CN103529115B - A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device - Google Patents
A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device Download PDFInfo
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- CN103529115B CN103529115B CN201210234821.2A CN201210234821A CN103529115B CN 103529115 B CN103529115 B CN 103529115B CN 201210234821 A CN201210234821 A CN 201210234821A CN 103529115 B CN103529115 B CN 103529115B
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Abstract
The present invention devises a kind of directly-heated type tubular film for on-line mass spectroscopy and is enriched with sampling device, including: tubular film, heater strip, film sample introduction cavity, carrier gas, sample introduction metal tube and emergency cut-off magnetic valve.Tubular film is atresia densification polydimethylsiloxane tubular film.Device use tubular film to sample feeding fast enriching；Outside film, uniform winding heater strip is as film heating device；Film outboard chambers is connected formation negative pressure state by metal capillary with mass spectrum；Added with carrier gas device outside film.Tubular film is under the effect of stretching, heating, pressure reduction and carrier gas, and sample can be enriched with through tubular film rapidly.Improve sample transmitance in film sampling device and transmission rates.
Description
Technical field
The invention belongs to mass spectrometer, particularly to a kind of directly-heated type for on-line mass spectroscopy
Tubular film enrichment sampling device.This device can realize volatility in fluid sample and gaseous sample to be had
The on-line preconcentration of organic pollutants.Analysis sample is made under the effect of stretching, pressure reduction, heating and carrier gas
Product fast strikethrough film is enriched with in film outboard chambers, and is brought into mass spectrum ionized region electricity by carrier gas
From.Improve sample transmitance in film sampling device and transmission rates.
Background technology
Volatilizable and although half volatile organic contaminant concentration is low in water and air, but greatly
There are pathogenic, teratogenesis and carcinogenesis more.So to the on-line checking of organic pollution in environment
It is constantly subjected to the extensive concern of people.After conventional detection method is usually field sample collection,
Carry out pretreatment and enrichment at the laboratory sample to collecting, re-use gas phase and liquid phase chromatograph-
Mass spectrum (GC/LC-MS) is analyzed.Although the method is highly sensitive, but spent time is longer
(general a few minutes are to dozens of minutes).From sampling analysis group laboratory treatment sample
Divide it may happen that change thus impact analysis result.Connecting online environmental sample can not be realized
Continuous detection.So it is dirty for Organic substance in magnanimity environmental sample to explore online quickly detection method
The analysis of dye thing is extremely important.
Film sample introduction utilizes pervaporation effect to achieve mass spectrographic direct, continuous sample introduction, connexus
Spectrum has become as one of online quickly analysis maximally effective technology of volatile organic matter.Meanwhile, by
In the selective penetrated property of semipermeable membrane, inorganic matter is more difficult passes through for nitrogen in water and air, oxygen etc.
Film, and volatility and semi-volatile organic matter are easy to be enriched with through film.But, ordinary tablet
Shape film sampling device makes membrane area little to meet mass spectrum vacuum requirement, and film is the thinnest easily
Rupture.Membrane area is little to be contacted with sample less, causes film sampling preconcentration efficiency to reduce.Conventional tubular
Although film specific surface area is relatively big, but wall thickness is few compared with making greatly sample transmitance, enrichment effect
Rate is low, and penetration speed is relatively slow, and the response time of film is longer, and is not suitable as the quickly side of detection
Method.
Thus, the present invention devises a kind of directly-heated type tubular film for on-line mass spectroscopy and is enriched with sample introduction
Device, sample can stretch at film, pressure reduction, heating and carrier gas effect under rapidly through film, with
Improve sample transmitance in film sampling device and transmission rates.
Summary of the invention
It is an object of the invention to provide a kind of directly-heated type tubular film for on-line mass spectroscopy to be enriched with
Sampling device.
A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device, including film sample cavity
Body, tubular film is placed in film sample cavity body, and tubular film can be stretched the length of 1-5 times vertically
Using after degree, the tubular film after stretching can effectively reduce tubular film wall thickness.Film two ends are even
Connect metal capillary as sample inlet and outlet, be provided with in sample inlet metal capillary
Grain drainage screen, heater strip is evenly around outside film, at film sample introduction cavity near the sidewall exported
On offer through hole as carrier gas inlet；Open on the sidewall of sample inlet at film sample introduction cavity
Be provided with through hole as connect mass spectrum ionized region interface, seam is provided with the second metal capillary,
Equipped with emergency cut-off magnetic valve on the second metal capillary of seam.
When sample introduction is fluid sample, sample inlet front end arranges peristaltic pump and fluid sample is sent into pipe
In shape film, discharge from using outlet；When sample introduction is gaseous sample, sample inlet front end arranges and takes out
Gaseous sample is sent in tubular film by air pump, from use outlet discharge, when sampling analysis sample relatively
Time few, circulation sample introduction can be set.
Tubular film material is PDMS membrane, and this film is semipermeable membrane, and can vertically by
Use after stretching the length of 1-5 times.Heater strip is nichrome wire, is connected by wire
DC voltage.Carrier gas interface is Capillary restrictor, and carrier gas is: helium (He) or nitrogen (N2).
Film sample introduction cavity is connected with mass spectrum ionized region by metal capillary, utilizes mass spectrum vacuum bar
Part maintains film outboard chambers to form negative pressure state.Sample through film enters matter under carrier gas effect
Spectrum ionized region is ionized.
In sampling process, liquid or gaseous sample enter in tubular film from sample inlet, at film
Promote sample molecule diffusion in film under inside and outside differential pressure action, improve passing through of sample
Rate and penetration speed speed.Outside film, the heater strip of uniform winding is tubular film heating, can accelerate
Sample is desorption from film surface, improves the sample speed by film.Carrier gas is rapidly by outside film
On analyte take mass spectrum ionized region in be ionized.
Advantages of the present invention:
Use after tubular film is stretched vertically the length of 1-5 times, effectively reduce pipe
Shape membranous wall is thick.And utilize mass spectrum vacuum condition to make tubular film outboard chambers form condition of negative pressure, film
The pressure reduction in interior outside accelerates sample molecule diffusion in film, improve sample transmitance and
Transmission rates.
Uniform winding heater strip outside tubular film, accelerates sample from film for the heating of tubular film outer surface
The desorption on surface.
Carrier gas can be by the sample purge desorption on tubular film outer surface and be brought into rapidly mass spectrum
Ionized region is ionized detection.The effect of stretching, pressure reduction, heating and carrier gas can increase sample
Speed and penetration speed rate through film.
Directly-heated type tubular film enrichment sampling device, it is possible to achieve the most online inspection to environmental sample
Survey.
Accompanying drawing explanation
Fig. 1 is that a kind of directly-heated type tubular film for on-line mass spectroscopy of the present invention is enriched with sampling device
Structural representation.
Detailed description of the invention
In order to improve sample transmitance in film sampling device and transmission rates.The present invention provides
A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device.
As it is shown in figure 1, the present invention is applied to mass spectrometer, wherein 1 is tubular film, and 2 for adding
Heated filament, 3 is film sample introduction cavity, and 4 is particle filtering net, and 5 is sample inlet, and 6 for sampling out
Mouthful, 7 is sampling metal capillary, and 8 is film outboard chambers, and 9 is carrier gas inlet, and 10 is the
Two metal capillaries are also directly connected to mass spectrum ionized region, and 11 is emergency cut-off magnetic valve.Wherein
During fluid sample, sample inlet 5 front end arranges peristaltic pump and is sent into by fluid sample in tubular film 1,
Discharge from sample outlet 6；During gaseous sample, sample inlet 5 front end arranges air pump by gas
Sample is sent in tubular film 1, discharges from sample outlet 6, can when sampling analysis sample is less
Circulation sample introduction is set.
A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device, including airtight film
Sample introduction cavity, tubular film is placed in film sample cavity body, and tubular film two ends connect metal kernel respectively
Tubule, it is external that metal capillary extend out to film sample cavity in film sample cavity body, the gold at film two ends
Belong to capillary tube respectively as sample inlet and outlet.It is in the metal capillary at sample inlet
Being provided with particle filtering net, heater strip is evenly around the outside at tubular film, at film sample introduction cavity
Through hole is offered as carrier gas inlet, at film sample introduction cavity near sampling on the sidewall of outlet
Offering through hole on the sidewall of import as connecting mass spectrum ionized region interface, seam is provided with the
Two metal capillaries, equipped with emergency cut-off magnetic valve on the second metal capillary of seam.
Directly-heated type tubular film enrichment sampling device is connected with mass spectrum and can realize environmental sample
On-line preconcentration and quickly detection.In directly-heated type tubular film of the present invention enrichment sampling device, utilize
Environmental sample is delivered in tubular film by peristaltic pump or air pump, adds a granule mistake before sampling injection port
Filter screen is removed particulate matter in sample and is carried out protecting film device.
The tubular film that the present invention uses is PDMS membrane, and is stretched 3 times of length
Rear use.During detection, analysis sample continues through sample inlet through particle filtering net filtration and enters
Enter in tubular film.When analyzing sample and being less, it is possible to use circulation sample introduction.Film outboard chambers
Maintaining negative pressure state by mass spectrum vacuum system, volatility and half volatile organic contaminant are at film
Rapidly through film under inside and outside differential pressure effect, it is enriched with in film outboard chambers.Uniformly twine outside film
Around heater strip heating and carrier gas effect under, make the Organic substance can be rapidly the most attached also from film surface desorption
It is brought into the ionization of mass spectrum ionized region analyzed detection by carrier gas.
Between sample introduction metal capillary between directly-heated type tubular film enrichment sampling device and mass spectrum
On equipped with emergency cut-off magnetic valve.When film rupture, mass spectrum vacuum can change rapidly, the tightliest
Eager power-off magnet valve can be closed rapidly, to protect mass spectrometer.
Claims (4)
1. the directly-heated type tubular film enrichment sampling device for on-line mass spectroscopy, it is characterised in that:
Including airtight film sample introduction cavity (3), tubular film (1) is placed in film sample introduction cavity (3),
Tubular film two ends connect metal capillary (7) respectively, and metal capillary (7) is from film sample introduction cavity (3)
Inside extend out to film sample introduction cavity (3) outward, the metal capillary (7) at film two ends respectively as sample into
Mouth (5) and outlet (6)；
Particle filtering net (4) it is provided with in being in the metal capillary (7) at sample inlet (5) place,
Heater strip (2) is evenly around the outside in tubular film (1), at film sample introduction cavity (3) near outlet
(6) through hole is offered on sidewall as carrier gas (9) import, at film sample introduction cavity (3) near adopting
Offer on the sidewall of sample import (5) through hole as connect mass spectrum ionized region interface, seam is provided with
Second metal capillary (10), equipped with emergency cut-off on second metal capillary (10) of seam
Electromagnetic valve (11), described tubular film (1) material is polydimethylsiloxane, polydimethylsiloxane
Film is semipermeable membrane, and commercially available tubular film can be stretched vertically after the length of 1-5 times and use,
Tubular film after stretching can effectively reduce tubular film wall thickness.
Directly-heated type tubular film the most according to claim 1 enrichment sampling device, it is characterised in that:
When sample introduction is fluid sample, described sample inlet (5) front end arranges peristaltic pump and is sent by fluid sample
Enter in tubular film (1), discharge from outlet (6)；
When sample introduction is gaseous sample, described sample inlet (5) front end arranges air pump and is sent by gaseous sample
Enter in tubular film (1), discharge from outlet (6).
Directly-heated type tubular film the most according to claim 1 enrichment sampling device, it is characterised in that:
Described heater strip (2) is nichrome wire, and it connects DC voltage by wire.
Directly-heated type tubular film the most according to claim 1 enrichment sampling device, it is characterised in that:
Described carrier gas (9) import uses Capillary restrictor, and carrier gas is: helium (He) or nitrogen (N2)。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210234821.2A CN103529115B (en) | 2012-07-05 | 2012-07-05 | A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210234821.2A CN103529115B (en) | 2012-07-05 | 2012-07-05 | A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device |
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| Publication Number | Publication Date |
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| CN103529115A CN103529115A (en) | 2014-01-22 |
| CN103529115B true CN103529115B (en) | 2016-12-21 |
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| CN201210234821.2A Active CN103529115B (en) | 2012-07-05 | 2012-07-05 | A kind of directly-heated type tubular film for on-line mass spectroscopy is enriched with sampling device |
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Families Citing this family (13)
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| AU2015230905B2 (en) * | 2014-03-19 | 2019-11-21 | Philip Morris Products S.A. | Aerosol-generating devices incorporating an intertwined wick and heating element |
| CN105655225B (en) * | 2014-11-13 | 2017-09-15 | 中国科学院大连化学物理研究所 | A kind of film sampling device of mass spectrum fast enriching Thermal desorption 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 |
| CN105181419B (en) * | 2015-10-22 | 2017-11-17 | 中国科学院合肥物质科学研究院 | The online and offline detection means and detection method of volatile organic matter in a kind of ultrasonic atomizatio extraction water body |
| CN105372357B (en) * | 2015-12-17 | 2017-04-05 | 吕梁学院 | A kind of ionization adsorption and enrichment device |
| CN109841482B (en) * | 2017-11-27 | 2020-07-21 | 中国科学院大连化学物理研究所 | Enrichment sampling and ionization device for volatile organic compounds in liquid sample |
| CN109839421A (en) * | 2017-11-27 | 2019-06-04 | 中国科学院大连化学物理研究所 | The method quickly detected for the direct mass spectrography of semi-volatile organic matter in liquid |
| CN111199861B (en) * | 2018-11-20 | 2020-12-15 | 中国科学院大连化学物理研究所 | Capillary micro-reaction ionization source |
| CN111220694B (en) * | 2018-11-27 | 2021-09-28 | 中国科学院大连化学物理研究所 | Mass spectrometry device and method for wide concentration range online monitoring |
| CN110144566B (en) * | 2019-06-20 | 2021-09-14 | 枣庄学院 | Physical vapor deposition sample heating device |
| CN113607800B (en) * | 2021-07-27 | 2023-08-25 | 中国计量科学研究院 | Rapid mass spectrum detection device and detection method for detecting rubber content in plants |
| CN114002306A (en) * | 2021-11-12 | 2022-02-01 | 暨南大学 | Membrane sample injection structure for extracting volatile organic compounds in water through bubble enrichment |
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