CN105510278A - Test method for particle filtering efficiency of thermal desorption liner tube - Google Patents
Test method for particle filtering efficiency of thermal desorption liner tube Download PDFInfo
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- CN105510278A CN105510278A CN201410495425.4A CN201410495425A CN105510278A CN 105510278 A CN105510278 A CN 105510278A CN 201410495425 A CN201410495425 A CN 201410495425A CN 105510278 A CN105510278 A CN 105510278A
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- thermal desorption
- bushing pipe
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Abstract
The invention discloses a test method for particle filtering efficiency of a thermal desorption liner tube. The test method includes the following steps: arranging the thermal desorption liner tube requiring filtering efficiency test into a thermal desorption device; adjusting the thermal desorption device into working status; injecting a certain volume of silicon dioxide microsphere solution dispersed in an organic solvent into the thermal desorption device through a micro-sample injector; collecting penetrated silicon dioxide microspheres with a pure liquid at the outlet of the thermal desorption device; detecting the concentration of the collected silicon dioxide microspheres with an evaporative light-scattering detector to obtain a peak area A; with a blank liner tube not filled with the filter medium, re-doing the operations above to obtain a peak area A0; and calculating the filtering efficiency of the thermal desorption liner tube to particles being x in particle size according to the following formula: (1-A/A0)*100%. The test method is reliable in result and is quick to carry out. The result can directly reflect the filtering efficiency of the thermal desorption liner tube filled with the filter medium.
Description
Technical field
The present invention relates to sampling sample preparation field, specifically, relate to and a kind ofly evaluate the method for Thermal desorption process to the filtration efficiency of particle in sample.
Background technology
Thermal desorption is a kind of Sample introduction commonly used in gas chromatography or field of mass spectrometry.Common Thermal desorption sampling technique is that the sample of Water demand is put into a Thermal desorption bushing pipe, carrier gas is passed into after bushing pipe sealing, to bushing pipe heating, the volatility in sample or half volatile component are parsed from sample, sent in gas chromatography or mass spectrum by carrier gas and analyze.The sample analyzed enter in chromatographic system or mass spectrometer system owing to may have particle can be carried by carrier gas in heating process, along with the accumulation of particle in gas chromatography or mass spectrometer system, accurate instrument system can break down very soon, also likely occurs to analyze the phenomenons such as thing loss, background signal rising, peak stretching, overlap of peaks.Therefore, before parsing air-flow introduces analytic system, the particle of suspension must be removed as far as possible.For addressing this problem, prior art in Thermal desorption bushing pipe, loads filter packing (as deactivation glass fiber, granular filter material etc.) filter.But, load the difference of material, filling operating parameter (as loaded density, loading volume etc.) impact on the filtration efficiency under Thermal desorption bushing pipe duty, still lack applicable method at present and carry out evaluating or testing.
Summary of the invention
The object of the present invention is to provide a kind of test loaded filtrate Thermal desorption bushing pipe to the method for particle filtration efficiency, to evaluate the impact on filter effect such as various filtrate and filling parameter quantitatively, obtain best filtering scheme, to protect follow-up gas chromatography or mass spectrometer system better; Also can be simultaneously and manufacture the Thermal desorption bushing pipe that processing has a good particle filtering function guidance is provided.
In order to realize foregoing invention object, the technical solution used in the present invention is:
A kind of method of testing of Thermal desorption bushing pipe particle filtration efficiency, containing filter medium in described Thermal desorption bushing pipe, Thermal desorption bushing pipe is placed in hot parser, and Thermal desorption carrier gas is introduced through Thermal desorption bushing pipe from hot parser upper end, flows out from the lower end outlet of hot parser.
1) in the Thermal desorption bushing pipe being in working temperature, inject dispersion silicon dioxide microsphere solution in organic solvent, the particle diameter of silicon dioxide microsphere is d; A conduit is provided with in the exit, lower end of hot parser, tube at one end exports with the lower end of hot parser and is connected, the conduit other end stretches under the liquid levels of splendid attire in container, the silicon dioxide microsphere penetrating filter medium in Thermal desorption bushing pipe carried out by carrier gas with liquid collection; By the silicon dioxide microsphere concentration of collecting in evaporative light-scattering detector tracer liquid, obtain peak area A;
2) adopt containing the blank bushing pipe of filter medium, repeat above step 1) operating process, obtain peak area A0;
3) by (1-A/A0) * 100% formulae discovery to obtain containing the Thermal desorption bushing pipe of filter medium be the filtration efficiency of the particle of d to particle diameter.
The mass concentration scope 0.05% ~ 10% of described dispersion silicon dioxide microsphere in organic solvent.
The particle diameter d scope 0.01 ~ 10 micron of described silicon dioxide microsphere.
The organic solvent of described dispersed silicon dioxide microballoon is boiling point lower than the organic solvent of 80 DEG C.
Described organic solvent is one or more mixed solutions in methyl alcohol, ethanol, acetone, acetonitrile.
Described liquid is any one or two kinds of mixing in pure water, methyl alcohol, ethanol, acetone, acetonitrile.
Filter medium in described Thermal desorption bushing pipe is one or more combinations in glass fibre hair, quartz fibre hair, silica sand or silica gel.
The working temperature of described Thermal desorption bushing pipe is more than or equal to the boiling point of organic solvent in silicon dioxde solution, usual 80 – 600 DEG C.
Described carrier gas is one in nitrogen or helium or two kinds; Thermal desorption bushing pipe internal diameter 2mm-1cm, injecting dispersion silicon dioxide microsphere solution injection rate IR in organic solvent in Thermal desorption bushing pipe is 1 microlitre-100 microlitre.
Technical scheme of the present invention is based on following Cleaning Principle:
When dispersion silicon dioxide microsphere solution in organic solvent injects and is in the Thermal desorption bushing pipe of working temperature, because the temperature in bushing pipe is greater than or equal to the boiling point of organic solvent, causes organic solvent to gasify rapidly and form silicon dioxide microsphere gasoloid.After filter medium, a part of silicon dioxide microsphere is absorbed or is adsorbed, and remaining particle flows out, by the liquid collection exported out with the outlet of Thermal desorption air-flow from hot parser.The silicon dioxide microsphere concentration collected uses evaporative light-scattering detector to detect, and obtains peak area A.When not loading filter packing in Thermal desorption bushing pipe, particle can all pass through, and the signal of now evaporative light-scattering detector detection is the strongest, obtains signal peak area A 0.The value of A is lower shows that the particle through filtrate is fewer, and the filtration efficiency of Thermal desorption bushing pipe is higher.By formula E=(1-A/A0) * 100%, filtration efficiency E can be calculated.
Beneficial effect main manifestations of the present invention is in the following areas:
One, the present invention tests in the hot parser course of work, and test condition is identical with actual Thermal desorption condition, reliable test result, detects and has feature accurately and rapidly.
Two, the present invention mainly tests the filtration efficiency of Thermal desorption bushing pipe in Thermal desorption process, can react the Thermal desorption bushing pipe being filled with filtering material be stopped by particle and make it not enter gas chromatography or mass spectrometer system, testing result directly reflects the quality of the Thermal desorption bushing pipe filtration efficiency loading filtrate.
Three, the present invention is applicable to test Thermal desorption bushing pipe to the filtration efficiency of the particle of different-grain diameter under Thermal desorption condition, the detailed dependence between filtration efficiency and particle size can be obtained, contribute to studying and load parameter (load density, the load volume) impact on filtration efficiency.
Four, the present invention is without the need to special filtration efficiency proving installation, and testing cost is low, simple to operate, be beneficial to promotion and implementation.
Embodiment
Below in conjunction with embodiment, the present invention is described, is used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1
One is loaded the deactivation glass fibre hair (10mg that diameter is 5 microns, load length 1cm) Thermal desorption bushing pipe (internal diameter 4mm) load in hot parser, open circuit and the air circuit breaker of hot parser, treat that hot parser resolution temperature and resolution gas flow velocity reach setting value (resolution temperature 150 DEG C, resolution gas flow velocity: 5mL/min), hot parser is in normal operating conditions, and hot parser outlet kapillary inserts one and is loaded with in the sample vial of 300 microlitre pure water;
In hot parser, the 100nm silicon dioxide single dispersing methanol solution that 2 microlitre mass concentrations are 2.5% is injected with micro-sampling pin;
Aqueous solution in sample vial is sent into evaporative light-scattering detector detect, the signal peak area A that recording solution enters evaporative light-scattering detector generation is 2mv.s.
Change an empty Thermal desorption bushing pipe, in hot parser, inject the 100nm silicon dioxide single dispersing methanol solution that 2 microlitre mass concentrations are 2.5%;
Aqueous solution in sample vial is sent into evaporative light-scattering detector detect, the signal peak area A 0 that recording solution enters evaporative light-scattering detector generation is 80mv.s.
Calculate according to formula E=(1-A/A0) * 100%, filtration efficiency E is 97.5%.
Embodiment 2
As described in Example 1, the silicon dioxide microsphere solution wherein injected is the silicon dioxide ethanolic solution of 50 microlitre 0.05% particle diameter 500nm, and the Thermal desorption temperature of test is 300 DEG C, and Thermal desorption gas velocity is 3mL/min, and acquisition A0 is 132mv.s, A is 4.7mv.s.
Calculate according to formula E=(1-A/A0) * 100%, filtration efficiency E is 96.4%.Result shows, same Thermal desorption bushing pipe is discrepant to the filtration efficiency of the particle of different-grain diameter under different operating conditions.
Embodiment 3
As described in Example 1, wherein Thermal desorption bushing pipe (internal diameter 3mm) is 120 ~ 160 micron quartz sand for having loaded 380mg particle diameter, loading length is 2 centimetres, the silicon dioxide microsphere solution of injection is the silicon dioxide acetonitrile solution of the 300nm of 2 microlitres 10%, the Thermal desorption temperature of test is 350 DEG C, Thermal desorption flow rate of carrier gas is 10mL/min, and acquisition A0 is 576mv.s, A is 36.7mv.s.
Calculate according to formula E=(1-A/A0) * 100%, filtration efficiency E is 93.6%.
Embodiment 4
As described in Example 1, wherein Thermal desorption bushing pipe (internal diameter 3mm) is 5 micron quartz fiber hair for having loaded 30mg diameter, loading length is 3 centimetres, the silicon dioxide microsphere solution of injection is the silicon dioxide methanol solution of the 100nm of 2 microlitres 2.5%, the Thermal desorption temperature of test is 300 DEG C, Thermal desorption gas velocity is 3mL/min, and acquisition A0 is 80mv.s, A is 0.5mv.s.
Calculate according to formula E=(1-A/A0) * 100%, filtration efficiency E is 99.9%.Can find out, load parameter and Thermal desorption condition (as Thermal desorption temperature etc.) by optimizing, higher filtration efficiency can be obtained, show that the method can instruct Thermal desorption bushing pipe to load the optimization of condition and Thermal desorption condition of work.
Claims (9)
1. the method for testing of a Thermal desorption bushing pipe particle filtration efficiency, containing filter medium in described Thermal desorption bushing pipe, Thermal desorption bushing pipe is placed in hot parser, and Thermal desorption carrier gas is introduced through Thermal desorption bushing pipe from hot parser upper end, flow out from the lower end outlet of hot parser, it is characterized in that:
1) in the Thermal desorption bushing pipe being in working temperature, inject dispersion silicon dioxide microsphere solution in organic solvent, the particle diameter of silicon dioxide microsphere is d; A conduit is provided with in the exit, lower end of hot parser, tube at one end exports with the lower end of hot parser and is connected, the conduit other end stretches under the liquid levels of splendid attire in container, the silicon dioxide microsphere penetrating filter medium in Thermal desorption bushing pipe carried out by carrier gas with liquid collection; By the silicon dioxide microsphere concentration of collecting in evaporative light-scattering detector tracer liquid, obtain peak area A;
2) adopt containing the blank bushing pipe of filter medium, repeat above step 1) operating process, obtain peak area A0;
3) by (1-A/A0) * 100% formulae discovery to obtain containing the Thermal desorption bushing pipe of filter medium be the filtration efficiency of the particle of d to particle diameter.
2. particle filtration efficiency method of testing according to claim 1, is characterized in that: the mass concentration scope 0.05% ~ 10% of described dispersion silicon dioxide microsphere in organic solvent.
3. particle filtration efficiency method of testing according to claim 1, is characterized in that: the particle diameter d scope 0.01 ~ 10 micron of described silicon dioxide microsphere.
4. particle filtration efficiency method of testing according to claim 1, is characterized in that: the organic solvent of described dispersed silicon dioxide microballoon is boiling point lower than the organic solvent of 80 DEG C.
5. particle filtration efficiency method of testing according to claim 4, is characterized in that: described organic solvent is one or more mixed solutions in methyl alcohol, ethanol, acetone, acetonitrile.
6. particle filtration efficiency method of testing according to claim 1, is characterized in that: described liquid is any one or two kinds of mixing in pure water, methyl alcohol, ethanol, acetone, acetonitrile.
7. particle filtration efficiency method of testing according to claim 1, is characterized in that: the filter medium in described Thermal desorption bushing pipe is one or two or more kinds combination in glass fibre hair, quartz fibre hair, silica sand or silica gel.
8. particle filtration efficiency method of testing according to claim 1, is characterized in that: the working temperature of described Thermal desorption bushing pipe is more than or equal to the boiling point of organic solvent in silicon dioxde solution, usual 80-600 DEG C.
9. particle filtration efficiency method of testing according to claim 1, is characterized in that: described carrier gas is one in nitrogen or helium or two kinds; Thermal desorption bushing pipe internal diameter 2mm-1cm, injecting dispersion silicon dioxide microsphere solution injection rate IR in organic solvent in Thermal desorption bushing pipe is 1 microlitre-100 microlitre.
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| CN201410495425.4A CN105510278B (en) | 2014-09-25 | 2014-09-25 | A kind of test method of Thermal desorption bushing pipe particulate matter filter efficiency |
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| US3810697A (en) * | 1972-08-10 | 1974-05-14 | Air Technologies Inc | Portable filter evaluation apparatus |
| CN101298625A (en) * | 2008-07-02 | 2008-11-05 | 中国人民解放军军事医学科学院微生物流行病研究所 | Highly effective particle filter biological detection method and positive-negative pressure facility detection system |
| CN101299037A (en) * | 2008-06-13 | 2008-11-05 | 中国人民解放军军事医学科学院卫生装备研究所 | Device and method for testing filtration efficiency of biologic aerosol for filtering or separating material |
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| CN103837460A (en) * | 2014-03-17 | 2014-06-04 | 天津三星电机有限公司 | Method for detecting and evaluating filtration efficiency of dust-free mask |
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2014
- 2014-09-25 CN CN201410495425.4A patent/CN105510278B/en active Active
Patent Citations (5)
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|---|---|---|---|---|
| US3810697A (en) * | 1972-08-10 | 1974-05-14 | Air Technologies Inc | Portable filter evaluation apparatus |
| CN101299037A (en) * | 2008-06-13 | 2008-11-05 | 中国人民解放军军事医学科学院卫生装备研究所 | Device and method for testing filtration efficiency of biologic aerosol for filtering or separating material |
| CN101298625A (en) * | 2008-07-02 | 2008-11-05 | 中国人民解放军军事医学科学院微生物流行病研究所 | Highly effective particle filter biological detection method and positive-negative pressure facility detection system |
| CN102183492A (en) * | 2010-12-15 | 2011-09-14 | 安徽循环经济技术工程院 | Three-band integrated atmospheric aerosol particle scattering coefficient measuring instrument and measuring method |
| CN103837460A (en) * | 2014-03-17 | 2014-06-04 | 天津三星电机有限公司 | Method for detecting and evaluating filtration efficiency of dust-free mask |
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| 武汉大学化学系高分子教研室: "《有机高分子化学 下》", 10 February 1978 * |
| 穆光照等: "《实用溶剂手册》", 30 September 1990, 上海：上海科学技术出版社 * |
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