CN102446692B - Mass spectrum analyzer with online cleaning function and working method of mass spectrum analyzer - Google Patents
Mass spectrum analyzer with online cleaning function and working method of mass spectrum analyzer Download PDFInfo
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- CN102446692B CN102446692B CN201110284595.4A CN201110284595A CN102446692B CN 102446692 B CN102446692 B CN 102446692B CN 201110284595 A CN201110284595 A CN 201110284595A CN 102446692 B CN102446692 B CN 102446692B
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- quadrupole rod
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- 238000004140 cleaning Methods 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims description 32
- 238000001819 mass spectrum Methods 0.000 title abstract 5
- 238000005040 ion trap Methods 0.000 claims abstract description 69
- 239000000126 substance Substances 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 238000000534 ion trap mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
The invention provides a mass spectrum analyzer with an online cleaning function, which comprises an ion trap, a radio frequency power supply, a vacuum unit and a control unit, wherein the radio frequency power supply is used for applying a constant voltage to the ion trap when in a cleaning state, and applying a constant voltage to the ion trap when in a working state; the vacuum unit is used for enabling the ion trap to be maintained in a low-vacuum state when in a cleaning state so as to ensure that an electrode of the ion trap generates plasma discharge when in the constant-voltage and low-vacuum state and enabling the ion trap to be maintained to be in a high-vacuum state when in the working state; and the control unit is used for selectively enabling the mass spectrum analyzer to be in a cleaning state, an idle state and a working state. The mass spectrum analyzer has the advantages of good cleaning effect, convenience for implementation, high automation degree and the like.
Description
Technical field
The present invention relates to the cleaning of mass spectrometer, particularly there is mass spectrometer and the method for work of function of on-line cleaning.
Background technology
Ion trap is a kind of mass analyzer of function admirable, the basic principle that it carries out quality analysis be first by the ion binding of different mass-to-charge ratioes in ion trap, then by electric field action, the ion of different mass-to-charge ratioes is distinguished out, reach the object of quality analysis.Ion strap mass analyzer have little, the easy processing of volume, to vacuum degree require low, maintenance cost is low, highly sensitive and can carry out the many merits such as multi-stage ms analysis, therefore, be widely used in various mass spectrometers based on ion strap mass analyzer, particularly miniaturization or portable mass spectrometer.
Although ion trap has numerous advantages, also there are some defects in it, and particularly ion trap surface is easily polluted at work, as adsorb some organic substances etc.Ion trap surface contamination meeting brings chemical noises to become the problems such as large, sensitivity and charge accumulated, has a strong impact on the performance of ion strap mass analyzer.
Traditional desk-top ion trap mass spectrometer adopts periodic cleaning ion trap to guarantee mass spectrometric sensitivity conventionally; ion trap is cleaned and need to be carried out a series of operation, and comprising that ion trap mass spectrometer is shut down with emptying vacuum, dismounting ion strap mass analyzer, ultrasonic cleaning, ion strap mass analyzer assembling, instrument restores, again vacuumizes and roasting trap etc.
The subject matter that the method for above-mentioned cleaning ion trap exists is:
1, dismounting ion trap needs complicated and loaded down with trivial details operation need to expend the plenty of time, and also higher to operating personnel's requirement.
2, use ultrasonic cleaning cannot remove the organic substance that some adsorptivities are very strong completely, may cause cleaning not thorough, cannot make instrument reach optimum state.
3, need auxiliary cleaning equipment and a large amount of cleaning fluid and solvents etc.
4, to small spectrometer, particularly portable mass spectrometer, its integrated level is very high, and dismounting ion strap mass analyzer is often very difficult, and concerning the client of use portable mass spectrometer, carrying out above-mentioned loaded down with trivial details operation is almost impossible mission.
summary of the invention
In order to solve the deficiency in above-mentioned prior art scheme, the invention provides that a kind of cleaning performance is good, convenient, the mass spectrometer of automation, also provide that a kind of cleaning performance is good, convenient, the method for work of the mass spectrometer of automation.
The object of the invention is to be achieved through the following technical solutions:
Have the mass spectrometer of function of on-line cleaning, described mass spectrometer comprises ion trap or quadrupole rod, and described mass spectrometer further comprises:
Radio-frequency power supply, described radio-frequency power supply for being that the electrode of ion trap or quadrupole rod applies high frequency voltage in the time that mass spectrometer is in running order; Apply constant voltage in the time cleaning state at mass spectrometer the electrode of described ion trap or quadrupole rod;
Vacuum unit, described vacuum unit is used for making described ion trap or quadrupole rod maintain low vacuum state in the time of the state of cleaning, thereby make the electrode of described ion trap or quadrupole rod, in the time of described constant voltage, low vacuum state, plasma discharge occur, and make described ion trap or quadrupole rod maintain high vacuum state in working order time;
Control personnel equipment, described control personnel equipment is for optionally making described mass spectrometer in cleaning state, operating state and idle condition.
According to above-mentioned mass spectrometer, preferably, the pressure limit of described low vacuum state is 10-1000mTorr.
According to above-mentioned mass spectrometer, preferably, the radio-frequency voltage that described constant voltage is constant amplitude, voltage range is 100-1000 volt.
According to above-mentioned mass spectrometer, alternatively, described mass spectrometer further comprises:
Timing personnel equipment, described timing personnel equipment is used for setting time started and the duration of cleaning state, and is sent to described control personnel equipment.
According to above-mentioned mass spectrometer, alternatively, described mass spectrometer further comprises:
Judgement personnel equipment, whether the described personnel's of judgement equipment is for according to discharging between electrode or whether whether the chemical noises of mass spectrometer exceed that threshold value determines should be in cleaning state, and judged result is sent to described control personnel equipment.
According to above-mentioned mass spectrometer, alternatively, described radio-frequency power supply is only a radio-frequency power supply, or is respectively described electrode the first radio-frequency power supply and the second source of high frequency voltage and constant voltage is provided.
According to above-mentioned mass spectrometer, alternatively, described vacuum unit is only a vacuum unit, or is respectively described ion trap or quadrupole rod and maintains the first vacuum unit and second vacuum unit of low vacuum state and high vacuum state.
Object of the present invention is also achieved by the following technical programs:
Have the method for work of the mass spectrometer of function of on-line cleaning, described method of work is:
Under the selection of the personnel of control equipment, described mass spectrometer is in on-line cleaning state, ion trap or quadrupole rod that radio-frequency power supply is mass spectrometer provide constant voltage, vacuum unit makes described ion trap or quadrupole rod maintain low vacuum state, make the electrode generation plasma discharge of described ion trap or quadrupole rod, thereby cleaned described electrode;
Under the selection of described control personnel equipment, described mass spectrometer is in running order, and described radio-frequency power supply provides high frequency voltage for described ion trap or quadrupole rod, and described vacuum unit is that described ion trap or quadrupole rod maintain high vacuum state.
According to above-mentioned method of work, preferably, the pressure limit of described low vacuum state is 10-1000mTorr.
According to above-mentioned method of work, preferably, the radio-frequency voltage that described constant voltage is constant amplitude, voltage range is 100-1000 volt.
According to above-mentioned method of work, alternatively, described method of work further comprises determining step:
Judge whether personnel's equipment is according to discharging between described electrode or whether the chemical noises of mass spectrometer exceedes that threshold value determines whether should be in cleaning state, and judged result is sent to described control personnel equipment.
According to above-mentioned method of work, alternatively, described method of work further comprises timing step:
On timing personnel equipment, set time started and the duration of described cleaning state, the output signal of timing personnel equipment is sent to described control personnel equipment.
Compared with prior art, the beneficial effect that the present invention has is:
1, without dismounting ion trap mass spectrometry instrument and mass analyzer, save a large amount of human and material resources and time.
2, cleaning process automatically realizes completely on instrument, without any external equipment and reagent.
3, make ion trap mass spectrometer user maintenance tool become very convenient, can realize small spectrometer that integrated level is high or cleaning and the maintenance of portable mass spectrometer intermediate ion trap simultaneously, the method before using may realize hardly.
4, plasma cleaning method is more effectively removed the pollutant of ion trap adsorption than ultrasonic cleaning method.
Accompanying drawing explanation
With reference to accompanying drawing, disclosure of the present invention will be easier to understand.Those skilled in the art hold intelligible: these accompanying drawings are only for illustrating technical scheme of the present invention, and are not intended to protection scope of the present invention to be construed as limiting.In figure:
Fig. 1 is the basic block diagram of mass spectrometer in embodiments of the invention.
Embodiment
Fig. 1 and following declarative description optional execution mode of the present invention how to implement and to reproduce the present invention with instruction those skilled in the art.In order to instruct technical solution of the present invention, simplify or omitted some conventional aspects.Those skilled in the art should understand that be derived from these execution modes modification or replace will be within the scope of the invention.Those skilled in the art should understand that following characteristics can combine to form multiple modification of the present invention in every way.Thus, the present invention is not limited to following optional execution mode, and is only limited by claim and their equivalent.
Embodiment 1:
Fig. 1 has schematically provided the basic block diagram of the mass spectrometer with function of on-line cleaning of the embodiment of the present invention.As shown in Figure 1, described mass spectrometer comprises:
Ion trap or quadrupole rod, these are state of the art, do not repeat them here.
Radio-frequency power supply, described radio-frequency power supply for being that the electrode of ion trap or quadrupole rod applies high frequency voltage in the time that mass spectrometer is in running order; Apply constant voltage in the time cleaning state at mass spectrometer the electrode of described ion trap or quadrupole rod;
Alternatively, the radio-frequency power supply that described radio-frequency power supply can only use existing mass spectrometer to be equipped with, be respectively described electrode high frequency voltage and constant voltage are provided, can certainly on the basis of original radio-frequency power supply that high frequency voltage is provided, add another provides the radio-frequency power supply of constant voltage for described electrode.Concrete radio-frequency power supply is the state of the art, does not repeat them here.
Vacuum unit, described vacuum unit is used for making described ion trap or quadrupole rod maintain low vacuum state in the time of the state of cleaning, thereby make the electrode of described ion trap or quadrupole rod, in the time of described constant voltage, low vacuum state, plasma discharge occur, and make described ion trap or quadrupole rod maintain high vacuum state in working order time;
Alternatively, the vacuum unit that described vacuum unit can only use existing mass spectrometer to be equipped with, be respectively described mass spectrometer low vacuum and high vacuum are provided, can certainly on the basis of original vacuum unit that high vacuum is provided, add another provides the vacuum unit of low vacuum for described mass spectrometer.Concrete vacuum unit is the state of the art, does not repeat them here.
Preferably, the pressure limit of described low vacuum state is 10-1000mTorr.
Preferably, the radio-frequency voltage that described constant voltage is constant amplitude, voltage range is 100-1000 volt.
Control personnel equipment, described control personnel equipment is for optionally making described mass spectrometer in cleaning state, operating state and idle condition, adjust the operating state of described radio-frequency power supply and vacuum unit by controlling personnel's equipment (as the height of the vacuum degree of the height of radio-frequency power supply output voltage, vacuum unit realization, whether work), thus make mass spectrometer in above-mentioned three kinds of states.Above-mentioned control personnel equipment can be realized or circuit, software are realized above-mentioned selection by attendant.
Alternatively, described mass spectrometer further comprises:
Timing personnel equipment, described timing personnel equipment is used for setting time started and the duration of cleaning state, and is sent to described control personnel equipment.Can realize or circuit, software are realized above-mentioned selection by attendant.
Alternatively, described mass spectrometer further comprises:
Judgement personnel equipment, whether the described personnel's of judgement equipment is for according to discharging between electrode or whether whether the chemical noises of mass spectrometer exceed that threshold value determines should be in cleaning state, and judged result is sent to described control personnel equipment.Described threshold value is to set flexibly according to the user's of the requirement of standard or mass spectrometer acceptable degree.Can realize or circuit, software are realized above-mentioned selection by attendant.
The present embodiment has also disclosed the method for work of mass spectrometer, and described method of work is:
Under the selection of the personnel of control equipment, described mass spectrometer is in on-line cleaning state, ion trap or quadrupole rod that radio-frequency power supply is mass spectrometer provide constant voltage, vacuum unit makes described ion trap or quadrupole rod maintain low vacuum state, make the electrode generation plasma discharge of described ion trap or quadrupole rod, thereby cleaned described electrode;
Preferably, the pressure limit of described low vacuum state is 10-1000mTorr.
Preferably, the radio-frequency voltage that described constant voltage is constant amplitude, voltage range is 100-1000 volt.
Under the selection of described control personnel equipment, described mass spectrometer is in running order, and described radio-frequency power supply provides high frequency voltage for described ion trap or quadrupole rod, and described vacuum unit is that described ion trap or quadrupole rod maintain high vacuum state.
Alternatively, described method of work further comprises determining step:
Judge that personnel's equipment is according to whether discharging between described electrode or whether the chemical noises of mass spectrometer exceedes that threshold value determines whether should be in cleaning state, judged result is sent to described control personnel equipment, to automatically start when needed function of on-line cleaning.
Alternatively, described method of work further comprises timing step:
On timing personnel equipment, set time started and the duration of described cleaning state, the output signal of timing personnel equipment is sent to described control personnel equipment, so that the personnel of control equipment optionally makes mass spectrometer automatically in cleaning state.
The benefit reaching according to the embodiment of the present invention is: can use the original radio-frequency power supply of mass spectrometer to provide constant voltage for electrode, and use the original vacuum unit of mass spectrometer that low vacuum state is provided, to realize function of on-line cleaning, creatively utilize device of the prior art to go to realize new function.Without dismounting, without using cleaning agent to clean, really realize on-line auto-cleaning function, cleaning performance is good.
Embodiment 2:
The application examples in VOC detects according to the mass spectrometer of the embodiment of the present invention 1 and method of work, as the detection of benzene homologues.Mass spectrometer adopts ion trap, only adopt a radio-frequency power supply, electrode for ion trap in working order time provides high frequency voltage: 5000 volts of peak-to-peak values, and cleaning the radio-frequency voltage that constant amplitude is provided for the electrode of ion trap when state: amplitude is 100 volts.Only adopt a vacuum unit, in working order time for ion trap provides high vacuum: 10uTorr, cleaning when state as ion trap provides low vacuum: 1Torr.
The attendant of above-mentioned mass spectrometer sets time started and the duration of cleaning state: under regular situation, the frequency of utilization of mass spectrometer and service time are all roughly determined, therefore can calculate the time that ion trap need to be cleaned.When ion trap uses after certain hour, attendant starts function of on-line cleaning.
Or use timing device, the record operating time each time, in the time that the operating time is accumulated to certain value, starts function of on-line cleaning automatically.
Embodiment 3:
The application examples in VOC detects according to the mass spectrometer of the embodiment of the present invention 1 and method of work, as the detection of alkanes substance.Mass spectrometer adopts ion trap, only adopt a radio-frequency power supply, electrode for ion trap in working order time provides high frequency voltage: 5000 volts of peak-to-peak values, and cleaning the radio-frequency voltage that constant amplitude is provided for the electrode of ion trap when state: amplitude is 500 volts.Only adopt a vacuum unit, in working order time for ion trap provides high vacuum: 10uTorr, cleaning when state as ion trap provides low vacuum: 0.5Torr.
The attendant of above-mentioned mass spectrometer sets time started and the duration of cleaning state: under regular situation, the frequency of utilization of mass spectrometer and service time are all roughly determined, therefore can calculate the time that ion trap need to be cleaned.When ion trap uses after certain hour, attendant starts function of on-line cleaning.
Or use timing device, the record operating time each time, in the time that the operating time is accumulated to certain value, starts function of on-line cleaning automatically.
Embodiment 4:
The application examples in VOC detects according to the on-line monitoring instrument of the embodiment of the present invention 1 and monitoring method, in the detection of Volatile Organohalides.Mass spectrometer adopts quadrupole rod, on the basis of original the first radio-frequency power supply, add second source, the electrode that in working order time, the first radio-frequency power supply is quadrupole rod provides high frequency voltage: 6000 volts of peak-to-peak values, the electrode that second source is quadrupole rod in the time of the state of cleaning provides the radio-frequency voltage of constant amplitude: amplitude is 1000 volts.On the basis of original the first vacuum unit, add the second vacuum unit, in working order time, the first vacuum unit provides high vacuum for quadrupole rod: 1uTorr, in the time of the state of cleaning, the second vacuum unit provides low vacuum for quadrupole rod: 10mTorr.
Judge whether personnel's equipment (mass spectrometer user of service or judgment means) discharges between the electrode of quadrupole rod or whether the chemical noises of mass spectrometer exceedes threshold value for monitoring, if electric discharge or exceed threshold value and show that quadrupole rod should be in cleaning state, judged result is sent to described control personnel equipment.Control personnel equipment is by selecting, make quadrupole rod in cleaning state: second source provides constant voltage for quadrupole rod, the second vacuum unit makes quadrupole rod in low vacuum state, thereby makes, between the electrode of quadrupole rod, plasma discharge occurs, thereby has cleared up the pollutant on electrode.
Claims (12)
1. have the mass spectrometer of function of on-line cleaning, described mass spectrometer comprises ion trap or quadrupole rod, it is characterized in that: described mass spectrometer further comprises:
Radio-frequency power supply, described radio-frequency power supply for being that the electrode of ion trap or quadrupole rod applies high frequency voltage in the time that mass spectrometer is in running order; Apply constant voltage in the time cleaning state at mass spectrometer the electrode of described ion trap or quadrupole rod;
Vacuum unit, described vacuum unit is used for making described ion trap or quadrupole rod maintain low vacuum state in the time of the state of cleaning, thereby make the electrode of described ion trap or quadrupole rod, in the time of described constant voltage, low vacuum state, plasma discharge occur, and make described ion trap or quadrupole rod maintain high vacuum state in working order time;
Control personnel equipment, described control personnel equipment is for optionally making described mass spectrometer in cleaning state, operating state and idle condition.
2. mass spectrometer according to claim 1, is characterized in that: the pressure limit of described low vacuum state is 10-1000mTorr.
3. mass spectrometer according to claim 1, is characterized in that: the radio-frequency voltage that described constant voltage is constant amplitude, voltage range is 100-1000 volt.
4. mass spectrometer according to claim 1, is characterized in that: described mass spectrometer further comprises:
Timing personnel equipment, described timing personnel equipment is used for setting time started and the duration of cleaning state, and is sent to described control personnel equipment.
5. mass spectrometer according to claim 4, is characterized in that: described mass spectrometer further comprises:
Judgement personnel equipment, whether the described personnel's of judgement equipment is for according to discharging between electrode or whether whether the chemical noises of mass spectrometer exceed that threshold value determines should be in cleaning state, and judged result is sent to described control personnel equipment.
6. mass spectrometer according to claim 1, is characterized in that: described radio-frequency power supply is only a radio-frequency power supply, or is respectively described electrode the first radio-frequency power supply and the second source of high frequency voltage and constant voltage is provided.
7. mass spectrometer according to claim 1, is characterized in that: described vacuum unit is only a vacuum unit, or is respectively described ion trap or quadrupole rod and maintains the first vacuum unit and second vacuum unit of low vacuum state and high vacuum state.
8. have the method for work of the mass spectrometer of function of on-line cleaning, described method of work is:
Under the selection of the personnel of control equipment, described mass spectrometer is in on-line cleaning state, ion trap or quadrupole rod that radio-frequency power supply is mass spectrometer provide constant voltage, vacuum unit makes described ion trap or quadrupole rod maintain low vacuum state, make the electrode generation plasma discharge of described ion trap or quadrupole rod, thereby cleaned described electrode;
Under the selection of described control personnel equipment, described mass spectrometer is in running order, and described radio-frequency power supply provides high frequency voltage for described ion trap or quadrupole rod, and described vacuum unit is that described ion trap or quadrupole rod maintain high vacuum state.
9. method of work according to claim 8, is characterized in that: the pressure limit of described low vacuum state is 10-1000mTorr.
10. method of work according to claim 8, is characterized in that: the radio-frequency voltage that described constant voltage is constant amplitude, voltage range is 100-1000 volt.
11. method of works according to claim 8, is characterized in that: described method of work further comprises determining step:
Judge whether personnel's equipment is according to discharging between described electrode or whether the chemical noises of mass spectrometer exceedes that threshold value determines whether should be in cleaning state, and judged result is sent to described control personnel equipment.
12. method of works according to claim 8, is characterized in that: described method of work further comprises timing step:
On timing personnel equipment, set time started and the duration of described cleaning state, the output signal of timing personnel equipment is sent to described control personnel equipment.
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| CN106841536A (en) * | 2017-03-31 | 2017-06-13 | 宇星科技发展(深圳)有限公司 | A kind of VOCs detectors |
| GB201808893D0 (en) | 2018-05-31 | 2018-07-18 | Micromass Ltd | Bench-top time of flight mass spectrometer |
| GB201808912D0 (en) | 2018-05-31 | 2018-07-18 | Micromass Ltd | Bench-top time of flight mass spectrometer |
| GB201808932D0 (en) | 2018-05-31 | 2018-07-18 | Micromass Ltd | Bench-top time of flight mass spectrometer |
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| CN1653582A (en) * | 2002-05-13 | 2005-08-10 | 热电子公司 | Improved mass spectrometer and mass filter for the mass spectrometer |
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| WO2005033663A2 (en) * | 2003-09-30 | 2005-04-14 | Sequenom, Inc. | Methods of making substrates for mass spectrometry analysis and related devices |
| US7005635B2 (en) * | 2004-02-05 | 2006-02-28 | Metara, Inc. | Nebulizer with plasma source |
| US7709790B2 (en) * | 2008-04-01 | 2010-05-04 | Thermo Finnigan Llc | Removable ion source that does not require venting of the vacuum chamber |
| CN101583233A (en) * | 2009-03-24 | 2009-11-18 | 新奥光伏能源有限公司 | Normal-pressure plasma device |
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