Endress+Hauser Analytik Jena PlasmaQuant MS Operating Manual
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Endress+Hauser Analytik Jena PlasmaQuant MS Operating Manual

Inductively coupled plasma mass spectrometer (icp-ms)
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Operating Manual
PlasmaQuant MS product family
Inductively Coupled Plasma Mass
Spectrometer (ICP-MS)

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Summary of Contents for Endress+Hauser Analytik Jena PlasmaQuant MS

  • Page 1 Operating Manual PlasmaQuant MS product family Inductively Coupled Plasma Mass Spectrometer (ICP-MS)
  • Page 2 Analytik Jena AG Manufacturer Konrad-Zuse-Str.1 07745 Jena  Germany Phone + 49 3641 / 77 70 + 49 3641 / 77 92 79 Email info@analytik-jena.com Analytik Jena AG Service Konrad-Zuse-Str. 1 07745 Jena  Germany Phone + 49 3641 / 77 74 07 (Hotline) Email service@analytik-jena.com Email...
  • Page 3 PlasmaQuant MS product family Contents Contents Basic information ....................... 9 User manual notes ......................9 Intended use ........................10 Safety instructions ....................11 General notes ........................11 Safety markings on the PlasmaQuant MS ..............11 Requirements for operating personnel ................. 12 Safety instructions, transport and commissioning ............
  • Page 4 Contents PlasmaQuant MS product family Optimizing hardware ....................58 Instrument Automated Setup ..................59 Torch alignment ......................59 Peak resolution and trim ....................60 Mass calibration ......................62 Detector voltage ......................63 Detector attenuation ...................... 64 Method development ....................65 Create new worksheet ....................
  • Page 5 PlasmaQuant MS product family Contents 11.3 Maintenance ......................... 123 11.3.1 Replacing the cannula and the sample tubing ............123 11.3.2 Replacing the pump tubing ..................125 11.3.3 Clean-up after cup overflow ..................125 11.3.4 Replacing the fuses....................... 126 Troubleshooting ..................... 127 Transport and storage ....................

  • Page 6: Table Of Contents

    Figures PlasmaQuant MS product family Figures Fig. 1 Safety markings on the PlasmaQuant MS ............12 Fig. 2 PlasmaQuant MS – Front view with major components ........21 Fig. 3 Sample introduction system in the PlasmaQuant MS ........22 Fig. 4 Concentric nebulizer (left) and spray chamber (right) ........
  • Page 7 PlasmaQuant MS product family Figures Fig. 52 Detector attenuation correction factors viewer ..........92 Fig. 53 Graphical representation of attenuation factors ..........93 Fig. 54 Saving attenuation correction factors ..............93 Fig. 55 Scan settings tab ....................94 Fig. 56 Selecting attenuation correction factors ............94 Fig.
  • Page 8 Summaries PlasmaQuant MS product family Summaries Summary 1 Common elements and Interferences ............27 Summary 2 Major components and their advantages ..........30 Summary 3 Environmental conditions for operation ..........31 Summary 4 Power supply ....................32 Summary 5 Gas supply ....................33 Summary 6 Exhaust unit requirements ................
  • Page 9 PlasmaQuant MS product family Basic information Basic information User manual notes The user manual describes the following spectrometers of the PlasmaQuant series:  PlasmaQuant MS  PlasmaQuant MS Q  PlasmaQuant MS Elite S  PlasmaQuant MS Elite In the text below these devices are collectively called PlasmaQuant MS. Differences in the devices concerning the analytical performance are detailed in the section 8.
  • Page 10 Basic information PlasmaQuant MS product family Intended use Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a powerful technique for elemental and isotopic analysis that combines the efficiency and ease of use of the inductively coupled plasma (ICP) with the sensitivity and selectivity of mass spectrometry (MS).
  • Page 11 PlasmaQuant MS product family Safety instructions Safety instructions General notes For your own safety and to ensure error-free and safe operation of the PlasmaQuant MS, please read this chapter carefully before using the instrument. Observe all safety notes listed in this user manual and all messages and notes displayed by the ASpect MS software.

  • Page 12: Fig. 1 Safety Markings On The Plasmaquant Ms

    Safety instructions PlasmaQuant MS product family The following safety markings are attached to the PlasmaQuant MS: On the rear side: WARNING! Use only hydrogen and/or helium. Do NOT connect air, oxygen, or any oxidizing gas or gas mix. WARNING! Shock Hazard High voltages inside No user-serviceable parts under covers.
  • Page 13 PlasmaQuant MS product family Safety instructions  The device may only be placed on surfaces, such as desks, which were designed to bear the specific load of the device.  The device must not be placed on an uneven or inclined surface to avoid tipping over.
  • Page 14 Safety instructions PlasmaQuant MS product family  Danger of frostbite. The spray chamber and the inner parts of the thermostated holder assembly may be very cold (≥ -15 °C). Do not touch these parts in normal operation and directly after operation. 2.5.2 Safety instructions relating to ambient conditions ...
  • Page 15 PlasmaQuant MS product family Safety instructions The PlasmaQuant MS has an interlock system which is designed to extinguish the plasma if either the plasma compartment lid or the interface door is opened. The device will also extinguish the plasma when the flow rate of the cooling water or of the argon gas and the extraction output drop below the required minimum.
  • Page 16 Safety instructions PlasmaQuant MS product family 2.5.6 Safety instructions relating to the formation of ozone and toxic vapors The interaction between the UV radiation from the plasma and the surrounding air results in the formation of a high concentration of toxic gases such as ozone and nitrogen oxides.
  • Page 17 PlasmaQuant MS product family Safety instructions Observe the following notes:  Instead of using pressurized gas cylinders as a source of hydrogen, consider using a hydrogen gas generator. These devices only produce the required amount of hydrogen. There is no storage of hydrogen gas when the system is not being used. ...
  • Page 18 Safety instructions PlasmaQuant MS product family Examples of dangerous organic solvents: Methyl isobutyl ketone (MIBK) Flammable, highly volatile, noxious-smelling Toluene Flammable, hazardous to health Kerosene Flammable, hazardous to the aquatic environment, hazardous to health Methanol, ethanol, propanol Flammable, partly acutely toxic Tetrahydrofuran (THF) Flammable, hazardous to health, extremely volatile, dissolves polyethylene and polystyrene...
  • Page 19 PlasmaQuant MS product family Safety instructions Safety instructions - maintenance and repair Observe the following notes:  The PlasmaQuant MS is always serviced by the service engineers of Analytik Jena or an authorized and trained representative. Otherwise the warranty is void. The operator may only carry out the tasks listed in the chapter "Maintenance and care".
  • Page 20 Function and setup of the PlasmaQuant MS PlasmaQuant MS product family Function and setup of the PlasmaQuant MS Physical principle of ICP-MS Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful technique for elemental and isotopic analysis that combines the efficiency and ease of use of the inductively coupled plasma (ICP) with the sensitivity and selectivity of mass spectrometry (MS).

  • Page 21: Fig. 2 Plasmaquant Ms - Front View With Major Components

    PlasmaQuant MS product family Function and setup of the PlasmaQuant MS Setup of the PlasmaQuant MS Essentially the PlasmaQuant MS consists of the following components  Sample introduction system with peristaltic pump, nebulizer, spray chamber and torch  Plasma compartment with plasma generation and interference management ...

  • Page 22: Fig. 3 Sample Introduction System In The Plasmaquant Ms

    Function and setup of the PlasmaQuant MS PlasmaQuant MS product family 3.2.1 Sample introduction system The sample introduction system is freely accessible in the sampling compartment. The PlasmaQuant MS uses a four-channel variable-speed peristaltic pump to deliver Pump, nebulizer and solution to the nebulizer and to drain waste from the spray chamber.

  • Page 23: Fig. 4 Concentric Nebulizer (Left) And Spray Chamber (Right)

    PlasmaQuant MS product family Function and setup of the PlasmaQuant MS Fig. 4 Concentric nebulizer (left) and spray chamber (right) The torch sits inside the plasma compartment of the spectrometer and can be seen Plasma Torch (when in operation) through the plasma viewing window. The torch compartment is heavily shielded to prevent emission of stray RF energy and UV light.

  • Page 24: Fig. 7 Torch And Induction Coil

    Function and setup of the PlasmaQuant MS PlasmaQuant MS product family  Inert sample introduction system for geochemical type samples containing hydrofluoric acid (torch with sapphire injector, PFA nebulizer, PFA spray chamber, PFA transfer tube)  Sample introduction system for organic samples recommended for alcohols, kerosene, etc.

  • Page 25: Fig. 8 Plasmaquant Ms With Unlatched Interface Door

    PlasmaQuant MS product family Function and setup of the PlasmaQuant MS This first stage of the vacuum rapidly expands the plasma at supersonic speeds producing a beam of particles that are guided later-on to the mass spectrometer system. This first part of the vacuum system can easily be brought to atmospheric pressure for maintenance while the mass spectrometer system remains under vacuum.

  • Page 26: Fig. 9 Sampler Cone Installed In The Plasmaquant Ms

    Function and setup of the PlasmaQuant MS PlasmaQuant MS product family Sampler cone Orifice Retaining clamp ring Fig. 9 Sampler cone installed in the PlasmaQuant MS Skimmer cone Orifice Fig. 10 Skimmer cone installed in the PlasmaQuant MS The vacuum is maintained by differential pumping, whereby the pressure is reduced in The Vacuum System three stages.

  • Page 27: Fig. 11 Relative Size Distinction Between Polyatomic And Analyte Ion

    PlasmaQuant MS product family Function and setup of the PlasmaQuant MS At this pressure, ions can be guided by ion optics. Neutral gas atoms, molecules and photons, on the other hand, diffuse into the vacuum chamber and are pumped away. The final stage of the vacuum system, containing the mass analyzer and the detector, is maintained at a pressure of around 7 x 10 mbar by a second turbomolecular pump.

  • Page 28: Fig. 12 Reflexion

    Function and setup of the PlasmaQuant MS PlasmaQuant MS product family The electric fields produced by ion optics can alter the path of ions in much the same Ion Optics way as optical components like lenses, prisms or a parabolic reflectors can alter the path of photons in a beam of light.

  • Page 29: Fig. 13 Curved Pre-Filters And Mass Analyzer

    PlasmaQuant MS product family Function and setup of the PlasmaQuant MS Fig. 13 Curved pre-filters and mass analyzer Opposite pairs of rods are connected electrically. Radio frequency and DC potentials are applied to each pair of rods so that they have equal potential of opposite sign. The ions to be analyzed enter at one end of the quadrupole and those having the selected mass-to-charge ratio emerge at the other.

  • Page 30: Fig. 15 Setup Of Plasmaquant Ms

    Function and setup of the PlasmaQuant MS PlasmaQuant MS product family 3.2.4 PlasmaQuant MS – at a look Fig. 15 Setup of PlasmaQuant MS Nebulizer and spray chamber Turbomolecular pump Virtually center grounded coil ReflexION Ion Mirror Fore-line roughing pump Curved pre-filters Sampler cone HD Quadrupole mass analyzer...
  • Page 31 PlasmaQuant MS product family Installation and commissioning Installation and commissioning CAUTION The device may only be assembled, installed and repaired by the service engineers from Analytik Jena or by technical personnel authorized by Analytik Jena. Any unauthorized interference voids warranty entitlements. When starting up your device, please observe the instructions provided in the section "Safety instructions"...
  • Page 32 Installation and commissioning PlasmaQuant MS product family 4.1.2 Power supply WARNING Shock hazard! During electrical installation, observe the VDE (German Association for Electrical Engineers) electrotechnical guidelines and local regulation requirements! The mains supply must be correctly earthed. Do not use an adapter in the mains cabling.
  • Page 33 PlasmaQuant MS product family Installation and commissioning 4.1.3 Gas supply WARNING Danger of explosions! Hydrogen is highly combustible. Oxygen is a powerful oxidizer. Further, any leak in the gas supplies (except for oxygen) can result in an oxygen- deficient atmosphere which can cause asphyxiation! The operator must ensure that the connector type used on the outlet side of the gas pressure controller is adequate for the national requirements that apply.
  • Page 34 Installation and commissioning PlasmaQuant MS product family 4.1.4 Exhaust unit CAUTION Danger from hazardous gases such as ozone and nitrous gases! Switch on the exhaust unit prior to igniting the plasma. The exhaust unit is meant to remove hazardous gases generated during plasma operation, such as ozone or nitrous gases.
  • Page 35 PlasmaQuant MS product family Installation and commissioning Parameters Properties Max. Water Pressure 500 kPa (72,5 psi) Pressure at the instrument water inlet Water purity Conductivity: permitted range 75-150 µS/cm, target range 100-120 µS/cm (particle size < 0.1 mm) pH: 7-9 Total Chlorine: <...
  • Page 36 Installation and commissioning PlasmaQuant MS product family Summary 10 Fore-line roughing pump XDS46i Parameters Properties Protection class Voltage 200-240 V Frequency 50/60 Hz Power consumption 0.52 VA Weight 48 kg The fore-line roughing pump is used as both the primary pump for the first vacuum stage and as a fore-line pump for the two turbomolecular pumps on the second- and third-stage vacuum chambers.
  • Page 37 PlasmaQuant MS product family Installation and commissioning  The workbench surface must be wipeable, corrosion resistant and must not absorb moisture.  It must be freely accessible from all sides. A distance of at least 200 mm to the next wall must be kept.

  • Page 38: Fig. 16 Dimensions Of The Plasmaquant Ms

    Installation and commissioning PlasmaQuant MS product family Fig. 16 Dimensions of the PlasmaQuant MS...

  • Page 39: Fig. 17 Connections And Interfaces On The Rear Side Of The Device

    PlasmaQuant MS product family Installation and commissioning Supply and control connections The supply lines for the instrument are connected during the installation of the PlasmaQuant MS by service engineers from Analytik Jena. On the rear side of the instrument there are the connections for PC and accessories as well as the connections for gases and the cooling water inlet and outlet.

  • Page 40: Fig. 18 Overview Of Connections On The Right Side Of The Instrument

    Installation and commissioning PlasmaQuant MS product family Fig. 18 Overview of connections on the right side of the instrument Plasma OFF Connection for water cooling (H O out) Argon – sheath gas (optional, connection to the Connection for water cooling (H O in) transfer tube) Nebulizer gas...
  • Page 41 PlasmaQuant MS product family Installation and commissioning Summary 11 Information on the type plate Manufacturer (with address) Analytik Jena AG, Konrad Zuse Str. 1, D-07745 Jena Device type and model PlasmaQuant MS PlasmaQuant MS Q PlasmaQuant MS Elite S PlasmaQuant MS Elite Voltage / frequency 200-240 V AC 50/60 Hz...
  • Page 42 Installation and commissioning PlasmaQuant MS product family Installing the PlasmaQuant MS NOTICE After transport, wait for 12 hours until the PlasmaQuant MS has reached room temperature. Only start up the device after this period has elapsed. The sensitive electronics may otherwise be damaged by condensed water. The PlasmaQuant MS is delivered directly to its final destination by a transportation company.
  • Page 43 PlasmaQuant MS product family Installation and commissioning 4.3.1 Installation of the torch CAUTION Danger of injury from breaking glass! Always take care when installing or removing the parts. Installation of the torch 1. Fit one quick-connect fitting to each length of tubing. 2.
  • Page 44 Installation and commissioning PlasmaQuant MS product family 7. Close and lock the clamp arm: push the locking knob down and turn it 90-degrees until it clicks in place. 8. Connect the torch to the glass transfer tube with the glassware clamp.
  • Page 45 PlasmaQuant MS product family Installation and commissioning 4.3.2 Installation of the nebulizer 1. Fit the gas and sample tubing to the nebulizer.  Insert the capillary tubing connector directly onto the sample inlet of the nebulizer as far as it will go to minimize the dead space in the nebulizer (1).
  • Page 46 Installation and commissioning PlasmaQuant MS product family 4.3.3 Installation of the spray chamber 1. Attach a ~10 cm piece of drain tubing to the waste outlet at the bottom of the spray chamber. 2. Open the holder assembly. Place the spray chamber into position in the lower half of the holder assembly.

  • Page 47: Fig. 20 Transfer Tube For Aerosol Dilution (Left), Standard Transfer Tube (Right)

    PlasmaQuant MS product family Installation and commissioning 4.3.4 Installation of the transfer tube There are two different transfer tubes:  Standard transfer tube  Transfer tube for Aerosol Dilution (optional) Fig. 20 Transfer tube for Aerosol Dilution (left), standard transfer tube (right) The transfer tube for Aerosol Dilution has an extra connection for sheath gas.
  • Page 48 Installation and commissioning PlasmaQuant MS product family 4. Hold the lever arm down. 5. Feed the spherical joint of the transfer tube into the torch compartment through the opening in the torch compartment wall. 6. Connect the torch to the transfer tube with the glassware clamp.
  • Page 49 PlasmaQuant MS product family Installation and commissioning 8. For Aerosol Dilution: attach the gas tubing from the transfer tube to the gas box outlet labeled “Sheath Gas”.

  • Page 50: Fig. 21 Sample Tubing

    Installation and commissioning PlasmaQuant MS product family 4.3.5 Installation of the peristaltic pump tubing CAUTION Risk of injury! Always switch off the peristaltic pump before installing or removing the pump tubing. Take care to keep loose clothing, jewelry, etc. clear of the pump while it is running. 1.

  • Page 51: Fig. 22 Peristaltic Pump - Tubing Connections

    PlasmaQuant MS product family Installation and commissioning Nebulizer tubing Pressure bars Pump rollers Sample tubing - to be placed in the sample or the autosampler tubing Drain tubing from the spray chamber Fig. 22 Peristaltic pump - tubing connections 6. Place the capillary that extends from the sample pump tubing into the sample or rinse solution.

  • Page 52: Fig. 23 Pump Tubing With Internal Standard Tubing

    Installation and commissioning PlasmaQuant MS product family Always change the sample and Internal Standard tubing at the same time to avoid uneven wear of the tubing. 1. Fit another pump tubing to the peristaltic pump in the next available channel. This will be the Internal Standard channel.
  • Page 53 PlasmaQuant MS product family Operation Operation This chapter gives an outline of how to get your PlasmaQuant MS up and running for analysis and how to shut it down. The following topics cover basic ICP-MS operations:  Starting the ASpect MS Software ...

  • Page 54: Fig. 25 Instrument Summary Window

    Operation PlasmaQuant MS product family Fig. 25 Instrument summary window Starting the vacuum system If the system does not reach the required vacuum pressure within 10 minutes, an error will be displayed and the vacuum system will be shut down. 1.
  • Page 55 PlasmaQuant MS product family Operation Igniting the plasma WARNING Risk of eye and skin injuries due to UV and electromagnetic radiation! To ensure safe torch operation, you must not ignite the plasma unless the following conditions are met:  The plasma compartment lid and the interface door are closed and latched. ...

  • Page 56: Fig. 26 Time Scan Displaying The Signal During Warm-Up

    Operation PlasmaQuant MS product family Warming up the PlasmaQuant MS With the plasma lit: 1. Open the P tab of the I window. LASMA LIGN NSTRUMENT 2. Select T for the scan type in the lower-left corner of the window. 3.
  • Page 57 PlasmaQuant MS product family Operation Shutting down the PlasmaQuant MS Normally the PlasmaQuant MS should be left in standby mode, with the vacuum system on and the plasma off, unless it is not going to be used for an extended period of time (>2 weeks) or needs to be shut down due to interruptions in the laboratory facilities such as a power outage.
  • Page 58 Optimizing hardware PlasmaQuant MS product family Optimizing hardware There is a difference between Hardware Optimization and Method Optimization. The information contained in the following section refers to parameters required to make the PlasmaQuant MS run at peak efficiency. These parameters are independent of any specific analytical method and are referred to as Hardware Optimization.
  • Page 59 PlasmaQuant MS product family Optimizing hardware Instrument Automated Setup The ASpect MS can automatically perform plasma alignment, resolution and trim and mass calibration routines. All routines use the same default System Setup-worksheet: System Setup.msws. They require the 1 µg/L (1 ppb) tuning solution. Some customers use the instrument automated setup as a daily start-up of the PlasmaQuant MS because you can add to the routine that the plasma is automatically ignited and the system is warmed up.

  • Page 60: Fig. 27 Automatic Torch Alignment

    Optimizing hardware PlasmaQuant MS product family Fig. 27 Automatic torch alignment 1. Click the arrow next to the Instrument icon on the Main Toolbar and select to open the I window. Alternatively select W NSTRUMENT SETUP NSTRUMENT INDOW I NSTRUMENT ETUP 2.

  • Page 61: Fig. 28 Peak Resolution And Trim

    PlasmaQuant MS product family Optimizing hardware After changing the resolution and trim settings, you must redo the mass calibration to set the position and resolution of the remaining spectrum. Resolution and trim should be checked routinely once a month and whenever mass calibration does not give satisfactory results for peak widths.

  • Page 62: Fig. 29 Mass Calibration

    Optimizing hardware PlasmaQuant MS product family Mass calibration To calibrate, the software finds and identifies the peaks across its operating mass range. Mass calibration is done using the tuning solution supplied with the instrument; it contains a series of isotopes across the mass range (3-260 AMU). The software finds these expected peaks, and can then extrapolate all other peak positions in the mass range from these known values.

  • Page 63: Fig. 30 Detector Voltage Calibration

    PlasmaQuant MS product family Optimizing hardware Detector voltage Over time, and with continued use, the detector “ages” and requires increased voltage to produce the same signal level from a given concentration of sample. Check the detector voltage weekly and keep the voltage set to the optimum. The software scans the detector voltage across the specified range, and recommends the ideal set point.

  • Page 64: Fig. 31 Setting Up Detector Attenuation

    Optimizing hardware PlasmaQuant MS product family 5. Make a note of the present . You need to compare this value to DETECTOR VOLTAGE the recommended voltage in a later step. 6. Click [S TART The PlasmaQuant MS scans the detector voltage across the scan range shown in the F and T boxes in the lower-left (e.g.
  • Page 65 PlasmaQuant MS product family Method development Method development Before running any samples, an analytical protocol, which will be referred to in this documentation as a "Method", must be developed. This method defines the software and hardware parameters used during data acquisition for the elements/isotopes of interest in the samples to be measured.

  • Page 66: Fig. 32 Main Page Of The Worksheet

    Method development PlasmaQuant MS product family 3. Click [S ] to create the new worksheet. The main page of the worksheet is opened. Fig. 32 Main page of the worksheet Consider using a consistent naming/numbering system for worksheet data files, such as the date the worksheet was created, as well as a short description of what that particular worksheet was for.

  • Page 67: Fig. 33 Selecting Elements And Isotopes

    PlasmaQuant MS product family Method development Select elements and isotopes Elements and isotopes can be selected for analysis in the method. 1. From the main page of the worksheet, click [E ETHOD 2. Select the E tab. LEMENT 3. Select each element to be included in the method as analyte, Internal Standard, or semi-quant analyte using the browser window: Click the element in the PERIODIC TABLE...

  • Page 68: Fig. 34 Quickly Adding Elements And Isotopes From The Periodic Table

    Method development PlasmaQuant MS product family Fig. 34 Quickly adding elements and isotopes from the periodic table 5. Add an Internal Standard correction for those analytes that require it. Interpolate correction is recommended if more than one Internal Standard is selected. ...

  • Page 69: Fig. 36 Adding Or Modifying Isotope Correction Equations

    PlasmaQuant MS product family Method development Fig. 36 Adding or modifying isotope correction equations  In the C field in the I list, enter or edit the ORRECTION EQUATION SOTOPES AND QUATIONS isotope correction equation. Calculate isotope ratios Slightly different acquisition parameters are required in order to make the best isotope ratio measurements.

  • Page 70: Fig. 38 Setting Up Calibration Standards

    Method development PlasmaQuant MS product family All elemental symbols, masses, signs, and many molecular combinations, such as CeO+ and Ba++, can be entered. For example, to measure the ratio of cerium oxide formation, enter ‘CeO+’ in the first species column (the software automatically interprets this as ) and Ce+ in the second species column.
  • Page 71 PlasmaQuant MS product family Method development 3. Select the A NALYSIS  Q : Typically used for routine quantitative elemental analysis UANTITATIVE  S UANTITATIVE  S TANDARD DDITIONS 4. Type the number of standards included in the analysis in the N UMBER OF TANDARDS field.

  • Page 72: Fig. 39 Scan Settings

    Method development PlasmaQuant MS product family Fig. 39 Scan settings 3. Select the S . For details on each S , see the software help. 4. Select the scan , or the distance between measurement points on a single SPACING mass peak.

  • Page 73: Fig. 40 Sampling Settings

    PlasmaQuant MS product family Method development Fig. 40 Sampling Settings 1. From the main page of the worksheet, click [E ETHOD 2. Click the S tab. AMPLING For details on the options available on this screen, see the software help. For aqueous samples, to reduce the amount of solvent entering into the plasma, set the spray chamber temperature to 3-4 °C.

  • Page 74: Fig. 41 Qc Test Settings

    Method development PlasmaQuant MS product family Fig. 41 QC test settings Enter notes and save method parameters The N page is a text editor. It can be used to enter any additional information OTES about the method. To include information entered in the N page in the printed report, select the OTES checkbox for M...
  • Page 75 PlasmaQuant MS product family Method optimization Method optimization Method optimization is used to fine-tune the plasma and ion optics settings, including the gas flows, sampling pump rate, sampling depth, and RF power settings for the plasma, as well as the voltages applied to the ion optics. iCRC gas settings for the interference management can also be modified.
  • Page 76 Method optimization PlasmaQuant MS product family Summary 13 Performance: PlasmaQuant MS Elite S, PlasmaQuant MS Elite Element Sensitivity PlasmaQuant MS Elite S PlasmaQuant MS Elite Tuning solution Be, Mg, Co, Ba, Ce, In, Pb 1 µg/L 1 µg/L Sensitivity >3,5 ∙ 10 >5,0 ∙...

  • Page 77: Fig. 42 Copying Optimization Settings

    PlasmaQuant MS product family Method optimization 1. Open the existing worksheet and select the O tab. PTIMIZATION 2. Use the mouse to highlight the optimization settings. 3. Right-click the highlighted area and click C . The highlighted optimization settings are stored on the computer’s clipboard. 4.

  • Page 78: Fig. 43 Default Settings In The Scan Setup Window

    Method optimization PlasmaQuant MS product family 8.2.2 Scan settings for method optimization The S window is opened by clicking the [T ] button on the ETUP ETUP tab. The default settings are shown below for this window (using several PTIMIZATION elements in the tuning solution to monitor sensitivity and interferences);...
  • Page 79 PlasmaQuant MS product family Method optimization 6. Slightly adjust the voltages applied to ion optics to achieve the required sensitivity for each isotope of interest. When close to optimum, any further changes to the ion optic settings will typically begin to bias the sensitivity towards the low-mass or high-mass element. As this is done, monitor the oxide ratio and doubly-charged ratio to make sure they all meet performance requirements (see Method optimization p.

  • Page 80: Fig. 44 Selecting An Optimization Routine

    Method optimization PlasmaQuant MS product family 8.3.2 Run automatic optimization Fig. 44 Selecting an optimization routine 1. Select an optimization routine from W  O INDOWS PTIMISE PITCS 2. Verify that the selected optimization routine is appropriate. There are routines for normal and high sensitivity and for the iCRC mode.

  • Page 81: Fig. 45 Starting Optimization

    PlasmaQuant MS product family Method optimization Fig. 45 Starting optimization 4. Present a tuning solution. 5. Allow the solution nebulization to stabilize, click [R 6. Select one of the three tabs during the optimization to view optimization details. : Shows overall response to the calibration. ISUAL ...

  • Page 82: Fig. 46 Signals Of Analyte, Interference And Analyte/Interference Ratio

    Method optimization PlasmaQuant MS product family Optimize the iCRC gas flows When running in iCRC-He or iCRC-H mode the gas flow rates need to be optimized to ensure best analytical results. The amount of the iCRC gas required to remove the interferences may vary, depending on the type of samples and interfering ions.
  • Page 83 PlasmaQuant MS product family Method optimization  Ensure the instrument has been warmed up for 15 minutes before starting the optimization procedure. During the warm-up period, a time scan should be run to ensure that the quadrupole is scanning. 1. Open a system setup worksheet, or create a new worksheet. Click on [E Optimization ETHOD and select the analytes/isotopes of interest from the E...
  • Page 84 Method optimization PlasmaQuant MS product family Once an optimal flow rate is determined and set, you can further enhance sensitivity by re-tuning the instruments ion optics parameters to achieve the highest possible sensitivity for each reference isotope in iCRC mode. For more information on auto-optimization of the ion optics in iCRC mode see section "Automatic optimization"...
  • Page 85 PlasmaQuant MS product family Method optimization If there are not significant improvements in the sensitivities, then check the next point; otherwise run the ion optics auto optimization again.  Run a plasma auto optimization by selecting a plasma optimization routine during auto optimization.

  • Page 86: Fig. 47 Schematic Of Detector Attenuation

    Detector calibration PlasmaQuant MS product family Detector calibration The PlasmaQuant MS features a unique all-digital extended dynamic range detector. If the option of auto attenuation is selected, the ASpect MS software automatically chooses a suitable attenuation mode for the detector. The auto attenuation offers a wide calibration range with the lowest possible detection limit.

  • Page 87: Fig. 48 Linear Dynamic Range Of Different Attenuation Modes

    PlasmaQuant MS product family Detector calibration There are four attenuation mode settings available for any isotope in a method:  No attenuation  Medium  High  Auto Each attenuation mode can be selected on a per mass basis and works best over different concentration ranges for any given isotope.
  • Page 88 Detector calibration PlasmaQuant MS product family Before any replicate measurements are made for a solution, one very short pre-read scan (100 µs) is performed using maximum attenuation; the detector is least sensitive in this mode. This pre-reading gives an indication of what the counts per second obtained will be for that solution;...
  • Page 89 PlasmaQuant MS product family Detector calibration  Prepare two detector calibration solutions, i.e., Solution A and Solution B, which must contain all the analytes of interest. Solution A is used to calibrate the medium attenuation factor, and Solution B is used to calibrate the high attenuation factor. To avoid possible detector over-range, it is recommended that the concentration for Solution A be around 1 µg/L and the concentration for Solution B be 50 µg/L.

  • Page 90: Fig. 49 Incorrect Settings For Detector Calibration

    Detector calibration PlasmaQuant MS product family Fig. 49 Incorrect settings for detector calibration 1. Create a new worksheet by selecting N from the F menu. 2. Enter a worksheet name in the N dialog box. ORKSHEET 3. Click [S ]. The new worksheet is created. 4.

  • Page 91: Fig. 50 Configuring Scan Settings For Attenuation Calibration

    PlasmaQuant MS product family Detector calibration to H for all isotopes. ATTENUATION  Set the to at least 50,000 µs. DWELL TIME  Fig. 50 Configuring scan settings for attenuation calibration 3. Open the S tab. AMPLING 4. Set appropriate sample introduction parameters, such as sample uptake delay, spray chamber temperature, and autosampler settings.

  • Page 92: Fig. 51 Detector Calibration Tab

    Detector calibration PlasmaQuant MS product family Fig. 51 Detector calibration tab 6. When the calibration is complete, a table is displayed. Fig. 52 Detector attenuation correction factors viewer 7. Review the D table and verify both ETECTOR TTENUATION ORRECTION ACTORS IEWER attenuation factors (Medium and High) are calibrated for all isotopes of interest.

  • Page 93: Fig. 53 Graphical Representation Of Attenuation Factors

    PlasmaQuant MS product family Detector calibration 8. Click [S ] to view a graphical representation of attenuation HOW GRAPH OF THE TABLE factors. Fig. 53 Graphical representation of attenuation factors 9. Click [S ] to set the newly-calibrated factors as the default factors. Click ET AS DEFAULT ] to save the new factors to the current worksheet and as a template for later use.

  • Page 94: Fig. 55 Scan Settings Tab

    Detector calibration PlasmaQuant MS product family Attenuation factors on the existing worksheet 1. After adding isotopes and analytes of interest, open the S tab from the ETTINGS Method Editor and in the A field click [B TTENUATION CORRECTION ROWSE Fig. 55 Scan settings tab 2.
  • Page 95 PlasmaQuant MS product family Detector calibration Attenuation factors calibration troubleshooting If no significant sensitivity is observed for selected isotope/s when running the detector calibration, then check the following:  Inspect the sample introduction system and verify that the detector calibration solution is pumped into the spray chamber and the solution waste from the spray chamber is drained out properly.
  • Page 96 Maintenance and care PlasmaQuant MS product family Maintenance and care This chapter contains all the instructions for care and maintenance which users can and must perform themselves. All maintenance work and repairs beyond this scope must only be performed by service engineers from Analytik Jena or persons authorized by Analytik Jena.
  • Page 97 PlasmaQuant MS product family Maintenance and care 10.1 Maintenance intervals The following maintenance tasks must be performed: Maintenance item Action Reason, frequency Base device Basic device Clean surface with soft cloth, water or a mild Daily detergent. Clean the air vents with a soft cloth, water or a mild Monthly detergent.
  • Page 98 Maintenance and care PlasmaQuant MS product family Maintenance item Action Reason, frequency Sample tubing/cannula Check that they are free of blockages. Daily, Blockages can falsify measurement results Pump tubing Check for flexibility and tightness. Daily, replace if necessary Wash cup Clean.
  • Page 99 PlasmaQuant MS product family Maintenance and care 10.3 Sample introduction system maintenance WARNING Risk of eye and skin injuries due to UV and electromagnetic radiation! Plasma emits UV radiation and high-frequency electromagnetic radiation which can cause serious eye and skin injuries as well as other health problems. Before removing the glass components of the sample introduction system for maintenance work, always extinguish the plasma from the software.

  • Page 100: Fig. 57 Nebulizer Cleaning Tool With Installed Nebulizer

    Maintenance and care PlasmaQuant MS product family 10.3.1 Cleaning the nebulizer The nebulizer must be cleaned if particles or high concentrations of salt in the samples have clogged it up. An indicator that this has occurred is an increase in the nebulizer gas pressure.
  • Page 101 PlasmaQuant MS product family Maintenance and care 3. Push the nebulizer with the tip first into the holder until the lateral carrier gas connection comes to rest in the holder groove. 4. Hold the nebulizer cleaning tool over a receptacle and push the plunger into the syringe.
  • Page 102 Maintenance and care PlasmaQuant MS product family 10.3.2 Cleaning the spray chamber The function of the spray chamber is to act as a filter for the sample droplets. Fine droplets go through the spray chamber up to the torch and the larger droplets hit the side of the spray chamber and coalesce to form larger droplets, which then move down the drain tubing to the waste liquid vessel.
  • Page 103 PlasmaQuant MS product family Maintenance and care 6. Lift the spray chamber from the lower cover. 7. Remove the drain tubing from the spray chamber. 8. Remove the plastic cap from the spray chamber by rotating it. 9. Inspect the two O-rings and replace them if necessary.
  • Page 104 Maintenance and care PlasmaQuant MS product family 10.3.3 Cleaning the transfer tube The following instruction shows the steps for cleaning the transfer tube for aerosol dilution. The maintenance of the standard transfer tube is largely identical. 1. Turn off the plasma by clicking on the Removing the transfer ] button on the main toolbar or tube...
  • Page 105 PlasmaQuant MS product family Maintenance and care 6. Remove the transfer tube via the opening in the side wall of the torch compartment. 7. With the transfer tube for Aerosol Dilution: Remove the tubing from the transfer tube. 1. Place the transfer tube in an ultrasonic bath containing a neutral surfactant for 5 Cleaning the transfer to 15 minutes.
  • Page 106 Maintenance and care PlasmaQuant MS product family 10.3.4 Cleaning the torch CAUTION Plasma is extremely hot. Risk of burns! Wait for approx. 5 min after extinguishing the plasma before you dismantle the torch! During normal operation, deposits may form on the torch that may interfere with the operation of the instrument.
  • Page 107 PlasmaQuant MS product family Maintenance and care Check the torch for cracks or deformation caused by overheating. You should replace Inspecting the torch the torch if any part of it is cracked, partly melted, or severely eroded. Specifically, inspect the torch for: ...

  • Page 108: Fig. 58 Sampler Cone In Position With Retaining Ring And Sampler Cone Tool

    Maintenance and care PlasmaQuant MS product family 10.4 Interface maintenance 10.4.1 Cleaning the sampler cone CAUTION Plasma is extremely hot. Risk of burns! Wait for approx. 5 min after extinguishing the plasma before servicing the interface cones! NOTICE The tips of the interface cones are fabricated from nickel, so the orifices are fragile. Take extreme care when handling the cones as microscopic defects in the cone tips will have adverse effects on analytical performance.
  • Page 109 PlasmaQuant MS product family Maintenance and care 1. Before opening the interface door, extinguish the plasma from the software by clicking on the [P ] button on LASMA the main toolbar or pressing [F4]. 2. Allow the interface to cool down for at least five minutes before servicing the sampler cone or wear heat-resistant gloves.
  • Page 110 Maintenance and care PlasmaQuant MS product family 7. Press your finger against the bottom tab to help remove the cone from the interface assembly flange. 8. Remove the sampler cone (1) and retaining ring (2) from the interface assembly. 9. There is a single silicone O-ring which fits into a grooved channel behind the sampler cone.

  • Page 111: Fig. 59 Skimmer Cone In Position And Skimmer Cone Tool

    PlasmaQuant MS product family Maintenance and care From an analytical viewpoint, there is no need to clean the sampler cone clamping ring. 1. Position the sampler cone in the Replacing the sampler interface. cone 2. There are three tabs on the cone which have a unique orientation, meaning there is only one way the cone will fit back into position.
  • Page 112 Maintenance and care PlasmaQuant MS product family 1. Insert the skimmer cone tool into the three slots provided on the cone. 2. Turn the tool counterclockwise and remove the cone from the interface assembly. 3. There are two O-rings on the skimmer cone, a larger one on the outer side and a smaller one on the inner side.

  • Page 113: Fig. 60 Extraction Lens 1, Extraction Lens 2 And Retainer Tool

    PlasmaQuant MS product family Maintenance and care 10.4.3 Cleaning the extraction lenses Extraction lens 1 and 2 are the first part of the ion optics. Placed behind the skimmer Removing the two cone they direct the ion beam through the gate valve into the second stage of the extraction lenses vacuum system.
  • Page 114 Maintenance and care PlasmaQuant MS product family 1. Only for heavily soiled lenses: Clean the lens surface using fine grade sandpaper Cleaning and reinstalling such as grade 800. Alternatively, create a paste by mixing Analytik Jena cleaning the extraction lenses powder with a suitable quantity of water.
  • Page 115 PlasmaQuant MS product family Maintenance and care  Cooling water additive (10 g biocide + 10 g corrosion inhibitor) Required equipment  Distilled / demineralized water (σ < 10 µS/cm)  Beaker (V = 1 L) for mixing the cooling water additive ...

  • Page 116: Fig. 61 Forevacuum Pump

    Maintenance and care PlasmaQuant MS product family 10.6 Maintenance of the fore-line roughing pump SV40BI WARNING Vacuum pump oil can be extremely hot if the pump has been running for an extended period of time. Used pump oil may contain residual contaminants from the samples or sample matrix.
  • Page 117 PlasmaQuant MS product family Maintenance and care Required equipment: Drain the pump oil  1 L fresh pump oil (Leybonol LVO420)  Blind flange for intake connector (DN 40 KF) or plastic cap  12 mm hexagon socket wrench  Large screwdriver ...
  • Page 118 Maintenance and care PlasmaQuant MS product family 8. Close the suction port with the blind flange. 9. Connect the pump with the mains. 10. Start the pump and run it for about 30 seconds. 11. Stop the pump and disconnect the mains power connection. 12.

  • Page 119: Fig. 62 Autosampler

    PlasmaQuant MS product family Autosampler ASPQ 3300 Autosampler ASPQ 3300 11.1 Function and setup Fig. 62 Autosampler The autosampler allows fully automated routine analysis. It can be equipped with three sample racks and two racks each with 6 or 11 special samples, e.g., standards and QC solutions.

  • Page 120: Fig. 63 Autosampler - Overview

    Autosampler ASPQ 3300 PlasmaQuant MS product family 11.2 Installation Connections Fig. 63 Autosampler – overview Autosampler arm Wash cup Autosampler with cannula holder Wash cup pump Cannula 10 Speed controller for wash cup pump 4, 5 Rack for standards & QC solutions 11 Mains LED Base plate for racks 12 Sample aspiration tubing...
  • Page 121 PlasmaQuant MS product family Autosampler ASPQ 3300 The autosampler is installed next to the PlasmaQuant MS. Between these two Installing the instruments 30 cm of clearance is required to allow space for opening the interface autosampler door. NOTICE The autosampler must not be connected to the mains during installation. 1.
  • Page 122 Autosampler ASPQ 3300 PlasmaQuant MS product family 4. Connect the pump tubing to the lower inlet connector (1a) of the wash cup. Clamp the tubing between two stoppers into the pump with the connection to the wash cup facing upwards. Connect the other end of the pump tubing (1b) with a coupling to the aspiration tubing for the wash solution.
  • Page 123 PlasmaQuant MS product family Autosampler ASPQ 3300 11. Set all eight DIP switches (1) to off (right position); none of the switches is set to "ON". 12. Connect the autosampler (2, "HOST") with the interface cable to the computer. Use the provided USB-adapter, if necessary. 13.

  • Page 124: Fig. 65 Cannula With Sample Tube Of The Autosampler

    Autosampler ASPQ 3300 PlasmaQuant MS product family 6. Insert the cannula into the holder in the automatic sampler. Use the coupling piece (4) to fix the cannula from below in the holder. To do this, screw the coupling pieces (1) and (4) together. 7.

  • Page 125: Fig. 67 Autosampler Pump

    PlasmaQuant MS product family Autosampler ASPQ 3300 11.3.2 Replacing the pump tubing 1. Switch off the autosampler at the power switch. 2. Place a tray or an absorbent cloth underneath the connectors of the wash cup. 3. Release the pressure bars at the pump and fold them down. 4.
  • Page 126 Autosampler ASPQ 3300 PlasmaQuant MS product family 11.3.4 Replacing the fuses Replace the fuses of the autosampler as follows: 1. Switch off the autosampler at the power switch and pull the mains cable from the connection on the autosampler. 2. Pull out the fuse holder. To do so, insert a screwdriver blade into the slot in the fuse holder and carefully pry out the holder.
  • Page 127 PlasmaQuant MS product family Troubleshooting Troubleshooting If the plasma wouldn´t light but there are no error messages indicating a hardware Plasma Will Not Light fault, check the following:  Has anything changed on the instrument since the plasma was last operated? Faulty connections anywhere in the sample introduction system can introduce air leaks into the torch, which prevent it from igniting the plasma.
  • Page 128 Troubleshooting PlasmaQuant MS product family  If the process fails after re-setting the resolution, then click the [D ] button EFAULTS to restore the default values set by the Analytik Jena service personnel during the last installation or service, and repeat the resolution and trim routine. ...
  • Page 129 PlasmaQuant MS product family Transport and storage Transport and storage 13.1 Preparing the PlasmaQuant MS for transport CAUTION The PlasmaQuant MS is very heavy (186 kg). Risk of injury if the device falls! NOTICE Use suitable transport packaging! Unsuitable packaging material may cause damage to the device! Only transport the PlasmaQuant MS in its original packaging! 1.
  • Page 130 Transport and storage PlasmaQuant MS product family 13.2 Ambient conditions for transport and storage Observe the safety instructions in the section "Safety instructions, transport and commissioning" p. 12. Transport the PlasmaQuant MS and its components very carefully to prevent damage from impact or vibration. The device should be transported in such a way that major temperature fluctuations are avoided and the formation of condensate is thus prevented.
  • Page 131 PlasmaQuant MS product family Disposal Disposal Typically, inductively coupled plasma mass spectrometry (ICP-MS) generates liquid waste which, besides metal or heavy metal ions, mainly contains various mineral acids that are involved in sample preparation procedures. For safe removal, such resulting waste solutions must be neutralized using, for example, diluted sodium hydroxide solution.
  • Page 132 Specification PlasmaQuant MS product family Specification 15.1 Technical data 15.1.1 ICP-MS data Sample introduction Type of sample Liquid system Pump Four-channel variable-speed peristaltic pump (max. speed 100 rpm) Type of nebulizer Micromist concentric nebulizer (0.4 mL/min), optional PFA nebulizer (0.1 mL/min) for semiconductor or geochemical type applications Spray chamber Scott type, double pass spray chamber, Peltier-cooled Transfer tube...
  • Page 133 PlasmaQuant MS product family Specification Mass spectrometer Ion Optics Ion optics system with ReflexION, a 3D focusing, 90 degree ion system mirror Mass analyzer Low noise, double off-axis HD mass analyzer consisting of two assemblies – the fringe filter and the quadrupole filter (3 MHz). Self- cleaning, maintenance free.
  • Page 134 Specification PlasmaQuant MS product family Altitude 0 to 2000 m Storage Temperature: +5 °C to +45 °C, use desiccant For optimum analytical performance, it is recommended that positive air pressure be maintained in the laboratory at all times. Exhaust unit Material Heat and corrosion resistant (recommended V2A steel) Extraction output...
  • Page 135 PlasmaQuant MS product family Specification Max. Water Pressure 500 kPa (72,5 psi) Pressure at the instrument water inlet Water Purity Conductivity: permitted range 75-150 µS/cm, target range 100- 120 µS/cm (particle size < 0.1 mm) pH: Between 7-9 Total Chlorine: < 20 mg/L (20 ppm), total Nitrate: < 10 mg/L (10 ppm), total Sulfate: <...
  • Page 136 Specification PlasmaQuant MS product family 15.2 Guidelines and standards  The PlasmaQuant MS belongs to protection class I. Protection class and protection type  The housing has protection type IP 20. The PlasmaQuant MS conforms to the safety standards Device safety ...
  • Page 137 PlasmaQuant MS product family Index Index Attenuation 64 Hydrofluoric acid 10 Modes 86 Autosampler Fuse 126 ICES standards compatibility (CAN) 136 Installation 120 ICP-MS Maintain 123 Physical principle 20 Replace cannula 123 iCRC 27 Replace pump tubing 125 Optimizing the gas flow 82 Installation Autosampler 120 Calibration Standards 70...
  • Page 138 Index PlasmaQuant MS product family Transport 12 Safety interlocks 15 Operating temperature 31 Sample introduction system 22 Operation 53 Sample racks 119 PlasmaQuant MS 53 Sampler cone 25 Vacuum System 54 Clean 108 Optimization 58 Sampling Settings 72 Detector 86 Scan Settings 71, 78, 90 Detector Voltage 63 Setup...
  • Page 139 PlasmaQuant MS product family Index Type plate 41 Vacuum System 26 Starting 54 Use 10 User manual conventions 9 Water cooler 34 Maintain 114 Weight 36 Worksheet 65 Vacuum pump Mainten 116...

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