CN108802164A - A method of implementing LDAR using vehicle-mounted chemical ionization mass spectrometry - Google Patents
A method of implementing LDAR using vehicle-mounted chemical ionization mass spectrometry Download PDFInfo
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- CN108802164A CN108802164A CN201810937673.8A CN201810937673A CN108802164A CN 108802164 A CN108802164 A CN 108802164A CN 201810937673 A CN201810937673 A CN 201810937673A CN 108802164 A CN108802164 A CN 108802164A
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- 238000000262 chemical ionisation mass spectrometry Methods 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 239000005416 organic matter Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 4
- 150000002500 ions Chemical class 0.000 claims description 61
- 238000004949 mass spectrometry Methods 0.000 claims description 8
- 238000013016 damping Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 239000000356 contaminant Substances 0.000 abstract description 8
- 239000004615 ingredient Substances 0.000 abstract description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000001819 mass spectrum Methods 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000012855 volatile organic compound Substances 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- -1 H3O+ Chemical class 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- VGQXTTSVLMQFHM-UHFFFAOYSA-N peroxyacetyl nitrate Chemical compound CC(=O)OO[N+]([O-])=O VGQXTTSVLMQFHM-UHFFFAOYSA-N 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating 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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Abstract
The invention discloses a kind of methods for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry, include the following steps：S1：Prepare：Prepare chemical ionization mass spectrometry device in advance；S2：In the ion source region of chemical ionization mass spectrometry device, the initial ion A of initial chemical ionization mass spectrometry is generated by hollow cathode discharge+, ion-molecule reaction occurs into the volatile organic matter molecule M in ion drift tube, with air；S3：Measure trace organic substance M；S4：Gas inside drift tube all is from external air, and the partial pressure concentration of M remains unchanged before and after entering drift tube, and the partial pressure concentration for the M that CI-MS is measured is that under test gas enters the concentration before drift tube.Reasonable design of the present invention can utilize chemical ionization mass spectrometry method to detect the ingredient and concentration of volatile organic contaminant, without being pre-processed to sample gas, reduce the detection used time, improve detection efficiency.
Description
Technical field
The present invention relates to gas detection technology field more particularly to a kind of vehicle-mounted chemical ionization mass spectrometry is utilized to implement LDAR
Method.
Background technology
LDAR technologies (i.e. leak detection and recovery technique), be by being detected to the potential leakage point of refinery device, and
There are the components of leakage phenomenon by Shi Faxian, and are repaired or replaced, and then realize that reducing leakage discharges.Volatile organic matter
（VOCs）A kind of main atmosphere pollution, caused by harm include：1）Part VOCs has toxicity and carcinogenicity；2）Ginseng
With photochemical fog, ozone, Peroxyacetyl nitrate etc. are formed；3）The formation of secondary organic aerosol in air is participated in, is formed
Secondary organic aerosol hide in fine grained（Grain size<2.5μm）Range, free settling, can not be stranded in air the long period, right
The scattering power of light is stronger, and to significantly reduce, there are visibility.Volatile organic matter is the weight of current atmospheric prevention and cure of pollution
Point.Through retrieval, application No. is 201810099383.0 patent documents to disclose a kind of chemi-ionization and photo-ionisation multiple source matter
The volatile organic compound detection device and detection method of spectrum, including discharge ion source and photo-ionisation lamp, internal diameter it is gradually smaller anti-
Ying Guan, adapter cavity, mass spectrum chamber, adapter cavity molecular pump, mass spectrum chamber molecular pump, fore pump, alternating current-direct current composite power source, injection port, from
Son detection mass spectrum, air source etc.；The detection method is the chemi-ionization and photo-ionisation by ion molecule reaction, and realization is waved various
Dual ionization while hair property organic matter realizes online highly sensitive detection by mass spectrum to determinand.The invention passes through chemical-electrical
It is realized to the multidimensional ionization of volatile organic matter and highly sensitive Mass Spectrometer Method from photo-ionisation, compensates for the changes such as Proton-Transfer Reactions
Learn the deficiency that photo-ionisation efficiency is low under the difficult detection alkanes volatile organic matter of ionization and vacuum condition.The invention may be implemented
The all standing of non-alkanes volatile organic matter and alkanes volatile organic matter highly sensitive on-line checking simultaneously.
But the prior art is required for concentrating detection gas greatly when being detected volatile organic contaminant
The pretreatments such as separation, detection efficiency is relatively low, and the used time is long, is unfavorable for using, therefore utilizing vehicle-mounted chemistry we have proposed a kind of
Ionization mass spectrometry implements the method for LDAR for solving the above problems.
Invention content
Technical problems based on background technology, the present invention propose a kind of vehicle-mounted chemical ionization mass spectrometry of utilization and implement
The method of LDAR.
A kind of method for being implemented LDAR using vehicle-mounted chemical ionization mass spectrometry proposed by the present invention, is included the following steps：
S1：Prepare：Prepare chemical ionization mass spectrometry device in advance；
S2：In the ion source region of chemical ionization mass spectrometry device, initial chemical ionization mass spectrometry is generated by hollow cathode discharge
Initial ion A+, ion-molecule reaction occurs into the volatile organic matter molecule M in ion drift tube, with air：
(1)
Formula（1）In, k is reaction rate constant, product ion concentration [BH in drift tube+] relationship that changes over time is：
(2)
Formula（2）In, [A+] and [M] be respectively the number density of initial ion and volatile organic matter M in drift tube；
S3：Measure trace organic substance M, the reactive ion A in drift tube+Number density be much larger than M number density [M], reacting
It is front and back, the number density [A+ of reactive ion+] constant is regarded as, in the number density [B of drift tube end products ion+] be：
(3)
Formula（3）In, t is ionic reaction time, the ion signal arrived equal to the time that ion migrates in drift tube, mass spectrometry detection
i(A+) and i (B+) it is proportional to the number density [A of drift tube intermediate ion+] and [B+], volatile organic trace compounds M's is dense in drift tube
Degree is：
(4)
Formula（4）In, τ be chemical ionization mass spectrometry device to the response factor of the ion of different mass-to-charge ratioes, measure ionic strength i (A+)
With i (B+), using ionic reaction rate constants k and ionic reaction time t, organic matter M to be measured in drift tube is obtained by (4) formula
Number density；
S4：Gas inside drift tube all is from external air, and the partial pressure concentration of M maintains not before and after entering drift tube
Become, the partial pressure concentration for the M that CI-MS is measured is that under test gas enters the concentration before drift tube.
Preferably, in the S1, chemical ionization mass spectrometry device includes ion source, drift tube, mass spectrometry system.
Preferably, in the S2, initial ion A+ chooses H3O+、O2 +、NO2 +、NO+In a kind of ion.
Preferably, in the S1, the vacuum degree of chemical ionization mass spectrometry device is less than 10-3Pa。
Preferably, in the S2, initial ion A is manufactured+When, initial ion A is generated by glow discharge+。
Preferably, in the S1, damping fixing device is set, chemical ionization mass spectrometry device is logical on chemical ionization mass spectrometry device
Damping fixing device is crossed to be fixed on automobile.
Preferably, in the S1, setting ionization generating means, is used for moisture electron discharge on chemical ionization mass spectrometry device.
Preferably, in the S3, when determining the numerical value of τ, pass through the number of experimental calibration τ on chemical ionization mass spectrometry device
Value.
Compared with prior art, the beneficial effects of the invention are as follows：
（1）The ingredient and concentration of volatile organic contaminant are quickly detected using chemical ionization mass spectrometry method；To quickly understand
The uncontrollable discharge situation of volatile organic contaminant.Since chemi-ionization reaction mass spectrometric analysis method is direct injection analysis,
Sample gas need not be carried out the pretreatment process such as being concentrated and separated；
（2）The initial ion A of initial chemical ionization mass spectrometry is generated by hollow cathode discharge+, initial ion A+Into ion
Ion-molecule reaction occurs with volatile organic matter molecule M after drift tube, wherein volatile organic matter include alcohols, aldehydes,
Ketone etc., gas can direct injected, sample need not be pre-processed, Instrumental Analysis detection time is short, equipment detection it is sensitive
Degree is high, and a variety of initial reaction ions, including H are generated by glow discharge3O+、O2 +、NO2 +、NO+Deng can realize that absolute partial pressure is dense
The quantitative measurment of degree need not calibrate.
Reasonable design of the present invention, can utilize chemical ionization mass spectrometry method detect volatile organic contaminant ingredient and
Concentration reduces the detection used time, improves detection efficiency without being pre-processed to sample gas.
Description of the drawings
Fig. 1 is chemical ionization mass spectrometry in a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry proposed by the present invention
The schematic diagram of device.
Specific implementation mode
The present invention is made further to explain with reference to specific embodiment.
Embodiment
With reference to figure 1, proposed in the present embodiment it is a kind of using vehicle-mounted chemical ionization mass spectrometry implement LDAR method, including with
Lower step：
S1：Prepare：Prepare chemical ionization mass spectrometry device in advance；
S2：In the ion source region of chemical ionization mass spectrometry device, initial chemical ionization mass spectrometry is generated by hollow cathode discharge
Initial ion A+, ion-molecule reaction occurs into the volatile organic matter molecule M in ion drift tube, with air：
(1)
Formula（1）In, k is reaction rate constant, product ion concentration [BH in drift tube+] relationship that changes over time is：
(2)
Formula（2）In, [A+] and [M] be respectively the number density of initial ion and volatile organic matter M in drift tube；
S3：Measure trace organic substance M, the reactive ion A in drift tube+Number density be much larger than M number density [M], reacting
It is front and back, the number density [A+ of reactive ion+] constant is regarded as, in the number density [B of drift tube end products ion+] be：
(3)
Formula（3）In, t is ionic reaction time, the ion signal arrived equal to the time that ion migrates in drift tube, mass spectrometry detection
i(A+) and i (B+) it is proportional to the number density [A of drift tube intermediate ion+] and [B+], volatile organic trace compounds M's is dense in drift tube
Degree is：
(4)
Formula（4）In, τ be chemical ionization mass spectrometry device to the response factor of the ion of different mass-to-charge ratioes, measure ionic strength i (A+)
With i (B+), using ionic reaction rate constants k and ionic reaction time t, organic matter M to be measured in drift tube is obtained by (4) formula
Number density；
S4：Gas inside drift tube all is from external air, and the partial pressure concentration of M maintains not before and after entering drift tube
Become, the partial pressure concentration for the M that CI-MS is measured is that under test gas enters the concentration before drift tube.
In the present embodiment, in S1, chemical ionization mass spectrometry device includes ion source, drift tube, mass spectrometry system, in S2,
Initial ion A+ chooses H3O+、O2 +、NO2 +、NO+In a kind of ion, in S1, the vacuum degree of chemical ionization mass spectrometry device is less than 10-3In Pa, S2, initial ion A is manufactured+When, initial ion A is generated by glow discharge+, in S1, on chemical ionization mass spectrometry device
Damping fixing device is set, and chemical ionization mass spectrometry device is fixed on by damping fixing device on automobile, in S1, in chemi-ionization
Setting ionization generating means, is used for moisture electron discharge on mass spectrometric apparatus, in S3, when determining the numerical value of τ, is filled in chemical ionization mass spectrometry
Set through the numerical value of experimental calibration τ, using chemical ionization mass spectrometry method quickly detect volatile organic contaminant ingredient and
Concentration；To quickly understand the uncontrollable discharge situation of volatile organic contaminant.Due to chemi-ionization reaction mass spectral analysis side
Method is direct injection analysis, need not carry out the pretreatment process such as being concentrated and separated to sample gas；It is produced by hollow cathode discharge
The initial ion A of raw initial chemical ionization mass spectrometry+, initial ion A+After into ion drift tube with volatile organic matter molecule M
Ion-molecule reaction occurs, wherein volatile organic matter includes alcohols, aldehydes, ketone etc., gas can direct injected, do not need
Sample is pre-processed, Instrumental Analysis detection time is short, and equipment detectivity is high, is generated by glow discharge a variety of initial
Reactive ion, including H3O+、O2 +、NO2 +、NO+Deng, it can realize the quantitative measurment of absolute partial pressure concentration, need not calibrate, the present invention
Reasonable design can utilize chemical ionization mass spectrometry method to detect the ingredient and concentration of volatile organic contaminant, without to sample
Product gas is pre-processed, and the detection used time is reduced, and improves detection efficiency.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry, which is characterized in that include the following steps：
S1：Prepare：Prepare chemical ionization mass spectrometry device in advance；
S2：In the ion source region of chemical ionization mass spectrometry device, initial chemical ionization mass spectrometry is generated by hollow cathode discharge
Initial ion A+, ion-molecule reaction occurs into the volatile organic matter molecule M in ion drift tube, with air：
(1)
Formula（1）In, k is reaction rate constant, product ion concentration [BH in drift tube+] relationship that changes over time is：
(2)
Formula（2）In, [A+] and [M] be respectively the number density of initial ion and volatile organic matter M in drift tube；
S3：Measure trace organic substance M, the reactive ion A in drift tube+Number density be much larger than M number density [M], before the reaction
Afterwards, the number density [A+ of reactive ion+] constant is regarded as, in the number density [B of drift tube end products ion+] be：
(3)
Formula（3）In, t is ionic reaction time, the ion signal arrived equal to the time that ion migrates in drift tube, mass spectrometry detection
i(A+) and i (B+) it is proportional to the number density [A of drift tube intermediate ion+] and [B+], volatile organic trace compounds M's is dense in drift tube
Degree is：
(4)
Formula（4）In, τ be chemical ionization mass spectrometry device to the response factor of the ion of different mass-to-charge ratioes, measure ionic strength i (A+)
With i (B+), using ionic reaction rate constants k and ionic reaction time t, organic matter M to be measured in drift tube is obtained by (4) formula
Number density；
S4：Gas inside drift tube all is from external air, and the partial pressure concentration of M maintains not before and after entering drift tube
Become, the partial pressure concentration for the M that CI-MS is measured is that under test gas enters the concentration before drift tube.
2. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S1, chemical ionization mass spectrometry device includes ion source, drift tube, mass spectrometry system.
3. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S2, initial ion A+ chooses H3O+、O2 +、NO2 +、NO+In a kind of ion.
4. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S1, the vacuum degree of chemical ionization mass spectrometry device is less than 10-3Pa。
5. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S2, manufacture initial ion A+When, initial ion A is generated by glow discharge+。
6. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S1, damping fixing device is set on chemical ionization mass spectrometry device, chemical ionization mass spectrometry device is solid by damping fixing device
It is scheduled on automobile.
7. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S1, setting ionization generating means, is used for moisture electron discharge on chemical ionization mass spectrometry device.
8. a kind of method for implementing LDAR using vehicle-mounted chemical ionization mass spectrometry according to claim 1, which is characterized in that institute
It states in S3, when determining the numerical value of τ, passes through the numerical value of experimental calibration τ on chemical ionization mass spectrometry device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109387559A (en) * | 2018-12-24 | 2019-02-26 | 中国科学院合肥物质科学研究院 | A kind of vehicle-mounted chemical ionization mass spectrometry of atmospheric volatile organic compounds is walked to navigate detection device and method |
| CN115332045A (en) * | 2022-08-19 | 2022-11-11 | 山东大学 | Photochemical ionization device for real-time online detection of mass spectrum of glyoxal in atmosphere |
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2018
- 2018-08-17 CN CN201810937673.8A patent/CN108802164A/en active Pending
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| CN205365373U (en) * | 2016-03-02 | 2016-07-06 | 龙岩市海德馨汽车有限公司 | Kitchen truck food monitoring devices |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109387559A (en) * | 2018-12-24 | 2019-02-26 | 中国科学院合肥物质科学研究院 | A kind of vehicle-mounted chemical ionization mass spectrometry of atmospheric volatile organic compounds is walked to navigate detection device and method |
| CN115332045A (en) * | 2022-08-19 | 2022-11-11 | 山东大学 | Photochemical ionization device for real-time online detection of mass spectrum of glyoxal in atmosphere |
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