CN101672734A - A dynamic membrane sampler for trace components in air and method for detecting the trace components in the air - Google Patents
A dynamic membrane sampler for trace components in air and method for detecting the trace components in the air Download PDFInfo
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- CN101672734A CN101672734A CN200810200836A CN200810200836A CN101672734A CN 101672734 A CN101672734 A CN 101672734A CN 200810200836 A CN200810200836 A CN 200810200836A CN 200810200836 A CN200810200836 A CN 200810200836A CN 101672734 A CN101672734 A CN 101672734A
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Abstract
The invention relates to a dynamic membrane sampler for trace components in the air. The sampler comprises a microporous membrane carrier, a connecting tube, an injector, an absorbent, an extractant and a sealant, wherein one end of the connecting tube is embedded with the injector, while the other end of the connecting tube is inserted into the microporous membrane carrier; the microporous membrane carrier is shaped like a hollow column; the extractant is filled in the hollow position of the microporous membrane carrier; the absorbent is loaded on the solid part of the microporous membrane carrier; the other end of the microporous membrane carrier is sealed by the first sealant; the inside of the injector is provided with the extractant; the tail end of the injector is provided with a piston; and the connecting tube is shaped like an injection needle. The invention also discloses a method for using the sampler to detect the trace components in the air. The invention realizes the dynamic absorption and extraction by making the processes of absorption, reaction, extraction and enrichment of pollutants be performed simultaneously, which is favorable for continuously collecting the low-concentration pollutants and directly carrying out the post corresponding analysis and detection.
Description
[technical field]
The present invention relates to a kind of device, relate in particular to a kind of air trace components Dynamic Membrane sampling thief and detection method thereof of being used for.
[background technology]
Along with scientific-technical progress, problem of environmental pollution increasingly sharpens.Worldwide urbanization process, also making people stay in the indoor time constantly increases.Air quality in the interior space has become important environmental problem, and in pollutant research, human beings'health in pollutant serious threats such as aldehydes, chloride, aromatic.
The general concentration of gas pollutant is very low, however, still can produce very big influence to people's health.With formaldehyde is example, and long term exposure can cause breathing problem and cancer in the formaldehyde contaminated environment.Therefore the content of estimating contaminant trace species in the room air is very important.For the analytical approach of low concentration unwanted poisonous substance in the environment, mostly comprise several stages such as sampling, separation, analysis.Sampling is an important link, has directly determined Sensitivity of Analytical Method.At present, the method for sampling of trace components mainly contains initiatively methods such as (active sample), passive (passive sample), solid absorption and drop sampling in the air.Initiatively sampling method is to utilize the absorption tube that fills absorption liquid to be connected on the pump equal power device to sample, this method has characteristics such as sample rate is fast, but needs certain power-equipment, difficult carrying, the cost height is so be subject to the restriction of sampling position, place, condition.Passive sampling is based on a kind of method of sampling that gas molecule diffusion or penetration theory are gathered gaseous state in the air or steam-like pollutant.Because sampling process need not power, the sampling thief volume is little, and is very light, the sampling place is variable flexibly, can the long period be positioned over the people playground, or the place that need monitor of large tracts of land, objectively respond a period of time to be studied the exposure concentrations of object in pollutant.At present, there is the defective that operation steps is many, consuming time, consume solvent in the sampling analysis at low concentration pollutant.
Chinese patent application: 200510131960.2, a kind of portable gas chromatograph that is used for the environmental gas analysizing trace organics is disclosed.Chinese patent application: 200510047011.6, disclose a kind of and the accelerated solvent extraction device and method gas chromatography on-line coupling.But yet there are no report about being used for air trace components Dynamic Membrane sampling thief.
[summary of the invention]
The objective of the invention is, a kind of air trace components Dynamic Membrane sampling thief that is used for is provided.
One purpose more of the present invention is that a kind of method of utilizing sampling thief to detect trace components in the air is provided.
For achieving the above object, the technical scheme that the present invention takes is: a kind of air trace components Dynamic Membrane sampling thief that is used for, described sampling thief comprises the microporous barrier carrier, connecting pipe, syringe, absorbing agent, extractant, fluid sealant, described connecting pipe one end and syringe tabling, the other end inserts in the microporous barrier carrier, described microporous barrier carrier is hollow circular cylinder, extractant is equipped with in the vacancy in the microporous barrier carrier, microporous barrier carrier entity section load absorbing agent, the other end of microporous barrier carrier seals with first fluid sealant, in the described syringe extractant is housed, injector tip is provided with piston, and described connecting pipe is the injection needle shape.
Described microporous barrier carrier interior diameter: 0.5-1.0 millimeter; Overall diameter: 0.51-1.02 millimeter; Length: 20-80 millimeter.
Described microporous barrier carrier material is selected from a kind of in polyvinylidene fluoride microporous film, acetate fiber microporous barrier or the polysulfone membrane.
A kind of in described connecting pipe material selection stainless steel or the polypropylene material.
Described absorbing agent is carried in the microporous barrier carrier entity portion by ultrasonic or heating means.
Connecting pipe inserts microporous barrier carrier gap and is provided with second fluid sealant.
Described first fluid sealant and second fluid sealant are selected from a kind of in macromolecule glue or the sealing wax.
For realizing above-mentioned second purpose, the technical scheme that the present invention takes is:
A kind of method of utilizing sampling thief to detect trace components in the air comprises following key step:
(a) apply or the dipping absorbing agent at the microporous barrier carrier surface;
(b) extract extractant in the microporous barrier carrier in vacancy and the syringe by piston;
(c) other end of microporous barrier carrier seals with fluid sealant;
(d) sampling thief is placed analysis environments;
(e) cut off hermetic unit, high performance liquid chromatography or gas chromatography direct injected are carried out compartment analysis.
Sampling thief places analysis environments to drive the tested pollutant of continuous acquisition with chemical force.
The invention has the advantages that: be used for air trace components Dynamic Membrane sampling thief by the microporous barrier carrier, pollutant absorption, reaction and extracting and enriching process are carried out simultaneously, realize dynamically absorbing extraction, the continuous acquisition that helps low concentration pollutant, have the characteristics of initiatively sampling and passive sampling concurrently, and can directly carry out follow-up corresponding analyzing and testing.The whole sampling to analytic process need not additional solvent wash-out and concentration process, and not only operating process is simple, and analysis speed is fast, and saves solvent, avoids the secondary pollution that a large amount of solvents produce air because of volatilization in the routine operation process.By changing absorbing agent composition in the sampling thief, can finish the variety classes gas sampling enrichment, can be applicable to the enrichment analysis field of trace contamination gas in the air, even be applicable to that there are strict demand, little particular surroundings and field, sample space in museum etc. to pollutant load.So the present invention is having broad application prospects aspect the analysis of low concentration dusty gas.
[description of drawings]
Fig. 1 is a kind of air trace components Dynamic Membrane sampling thief structural representation that is used for.
Fig. 2 is Figure 1A-A place microporous barrier carrier sectional view.
Fig. 3 is a formaldehyde gas collection analysis high-efficient liquid phase chromatogram.
[embodiment]
Below in conjunction with accompanying drawing a kind of embodiment that is used for air trace components Dynamic Membrane sampling thief and detection method thereof provided by the invention is elaborated.
The Reference numeral and the ingredient that relate in the accompanying drawing are as follows:
1. microporous barrier carrier 2. connecting pipes
3. syringe 4. absorbing agents
5. extractant 7. pistons
61. first fluid sealant, 62. second fluid sealants
Please refer to Fig. 1, Fig. 2.
Fig. 1 is a kind of air trace components Dynamic Membrane sampling thief that is used for, this sampling thief is provided with microporous barrier carrier 1, connecting pipe 2, syringe 3, absorbing agent 4, extractant 5, first fluid sealant 61, second fluid sealant 62, described connecting pipe 2 one ends and syringe 3 tablings, the other end inserts in the microporous barrier carrier 1.Please referring to Fig. 2, described microporous barrier carrier 1 is hollow circular cylinder, and extractant 5 is equipped with in the vacancy in the microporous barrier carrier 1, microporous barrier carrier entity section load absorbing agent 4.Microporous barrier carrier 1 inside radius 11:0.5 millimeter; External radius 12:0.501 millimeter; Length: 40 millimeters.Please referring again to Fig. 1, the other end of microporous barrier carrier 1 is provided with second fluid sealant 62 with first fluid sealant, 61 sealings, connecting pipe 2 insertion microporous barrier carriers 1 gap.In the described syringe 3 extractant 5 is housed, syringe 3 ends are provided with piston 7, and described connecting pipe 2 is the injection needle shape.Described microporous barrier carrier 1 material is a polyvinylidene fluoride microporous film.Described connecting pipe 2 materials are polypropylene materials.Described absorbing agent 4 is carried in the microporous barrier carrier 1 entity portion by heating means.Described first fluid sealant, 61, the second fluid sealants 62 are sealing waxs.
Need to prove:
1,, selects and the configuration absorbing agent according to the characteristic of collected gas.Select the concrete size of microporous barrier carrier 1 according to the concentration range of collected gas.Absorbing agent is dissolved in the appropriate solvent, and solvent should have bigger viscosity and less volatility, and by ultrasonic or heating means absorbing agent is carried on the microporous barrier carrier 1.
2, extract a certain amount of extractant 5 by syringe piston 7 and inject microporous barrier carriers 1, make be full of extractant 5 in the film after, the other end seals with inertia first fluid sealant 61 at once; Extractant 5 can have dissolving power preferably to the reaction product of component to be measured and absorbing agent 4, but absorbent solvent is not dissolved or less dissolving.
3, trace components is by absorbing agent 4 reactions in diffusion and the microporous barrier carrier 1 in the analyzed air, and reaction product is further by the extractant 5 timely extracting and enrichings of microporous barrier carrier 1 inside.This is a dynamic process, and airborne pollutant constantly is absorbed, and is diffused in the extractant 5, keeps the concentration of surperficial upward product lower, and reaction velocity is faster.Avoid local absorption equilibrium, reach better concentration effect.
4, cut off first fluid sealant 61, mobile syringe piston 7 is with in the 5 whole inhalation syringes 3 of the extractant in the sampling thief.Further remove microporous barrier carrier 1.
5, extractant 5 is suitably flung to,, reached good concentration effect so that the concentration of analysans improves.
6, after extractant 5 is suitably flung to, extractant 5 is injected the high performance liquid chromatography compartment analysis of being with the quantitative sample injection ring, obtain the correlation analysis data.
The configuration of formaldehyde adsorbent: in 10ml glycerine (analyzing pure), add the 0.0010 g 2,4 dinitrophenyl hydrazine, ultrasonic concussion is standby after 2 hours.
Get the polyvinylidene fluoride microporous film of i.d * L=1 * 40mm with tweezers, place 10ml tool plug test tube (i.d=1cm), pour formaldehyde adsorbent 8ml into, ultrasonic concussion 2 hours obtains the microporous barrier carrier that load has the formaldehyde absorbing agent.
Getting external diameter is the stainless steel connecting pipe of 1mm, and an end inserts microporous barrier carrier, the other end and syringe tabling.Connecting pipe inserts microporous barrier carrier gap and is provided with the second paraffin fluid sealant.
Mobile piston, the solid first paraffin fluid sealant with fusion seals immediately behind the openend suction 200 μ l acetonitrile solvents of microporous barrier carrier, promptly makes to be used for air trace components Dynamic Membrane sampling thief.
The liquid-phase chromatographic analysis condition: high performance liquid chromatograph (Agilent, America), moving phase is acetonitrile+water=65+35, flow velocity 1ml/min, detect wavelength 365nm, analytical column be dress Inertsil ODS-3 in 250mm * 4.6mm i.d stainless-steel tube (GL Sciences, Japan).
To be used for air trace components Dynamic Membrane sampling thief vertical fixing in the formaldehyde generator, under 20 ℃ through 24 hours the sampling enrichment after, taking-up is used for air trace components Dynamic Membrane sampling thief, cut off the first paraffin fluid sealant and seal the place, mobile piston is with in the whole inhalation syringes of the extractant in the sampling thief, remove the microporous barrier carrier, directly extractant is injected the high performance liquid chromatography compartment analysis that contains 20 μ l quantitative sample injection rings, obtain correlation analysis data such as Fig. 3.(Fig. 3 is the high performance liquid chromatography elution curve, and 2,4 dinitrophenyl hydrazine is the absorbing agent ultraviolet absorption peak, and the formaldehyde phenylhydrazone is the reaction product ultraviolet absorption peak.)
Experimental group: be used for the formaldehyde (preparation is used for the method for air trace components Dynamic Membrane sampling thief with embodiment 2, and sampling thief detects the method for the formaldehyde in the trace formaldehyde generator with embodiment 2) in the air trace components Dynamic Membrane sampling thief detection trace formaldehyde generator.
Contrast experiment's group:
Equipment: spectrophotometer (U.S.'s Varian ultraviolet spectrophotometer), bubble absorption tube (glass apparatus portion of Chemical Reagent Co., Ltd., Sinopharm Group), air sampler (the grand space environmental protection in Shanghai Applied Research Laboratory), color-comparison tube (glass apparatus portion of Chemical Reagent Co., Ltd., Sinopharm Group).
Detection method: the standard determination method of formaldehyde in the indoor air: national standard " method for determining formaldehyde in the public place air " (GB/T18204.26-2000).
In table 1, list the test result of experimental group and contrast experiment group.
Table 1:
| Experimental group | Contrast experiment's group | |
| Minimal detectable concentration | ??3μg/m 3 | ??10μg/m 3 |
| Sensing range | ??5μg/m 3-400μg/m 3 | ??20μg/m 3-400μg/m 3 |
| Solvent loss | ??200μL | ??10,000μL |
Sampling thief of the present invention detects the method for trace formaldehyde and compares with gas collecting analytical approach commonly used, and it is low to detect concentration, and sensing range is big, and solvent loss is few, and is fast and convenient.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the inventive method; can also make some improvement and replenish, these improvement and replenish and also should be considered as protection scope of the present invention.
Claims (9)
1. one kind is used for air trace components Dynamic Membrane sampling thief, it is characterized in that, described sampling thief comprises the microporous barrier carrier, connecting pipe, syringe, absorbing agent, extractant, fluid sealant, described connecting pipe one end and syringe tabling, the other end inserts in the microporous barrier carrier, described microporous barrier carrier is hollow circular cylinder, extractant is equipped with in the vacancy in the microporous barrier carrier, microporous barrier carrier entity section load has absorbing agent, the other end of microporous barrier carrier seals with first fluid sealant, in the described syringe extractant is housed, injector tip is provided with piston, and described connecting pipe is the injection needle shape.
2. sampling thief according to claim 1 is characterized in that, described microporous barrier carrier interior diameter: 0.5-1.0 millimeter, overall diameter: 0.51-1.02 millimeter, length: 20-80 millimeter.
3. sampling thief according to claim 1 is characterized in that, described microporous barrier carrier material is selected from a kind of in polyvinylidene fluoride microporous film, acetate fiber microporous barrier or the polysulfone membrane.
4. sampling thief according to claim 1 is characterized in that, a kind of in described connecting pipe material selection stainless steel or the polypropylene material.
5. sampling thief according to claim 1 is characterized in that, described absorbing agent is carried in the microporous barrier carrier entity portion by ultrasonic or heating means.
6. sampling thief according to claim 1 is characterized in that, connecting pipe inserts microporous barrier carrier gap and is provided with second fluid sealant.
7. sampling thief according to claim 6 is characterized in that, described first fluid sealant and second fluid sealant are selected from a kind of in macromolecule glue or the sealing wax.
8. method of utilizing the arbitrary described sampling thief of claim 1-7 to detect trace components in the air comprises following key step:
(a) apply or the dipping absorbing agent at the microporous barrier carrier surface;
(b) extract extractant in the microporous barrier carrier in vacancy and the syringe by piston;
(c) other end of microporous barrier carrier seals with fluid sealant;
(d) sampling thief is placed analysis environments;
(e) cut off hermetic unit, high performance liquid chromatography or gas chromatography direct injected are carried out compartment analysis.
9. sampling thief according to claim 8 is characterized in that, sampling thief places analysis environments to drive the tested pollutant of continuous acquisition with chemical force.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008102008360A CN101672734B (en) | 2008-10-04 | 2008-10-04 | A dynamic membrane sampler for trace components in air and method for detecting the trace components in the air |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102008360A CN101672734B (en) | 2008-10-04 | 2008-10-04 | A dynamic membrane sampler for trace components in air and method for detecting the trace components in the air |
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| CN101672734A true CN101672734A (en) | 2010-03-17 |
| CN101672734B CN101672734B (en) | 2011-08-31 |
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| CN101907531A (en) * | 2010-07-16 | 2010-12-08 | 浙江大学 | Piston-type underwater free gas sampler and using method thereof |
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