CN103165388A - Device for mass flow air enrichment analysis mass spectrum sampling in confined space - Google Patents
Device for mass flow air enrichment analysis mass spectrum sampling in confined space Download PDFInfo
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- CN103165388A CN103165388A CN2011104272798A CN201110427279A CN103165388A CN 103165388 A CN103165388 A CN 103165388A CN 2011104272798 A CN2011104272798 A CN 2011104272798A CN 201110427279 A CN201110427279 A CN 201110427279A CN 103165388 A CN103165388 A CN 103165388A
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Abstract
The invention discloses a device for mass flow air enrichment analysis mass spectrum sampling in a confined space. The device for the mass flow air enrichment analysis mass spectrum sampling in the confined space achieves mass flow sampling on air in the confined space. Sampling is carried out, and solydimethyl siloxane tubular film carries out enrichment on organics in an air sample at the same time. After the sampling is finished, the organics adsorbed on the solydimethyl siloxane tubular film are heated to release, and enter mass spectra so as to be analyzed. The device for the mass flow air enrichment analysis mass spectrum sampling in the confined space is simple in operation, can obtain a higher detection sensitivity in a short time, and is applicable to rapid detection of trace air organics inside the confined space.
Description
Technical field
The invention belongs to mass spectrometer, particularly a kind of for the large flow gas of confined space enrichment parsing mass spectrum sampling device.This sampling device utilizes the dimethyl silicone polymer tubular film to carry out enrichment to the organic substance in gaseous sample, and carries out fast pyrogenation and analyse, and is analyzed by mass spectrometer at last.This organic substance mass spectrum sample injection method is simple to operate, and can obtain higher detection sensitivity within a short period of time, is applicable to the organic fast detecting of trace gas in confined space.
Background technology
The rapid analysis of gaseous sample is importance of analysis field, and a lot of analytical methods all have been used for the organic analyzing and testing rapidly and sensitively of gaseous sample.Current, most gaseous sample analytical method institute towards object be all gas for open spaces, and develop less for the rapid analysis of the gaseous sample in confined space.Confined space such as container, airtight transportation instrument etc., its inner gaseous sample is difficult to effectively be gathered usually.In recent years, utilize the confined spaces such as container and airtight transportation instrument to hide dangerous goods and drugs etc., become distinct issues.In addition, a lot of confined spaces such as the airtight warehouse in chemical plant have all proposed an urgent demand to the rapid analysis of gaseous sample in confined space.
Traditional gaseous sample analytical method is mainly gas chromatography.Because its analysis speed is slow, the characteristics such as complex steps can't satisfy the needs of gaseous sample rapid analysis.Flight time mass spectrum has rapid analysis speed, macroion transfer rate, high sensitivity, the high-quality of Microsecond grade and measures precision and high-resolution, and single pass namely gets the advantage of spectrum entirely.Flight time mass spectrum is in conjunction with can directly obtaining organic molecular ion peak in the resulting mass spectrogram of vacuum UV lamp soft ionization technology, and spectrogram is simple, therefore can carry out qualitative and quantitative analysis rapidly to organic pollutant.
Summary of the invention
The purpose of this invention is to provide and a kind ofly resolve mass spectrum sampling device (Fig. 1) for the enrichment of the large flow gas of confined space, can fast and effeciently analyze the gaseous sample in confined space (as container) with the coupling of Miniature Vehicle time mass spectrum instrument.
For achieving the above object, the technical solution used in the present invention is:
A kind of for the large flow gas of confined space enrichment parsing mass spectrum sampling device, comprise metal tube, heater strip, dimethyl silicone polymer tubular film and quartz capillary;
A port in metal tube is connected with the sampling electromagnetically operated valve, and the another port is connected with solenoid valve for sampling, and the another port of sampling electromagnetically operated valve is connected with sampling pipe, and the another port of solenoid valve for sampling is connected with the mass spectrum ionized region; The metal tube side has and is welded with successively two electrode columns and a side metal tube on three holes, hole, and the side metal tube is between two electrode columns and solenoid valve for sampling;
Two electrode columns space on metal tube; Heater strip is placed in metal tube, and the two ends of heater strip are welded in respectively the electrode tip place of two electrode columns; The heater strip outer cover is provided with the dimethyl silicone polymer tubular film;
Be connected with the bleeding point of aspiration pump by the electromagnetically operated valve of bleeding on the side metal tube.
One port of sampling electromagnetically operated valve is connected with metal tube, and a port of another port and sampling pipe joins; Sampling pipe is soft tube connector, and the other port of sampling pipe is installed with filter screen.
Solenoid valve for sampling one end is connected with metal pipe end opening, and the other end is connected with the mass spectrum ionized region, is fixed with quartz capillary in both junction sealings; Connect solenoid valve for sampling and mass spectrum ionized region by quartz capillary.
Electromagnetically operated valve one port of bleeding is connected in side metal tube exit, and the another port is connected with the bleeding point of aspiration pump.
The present invention stretches to confined space with sampling pipe, by aspiration pump, the gaseous sample in confined space is carried out large flow collection; Organic substance in gaseous sample carries out enrichment through the dimethyl silicone polymer tubular film; After sampling finished, organic substance was resolved through Rapid Thermal and is discharged, and enters at last mass spectrometer analysis, thereby obtains composition and the concentration of gas in confined space.
Description of drawings
Fig. 1 is of the present invention a kind of for the large flow gas of confined space enrichment parsing mass spectrum sampling device.
Embodiment
Elongated sampling pipe is inserted in confined space (as container), and the employing aspiration pump carries out the extraction of large flow to the gaseous sample of confined space inside.The gaseous sample that extracts is through dimethyl silicone polymer tubular film zone, and fully contact, make the organic substance enrichment on the dimethyl silicone polymer tubular film in gaseous sample with it, and the organic substance of last institute enrichment enters mass spectrum analysis after pyrolysis is analysed.
As shown in Figure 1, this device basic composition is sampling pipe, metal tube, heater strip, dimethyl silicone polymer tubular film and aspiration pump etc.The two ends of metal tube are connected with solenoid valve for sampling with the sampling electromagnetically operated valve respectively; The metal tube side is welded with two electrode columns and side metal tube successively, wherein the certain distance in interval between two electrode columns.The position of two electrode columns is near the sampling electromagnetically operated valve, and the position of side metal tube is near solenoid valve for sampling.Electromagnetically operated valve one port of bleeding is connected in side metal tube exit, and the another port is connected with the bleeding point of aspiration pump.Aspiration pump provides extraction power for large flow gaseous sample collection.
One port of sampling electromagnetically operated valve is connected with metal tube, and a port of another port and sampling pipe joins.Sampling pipe length is 0.1m-50m, in order to the remote conveying of gaseous sample.The other port of sampling pipe is installed with filter screen, and filter screen is in order to the solid particle etc. that extracts in elimination gas sampling process, to keep the cleaning of whole sampling apparatus.
Two electrode columns are welded in respectively the metal tube side, and both spacing distances are 0.01m-1m; The two ends of one heater strip are welded in respectively the cartridge place of two electrode columns; The heater strip outer cover has the dimethyl silicone polymer tubular film.Heater strip has played supporting role to the dimethyl silicone polymer tubular film, and it is fixed well.When organic matter pyrolysis was analysed, two electrode columns switched on power for heater strip provides voltage, and heater strip is rapidly heated, and the maintaining heat resolution temperature is 50-400 ℃, the organic substance on the dimethyl silicone polymer tubular film is carried out pyrolysis rapidly analyse.
Solenoid valve for sampling one end is connected with metal pipe end opening, and the other end is connected with the mass spectrum ionized region, and its both junction sealings are fixed with quartz capillary; Quartz capillary connects solenoid valve for sampling and mass spectrum ionized region, is sent to the mass spectrum ionized region in order to the organic substance that pyrolysis is analysed, and carries out mass spectral analysis.
Sampling electromagnetically operated valve, solenoid valve for sampling and the electromagnetically operated valve of bleeding are by software control, and each comfortable various process is in different open/close states, and guarantees mass spectral:mass spectrographic vacuum degree requirement etc.During sampling, aspiration pump is opened, and sampling electromagnetically operated valve, the electromagnetically operated valve of bleeding are opened, and solenoid valve for sampling is closed; After sampling finished, aspiration pump cut out, sampling electromagnetically operated valve, the closed electromagnetic valve of bleeding; Solenoid valve for sampling is opened, and electrode column begins power supply simultaneously, makes heater strip carry out Fast Heating to PDMS membrane.
This device basic composition is sampling pipe 2, metal tube 3, heater strip 7, dimethyl silicone polymer tubular film 9 and aspiration pump 10 etc.The two ends of metal tube 3 are connected with solenoid valve for sampling 5 with sampling electromagnetically operated valve 4 respectively; Metal tube 3 sides have and are welded with successively two electrode columns 8 and side metal tube 13 on three holes, hole, the certain distance in interval between two electrode columns 8 wherein, and near sampling electromagnetically operated valve 4, and the position of side metal tube 13 is near solenoid valve for sampling 5.
One port of sampling electromagnetically operated valve 4 is connected with metal tube 3, and a port of another port and sampling pipe 2 joins.Sampling pipe 2 length are 0.1m-50m, in order to the remote extraction of gaseous sample.The other port of sampling pipe 2 is installed with filter screen 1, and filter screen 1 is in order to the solid particle etc. that extracts in elimination gas sampling process, to keep the cleaning of whole sampling apparatus.
Two electrode columns 8 are welded in respectively metal tube 3 sides, and both spacing distances are 0.01m-1m; The two ends of one heater strip 7 are welded in respectively the cartridge place of two electrode columns 8; Heater strip 7 outer cover have dimethyl silicone polymer tubular film 9.7 pairs of dimethyl silicone polymer tubular films 9 of heater strip have played supporting role, and it is fixed well.When organic matter pyrolysis was analysed, two electrode columns 8 switched on power for heater strip 7 provides voltage, and heater strip 7 is rapidly heated, and the maintaining heat resolution temperature is 50-400 ℃, the organic substance on dimethyl silicone polymer tubular film 9 is carried out pyrolysis rapidly analyse.
Solenoid valve for sampling 5 one ends are connected with metal tube 3 ports, and the other end is connected with mass spectrum ionized region 12, and its both junction sealings are fixed with quartz capillary 11; Quartz capillary 11 connects solenoid valve for sampling 5 and mass spectrum ionized region 12, is sent to mass spectrum ionized region 12 in order to the organic substance that pyrolysis is analysed, and carries out mass spectral analysis.
Concrete operations:
Before sampling beginning, aspiration pump 10, sampling electromagnetically operated valve 4, bleed electromagnetically operated valve 6 and solenoid valve for sampling 5 all are in closed condition.
Sampling: open aspiration pump 10, the sampling head of sampling pipe 2 is stretched in sample area (as container and airtight transportation instrument); Software control sampling electromagnetically operated valve 4 and the electromagnetically operated valve 6 of bleeding are opened simultaneously, and be extracted this moment under the dynamic action of aspiration pump 10 the large flow of gaseous sample in sample area; Gaseous sample is through filter screen 1, its floating particle thing that may contain with elimination; Gaseous sample is through dimethyl silicone polymer tubular film 9 zones, its organic substance that contains enrichment on dimethyl silicone polymer tubular film 9; After dimethyl silicone polymer tubular film 9 rich regions, gaseous sample is discharged by the gas outlet through aspiration pump 10; After certain sampling time, close simultaneously sampling electromagnetically operated valve 4 and the electromagnetically operated valve 6 of bleeding, close aspiration pump 10, sampling finishes.
Process is analysed in pyrolysis: open solenoid valve for sampling 5, control electrode post 8 begins power supply simultaneously, controls heater strip 7 and carries out Fast Heating, and the maintaining heat resolution temperature is 50-400 ℃; 7 pairs of dimethyl silicone polymer tubular films of heater strip 9 carry out Fast Heating.Organic substance at high temperature discharges from dimethyl silicone polymer tubular film 9, under the low pressure effect of mass spectrum ionized region 12, in quartz capillary 11 enters into mass spectrum ionized region 12, carries out mass spectral:mass spectrographic rapid analysis.
Claims (4)
1. one kind is used for the large flow gas of confined space enrichment parsing mass spectrum sampling device, it is characterized in that: comprise metal tube (3), heater strip (7), dimethyl silicone polymer tubular film (9) and quartz capillary (11);
A port in metal tube (3) is connected with sampling electromagnetically operated valve (4), the another port is connected with solenoid valve for sampling (5), the another port of sampling electromagnetically operated valve (4) is connected with sampling pipe (2), and the another port of solenoid valve for sampling (5) is connected with mass spectrum ionized region (12); Metal tube (3) side has and is welded with successively two electrode columns (8) and a side metal tube (13) on three holes, hole, and side metal tube (13) is positioned between two electrode columns (8) and solenoid valve for sampling (5);
Two electrode columns (8) are in the upper space of metal tube (3); Heater strip (7) is placed in metal tube (3), and the two ends of heater strip (7) are welded in respectively the electrode tip place of two electrode columns (8); Heater strip (7) outer cover is provided with dimethyl silicone polymer tubular film (9);
Side metal tube (13) is upper to be connected by the bleeding point of the electromagnetically operated valve of bleeding (6) with aspiration pump (10).
2. sampling device according to claim 1 is characterized in that: a port of sampling electromagnetically operated valve (4) is connected with metal tube (3), and a port of another port and sampling pipe (2) joins; Sampling pipe (2) is soft tube connector, and the other port of sampling pipe (2) is installed with filter screen (1).
3. sampling device according to claim 1, it is characterized in that: solenoid valve for sampling (5) one ends are connected with metal tube (3) port, the other end is connected with mass spectrum ionized region (12), is fixed with quartz capillary (11) in both junction sealings; Connect solenoid valve for sampling (5) and mass spectrum ionized region (12) by quartz capillary (11).
4. sampling device according to claim 1 is characterized in that: electromagnetically operated valve (6) one ports of bleeding are connected in side metal tube (13) exit, and the another port is connected with the bleeding point of aspiration pump (10).
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| CN2011104272798A CN103165388A (en) | 2011-12-19 | 2011-12-19 | Device for mass flow air enrichment analysis mass spectrum sampling in confined space |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104714043A (en) * | 2013-12-13 | 2015-06-17 | 中国科学院大连化学物理研究所 | Fully automatic sample introduction device for real-time analysis of dioxin precursor in online mass spectrometry |
| CN104716004A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Sampling device for non-contact type heating tubular film in mass spectrum ionization source |
| CN105372357A (en) * | 2015-12-17 | 2016-03-02 | 吕梁学院 | Ionization, adsorption and enrichment device |
| CN105590827A (en) * | 2014-11-13 | 2016-05-18 | 中国科学院大连化学物理研究所 | Mass spectrum low-temperature enrichment high-temperature thermal analysis sweeping type membrane sample feeding apparatus and application |
| CN105719934A (en) * | 2014-12-05 | 2016-06-29 | 中国科学院大连化学物理研究所 | Double film sample introduction apparatus |
| CN108072550A (en) * | 2016-11-17 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of absorption-thermal desorption device of ceramic heat |
| CN109308990A (en) * | 2018-09-25 | 2019-02-05 | 公安部第三研究所 | Sampling system for ionic migration spectrum detector |
| CN109839295A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | One kind being enriched with absorption-thermal desorption device for trace samplings |
| CN111289604A (en) * | 2020-03-16 | 2020-06-16 | 北京卫星环境工程研究所 | Membrane separation type trace gas detection device used in low-pressure hydrogen environment |
| CN108692998B (en) * | 2018-05-14 | 2020-09-22 | 清华大学深圳研究生院 | Sample introduction method for gas detection |
| CN112103171A (en) * | 2020-09-18 | 2020-12-18 | 中国科学院空天信息创新研究院 | Passive sample introduction device and application |
| CN113466316A (en) * | 2021-07-02 | 2021-10-01 | 中国科学院合肥物质科学研究院 | Mass spectrum detection method and device for rapidly analyzing chemical components of particles on filter membrane |
| CN113917050A (en) * | 2021-07-21 | 2022-01-11 | 北京师范大学 | Total volatile organic compound navigation monitor |
| CN114235513A (en) * | 2021-12-27 | 2022-03-25 | 盐城工学院 | Indoor volatile pollutant adsorption sampling device and sampling method |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104714043A (en) * | 2013-12-13 | 2015-06-17 | 中国科学院大连化学物理研究所 | Fully automatic sample introduction device for real-time analysis of dioxin precursor in online mass spectrometry |
| CN104716004A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Sampling device for non-contact type heating tubular film in mass spectrum ionization source |
| CN104716004B (en) * | 2013-12-15 | 2017-06-06 | 中国科学院大连化学物理研究所 | Non-contact thermal tubular film sampling device in a kind of mass spectrum ionization source |
| CN105590827A (en) * | 2014-11-13 | 2016-05-18 | 中国科学院大连化学物理研究所 | Mass spectrum low-temperature enrichment high-temperature thermal analysis sweeping type membrane sample feeding apparatus and application |
| CN105590827B (en) * | 2014-11-13 | 2017-07-28 | 中国科学院大连化学物理研究所 | A kind of sweeping type film sampling device of mass spectrum low temperature enrichment high temperature pyrolysis analysis and application |
| CN105719934A (en) * | 2014-12-05 | 2016-06-29 | 中国科学院大连化学物理研究所 | Double film sample introduction apparatus |
| CN105372357A (en) * | 2015-12-17 | 2016-03-02 | 吕梁学院 | Ionization, adsorption and enrichment device |
| CN105372357B (en) * | 2015-12-17 | 2017-04-05 | 吕梁学院 | A kind of ionization adsorption and enrichment device |
| CN108072550A (en) * | 2016-11-17 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of absorption-thermal desorption device of ceramic heat |
| CN108072550B (en) * | 2016-11-17 | 2020-03-10 | 中国科学院大连化学物理研究所 | Adsorption-thermal desorption device for ceramic heating |
| CN109839295A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | One kind being enriched with absorption-thermal desorption device for trace samplings |
| CN108692998B (en) * | 2018-05-14 | 2020-09-22 | 清华大学深圳研究生院 | Sample introduction method for gas detection |
| CN109308990A (en) * | 2018-09-25 | 2019-02-05 | 公安部第三研究所 | Sampling system for ionic migration spectrum detector |
| CN111289604A (en) * | 2020-03-16 | 2020-06-16 | 北京卫星环境工程研究所 | Membrane separation type trace gas detection device used in low-pressure hydrogen environment |
| CN112103171A (en) * | 2020-09-18 | 2020-12-18 | 中国科学院空天信息创新研究院 | Passive sample introduction device and application |
| CN112103171B (en) * | 2020-09-18 | 2023-10-13 | 中国科学院空天信息创新研究院 | Passive sample injection device and application |
| CN113466316A (en) * | 2021-07-02 | 2021-10-01 | 中国科学院合肥物质科学研究院 | Mass spectrum detection method and device for rapidly analyzing chemical components of particles on filter membrane |
| CN113917050A (en) * | 2021-07-21 | 2022-01-11 | 北京师范大学 | Total volatile organic compound navigation monitor |
| CN113917050B (en) * | 2021-07-21 | 2022-05-27 | 北京师范大学 | Total volatile organic compound navigation monitor |
| CN114235513A (en) * | 2021-12-27 | 2022-03-25 | 盐城工学院 | Indoor volatile pollutant adsorption sampling device and sampling method |
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Application publication date: 20130619 |