CN103675080A - Headspace sampler and ion mobility spectrometry combined system - Google Patents
Headspace sampler and ion mobility spectrometry combined system Download PDFInfo
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- CN103675080A CN103675080A CN201210337677.5A CN201210337677A CN103675080A CN 103675080 A CN103675080 A CN 103675080A CN 201210337677 A CN201210337677 A CN 201210337677A CN 103675080 A CN103675080 A CN 103675080A
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Abstract
The invention discloses a headspace sampler and ion mobility spectrometry combined system. The system is composed of a headspace sampler (with an air generator or an air bottle), a gas pipeline connection component (comprising a pressure gauge and a flow gauge) and an ion mobility spectrometry. According to the principle of the headspace sampler, a to-be-detected sample is placed in a sealed container, by virtue of heating up, volatile constituents in the to-be-detected sample are volatilized from a sample matrix, then balance in gas-liquid (or gas-solid) phases is achieved, upper gas is directly extracted and enters the ion mobility spectrometry to be analyzed, and thus, the ingredients and content of the volatile constituents in the sample are detected.
Description
Technical field
The present invention relates to the system of a kind of head-space sampler and ion mobility spectrometry coupling.By head-space sampler (wearing air generator or gas cylinder), gas piping coupling assembling (containing tensimeter and flowmeter) and ion mobility spectrometry, formed.The injection port that the sample gas outlet of head-space sampler is analysed injector with the vapour-phase pyrolysis of ion mobility spectrometry is connected by sample introduction needle; Its principle of head-space sampler is that testing sample is placed in to an airtight container, by heat temperature raising, volatile constituent in testing sample is evaporated from sample matrices, in solution-air (or gas-solid) two-phase, reach balance, directly extract upper gas and carry out ion mobility spectrometry analysis, thereby detect composition and the content of volatile component in sample.
Background technology
Headspace analysis is to measure the content of these components in raw sample by the gas componant of sample substrate top.Obviously, this is a kind of indirect analysis method, and its main theoretical basis of the reform of Chinese economic structure is between gas phase and condensed phase (liquid phase and solid phase), to exist partition equilibrium under certain condition.So the composition of gas phase can reflect the composition of condensed phase.We can regard a kind of gaseous extraction method as headspace analysis, with gas, make " solvent " and extract the volatile ingredient in sample.Thereby headspace analysis is exactly a kind of desirable sample purification method.Traditional liquid-liquid extraction and solid phase micro-extraction technique are all that sample is dissolved in liquid, inevitably have some coextraction thing interference analyses.Moreover the purity of solvent itself is also a problem, and this is particularly important in trace analysis.And gas makes solvent and just can avoid unnecessary interference, because high-pure gas is easy to obtain, and cost is lower, and this is also the major reason that Ding Kong – gas chromatography (GC) is widely adopted.
As a kind of analytical approach, headspace analysis is first simple, and it is only got gas phase and partly analyzes, and has greatly reduced sample substrate to the interference of analyzing.The sample treatment of analyzing as GC, head space is the easiest.Secondly, headspace analysis has different mode, can be suitable for various samples by Optimum Operation parameter.The 3rd, the sensitivity of headspace analysis can meet the requirement of regulation.Finally, combine with the quantitative test ability of GC, GC with Headspace can be carried out quantitative test accurately completely.
A kind of separated detection technique that ion mobility spectrometry (Ion Mobility Spectrometry, IMS) technology 20 century 70s occur, compares with traditional mass spectrum, chromatographic apparatus, he has simple in structure, highly sensitive, analysis speed is fast, the feature of reliable results.Can in atmospheric environment, to micro substance, detect, be suitable for on-the-spot use.Therefore this technology can be applied to the online detection of precursor chemicals.The ionization source of ion mobility spectrometry, is easy to make sample molecule, N
2, O
2with water vapor ionization, ion be easy to and molecule between there is ion, molecular reaction, obtain multi-products, thereby make the spectral line that records very complicated.Ion mobility spectrometry is mainly comprised of chamber, ion gate, drift region and detecting device.Sample gas produces molecule, ion in chamber ionization.The ion gate that ion is opened by periodicity under the ordering about of electric field enters drift region.In the process of constantly colliding at the neutral drift gas molecule with adverse current, due to these ions, in electric field, migration rate is different separately, makes different ions obtain separation, successively arrives collector detected.Therefore by transit time, just can determine the existence of evaluating objects material.
Summary of the invention
The object of the present invention is to provide the system of a kind of head-space sampler and ion mobility spectrometry coupling.Employing technical scheme is:
A system for head-space sampler and ion mobility spectrometry coupling, is comprised of head-space sampler, gas piping and ion mobility spectrometry; The injection port that the sample gas outlet of head-space sampler is analysed injector with the vapour-phase pyrolysis of ion mobility spectrometry is connected by sample introduction needle.
Head-space sampler can be type hand head-space sampler, semi-automatic head-space sampler or automatic type head-space sampler.Its principle of head-space sampler is that testing sample is placed in to an airtight container, by heat temperature raising, volatile constituent in testing sample is evaporated from sample matrices, in solution-air (or gas-solid) two-phase, reach balance, directly extract upper gas and enter ion mobility spectrometry analysis, thereby detect composition and the content of volatile component in sample.
The assembly of head-space sampler comprises: sample bottle constant temperature oven, can be from room temperature-150 ℃ with heating arrangement; Sampling and sample introduction pipeline, can be from room temperature-150 ℃ with heating arrangement; Sample introduction six-way valve, can be from room temperature-150 ℃ with heating arrangement automatically; Vapour-phase pyrolysis is analysed injector with heating arrangement, can be from room temperature-250 ℃; Transference tube, can be from room temperature-120 ℃ with heating arrangement.The system of head-space sampler and ion mobility spectrometry coupling can total system heating, can set temperature, eliminate system cold spot, reduce sample peak broadening, increase degree of separation, make sample analysis more accurate, improve ion mobility spectrometry detection sensitivity.
The sample bottle constant temperature oven station design of head-space sampler adopts circle distribution, more reasonable, the thermograde that makes all head space bottles add thermal potential minimizes, sample bottle constant temperature oven temperature can be set in room temperature-150 ℃, sample equilibration time is greater than 30min, can improve stability and the reliability of ion mobility spectrometry analysis result.
Ion mobility spectrometry ionization source can be nickel source ionization source, uviol lamp ionization source or corona discharge ionization source; Injector be can pin sample introduction pyrolysis analyse injector.
Head-space sampler sampling probe negative pressure form from testing sample matrix extracts volatile constituent and enters quantitative ring, and then carrier gas is carried sample gas in quantitative ring and directly sent into ion mobility spectrometry injector, by ion mobility spectrometry, detects analysis.
The carrier gas of using in experiment, float gas and sweep gas is Purge gas, can be purify air, nitrogen, oxygen or inert gas; Purge gas must be according to the request for utilization of migration spectrum air feed source of the gas, and process dewaters, organism.
Head-space sampler has been worn air generator or gas cylinder; Gas piping comprises gas piping that carrier gas source of the gas is connected with head-space sampler, float the gas piping that gas source of the gas is connected with ion mobility spectrometry, the gas piping that sweep gas source of the gas is connected with head-space sampler, the gas piping that carrier gas source of the gas is connected with ion mobility spectrometry; Gas piping material therefor in system is required to be teflon, stainless steel, metallic iron or aluminium.
The gas piping that the gas piping that carrier gas source of the gas is connected with head-space sampler and sweep gas source of the gas are connected with head-space sampler is provided with tensimeter; Float the gas piping that gas piping that gas source of the gas is connected with ion mobility spectrometry and carrier gas source of the gas be connected with ion mobility spectrometry and be provided with flowmeter.
Head-space sampler output sample gas flow pressure is within the scope of 0.3-0.4MPa.Ion mobility spectrometry output carrier gas is 0mL/min, and head-space sampler sample gas is double serves as carrier gas, meets ion mobility spectrometry circulating air service condition.
After sample test completes, head-space sampler system adopts Purge gas to purge sample lines, quantitatively encircle automatically, prevents cross pollution; Ion mobility spectrometry is closed carrier gas, floats gas blowback detection system, pollution abatement.
Head-space sampler and ion mobility spectrometry combined system can be realized automatic operation, analyze continuously, farthest bring into play work efficiency.
Advantage of the present invention is as follows:
(1) sample bottle constant temperature oven, sampling and sample introduction pipeline, automatic sample introduction six-way valve, vapour-phase pyrolysis are analysed injector and transference tube, total system heating, can set temperature, elimination system cold spot, reduce sample peak broadening, increase degree of separation, make sample analysis more accurate, improve ion mobility spectrometry detection sensitivity.
(2) head-space sampler and ion mobility spectrometry combined system can be realized automatic operation, analyze continuously, farthest bring into play work efficiency.
(3), after each sample introduction completes, system adopts Purge gas to purge sample lines, quantitatively encircle and transference tube automatically, prevents cross pollution.
Below in conjunction with drawings and Examples, the present invention is further detailed explanation:
Accompanying drawing explanation
Fig. 1 is head-space sampler and ion mobility spectrometry combined system structural representation, and the present invention is given and explanation;
Fig. 2 is background signal (RIP) the positive ion mode ion mobility spectrometry figure of head-space sampler and ion mobility spectrometry combined system;
Fig. 3 is background signal (RIP) the negative ion mode ion mobility spectrometry figure of head-space sampler and ion mobility spectrometry combined system;
Embodiment
Head-space sampler is used AC supply voltage 220V, frequency 50 ~ 60HZ.Environment temperature: positive and negative 5 ℃ ~ 35 ℃.The carrier gas of ion mobility spectrometry fast detector and sample gas (air) be 400mL/min altogether, floats gas (air) 600mL/min, 100 ℃ of migration tube temperature, 100 ℃ of injector temperature.Following embodiment operates under above-mentioned experiment condition.
Sample bottle constant temperature oven (80 ℃), sampling and sample introduction pipeline (120 ℃), automatic sample introduction six-way valve (120 ℃ of room temperatures), vapour-phase pyrolysis are analysed injector (100 ℃) and transference tube (100 ℃), sample equilibration time 30min.
Embodiment 1
If Fig. 1 is head-space sampler and ion mobility spectrometry combined system structural representation, to the present invention, giving with explanation: 1-6 is first to the 6th interface of Full-automatic quantitative six-way valve in head-space sampler, 7 analyse injector for vapour-phase pyrolysis, and 8 is ion mobility spectrometry detecting device transference tube.In work, first is connected quantitatively ring with the 4th interface, and second interface connects carrier gas, and the 3rd interface inserts dottle pin connection vapour-phase pyrolysis by sample introduction needle and analyse injector, and the 5th interface connects aspiration pump, and the 6th interface connects sampling probe and insert in sample bottle.During sampling, 1,4,5,6 are connected; During sample introduction, 1,2,3,4 are connected.
Air generator or gas cylinder output gas connect head-space sampler, head-space sampler has two-way gas piping to connect sample introduction needle, a sample introduction needle connects sealed sample bottle, from testing sample matrix, extract volatile constituent, then directly send in Full-automatic quantitative six-way valve quantity tube (using 1mL in test)
。Subsequently can be automatically in head-space sampler carrier gas carry sample gas and by another root, insert vapour-phase pyrolysis and analyse the sample introduction needle of injector and enter ion mobility spectrometry analysis.
Embodiment 2
Fig. 2 is background signal (RIP) the positive ion mode ion mobility spectrometry figure of head-space sampler and ion mobility spectrometry combined system;
In background signal, 4.84ms and 7.28ms material release signal, can eliminate by cleaning.
Embodiment 3
Fig. 3 is background signal (RIP) the negative ion mode ion mobility spectrometry figure of head-space sampler and ion mobility spectrometry combined system.
Under test condition, reagent ion peak appears at 3.76ms, as shown in the figure, does not have signal to disturb, and can detect by Direct Analysis.
Claims (10)
1. a system for head-space sampler and ion mobility spectrometry coupling, is characterized in that: head-space sampler, gas piping and ion mobility spectrometry, consist of;
The injection port that the sample gas outlet of head-space sampler is analysed injector with the vapour-phase pyrolysis of ion mobility spectrometry is connected by sample introduction needle.
2. system according to claim 1, is characterized in that:
Head-space sampler sampling probe negative pressure form from testing sample matrix extracts volatile constituent and enters quantitative ring, and then carrier gas is carried sample gas in quantitative ring and directly sent into ion mobility spectrometry injector, by ion mobility spectrometry, detects analysis.
3. system according to claim 1, is characterized in that: head-space sampler can be type hand head-space sampler, semi-automatic head-space sampler or automatic type head-space sampler.
4. system according to claim 1, is characterized in that: ion mobility spectrometry ionization source can be nickel source ionization source, uviol lamp ionization source or corona discharge ionization source; Injector be can pin sample introduction pyrolysis analyse injector.
5. system according to claim 1, is characterized in that:
The assembly of head-space sampler comprises: sample bottle constant temperature oven, can be from room temperature-150 ℃ with heating arrangement; Sampling and sample introduction pipeline, can be from room temperature-150 ℃ with heating arrangement; Sample introduction six-way valve, can be from room temperature-150 ℃ with heating arrangement automatically; Vapour-phase pyrolysis is analysed injector with heating arrangement, can be from room temperature-250 ℃; Transference tube, can be from room temperature-120 ℃ with heating arrangement;
The system of head-space sampler and ion mobility spectrometry coupling can total system heating, can set temperature, eliminate system cold spot, reduce sample peak broadening, increase degree of separation, make sample analysis more accurate, improve ion mobility spectrometry detection sensitivity.
6. system according to claim 1, is characterized in that: the carrier gas of using in experiment, float gas and sweep gas is Purge gas, can be purify air, nitrogen, oxygen or inert gas; Purge gas must be according to the request for utilization of migration spectrum air feed source of the gas, and process dewaters, organism.
7. according to the system described in claim 1 or 6, it is characterized in that: after sample test completes, head-space sampler system adopts Purge gas to purge sample lines, quantitatively encircle automatically, prevents cross pollution; Ion mobility spectrometry is closed carrier gas, floats gas blowback detection system, pollution abatement.
8. system according to claim 1, is characterized in that: the gas piping material therefor in system is required to be teflon, stainless steel, metallic iron or aluminium.
9. system according to claim 1, is characterized in that: head-space sampler and ion mobility spectrometry combined system can be realized automatic operation, analyzes continuously, farthest brings into play work efficiency.
10. system according to claim 1, is characterized in that: described head-space sampler has been worn air generator or gas cylinder;
Gas piping comprises gas piping that carrier gas source of the gas is connected with head-space sampler, float the gas piping that gas source of the gas is connected with ion mobility spectrometry, the gas piping that sweep gas source of the gas is connected with head-space sampler, the gas piping that carrier gas source of the gas is connected with ion mobility spectrometry;
The gas piping that the gas piping that carrier gas source of the gas is connected with head-space sampler and sweep gas source of the gas are connected with head-space sampler is provided with tensimeter; Float the gas piping that gas piping that gas source of the gas is connected with ion mobility spectrometry and carrier gas source of the gas be connected with ion mobility spectrometry and be provided with flowmeter.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105004782A (en) * | 2015-07-13 | 2015-10-28 | 天津出入境检验检疫局动植物与食品检测中心 | Method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry |
| CN106706745A (en) * | 2017-02-17 | 2017-05-24 | 神华集团有限责任公司 | Measuring device and measuring method of water content in coal liquefaction oil product |
| CN109324124A (en) * | 2018-06-29 | 2019-02-12 | 天津科技大学 | The detection method of difference small-molecule substance in efficient identification xanthochromia and normal paddy |
| CN109557226A (en) * | 2018-12-04 | 2019-04-02 | 中国科学院地质与地球物理研究所 | It is a kind of for measuring the sampling system and its sample injection method of nitrogen isotope |
| CN109781867A (en) * | 2017-11-10 | 2019-05-21 | 中国科学院大连化学物理研究所 | A kind of gas-chromatography-ion mobility spectrometry combination device for sulfur hexafluoride decomposer detection |
| CN109900769A (en) * | 2017-12-08 | 2019-06-18 | 中国科学院大连化学物理研究所 | The method and device of ammonia nitrogen in a kind of ion mobility spectrometry quantitative measurment water |
| CN110880445A (en) * | 2018-09-06 | 2020-03-13 | 同方威视技术股份有限公司 | Ion mobility spectrometer based on pulse sampling and sniffing device |
| CN113740448A (en) * | 2021-07-12 | 2021-12-03 | 南京财经大学 | Olive oil flavor detection method based on electronic nose and gas phase-ion mobility spectrometry |
| CN114242558A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Pulse purging negative-pressure pyrolysis sample suction method for ion mobility spectrometry and sample injector |
| CN114264539A (en) * | 2020-09-16 | 2022-04-01 | 中国烟草总公司郑州烟草研究院 | Solvent-assisted thermal desorption apparatus |
| CN115808462A (en) * | 2022-12-05 | 2023-03-17 | 苏州盖世生物医疗科技有限公司 | Method for eliminating ammonia gas signal and/or volatile organic amine in ion mobility spectrometry and method for detecting sample |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004782A (en) * | 2015-07-13 | 2015-10-28 | 天津出入境检验检疫局动植物与食品检测中心 | Method for fast detecting fumigation agent bromomethane residues in foods by headspace sample injection and ion mobility spectrometry |
| CN106706745A (en) * | 2017-02-17 | 2017-05-24 | 神华集团有限责任公司 | Measuring device and measuring method of water content in coal liquefaction oil product |
| CN109781867A (en) * | 2017-11-10 | 2019-05-21 | 中国科学院大连化学物理研究所 | A kind of gas-chromatography-ion mobility spectrometry combination device for sulfur hexafluoride decomposer detection |
| CN109900769A (en) * | 2017-12-08 | 2019-06-18 | 中国科学院大连化学物理研究所 | The method and device of ammonia nitrogen in a kind of ion mobility spectrometry quantitative measurment water |
| CN109324124A (en) * | 2018-06-29 | 2019-02-12 | 天津科技大学 | The detection method of difference small-molecule substance in efficient identification xanthochromia and normal paddy |
| CN110880445A (en) * | 2018-09-06 | 2020-03-13 | 同方威视技术股份有限公司 | Ion mobility spectrometer based on pulse sampling and sniffing device |
| CN109557226A (en) * | 2018-12-04 | 2019-04-02 | 中国科学院地质与地球物理研究所 | It is a kind of for measuring the sampling system and its sample injection method of nitrogen isotope |
| CN114264539A (en) * | 2020-09-16 | 2022-04-01 | 中国烟草总公司郑州烟草研究院 | Solvent-assisted thermal desorption apparatus |
| CN113740448A (en) * | 2021-07-12 | 2021-12-03 | 南京财经大学 | Olive oil flavor detection method based on electronic nose and gas phase-ion mobility spectrometry |
| CN114242558A (en) * | 2021-12-14 | 2022-03-25 | 中国科学院大连化学物理研究所 | Pulse purging negative-pressure pyrolysis sample suction method for ion mobility spectrometry and sample injector |
| CN114242558B (en) * | 2021-12-14 | 2023-11-14 | 中国科学院大连化学物理研究所 | Ion mobility spectrometry pulse purging negative pressure thermal desorption sample injector and sample injection method |
| CN115808462A (en) * | 2022-12-05 | 2023-03-17 | 苏州盖世生物医疗科技有限公司 | Method for eliminating ammonia gas signal and/or volatile organic amine in ion mobility spectrometry and method for detecting sample |
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