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Drawell GC-MS-II User Manual

Gas chromatograph-mass spectrometer
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Gas Chromatograph-Mass Spectrometer
Please read operating manual before installation and operation.
Drawell International Technology Limited
Chongqing Drawell Instrument Co., Ltd.
Shanghai Drawell Scientific Instrument Co.,Ltd.
Chongqing Center : Suite 2705,Building No.12,Shiyou Road No.1, Yuzhong District,
Shanghai Office : Suite 1117,Lane561 XiuChuan Rd.,PuDong New
Homepage : www.drawell.com.cn
Tel : 0086-023-63268643
Email : sales02@drawell.com.cn
GC-MS-II
User Manual
Chongqing, China.
Area,Shanghai,China

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  • Page 1 GC-MS-II User Manual Please read operating manual before installation and operation. Drawell International Technology Limited Chongqing Drawell Instrument Co., Ltd. Shanghai Drawell Scientific Instrument Co.,Ltd. Chongqing Center : Suite 2705,Building No.12,Shiyou Road No.1, Yuzhong District, Chongqing, China. Shanghai Office : Suite 1117,Lane561 XiuChuan Rd.,PuDong New Area,Shanghai,China Homepage : www.drawell.com.cn...

  • Page 2: Precautions For Safe Operation

    General This Operation Guide describes the procedures for properly operating and maintaining the instrument. The operator of the instrument should carefully read and fully understand this guide herein before running the instrument. This guide should be readily available for reference by operators who will operate and maintain the instrument.

  • Page 3: Operation Precautions

    Operation Precautions Warning Always wear safety glasses or goggles when handling solvents. If solvent gets into the eyes, blindness could occur. Should solvent get into the eyes, immediately flush with large amounts of water and seek medical attention. Warning: Do not place solvents near PCs or printers, as fire or instrument damage may occur. Warning: Do not use flammable sprays (hair sprays, insecticide sprays, etc.) near this instrument, as they may ignite and cause a fire.
  • Page 4 High-Pressure Gas Cylinder Precautions Warning A high-pressure gas cylinder will be used to supply the carrier gas. When handling the gas cylinders, observe the following precautions. 1. Keep gas cylinders in a well-ventilated area outside of the instrument installation site. Avoid direct sunlight. Use lines to transport the gas from the cylinders to the instrument.
  • Page 5 Handling Emergencies The following measures should be taken in case of an emergency. Reuse the instrument with great care and contact Drawell after-sales service dept. if necessary. In the event of an emergency, 1. Turn off the gas chromatograph and mass spectrometer.

  • Page 6: Table Of Contents

    Table of contents 1. Introduction..........................2 1.1 Some Abbrs........................2 1.2 Important Safety Warning.................... 3 Mark............................4 Note............................. 4 2. Instrument installation......................5 2.1 Outer Configuration Requirements................5 2.2 Installation and Connection..................7 2.3 External gas path installation..................9 2.4 External Gas path leakage check................11 2.5 Septum, glass liner installation...................12 2.5.1 Glass liner installation.....................

  • Page 7: Introduction

    1. Introduction Some Abbrs For your reading convenience, the abbreviations used in this manual are listed below. Table 1 Abbr Abbr. Def. Atomic mass unit DC voltage Electronic Flow Control Electron impact ionization source Electronic Pressure Control Full scan Full scan Gas Chromatograph High dynode mass-to-charge rate...

  • Page 8: Important Safety Warning

    1.2 Important Safety Warning Using GC-MS-II, you should always pay attention to the following important safety precautions: If the MS is connected to the power supply even when the power switch is turned off, following components will still exist potentially dangerous voltages: The wiring connecting MS power cord with AC source;...

  • Page 9: Mark

    The best way to maintain MS normal operation is to keep “Turn on” and maintain a higher temperature under the condition of carrier air flow. If intend to move or store MS, it is recommended to consult Drawell service department for information. MS must always remain upright and be taken great care when moving.

  • Page 10: Instrument Installation

    Physical Characteristics 2.1.1 The whole package of GC-MS-II is rectangular with a length of 105 cm, width 60 cm, height 50 cm, among which the mechanical pump weighs 23 kg, while the whole machine (excluding mechanical pump) weighs 100 kg.
  • Page 11 Warning The solvent used by GCMS is flammable and toxic, so the instrument should be placed in an adequately ventilated room, otherwise poisoning or fire will be easily caused. Do not use in an environment with explosive, flammable gas, to avoid fire risk. Warning Do not place flammable materials near the column oven vent at the rear of GC to avoid fire risk.

  • Page 12: Installation And Connection

    Place the instrument in sequence as in Figure 2-1; connect the power cords of GC, MS and mechanical pump to the appropriate source (see Figure 2-2). Figure 2-1 GC-MS-II Schematic front view 1-Status Lamp 2-Injection 3- GC Oven door 4-GC Control Panel...
  • Page 13 Figure 2-2 GC-MS-II Schematic rear view 1—Exhaust Opening 2—Carrier Gas Inlet 3、8—Power Switch 4—GC Power Socket 5—Vacuum Line 6—Mechanical Pump Power 7—MS Power Socket...

  • Page 14: External Gas Path Installation

    2.3External gas path installation Related consumables and tools Part name Part No. Valve connector 3010605408 3010603528 Nuts（Ф3.2） 1/8”front ferrule 304760233 1/8”back ferrule 304760234 Double wrench（1/4-5/16） 3802000722 Wrench 3802000121 O-ring 3×1.8（optional） 304570322 Installation steps The installation of the external gas path is as shown in Figure 2-3; Keep cylinders upright and be fastened in the anti-falling base;...
  • Page 15 Warning For safety regulations on air source, please refer to the above mentioned High pressure cylinders Use Precautions. The quality of the gas should meet the gas source requirements of GC-MS, to avoid affecting the results or contaminating or even damaging the instrument. Mechanical pump exhaust outlet uses pipeline to exhaust gas outside, to prevent indoor air pollution when analyzing toxic substances.

  • Page 16: External Gas Path Leakage Check

    2.4External Gas path leakage check There’s a need of leakage check for the installed the external gas path. The check steps are as following: Set the cylinder valve regulator handle at a relaxed state, open the cylinder pressure valve, then slowly adjust the handle until the low-pressure gauge indicates at 0.4MPa;...

  • Page 17: Septum, Glass Liner Installation

    2.5Septum, glass liner installation Figure 2-4 depicts GC split / splitless inlet exploded view. Figure 2-4 Split / splitless inlet exploded view 1— Septum Nut 2—Septum 3—Nut(Injection Port) 4—Injection Port 5—Fluororubber O-Ring 6—Glass Insert Port 7—Nut(Heat Block) 8—SS Ferrule 9—Nut(SS Ferrule) 10— Ferrule(Graphite /Vespel) 11—Nut(Ferrule) Glass liner installation...

  • Page 18: Septum Installation

    Figure 2-5 Loading position of quartz wool in the glass liner (2) Install O-ring: O-ring installed onto the glass liner about 7mm from the top; put the glass liner into the nebulization chamber and push to the bottom where the ring is about 5mm from the top. (3) Fasten glass liner: Carefully tighten the fastening nut by special inlet wrench.

  • Page 19: Gc Column Installation

    Warning Do not directly touch the glass liner or septum. 2.6GC Column Installation Related consumables and tools: Part name Part No. Column 3709400080 Column cutter 3802000251 15% Graphite /85%Vespel pressure ring 304650006 Pressure ring ferrule 3010205443 Interface column nut 3041810051 Column mounting jig (for interface end use) 3010211139 Wrench (1/4 inch×5/16 inch)
  • Page 20 Figure 2-7 Column installation at the inlet end 2.6.2 MS interface end installation (1) Pass the position markers (such as old septa), pressure ring ferrule and the pressure ring through the free end of the column (as shown in Figure 2-8) in sequence.

  • Page 21: Filament Installation

    Warning When the oven and interface are heated, pressure ring will shrink slightly; it needs leakage check after one or two heating cycles. Please make sure that the MS interface has been cooled to normal temperature; disassemble the nuts at high temperature will damage the thread of MS interface. 2.7Filament installation Related consumables and tools Part name...
  • Page 22 Figure 2-9 Ion source 1—GC-MS Interface 2—Heating Assembly Terminals 3—Lens1 4—Lens2 5—Lens3 6—Sensor Terminals 7、9—Filament 8—Repeller Electrode Terminal (1) Make sure that the main power of the instrument is switched off. (2) Loosen the 4 nuts on the front panel with a sleeve; remove the front panel. (3) Use a tweezer wiped by alcohol or acetone to remove the filament lead terminal (see Figure 2-9).
  • Page 23 (1) Install the new filament and tighten the nuts. (2) Push the lead terminal into the lead pin, reconnect the filament. Warning The filament should be fully inserted and well contacted when installing, and avoid the filament wire contacting other parts.

  • Page 24: Install Ion Source Electrode Box And Repulsion Electrode

    2.8Install ion source electrode box and repulsion electrode Related consumables and tools Part name Part number Electrode holder 1 3010211123 Electrode holder 2 3010211125 Insulating ceramic 1 305301217 Repulsion electrode 3010211131 Ion source holder 3010211100 Nut M2 304050001 Flat washer M2 304070001 Flat washer M3 304070002...
  • Page 25 Figure 2-11 Ion source box and repulsion electrode 1—Ion Source Holder 2—Nut 3—Gasket(M2) 4- Ceram Gasket 5—Repeller Electrode 6—Screw 7-Gasket(M3) 8—Electrode Trestle 1 9—Electrode Trestle 2 10—Electrode Box (1) Install the parts in an upward order, as shown in Figure 2-11. (2) Put the repulsion electrode into the ion source electrode box and adjust it to situate the repulsion electrode in the center of the electrode box.

  • Page 26: Instrument Startup And Shutdown

    3. Instrument Startup and Shutdown Turn on the instrument 3.1.1 Power on (1) Start computer and printer. Start Windows. (2) Open the valve of the helium cylinder after ensuring that the pressure shown on the high pressure gauge is not lower than 3 MPa. (3) Make sure the power supply of the instrument is switched on;...
  • Page 27 (1) Click the function icon [Monitor] on the left of the software interface. Figure 3-1 the Monitor icon (2) A dialog box [System monitoring] will be displayed on the screen, as shown in Figure 3-2. Figure 3-2 System Monitoring (3) Click [Auto Start] or [Auto Shutdown], the system will start or shutdown the vacuum automatically.
  • Page 28 After clicking [Auto Start], the system will start the mechanical pump first, and then start the turbo molecular pump when the vacuum degree is below 22 mbar. If an alert of [Mechanical Pump Startup Timeout] or [Molecular Pump Startup Timeout] pops up, the instrument may have a gas leak. Please check if the O-ring is well-placed or if the screws are tightened at the places such as the front panel of the ion source, GC-MS interface, and so Click [Auto Start] again, the green indicator on the MS panel will light up...

  • Page 29: System Standby Settings

    3.1.4 Power off (1) Power off the computer, monitor and printer. (2) Switch off GC. (3) Switch off MS. (4) Close the main valve of the gas cylinder. System standby settings (1) Click [Instrument] [Standby], the instrument will switch to Standby status. (2) At the Standby status, MS turn off the detector high voltage and RF, and lower the speed of the molecular pump to less than 1000 rps while the temperature of ion source keeps at 200℃.
  • Page 30 Note If the vacuum degree does not reach 5.0E-005mbar, do not light up filament or collect data, otherwise it may shorten lifetime of filament or even cause damage to the other parts. Figure 3-3 Tuning Panel (7) If the peak intensity of the spectrum is m/z 18(H2O) ＞m/z 28(nitrogen) ＞ m/z 32(oxygen) (As shown in Figure3-3), and the nitrogen- oxygen ratio is lower than 3.7, the instrument has no gas leak.

  • Page 31: Tuning And Calibrating

    4. Tuning and calibrating Tuning the instrument is to correct the instrument, adjusting various parameters of ion source, mass analyzer and detector to acquire desired resolution, sensitivity, and accurate mass axis and the correct ion abundance ratio. One of the purposes of tuning is to know about the state of the instrument and check if the instrument runs properly and the performance can meet the specifications.

  • Page 32: Manual Tuning

    created. (7)Click [File], [Automatic tuning report] and choose tuning files to create corresponding reports if needed. Manual tuning 4.2.1 Start scanning (1) Open a tuning file, select perfluorotributylamine mode, select filament, open the tuning valve, click [Set parameters], [Start scanning]. (2) Adjust [Delay electrode voltage], [Introduce electrode voltage], [Focus electrode voltage] in turn to achieve optimal peak intensity and ratio.

  • Page 33: Calibrate Mass Number

    Figure 4-3 RF Parameter Setting Panel Calibrate mass number (1) Click [Tune], [Automatic tuning] to open the mass number calibrating page. (2) Click [Add] to add the corresponding numbers of peaks to be calibrated. (3) Enter the number 69, 131, 219 and 502 in turn in the [Calibrate peak] column. (4) Start [Tune valve].
  • Page 34 Figure 4-4 Mass Axis Calibration Panel...

  • Page 35: Method Setting

    5. Method Setting Set GC method 5.1.1 Set method on GC control panel Figure 5-1 GC Control Panel (1) Set the inlet temperature: [Inlet] – [Settings], input the temperature value you want to set, [Enter]. (2) Set the chromatographic column parameters: [Chromatographic Column] –...

  • Page 36: Set Ms Method

    (5) Click [Retrieve all], all set value on GC panel can be received by the software. (6) Click [Download all], all set value on GC panel can be r downloaded to GC. Figure 5-2 GC Method Setting Panel Set MS method (1) Click [MS Settings] to go to MS settings page, as shown in Figure 5-3.
  • Page 37 Figure 5-3 MS Settings Panel 5.2.1 Full Scan Mode (1) [Duration] plus [Solvent Cut Time] equals the total scanning time. (2) Select [Full] from [Scan Mode], set the mass range for scanning, dwell time for each point is as the default value. Figure 4-4 Full Scan 5.2.2 Selected Ion Monitoring (SIM) Scan Mode (1) Add or delete SIM segment with [Add] or [Delete].
  • Page 38 Figure 5-5 SIM Scan Mode Settings (4) The time used for one time SIM scanning T(ms)= Width10 *4* the number of mass number; under the conditions set in Figure 5-5, T=1*10*4*3=120ms, i.e. it can scan 8.3 times in 1 second. 5.2.3 Advanced settings (1) Click [Advanced Settings], click the advanced function during acquisition, as shown in Figure 5-6.

  • Page 39: Sequence

    6. Sequence Sequence Settings (1) Click [Sequence] to switch to sequence acquisition window, as shown in Figure 6-1. (2) Add sequences. (3) Set the data file information and sample information. (4) Click the Start Acquisition button on the toolbar to be ready for acquisition. (5) If GC and MS are [Not Ready], the sequence will be waiting and not enter the waiting-for-injection status until GC and MS are Ready.

  • Page 40: Sample Injection And Data Acquisition

    Sample injection and data acquisition (1) As shown in Figure 6-2, use a syringe to extract 1μL of sample, quickly insert the syringe into the inlet to the bottom, quickly inject the sample into GC and pull out the syringe quickly. Figure 6-2 Sample Injection (2) As shown in Figure 6-3, after quickly pulling out the syringe, immediately press the [Start] button on GC control panel to...

  • Page 41: Data Processing

    7. Data Processing Double-click the icon of the data analysis software on the desktop of the computer with the left mouse button, start running the data processing software. Function introduction of the menu icon on the toolbar Figure 7-1 Toolbar files, used to open data files.
  • Page 42 (1) Click the icon on the menu toolbar to open the standard and sample chromatograms and compare the retention times. If they are the same or similar, the sample peak may be the target peak, and then compare its mass spectrogram with the standard mass spectrogram, as shown in Figure 7-2.
  • Page 43 target compound in the below interface poppedup, click to check the Mass Chromatogram (MC) of the ion, as shown in Figure 7-3, 7-4. Figure 7-3 Search the Characteristic Ion Figure 7-4 MC Displayed If the shape of peak on MC diagram is similar with the chromatographic peak, and the retention times are close, that peak might be the target peak;...

  • Page 44: Remove Background

    Figure 7-5 Check Mass Spectrogram 7.3.4 Remove Background (3) Click the icon on the toolbar, press and hold the left mouse button to select a segment of straight baseline on the left or right side of the target chromatographic peak as the mean noise level, as shown in Figure 7-6.
  • Page 45 Figure 7-7 Range for Removing Background (5) Press the Shift key and hold down, click the mass spectrogram or hold the left mouse button and drag for a short distance, the mass chromatogram without background will be seen, as shown in Figure 7-8. Figure 7-8 Check Average Spectrum 7.3.5 Spectral Library Search (6) Click the right mouse button on the centroidal mass...
  • Page 46 Figure 7-9 Search from NIST and Preview (7) Click the right mouse button on the mass spectrogram or integral component and select [Register to Qualitative Table]. Click the icon to open the Qualitative Table where batch searching from NIST library can be performed. Double-click to check the search results.

  • Page 47: Quantitative Analysis

    Figure 7-11 Index Search (9) Select an index database. (10)Conduct search according to [Name and Synonym], [Molecular Weight], [Chemical Formula], [CAS Number] or [NIST Library Number] in the dialog box of [Edit Database]; as shown in the below Figure, search the matter with CAS Number 64-17-5 . Figure 7-12 Index Search 7.4 Quantitative Analysis...
  • Page 48 Figure 7-13 Integration Toolbar 7.4.1 Automatic Integration (11) Click the icon, and users can set Automatic Integration parameters in the dialog box as required, as shown in Figure7-14. Figure 7-14 Parameter Settings for Automatic Integration 7.4.2 Manual Integration (12) Click the baseline icon. (13) Click the start point and end point of chromatogram peak respectively, as shown in Figure 7-15.
  • Page 49 Figure 7-15 Manual Integration The following is the introduction of other icons on the Integration toolbar: Split the chromatogram which cannot be completely separated. Slash shoulder peak and perform integration. Delete integration of selected chromatographic peak: click the icon and the selected integration will be deleted. Delete all integration data andcomponents data.
  • Page 50 Figure 7-16 Quantitative Analysis Guide (2)Select a data file and click [Add] to add it to the below textbox. (3)Select a data file in the below textbox, press the Delete key on the keyboard to delete the selected file. (4)Under the Quantitative mode, TIC or corresponding quantitative ions can be selected in the [Quantitative Ion] box.
  • Page 51 (9)Enter [Sample Weight], [Dilution Ratio]. (10)Click [Start Analysis], and the standard curve window will pop up, as shown in Figure 7-18. Figure 7-18 the Curve- External Standard Method (11)Click icon on the upper right corner of the window, the unknown sample can be added to the standard curve for analysis.
  • Page 52 Figure 7-17 Internal Standard Method (2)[Calculating Method], select [Internal Standard]. (3)Select [Internal Standard Matter], and input the concentration of non- internal-standard matter in the standard sample. (4)Click [Start Calculating], and the result is as shown in the below figure. Figure 7-20 the Curve- Internal Standard Method...

  • Page 53: Functions Of Other Icons

    7.5 Functions of other icons Comparison of mass chromatograms: if the button is selected, the newly opened mass chromatogram will be added to current TIC diagram directly. If the button is not selected, the newly opened mass chromatogram will be shown separately in a new window.
  • Page 54 Display the next mass spectrum: click to display the next one mass spectrum according to the current retention time. The way of display is similar to the above. (10) Annotation switch, click to switch the peak point to display the peak area. (11) Annotation of area, time, name and ratio.

  • Page 55: Analysis Report

    8. Analysis Report Print Report （1） Click in the menu bar and enter the print interface, as shown in Figure 8-1: Figure 8-1 Print Report （2） Select the data file: here you can select the data file you want to print. Click to change the file directory.
  • Page 56 to open it; drag the template tab into EXCEL, as shown in Figure 8-2: Figure 8-2 Report Template a) SampleInfor: basic information of the sample. b) GC Param/MS Param: basic parameters of GC and MS. c) Chromatogram Info: the related information of chromatogram. d) MassInfor: the related information of mass spectrogram.

  • Page 57: Trouble Shooting

    1. GC power is not well connected. 1. Check the power supply of GC. display and the oven fan has no response. 2. Replace the fuses. Contact Drawell after-sales service 2. Fuses of GC main power are blown. department for details.
  • Page 58 Contact Drawell after-sales service department. 1. Open the panel of tuned liquid on MS to check its amount. 1. Short of tuned liquid. 2. If the tuned liquid runs out, please contact Drawell after-sales There is no PFTBA peak while tuning. service department.

  • Page 59: Appendix 1: Pftba Mass Fragment Information Table

    Appendix 1: PFTBA Mass Fragment Information Table Figure 10-1 Standard Mass Spectrum of PFTBA/FC43 Table 10-1 MS Data of PFTBA/FC43 Relative Intensity Relative Intensity 49.99379 0.73 218.9856 38.07 68.99518 225.9903 0.56 92.99518 0.56 230.9856 0.47 99.99358 6.31 263.98705 8.38 113.99669 2.34 313.98386 0.32...
  • Page 60 Drawell International Technology Limited Chongqing Drawell Instrument Co., Ltd. Shanghai Drawell Scientific Instrument Co.,Ltd. Chongqing Center : Suite 2705,Building No.12,Shiyou Road No.1, Yuzhong District, Chongqing, China. Shanghai Office : Suite 1117,Lane561 XiuChuan Rd.,PuDong New Area,Shanghai,China Homepage : www.drawell.com.cn Tel : 0086-023-63268643...

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