CN108195923A - The method and mass spectrometer arrangement detected for volatile organic compounds in sample - Google Patents

The method and mass spectrometer arrangement detected for volatile organic compounds in sample Download PDF

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Publication number
CN108195923A
CN108195923A CN201810002041.2A CN201810002041A CN108195923A CN 108195923 A CN108195923 A CN 108195923A CN 201810002041 A CN201810002041 A CN 201810002041A CN 108195923 A CN108195923 A CN 108195923A
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cavity
sample
mass
mass spectrograph
sample container
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CN201810002041.2A
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余泉
张乾
王晓浩
钱翔
倪凯
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Shenzhen Graduate School Tsinghua University
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Shenzhen Graduate School Tsinghua University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

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  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a kind of method detected for volatile organic compounds in sample and mass spectrometer arrangements, the device includes sample container, mass spectrograph cavity and vacuum pump, the mass spectrograph cavity is provided with ionization source and mass analyzer, the sample container is tightly connected the mass spectrograph cavity by gas pipeline, the gas pipeline does not contact the sample in the sample container, the mass spectrograph cavity connects the vacuum pump, the vacuum pump generates vacuum environment through controlling in the mass spectrograph cavity, and make the volatile organic matter contained by sample in the sample container subjected to a vacuum and volatilize and be diffused as gaseous state, after the gas pipeline, it is ionized in the mass spectrograph cavity by the ionization source, finally detected by the mass analyzer.Apparatus and method of the present invention rapidly can detach and detect volatile organic compounds in sample, and without complicated pre-treatment, constructional device is simple.

Description

The method and mass spectrometer arrangement detected for volatile organic compounds in sample
Technical field
The present invention relates to mass spectral analysis field, more particularly to a kind of for volatile organic compounds detection in sample Method and mass spectrometer arrangement.
Background technology
Mass spectral analysis is a kind of quick, efficient substance determination method, is widely used in food and drug safety, sky Between the fields such as Science Explorations, public safety.Volatile organic compounds such as toluene, methyl phenyl ethers anisole, formaldehyde are often dissolved in liquid, Or by solid sorbent.As during volatile organic matter sample detection, needed in the waste waste liquid of chemical plant distillation and etc. gasification use again Mass spectrograph is detected its gaseous matter;The sample detection of Volatile Organic Compounds in Soil then needs the methods of purge and trap to receive Collect volatile organic matter, complex disposal process is cumbersome, takes long.
Invention content
It is a kind of for volatile organic in sample it is a primary object of the present invention in view of the deficiencies of the prior art, provide Close the method and mass spectrometer arrangement of analyte detection.
To achieve the above object, the present invention uses following technical scheme:
A kind of mass spectrometer arrangement detected for volatile organic compounds in sample, including sample container, mass spectrograph chamber Body and vacuum pump, the mass spectrograph cavity are provided with ionization source and mass analyzer, and the sample container is close by gas pipeline Envelope connects the mass spectrograph cavity, and the gas pipeline does not contact the sample in the sample container, and the mass spectrograph cavity connects The vacuum pump is connect, the vacuum pump generates vacuum environment, and make the sample container through controlling in the mass spectrograph cavity In sample contained by volatile organic matter it is subjected to a vacuum and volatilize be diffused as gaseous state, after the gas pipeline, It is ionized by the ionization source in the mass spectrograph cavity, is finally detected by the mass analyzer.
Further:
The vacuum pump through control in the mass spectrograph cavity and the sample container producible air pressure range 10-4-200Pa。
The vacuum pump includes mechanical pump and turbo-molecular, and the vacuum in the mass spectrograph cavity is by the turbomolecular pump It keeps, the mechanical pump is connect with the turbomolecular pump, the fore pump as the turbomolecular pump.
Valve is provided on the gas pipeline, the valve control sample is continuously or discontinuously transported to property the matter In spectrometer cavity.
Temperature is 0~200 DEG C in the sample container.
The gas pipeline stretches into the port of the mass spectrograph cavity and the preceding pole plate distance 0- of the mass analyzer 1cm。
The ionization source is light ionization source, appointing in electron bombardment ionization source, vacuum electric spray ion source, ullrasonic spraying ion source It is a kind of.
A kind of method detected for volatile organic compounds in sample, using the mass spectrometer arrangement, wherein sample Product container is tightly connected mass spectrograph cavity by gas pipeline, and the gas pipeline does not contact the sample in the sample container, The mass spectrograph cavity connects vacuum pump, and the vacuum pump generates vacuum environment, and make through controlling in the mass spectrograph cavity The volatile organic matter contained by sample in the sample container is subjected to a vacuum and volatilizees and is diffused as gaseous state, by described After gas pipeline, ionized by ionization source in the mass spectrograph cavity, finally detected by mass analyzer.
The present invention has the advantages that:
The method and mass spectrometer arrangement detected the present invention provides volatile organic compounds in a kind of sample, without to sample The special gasification step of volatile organic compounds to be detected progress is again detected its gaseous matter in product, of the invention Mass spectrometer arrangement is volatilized under vacuum conditions using volatile organic matter is diffused as gaseous characteristic, is connected using mass spectrograph cavity Vacuum pump provide vacuum environment for sample container by gas pipeline, realize volatile organic compound in liquid or solid sample The gasification of object is detached with other substances, and the volatile organic compounds of gasification enters mass spectrograph by closed gas pipeline again In cavity, ionized by mass spectrograph cavity internal ionization source, be finally mass analyzed device and detect.The present invention can be conveniently and efficiently to sample Product are isolated volatile organic compounds therein, and equipment making cost is relatively low, and detection process cost is relatively low, place Reason mode is simple, efficient, it can be achieved that on-line real-time measuremen, is particularly adapted to pollution situ liquid or solid continuously detects.
Description of the drawings
Fig. 1 is the knot of the mass spectrometer arrangement detected for volatile organic compounds in sample of an embodiment of the present invention Structure schematic diagram.
Specific embodiment
It elaborates below to embodiments of the present invention.It is emphasized that the description below is only exemplary, The range being not intended to be limiting of the invention and its application.
As shown in Figure 1, in one embodiment, a kind of mass spectrograph dress detected for volatile organic compounds in sample It puts, including sample container 1, mass spectrograph cavity 4 and vacuum pump, the mass spectrograph cavity 4 is provided with ionization source 5 and mass analyzer 6, the sample container 1 is tightly connected the mass spectrograph cavity 4 by gas pipeline 3, and the gas pipeline 3 does not contact the sample Sample in product container 1, the mass spectrograph cavity 4 connect the vacuum pump, and the vacuum pump is through controlling in the mass spectrograph chamber Vacuum environment is generated in body 4, and make the volatile organic matter contained by the sample in the sample container 1 subjected to a vacuum and Volatilization is diffused as gaseous state, after the gas pipeline 3, is ionized in the mass spectrograph cavity 4 by the ionization source 5, finally It is detected by the mass analyzer 6.
It is special without being carried out to volatile organic compounds to be detected in sample using mass spectrometer arrangement provided by the invention The complicated tedious steps such as gasification of door are again detected its gaseous matter, and mass spectrometer arrangement of the invention is organic using volatility Object volatilizees under vacuum conditions is diffused as gaseous characteristic, is by gas pipeline 3 using 4 connected vacuum pump of mass spectrograph cavity Sample container 1 provides vacuum environment, realizes the gasification of volatile organic compounds in solid or fluid sample, with other substances point From the volatile organic compounds of gasification is entered by closed gas pipeline 3 in mass spectrograph cavity 4 again, by mass spectrograph cavity 4 Internal ionization source 5 ionizes, and is finally mass analyzed device 6 and detects.The present invention mass spectrometer arrangement can conveniently and efficiently to sample into Row is isolated volatile organic compounds therein, and equipment making cost is relatively low, and detection process cost is relatively low, processing side Formula is simple, efficient, it can be achieved that on-line real-time measuremen, is particularly adapted to pollution field sample and continuously detects.
In a preferred embodiment, the vacuum pump can in the mass spectrograph cavity 4 and the sample container 1 through control The air pressure range of generation is 10-4-200Pa。
In a preferred embodiment, the vacuum pump includes mechanical pump 8 and turbo-molecular, in the mass spectrograph cavity 4 Vacuum is kept by the turbomolecular pump 7, and the mechanical pump 8 is connect with the turbomolecular pump 7, as the turbomolecular pump 7 fore pump.
In a preferred embodiment, it is provided with valve 2 on the gas pipeline 3.
In various embodiments, the valve 2 can control sample to be continuously or discontinuously transported to property the mass spectrograph In cavity 4.
In a preferred embodiment, temperature is 0~200 DEG C in the sample container 1.It can be according to the property of tested substance Matter selects vessel temp.
In a preferred embodiment, the gas pipeline 3 stretches into the port of the mass spectrograph cavity 4 and the quality analysis The preceding pole plate distance 0-1cm of device 6.
In various embodiments, the ionization source 5 is without restriction, can be light ionization source 5, electron bombardment ionization source, vacuum electric The ionization sources such as esi ion source or ullrasonic spraying ion source 5.
Refering to Fig. 1, in another embodiment, a kind of method detected for volatile organic compounds in sample is adopted With the mass spectrometer arrangement of aforementioned any embodiment, wherein sample container 1 is tightly connected mass spectrograph cavity 4, institute by gas pipeline 3 It states gas pipeline 3 and does not contact sample in the sample container 1, the mass spectrograph cavity 4 connects vacuum pump, the vacuum pump warp Control generates vacuum environment in the mass spectrograph cavity 4, and makes contained by the solid or fluid sample in the sample container 1 Volatile organic matter is subjected to a vacuum and volatilizees and is diffused as gaseous state, after the gas pipeline 3, in the mass spectrograph chamber It is ionized by ionization source 5 in body 4, is finally detected by mass analyzer 6.
As shown in Figure 1, in a typical embodiment, the mass spectrograph detected for volatile organic compounds in sample Device includes sample container 1, valve 2, gas pipeline 3, mass spectrograph cavity 4, ionization source 5, mass analyzer 6, turbomolecular pump 7th, mechanical pump 8.Described 3 one end of gas pipeline is placed in sample container 1, and the other end is placed in mass spectrograph cavity 4, gas pipeline 3 Centre be provided with valve 2, control its break-make, realize volatile organic compounds continuous sample introduction in sample or noncontinuity into Sample, the gas of sample introduction are ionized by ionization source 5 in mass spectrograph cavity 4, are finally mass analyzed device 6 and detect.
Apparatus and method of the present invention rapidly can detach and detect volatile organic compounds in sample, without multiple Miscellaneous pre-treatment, constructional device are simple.
The above content is combine specific/preferred embodiment further description made for the present invention, it is impossible to recognize The specific implementation of the fixed present invention is confined to these explanations.For those of ordinary skill in the art to which the present invention belongs, Without departing from the inventive concept of the premise, some replacements or modification can also be made to the embodiment that these have been described, And these are substituted or variant should all be considered as belonging to protection scope of the present invention.

Claims (8)

1. a kind of mass spectrometer arrangement detected for volatile organic compounds in sample, which is characterized in that including sample container, Mass spectrograph cavity and vacuum pump, the mass spectrograph cavity are provided with ionization source and mass analyzer, and the sample container passes through gas Body seal for pipe joints connects the mass spectrograph cavity, and the gas pipeline does not contact the sample in the sample container, the mass spectrum Instrument cavity connects the vacuum pump, and the vacuum pump generates vacuum environment through controlling in the mass spectrograph cavity, and makes described The volatile organic matter contained by sample in sample container is subjected to a vacuum and volatilizees and is diffused as gaseous state, by the gas After pipeline, ionized by the ionization source in the mass spectrograph cavity, finally detected by the mass analyzer.
2. mass spectrometer arrangement as described in claim 1, which is characterized in that the vacuum pump is through controlling in the mass spectrograph cavity With air pressure range producible in the sample container 10-4-200Pa。
3. mass spectrometer arrangement as claimed in claim 1 or 2, which is characterized in that the vacuum pump includes mechanical pump and turbine point Son, the vacuum in the mass spectrograph cavity are kept by the turbomolecular pump, and the mechanical pump is connect with the turbomolecular pump, Fore pump as the turbomolecular pump.
4. mass spectrometer arrangement as described in any one of claims 1 to 3, which is characterized in that be provided with valve on the gas pipeline Door, the valve control sample are continuously or discontinuously transported to property in the mass spectrograph cavity.
5. such as Claims 1-4 any one of them mass spectrometer arrangement, which is characterized in that in the sample container temperature for 0~ 200℃。
6. such as mass spectrometer arrangement described in any one of claim 1 to 5, which is characterized in that the gas pipeline stretches into the matter The port of spectrometer cavity and the preceding pole plate distance 0-1cm of the mass analyzer.
7. such as claim 1 to 6 any one of them mass spectrometer arrangement, which is characterized in that the ionization source is light ionization source, electricity Any one of sub- bombardment source, vacuum electric spray ion source, ullrasonic spraying ion source.
A kind of 8. method detected for volatile organic compounds in sample, which is characterized in that using such as claim 1 to 7 Any one of them mass spectrometer arrangement, wherein sample container are tightly connected mass spectrograph cavity, the flue by gas pipeline Road does not contact the sample in the sample container, and the mass spectrograph cavity connects vacuum pump, and the vacuum pump is through controlling described Vacuum environment is generated in mass spectrograph cavity, and makes the volatile organic matter contained by the sample in the sample container by vacuum Effect and volatilize be diffused as gaseous state, after the gas pipeline, ionized in the mass spectrograph cavity by ionization source, finally by Mass analyzer detects.
CN201810002041.2A 2018-01-02 2018-01-02 The method and mass spectrometer arrangement detected for volatile organic compounds in sample Pending CN108195923A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111982952A (en) * 2020-09-03 2020-11-24 北京赛诺新炜科技有限公司 Organic halide detection device and use method
CN112362720A (en) * 2020-10-29 2021-02-12 河南中烟工业有限责任公司 Detection method for mildew of boxed tobacco leaves
CN112782262A (en) * 2020-12-01 2021-05-11 广西电网有限责任公司电力科学研究院 Device and method for improving vacuum efficiency of portable mass spectrometer
CN113624565A (en) * 2021-08-11 2021-11-09 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) Trace atmosphere sampling detection device and trace atmosphere sampling detection method
CN114994224A (en) * 2022-07-06 2022-09-02 核工业理化工程研究院 Liquid sample introduction device and method for gas isotope mass spectrometer
CN113624565B (en) * 2021-08-11 2024-05-28 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) Trace atmosphere sampling detection device and trace atmosphere sampling detection method

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CN103512943A (en) * 2012-06-26 2014-01-15 吉林省维远科技有限公司 Special mass spectrometer for online detection of volatile organic compounds
CN102928499B (en) * 2012-11-03 2014-09-24 中国烟草总公司郑州烟草研究院 Rapid analysis device and method for ambient air volatile organic compounds
CN105489467A (en) * 2015-12-31 2016-04-13 上海华质生物技术有限公司 Chemical ionization source device and ionization detection method therefor
CN107039232A (en) * 2017-04-12 2017-08-11 清华大学深圳研究生院 A kind of vacuum electric spray ion source and mass spectrograph
CN207020123U (en) * 2017-07-27 2018-02-16 山东省科学院海洋仪器仪表研究所 A variety of soluble gas field monitoring instrument in a kind of seawater

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103512943A (en) * 2012-06-26 2014-01-15 吉林省维远科技有限公司 Special mass spectrometer for online detection of volatile organic compounds
CN102928499B (en) * 2012-11-03 2014-09-24 中国烟草总公司郑州烟草研究院 Rapid analysis device and method for ambient air volatile organic compounds
CN105489467A (en) * 2015-12-31 2016-04-13 上海华质生物技术有限公司 Chemical ionization source device and ionization detection method therefor
CN107039232A (en) * 2017-04-12 2017-08-11 清华大学深圳研究生院 A kind of vacuum electric spray ion source and mass spectrograph
CN207020123U (en) * 2017-07-27 2018-02-16 山东省科学院海洋仪器仪表研究所 A variety of soluble gas field monitoring instrument in a kind of seawater

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111982952A (en) * 2020-09-03 2020-11-24 北京赛诺新炜科技有限公司 Organic halide detection device and use method
CN112362720A (en) * 2020-10-29 2021-02-12 河南中烟工业有限责任公司 Detection method for mildew of boxed tobacco leaves
CN112782262A (en) * 2020-12-01 2021-05-11 广西电网有限责任公司电力科学研究院 Device and method for improving vacuum efficiency of portable mass spectrometer
CN113624565A (en) * 2021-08-11 2021-11-09 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) Trace atmosphere sampling detection device and trace atmosphere sampling detection method
CN113624565B (en) * 2021-08-11 2024-05-28 中国电子产品可靠性与环境试验研究所((工业和信息化部电子第五研究所)(中国赛宝实验室)) Trace atmosphere sampling detection device and trace atmosphere sampling detection method
CN114994224A (en) * 2022-07-06 2022-09-02 核工业理化工程研究院 Liquid sample introduction device and method for gas isotope mass spectrometer

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