Mass spectrometry has high sensitivity and resolution, and it has great advantages in qualitative and quantitative. Therefore, there are more and more laboratories that configure mass spectrometry. Compared with chromatogram, mass spectrometry requires extremely high environmental requirements, operation and Maintenance is also more frequent.
There are many types of mass spectrometers, and the working principle and application range are also very different. From the application point of view, mass spectrometers can be divided into the following categories:
1. Organic mass spectrometer <br> Due to different application characteristics, it is divided into:
1 gas chromatography-mass spectrometer (GC-MS)
In this kind of instrument, due to the different working principle of the mass spectrometer, there are gas chromatography-quadrupole mass spectrometer, gas chromatography-time-of-flight mass spectrometer, gas chromatography-ion trap mass spectrometer and so on.
2 liquid chromatography-mass spectrometer (LC-MS)
Similarly, there are liquid chromatography-quadrupole mass spectrometers, liquid chromatography-ion trap mass spectrometers, liquid chromatography-time-of-flight mass spectrometers, and various liquid chromatography-mass spectrometry-mass spectrometers.
3 Other organic mass spectrometers are: matrix-assisted laser desorption time-of-flight mass spectrometry (MALDI-TOFMS), Fourier transform mass spectrometer (FT-MS)
2. Inorganic mass spectrometer <br> Includes: spark source dual focus mass spectrometer.
Inductively Coupled Plasma Mass Spectrometer (ICP-MS).
Secondary ion mass spectrometer (SI-MS)
In addition to the above classification, the mass spectrometer can be divided into a dual focus mass spectrometer, a quadrupole mass spectrometer, a time-of-flight mass spectrometer, an ion trap mass spectrometer, a Fourier transform mass spectrometer, and the like, depending on the mass analyzer used in the mass spectrometer.
Mass spectrometer maintenance tips
Environmental requirements for the mass spectrometer:
1 There is no strong oscillation source and electromagnetic induction device around;
2 power requirements are grounded AC;
3 room temperature requirements: 15-28 ° C;
4 relative humidity requirements: 20% ~ 80%;
It can be seen that special attention should be paid to the control of indoor temperature and humidity during use. Generally, the time-of-flight mass spectrometer without an external flight tube has stricter requirements on the environment, and the external environment directly affects the accuracy of the mass axis. The mass spectrometer uses a two-stage pumping structure, the front stage is a mechanical pump, and the latter stage is a molecular turbo pump. When working, the pressure in the vacuum chamber is reduced by several orders of magnitude by the foreline pump, and then the post-stage pump is reduced to the required pressure.
1. Boot:
The mass spectrometer is turned on first, then the mechanical pump is turned on, and then the power of the mass spectrometer is turned on. After the vacuum is reached, the molecular turbo pump is turned on, and the calibration can be performed after the vacuum is reached. Generally, at least 12 hours are required. achieve. The mass spectrometer can only be used after each turn-on.
2. Sample testing process:
When used in combination with liquid chromatography, the mobile phase needs to be first filtered with a membrane. The organic membrane and the water membrane need to be distinguished. The sample also needs to be filtered or centrifuged at >10000 rpm to remove solid impurities.
The mobile phase cannot use difficult-to-volatile acids or salts, such as phosphates and borate. TFA, which is commonly used in liquid phase, inhibits ionization and is not recommended. Surfactants have high response in mass spectrometry, especially ESI sources. Therefore, all tubes and utensils cannot be cleaned with detergent. Ion pairing reagents used to improve separation and peak shape should also be used with caution. For use with mass spectrometry, it is recommended to use formic acid, acetic acid, ammonium formate, ammonium acetate and ammonia. Wait.
According to the selected ion source adjustment liquid phase method, the ESI source is generally 0.3-0.6mL/min. The specification of the conventional HPLC analysis column is 5μm, 4.6×250mm, the general flow rate is 1mL/min, and the post-column split mode can be adopted. To adjust the flow into the mass spectrum. At the same time, the atomizing gas temperature and the atomizing gas flow rate are adjusted according to the flow rate into the mass spectrometer and the nature of the sample.
After the sample test is finished, the injection line needs to be cleaned, and the pump is stopped after cleaning. After the temperature of the ion source is lowered, the standby state is selected.
3. Daily regular maintenance:
In the early stage, the mechanical pump will enter the pump with the detection of the sample. It is necessary to periodically open the vibration valve for about 20 minutes, and the vibration time should not be too long. Too long will cause the pump oil to consume too fast. It is recommended to adjust the frequency of the earthquake according to the amount of detection. It is generally recommended once a week.
The ion source chamber and the sampling cone and the cover are cleaned with dust-free paper and 50% methanol water, usually once a week.
The pump oil of the mechanical pump needs to be replaced regularly. It is usually replaced once every six months. If the pump oil looks dirty, it needs to be replaced in advance. When replacing the pump oil, all the pump oil needs to be poured out, and then the new pump oil is replaced. The pump oil of different brands cannot be mixed. General laboratory mass spectrometers perform large maintenance during long vacations.
In general, except for the replacement of the pump oil, it is not necessary to carry out the vacuum discharge. The internal cleaning and maintenance of the mass spectrometer is generally less. It is recommended to be handed over to the maintenance engineer for the internal metal parts. To polish, other components should be careful not to touch organic reagents, especially seals and the like.
4. Shutdown:
To shut down, you need to vent, vent the system, and then turn off the mechanical pump.
MS operation instructions and precautions
MS operation instructions and daily use precautions:
1. Boot
1) Turn on the main power, turn on the bypass pump power, and turn on the capillary heater (CPS).
2) Observe the pressure display panel, use the ▲▼ arrows to adjust the black bar display position to adjust to the Turbo Back option, press the enter key twice (〇) to turn on the turbo molecular pump and the background pump; press the return key (〓) to return Main panel. Observe the Turbo progress to get it to work (black bars to the end). Press the ▼ arrow to adjust to the AIMX option and observe the pressure display so that it is below 1*10-6. Zui Jia work pressure is 5*10-6 or less.
3) After the pressure reaches the requirement, open the control box (RC Interface), hear a drop, and open the MA soft software to start the experiment setup.
2. Software operation
1) New file: File-New File creates a new file, the main window appears;
2) Check the parameters in Global: RGA and Shutdown, confirm the filament status, click on the Global: RGA filament, and the filament is completely extinguished in Shutdown, select OK;
3) Double-click Scan mass to select the experiment mode. There are three modes: Bar, Profile and MID. Bar or Profile is used for full-spectrum scanning. Generally, the profile can be used to adjust the scanning rate and accuracy. MID mode for scanning for a specific mass. When using Profile mode, the scan range can be selected. When a segmented scan is required, first select Scan mass and click on the option on the toolbar to add a channel.
4) When selecting different detectors for different scanning ranges, double-click the detector unit and a dialog box appears. Select different monitors according to the gas pressure range. The pressure range of the Faraday detector is: 1*10-5-10-10 The pressure range of the SEM detector is: 1*10-7-10-14.
5) Select Scan mass, hold down Ctrl to select multiple, click New Graph View, and the scan window appears.
6) Light up the filament and observe the status of the filament on the control box. When the filament is on, click the green start button to start scanning.
Note: The two filaments cannot be turned on at the same time. Do not click on the Degas analysis Source. It is easy to burn the filament. Please contact the company engineer before clicking this button.
7) When you need to view the number of cycles, you can select the Scan window to view, right click and select Mode-Historical data. When you need to convert to the current scan window, select Real time.
8) When the scan ends, click the yellow light to end the current cycle and stop, and the red light will stop scanning immediately.
9) Select the path to save the data File-Save As, you can export the Excel data File-Export-File
10) Format selectable curve color: Views—Trend View setup; The window form can be changed in Windows.
11) In the Edit-Library-compound, you can view the peak content map of each substance. Click New to add a new substance.
12) Double-click Repeated, a dialog box appears (Scan structure Cycles), "Shutdown after Scanning" indicates the status of the filament. If you squat in front of the box, it means that the experiment filament is automatically turned off; if not, it means There is no need to open the filament for the next experiment.
3. Shutdown
1) Close the MAS soft software and close the control box.
2) Turn off the pump, use the ▲▼ arrows to adjust the black bar display position to adjust to the Turbo Back option, press the enter key twice (〇) to turn off the turbo molecular pump and the background pump; press the return key (〓) to return to the main panel. Observe the progress of the Turbo. When you hear the sound of the turbo molecular pump deflation, observe the black bar progress and confirm that the molecular pump is completely closed (the black bars are not). Turn off the CPS, turn off the bypass pump, and turn off the main power.
4. Note:
1) During the experiment, do not use soap bubbles to check the gas path, including your own gas path. It must be disconnected from the mass spectrometer when inspecting. (It is very important. Many mass spectrometers are caused by students using soap bubbles to detect leaks. Can't continue to use);
2) Under normal circumstances, the mass spectrometer should be kept in normal operation, unless it is used for more than 15 days. Because mass spectrometry requires a certain amount of time to stabilize (more than 24h), frequent switching mass spectrometry can also accelerate vacuum gauge contamination. In case of a power outage, please turn off the mass spectrum in advance.
3) Replacement of pump oil: Always observe the color of the pump oil and replace it immediately when it turns yellowish brown. If the instrument is used frequently and the gas is dirty, it is required to be replaced at least once every six months, and the amount of oil added does not exceed the uppermost level.
4) QIC20 heat-dissipating filter should be cleaned regularly (clean every two months). When using the air-conditioned room in summer, open the top cover as much as possible to prevent the heat from being affected.
5) When the capillary is not connected to the external instrument, do not place it directly on the dirty table, and place it as far as possible. The filter inside the capillary should be cleaned regularly, so be careful not to lose parts during the disassembly process.
6) During the transportation of the instrument, if there is an oil pump, it is necessary to release the pump oil (some nets can be used after collection), and the RF head is removed and transported separately.
The National Standard Material Resource Platform lists the national standard materials and the standards, reference materials and chemical reagents developed by the company, which facilitates the customer's inquiry of standard substances and chemical reagents! All the orders received were changed from door-to-door to express delivery, which not only speeded up the use of products by foreign customers, but also standardized the internal warehouse structure! Make the purchase of one-stop standard materials more accurate and efficient!
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There are many types of mass spectrometers, and the working principle and application range are also very different. From the application point of view, mass spectrometers can be divided into the following categories:
1. Organic mass spectrometer <br> Due to different application characteristics, it is divided into:
1 gas chromatography-mass spectrometer (GC-MS)
In this kind of instrument, due to the different working principle of the mass spectrometer, there are gas chromatography-quadrupole mass spectrometer, gas chromatography-time-of-flight mass spectrometer, gas chromatography-ion trap mass spectrometer and so on.
2 liquid chromatography-mass spectrometer (LC-MS)
Similarly, there are liquid chromatography-quadrupole mass spectrometers, liquid chromatography-ion trap mass spectrometers, liquid chromatography-time-of-flight mass spectrometers, and various liquid chromatography-mass spectrometry-mass spectrometers.
3 Other organic mass spectrometers are: matrix-assisted laser desorption time-of-flight mass spectrometry (MALDI-TOFMS), Fourier transform mass spectrometer (FT-MS)
2. Inorganic mass spectrometer <br> Includes: spark source dual focus mass spectrometer.
Inductively Coupled Plasma Mass Spectrometer (ICP-MS).
Secondary ion mass spectrometer (SI-MS)
In addition to the above classification, the mass spectrometer can be divided into a dual focus mass spectrometer, a quadrupole mass spectrometer, a time-of-flight mass spectrometer, an ion trap mass spectrometer, a Fourier transform mass spectrometer, and the like, depending on the mass analyzer used in the mass spectrometer.
Mass spectrometer maintenance tips
Environmental requirements for the mass spectrometer:
1 There is no strong oscillation source and electromagnetic induction device around;
2 power requirements are grounded AC;
3 room temperature requirements: 15-28 ° C;
4 relative humidity requirements: 20% ~ 80%;
It can be seen that special attention should be paid to the control of indoor temperature and humidity during use. Generally, the time-of-flight mass spectrometer without an external flight tube has stricter requirements on the environment, and the external environment directly affects the accuracy of the mass axis. The mass spectrometer uses a two-stage pumping structure, the front stage is a mechanical pump, and the latter stage is a molecular turbo pump. When working, the pressure in the vacuum chamber is reduced by several orders of magnitude by the foreline pump, and then the post-stage pump is reduced to the required pressure.
1. Boot:
The mass spectrometer is turned on first, then the mechanical pump is turned on, and then the power of the mass spectrometer is turned on. After the vacuum is reached, the molecular turbo pump is turned on, and the calibration can be performed after the vacuum is reached. Generally, at least 12 hours are required. achieve. The mass spectrometer can only be used after each turn-on.
2. Sample testing process:
When used in combination with liquid chromatography, the mobile phase needs to be first filtered with a membrane. The organic membrane and the water membrane need to be distinguished. The sample also needs to be filtered or centrifuged at >10000 rpm to remove solid impurities.
The mobile phase cannot use difficult-to-volatile acids or salts, such as phosphates and borate. TFA, which is commonly used in liquid phase, inhibits ionization and is not recommended. Surfactants have high response in mass spectrometry, especially ESI sources. Therefore, all tubes and utensils cannot be cleaned with detergent. Ion pairing reagents used to improve separation and peak shape should also be used with caution. For use with mass spectrometry, it is recommended to use formic acid, acetic acid, ammonium formate, ammonium acetate and ammonia. Wait.
According to the selected ion source adjustment liquid phase method, the ESI source is generally 0.3-0.6mL/min. The specification of the conventional HPLC analysis column is 5μm, 4.6×250mm, the general flow rate is 1mL/min, and the post-column split mode can be adopted. To adjust the flow into the mass spectrum. At the same time, the atomizing gas temperature and the atomizing gas flow rate are adjusted according to the flow rate into the mass spectrometer and the nature of the sample.
After the sample test is finished, the injection line needs to be cleaned, and the pump is stopped after cleaning. After the temperature of the ion source is lowered, the standby state is selected.
3. Daily regular maintenance:
In the early stage, the mechanical pump will enter the pump with the detection of the sample. It is necessary to periodically open the vibration valve for about 20 minutes, and the vibration time should not be too long. Too long will cause the pump oil to consume too fast. It is recommended to adjust the frequency of the earthquake according to the amount of detection. It is generally recommended once a week.
The ion source chamber and the sampling cone and the cover are cleaned with dust-free paper and 50% methanol water, usually once a week.
The pump oil of the mechanical pump needs to be replaced regularly. It is usually replaced once every six months. If the pump oil looks dirty, it needs to be replaced in advance. When replacing the pump oil, all the pump oil needs to be poured out, and then the new pump oil is replaced. The pump oil of different brands cannot be mixed. General laboratory mass spectrometers perform large maintenance during long vacations.
In general, except for the replacement of the pump oil, it is not necessary to carry out the vacuum discharge. The internal cleaning and maintenance of the mass spectrometer is generally less. It is recommended to be handed over to the maintenance engineer for the internal metal parts. To polish, other components should be careful not to touch organic reagents, especially seals and the like.
4. Shutdown:
To shut down, you need to vent, vent the system, and then turn off the mechanical pump.
MS operation instructions and precautions
MS operation instructions and daily use precautions:
1. Boot
1) Turn on the main power, turn on the bypass pump power, and turn on the capillary heater (CPS).
2) Observe the pressure display panel, use the ▲▼ arrows to adjust the black bar display position to adjust to the Turbo Back option, press the enter key twice (〇) to turn on the turbo molecular pump and the background pump; press the return key (〓) to return Main panel. Observe the Turbo progress to get it to work (black bars to the end). Press the ▼ arrow to adjust to the AIMX option and observe the pressure display so that it is below 1*10-6. Zui Jia work pressure is 5*10-6 or less.
3) After the pressure reaches the requirement, open the control box (RC Interface), hear a drop, and open the MA soft software to start the experiment setup.
2. Software operation
1) New file: File-New File creates a new file, the main window appears;
2) Check the parameters in Global: RGA and Shutdown, confirm the filament status, click on the Global: RGA filament, and the filament is completely extinguished in Shutdown, select OK;
3) Double-click Scan mass to select the experiment mode. There are three modes: Bar, Profile and MID. Bar or Profile is used for full-spectrum scanning. Generally, the profile can be used to adjust the scanning rate and accuracy. MID mode for scanning for a specific mass. When using Profile mode, the scan range can be selected. When a segmented scan is required, first select Scan mass and click on the option on the toolbar to add a channel.
4) When selecting different detectors for different scanning ranges, double-click the detector unit and a dialog box appears. Select different monitors according to the gas pressure range. The pressure range of the Faraday detector is: 1*10-5-10-10 The pressure range of the SEM detector is: 1*10-7-10-14.
5) Select Scan mass, hold down Ctrl to select multiple, click New Graph View, and the scan window appears.
6) Light up the filament and observe the status of the filament on the control box. When the filament is on, click the green start button to start scanning.
Note: The two filaments cannot be turned on at the same time. Do not click on the Degas analysis Source. It is easy to burn the filament. Please contact the company engineer before clicking this button.
7) When you need to view the number of cycles, you can select the Scan window to view, right click and select Mode-Historical data. When you need to convert to the current scan window, select Real time.
8) When the scan ends, click the yellow light to end the current cycle and stop, and the red light will stop scanning immediately.
9) Select the path to save the data File-Save As, you can export the Excel data File-Export-File
10) Format selectable curve color: Views—Trend View setup; The window form can be changed in Windows.
11) In the Edit-Library-compound, you can view the peak content map of each substance. Click New to add a new substance.
12) Double-click Repeated, a dialog box appears (Scan structure Cycles), "Shutdown after Scanning" indicates the status of the filament. If you squat in front of the box, it means that the experiment filament is automatically turned off; if not, it means There is no need to open the filament for the next experiment.
3. Shutdown
1) Close the MAS soft software and close the control box.
2) Turn off the pump, use the ▲▼ arrows to adjust the black bar display position to adjust to the Turbo Back option, press the enter key twice (〇) to turn off the turbo molecular pump and the background pump; press the return key (〓) to return to the main panel. Observe the progress of the Turbo. When you hear the sound of the turbo molecular pump deflation, observe the black bar progress and confirm that the molecular pump is completely closed (the black bars are not). Turn off the CPS, turn off the bypass pump, and turn off the main power.
4. Note:
1) During the experiment, do not use soap bubbles to check the gas path, including your own gas path. It must be disconnected from the mass spectrometer when inspecting. (It is very important. Many mass spectrometers are caused by students using soap bubbles to detect leaks. Can't continue to use);
2) Under normal circumstances, the mass spectrometer should be kept in normal operation, unless it is used for more than 15 days. Because mass spectrometry requires a certain amount of time to stabilize (more than 24h), frequent switching mass spectrometry can also accelerate vacuum gauge contamination. In case of a power outage, please turn off the mass spectrum in advance.
3) Replacement of pump oil: Always observe the color of the pump oil and replace it immediately when it turns yellowish brown. If the instrument is used frequently and the gas is dirty, it is required to be replaced at least once every six months, and the amount of oil added does not exceed the uppermost level.
4) QIC20 heat-dissipating filter should be cleaned regularly (clean every two months). When using the air-conditioned room in summer, open the top cover as much as possible to prevent the heat from being affected.
5) When the capillary is not connected to the external instrument, do not place it directly on the dirty table, and place it as far as possible. The filter inside the capillary should be cleaned regularly, so be careful not to lose parts during the disassembly process.
6) During the transportation of the instrument, if there is an oil pump, it is necessary to release the pump oil (some nets can be used after collection), and the RF head is removed and transported separately.
The National Standard Material Resource Platform lists the national standard materials and the standards, reference materials and chemical reagents developed by the company, which facilitates the customer's inquiry of standard substances and chemical reagents! All the orders received were changed from door-to-door to express delivery, which not only speeded up the use of products by foreign customers, but also standardized the internal warehouse structure! Make the purchase of one-stop standard materials more accurate and efficient!
Http://
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