the nebulizer see Removing the Nebulizer on page 8 11 2 Remove the spray chamber see Removing the Spray Chamber on page 8 13 3 Carefully pull out the injector 4 Press the red button at the torch holder 3 in Figure 8 6 and turn the torch assembly counterclockwise to release t...

Страница 106: ...h spray chamber injector 1 Insert the glassware in 10 20 high purity grade nitric acid 2 Clean it in an ultrasonic bath 3 Remove it from the nitric acid and wash it at least three times in fresh deionized water 4 Allow it to air dry completely If any components are to be stored for some time before use they should be placed in metal free sealed plastic bags CAUTION Corrosive Acids When handling th...

Страница 107: ...cone tool for easy disassembly of the cones The cone tool is magnetic to hold the cones in place when removing them from the interface block Figure 8 7 shows the cone tools with the cones arranged at their respective tool side Maintaining the Sample Cone Removing the Sample Cone To remove the sample cone 1 Open the plasma chamber door 2 Use the cone tool to remove the sample cone a Place the cone ...

Страница 108: ... Thermo Fisher Scientific c Slightly turn counterclockwise to unscrew the sample cone and the sample cone holder d Remove the sample cone and the cone holder from the tool The sample cone can now be cleaned Figure 8 8 Cone tool at cone housing Figure 8 9 Sample cone and holder in cone tool ...

Страница 109: ... to air dry Inserting the Sample Cone To insert the sample cone 1 Make sure that the sample cone gasket is in good condition see Figure 8 11 Replace it if required Figure 8 10 Cone tool sample cone holder and sample cone CAUTION Corrosive Acids When handling the corrosive acids required to perform the cleaning procedures described below take the following precautions Wear protective clothing Use a...

Страница 110: ...the cone must be sharp and regular If there is evidence of damage to the tip it should be replaced The skimmer cone has a replaceable insert that must be replaced depending on operation conditions Removing the Skimmer Cone To remove the skimmer cone 1 Open the plasma chamber door 2 Remove the sample cone see Removing the Sample Cone on page 8 17 3 Remove the skimmer cone a Carefully insert the con...

Страница 111: ...mer cone see Maintaining the Skimmer Cone Insert on page 8 21 Cleaning the Skimmer Cone For the cleaning procedure of the cone see Cleaning the Sample Cone and the Skimmer Cone on page 8 19 Maintaining the Skimmer Cone Insert To replace the skimmer cone insert using the insert tool 1 Align the insert tool with the holes in the skimmer cone insert Figure 8 12 Cone tool with skimmer cone Figure 8 13...

Страница 112: ...ean the insert Proceed as described in Cleaning the Sample Cone and the Skimmer Cone on page 8 19 using a 10 solution of nitric acid 5 After the cleaning procedure is completed position the insert at the tool again see Figure 8 15 NOTICE Make sure to mount the insert with the correct side facing the tool see Figure 8 15 Figure 8 14 Insert tool and skimmer cone insert Figure 8 15 Skimmer cone inser...

Страница 113: ...he sample cone and the cone holder see Inserting the Sample Cone on page 8 19 3 Close the plasma door Maintaining the Extraction Lens Depending on the type of applications and on the general operating conditions the extraction lens must be cleaned or replaced Removing the Extraction Lens To remove the extraction lens 1 Set the instrument to standby mode 2 Open the interface door 3 Turn the extract...

Страница 114: ...action lens Cleaning the Extraction Lens Figure 8 17 Pull out the extraction lens Figure 8 18 Extraction lens CAUTION Corrosive Acids When handling the corrosive acids required to perform the cleaning procedures described below take the following precautions Wear protective clothing Use acid resistant laboratory gloves and glasses Make yourself aware of all safety procedures in case of spillage or...

Страница 115: ...s for 5 minutes with deionized water 4 Dry it carefully with a non fiber shedding laboratory wipe or leave it to air dry Inserting the Extraction Lens To insert the extraction lens 1 Reassemble the extraction lens the extraction lens holder and the spring washer 2 Insert the extraction lens assembly in the housing see Figure 8 17 Be careful not to tilt the assembly 3 Turn the extraction lens clock...

Страница 116: ...tion CAUTION Hazardous Chemicals Hazardous material might contaminate certain parts of your system during analysis To protect our employees we ask you to adhere to special precautions when returning parts for exchange or repair If hazardous materials have contaminated mass spectrometer parts Thermo Fisher Scientific can only accept these parts for repair if they have been properly decontaminated M...

Страница 117: ... Safety Information This chapter contains excerpts from component suppliers documents with safety relevant information that may concern users of the iCAP Q mass spectrometer It contains the following topics Fore Vacuum Pump on page 9 2 Recirculating Chiller on page 9 4 Dionex ICS 5000 on page 9 5 ...

Страница 118: ...mbol must only be opened by trained electricians after having reliably deenergized lockout tagout the equipment Always operate the pump with a properly connected protective earth conductor and make sure that the motor FC connection box are closed Observe the manufacturer s information and operating instructions for the respective frequency converter enclosed Use only the OLV frequency converter fo...

Страница 119: ...or take appropriate precautions It is recommended to use an oil casing or pump touching protection at high ambient temperatures As a touching protection you can use the noise reduction cover All work on a pump which is still warm from operation must be done only whilst wearing protective gloves Handle the pump only while vented and after having let it cool down Never remove the oil fill or oil dra...

Страница 120: ...outlet It is the user s responsibility to assure a proper ground connection is provided Always turn off the unit and disconnect the power cord from the power source before performing any service or maintenance procedures or before moving the unit Never operate the unit with panels removed Never operate equipment with damaged power cords CAUTION Sharp Edges Danger of injury The condenser framing an...

Страница 121: ... an uncapped waste container Connect the Waste Gas Separator line to the waste tube CAUTION Hot Surface Risk of burns To avoid injury wait for the device to cool down before opening the door or performing any maintenance or service procedures CAUTION Hot Surface Risk of burns Do not touch any metal parts inside the Thermal Compartment TC while it is heating up or after it reaches the set point tem...

Страница 122: ...Additional Safety Information Dionex ICS 5000 9 6 iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific ...

Страница 123: ...rating Manual P N 1288090 Revision B D 1 Legal Documents This chapter provides legal documents It contains the following documentation FCC Compliance Statement on page D 2 WEEE Compliance on page D 3 Declaration of Conformity on page D 4 ...

Страница 124: ...Legal Documents FCC Compliance Statement D 2 iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific FCC Compliance Statement This device complies with part 18 of the FCC rules ...

Страница 125: ...ng symbol Thermo Fisher Scientific has contracted with one or more recycling disposal companies in each EU Member State and this product should be disposed of or recycled through them Further information on Thermo Fisher Scientific s compliance with these Directives the recyclers in your country and information on Thermo Fisher Scientific products which may assist the detection of substances subje...

Страница 126: ...Legal Documents Declaration of Conformity D 4 iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific Declaration of Conformity ...

Страница 127: ...tive Pirani Gauge used for vacuum pressure measurement atomic mass unit Atomic Mass Unit u defined by taking the mass of one atom of carbon12 as being 12u unit of mass for expressing masses of atoms or molecules aux gas auxiliary gas argon serves to generate the plasma B BEC Abbr for Background Equivalent Concentration normally in ppt n 10 depends on the concentration in the blank BLK Abbr for a b...

Страница 128: ...cles per second I ICIS Interactive Chemical Information System ID inside diameter in inch internal standards are used in ICP MS analyses to compensate for drift effects in response or sensitivity caused by various processes in sample introduction or ion extraction I O input output ISO Abbr for isotope dilution analyte L LAN local area network lb pound LC liquid chromatograph liquid chromatography ...

Страница 129: ...reation of calibration curves during a sequence of analyses the software offers four types linear thru zero weighted and square fit RF radio frequency S s second square fit regression type the fit is performed with a second order quadratic function STD Abbr for standard solution analyte T TCP IP transmission control protocol Internet protocol U u see atomic mass unit UPW abbr Ultra Pure Water V V ...

Страница 130: ...Glossary WEEE WEEE G 4 iCAP Q Operating Manual P N 1288090 Revision B Thermo Fisher Scientific ...

Страница 131: ...losure signals 3 25 cooling water 3 19 D DA lens 3 10 DA plate 3 10 Dashboard 3 12 dashboard 7 4 deposition of matrix 7 8 diagnosing potential problems 7 2 Door Lock interlock 7 10 E emergency shutdown 4 12 eQuant 6 14 error messages 7 4 exhaust ports 3 21 exhaust system 3 21 extraction lens 3 8 F flatapole fpole 3 9 floor space with autosampler 5 4 without autosampler 5 3 fore vacuum pump connect...

Страница 132: ...lizer 3 5 O organic solvents 3 17 oxygen 3 17 P Peltier cooler 3 6 performance report 6 9 peristaltic pump 8 12 personal protective equipment PPE 4 10 plasma door 3 7 plasma gas regulator 3 16 Plasma Lit Sensor interlock 7 12 polyatomic interferences 3 15 Power LED 6 4 power requirements 5 7 pressure two stage gas regulator 3 16 Q QCell 3 9 Qtegra Administrator 7 6 Qtegra User 7 2 quadrupole mass ...

Страница 133: ... W laboratory 7 8 7 9 tension on peristaltic pump tubing 7 8 torch 3 6 total dissolved solids level 7 8 7 9 tQuant 6 14 transport pallet 5 4 trQuant 6 14 turbomolecular pump 3 12 V Vacuum LED 6 4 vibration 5 9 W wall receptacle 5 7 warning labels 8 7 Water Valve Closed interlock 7 11 ...

Страница 134: ...Thermo Fisher Scientific Inc 81 Wyman Street P O Box 9046 Waltham Massachussetts 02454 9046 United States www thermoscientific com Part of Thermo Fisher Scientific ...

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