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CN103163013A - Thermal analysis and permeable membrane compound device for solid and liquid sample injection - Google Patents

Thermal analysis and permeable membrane compound device for solid and liquid sample injection Download PDF

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Publication number
CN103163013A
CN103163013A CN2011104199010A CN201110419901A CN103163013A CN 103163013 A CN103163013 A CN 103163013A CN 2011104199010 A CN2011104199010 A CN 2011104199010A CN 201110419901 A CN201110419901 A CN 201110419901A CN 103163013 A CN103163013 A CN 103163013A
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thermal analysis
permeable membrane
upper cover
pyrolysis
hole
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CN103163013B (en
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李京华
仓怀文
王新
渠团帅
李林
李海洋
史喜成
董艳春
高晓强
王丽
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Abstract

一种固体液体进样热解析与渗透膜的复合装置,由上盖体、渗透膜、热解析体、采样布、螺栓和开关电磁阀组成,上盖体和热解析体之间安装有渗透膜,上盖体和热解析体通过螺栓紧固在一起。将载有固体液体样品的采样布,插入到采样布腔、用开关电磁阀压紧在热解析体上进行加热,得到的样品气体,透过渗透膜扩散到膜后端腔,由流过膜后端进气口、膜后端出气口的载气带走进行分析。残留在热解析腔的样品,由流过膜前端进气口、膜前端出气口的载气进行吹扫和清洗。这种固体液体进样热解析与渗透膜的复合装置,结构紧凑、死体积小,可以实现样品的热解析、高效通过渗透膜、快速分析。

Figure 201110419901

A compound device for thermal analysis and permeable membrane of solid liquid sampling, which is composed of upper cover, permeable membrane, thermal analysis body, sampling cloth, bolts and switch solenoid valve, and permeable membrane is installed between the upper cover and the thermal analysis body , the upper cover body and the thermal analysis body are fastened together by bolts. Insert the sampling cloth loaded with solid and liquid samples into the sampling cloth cavity, and press it on the thermal analysis body with the switch solenoid valve for heating. The carrier gas at the rear inlet and membrane rear outlet is taken away for analysis. The sample remaining in the thermal analysis chamber is purged and cleaned by the carrier gas flowing through the air inlet at the front end of the membrane and the gas outlet at the front end of the membrane. This composite device of thermal analysis and permeable membrane for solid liquid sampling has a compact structure and small dead volume, which can realize thermal analysis of samples, efficiently pass through the permeable membrane, and rapid analysis.

Figure 201110419901

Description

The set composite with permeable membrane is analysed in the pyrolysis of a kind of solid-liquid sample introduction
Technical field
The invention belongs to the analytical technology of the solid-liquid of chemical analysis field, specifically the set composite with permeable membrane is analysed in the pyrolysis of a kind of solid-liquid sample introduction.
Background technology
When adopting gas analysis technology to analyze, usually need at first solid, fluid sample heat hot to be resolved to form corresponding gaseous sample, then this gaseous sample is analyzed, for example a kind of solid of inventing of number of patent application ZL 200610088949.7, the sampling device of fluid sample.
Simultaneously, due to solid, fluid sample potpourri often, when adding thermosetting gas except compound itself, also comprise water vapor and other gaseous impurities, the accuracy of interference analysis and sensitivity, therefore can adopt infiltrate membrane technology, what stop water vapor sees through film through film, assurance solid-liquid compound to be analyzed, is analyzed accurately.
Adopt respectively the device that the solid-liquid heat hot is resolved, device with permeable membrane, sample heating vaporization, gaseous sample are seen through film, analyze, increased connecting line, increased the volume at gaseous sample place, also needed to increase Insulation, finally affected the accuracy of analyzing.
Therefore the present invention has designed the pyrolysis of solid-liquid sample introduction and has analysed set composite with permeable membrane, to address the above problem.
Summary of the invention
The object of the present invention is to provide the pyrolysis of a kind of gas solid-liquid sample introduction to analyse set composite with permeable membrane.
For achieving the above object, the technical solution used in the present invention is:
The set composite with permeable membrane is analysed in the pyrolysis of a kind of solid-liquid sample introduction, comprises that body is analysed in upper cover body, permeable membrane, pyrolysis, sample cloth and switch electromagnetic valve,
The bottom of upper cover body is provided with groove, and the sidewall of upper cover body is provided with air intake opening and the gas outlet that is connected with groove;
Pyrolysis is provided with the through hole that penetration heat is resolved body in the middle part of analysing body, and the sidewall that body is analysed in pyrolysis is provided with air intake opening and the gas outlet that is connected with through hole, and pyrolysis is analysed and is provided with heating rod in body; The sidewall that body is analysed in pyrolysis is provided with the sampling cloth that is connected with through hole and picks and places mouth; Heating rod is electrically connected to external power;
Upper cover body and pyrolysis are analysed body and are snapped together, and permeable membrane is placed in upper cover body and pyrolysis is analysed between body, and the both sides of permeable membrane are respectively the groove of upper cover body and the through hole that body is analysed in pyrolysis;
The other end that the body through hole is analysed in pyrolysis is provided with switch electromagnetic valve, and spool one end of switch electromagnetic valve is placed in through hole.
Upper cover body is analysed body with pyrolysis and is in the same place by bolted.
In the groove of upper cover body and pyrolysis analyse in the through hole of body and be respectively equipped with the inserted film supporter that is complementary with groove and through hole.
The inserted film supporter is the sheet metal of porous.
Sampling cloth picks and places in mouthful receiving through-hole by sampling cloth.
Permeable membrane is the silicone rubber membrane of heatproof, and the thickness of permeable membrane is the 25-500 micron.
Pyrolysis is analysed and is provided with temperature sensor probe in body; Temperature sensor probe is connected with temperature controller by wire; Pyrolysis is analysed the heating-up temperature of body at the 50-200 degree.
The set composite with permeable membrane is analysed in the pyrolysis of this solid-liquid sample introduction, and compact conformation, dead volume are little, can realize that the pyrolysis of sample is analysed, efficiently by permeable membrane, express-analysis.
Description of drawings
Describe in further detail below in conjunction with accompanying drawing.
Fig. 1 is that the schematic diagram with the set composite of permeable membrane is analysed in the pyrolysis of solid-liquid sample introduction.
Embodiment
The set composite with permeable membrane is analysed in the pyrolysis of a kind of solid-liquid sample introduction, analysing body 4, sampling cloth 5, bolt 15 and switch electromagnetic valve 6 by upper cover body 1, permeable membrane 3, pyrolysis forms, upper cover body 1 and pyrolysis are analysed permeable membrane 3 are installed between body 4, and upper cover body 1 and pyrolysis are analysed body 4 and tightened together by bolt 15.
Chamber, film rear end 11, inserted film supporter 2, film rear end air intake opening 9, gas outlet, film rear end 13, bolt hole 10 are wherein arranged on upper cover body 1.
Pyrolysis is analysed has pyrolysis to analyse chamber 12, inserted film supporter 2, film front end airflow mouth 16, film front end gas outlet 17, sampling cloth chamber 14, heating rod hole 8, temperature sensor hole 7, bolt hole 10 on body 4.
The sampling cloth 5 of solid-liquid sample will be loaded with, be inserted into sampling cloth chamber 14, be pressed on pyrolysis with the spool of switch electromagnetic valve 6 and analyse on body 4 and heat, the sample gas that obtains, see through permeable membrane 3 and be diffused into chamber, film rear end 11, taken away by the carrier gas of flowing through film rear end air intake opening 9, gas outlet, film rear end 13 and analyze.
Remain in pyrolysis and analyse the sample in chamber 12, purge and clean by the carrier gas of flowing through film front end airflow mouth 16, film front end gas outlet 17.
When sampling cloth chamber do not sample cloth, be pressed on pyrolysis with the spool of switch electromagnetic valve and analyse pyrolysis on body when analysing the chamber, the gaseous sample direct injected by flowing through film front end airflow mouth, film front end gas outlet can realize the analysis of gaseous sample.
The set composite with permeable membrane is analysed in the pyrolysis of this solid-liquid sample introduction, and compact conformation, dead volume are little, can realize that the pyrolysis of sample is analysed, efficiently by permeable membrane, express-analysis.
Embodiment 1:
The set composite with permeable membrane is analysed in the pyrolysis of a kind of solid-liquid sample introduction, analysing body, sampling cloth, bolt and switch electromagnetic valve by upper cover body, permeable membrane, pyrolysis forms, upper cover body and pyrolysis are analysed permeable membrane are installed between body, and upper cover body is analysed body with pyrolysis and is in the same place by bolted.
The sampling cloth of 100 nanogram TNT solid samples will be loaded with, being inserted into sampling cloth chamber carries out 50 degree pyrolysis and analyses, permeable membrane thickness is 25 microns, after the TNT gaseous sample sees through the permeable membrane diffusion, taken away by the carrier gas of flowing through film rear end air intake opening, gas outlet, film rear end, be sent in ion mobility spectrometry, adopt negative ion mode to analyze, can obtain the detection signal of TNT.
Embodiment 2:
The set composite with permeable membrane is analysed in the pyrolysis of a kind of solid-liquid sample introduction, analysing body, sampling cloth, bolt and switch electromagnetic valve by upper cover body, permeable membrane, pyrolysis forms, upper cover body and pyrolysis are analysed permeable membrane are installed between body, and upper cover body is analysed body with pyrolysis and is in the same place by bolted.
The sampling cloth of 10 microlitre dimethyl sulfoxide (DMSO) liquid samples will be loaded with, being inserted into sampling cloth chamber carries out 200 degree pyrolysis and analyses, permeable membrane thickness is 500 microns, after the dimethyl sulfoxide (DMSO) gaseous sample sees through the permeable membrane diffusion, taken away by the carrier gas of flowing through film rear end air intake opening, gas outlet, film rear end, be sent in ion mobility spectrometry, adopt positive ion mode to analyze, can obtain the detection signal of dimethyl sulfoxide (DMSO).

Claims (7)

1.一种固体液体进样热解析与渗透膜的复合装置,包括上盖体、渗透膜、热解析体、采样布和开关电磁阀,1. A compound device for thermal analysis and permeable membrane of solid liquid sampling, including upper cover, permeable membrane, thermal analysis body, sampling cloth and switch solenoid valve, 上盖体的下部设有凹槽,上盖体的侧壁上设有与凹槽相连通的进气口和出气口;The lower part of the upper cover is provided with a groove, and the side wall of the upper cover is provided with an air inlet and an air outlet connected with the groove; 热解析体中部设有贯穿热解析体的通孔,热解析体的侧壁上设有与通孔相连通的进气口和出气口,热解析体内设有加热棒;热解析体的侧壁上设有与通孔相连通的采样布取放口;加热棒与外电源电连接;The middle part of the pyrolysis body is provided with a through hole through the pyrolysis body, the side wall of the pyrolysis body is provided with an air inlet and an air outlet connected with the through hole, and a heating rod is arranged in the pyrolysis body; the side wall of the pyrolysis body There is a sampling cloth take-out port connected to the through hole; the heating rod is electrically connected to the external power supply; 上盖体和热解析体扣合在一起,渗透膜置于上盖体和热解析体之间,渗透膜的两侧分别为上盖体的凹槽和热解析体的通孔;The upper cover body and the thermal analysis body are fastened together, the permeable membrane is placed between the upper cover body and the thermal analysis body, and the two sides of the permeable membrane are respectively the groove of the upper cover body and the through hole of the thermal analysis body; 热解析体通孔的另一端设有开关电磁阀,开关电磁阀的阀芯一端置于通孔内。The other end of the through hole of the thermal analysis body is provided with a switch solenoid valve, and one end of the valve core of the switch solenoid valve is placed in the through hole. 2.根据权利要求1所述复合装置,其特征在于:2. The composite device according to claim 1, characterized in that: 上盖体和热解析体通过螺栓紧固在一起。The upper cover body and the thermal analysis body are fastened together by bolts. 3.根据权利要求1所述复合装置,其特征在于:3. The composite device according to claim 1, characterized in that: 上盖体的凹槽内和热解析体的通孔内分别设有与凹槽和通孔相匹配的嵌入式膜支撑体。Embedded membrane supports matching the grooves and the through holes are respectively arranged in the groove of the upper cover body and in the through hole of the thermal analysis body. 4.根据权利要求3所述复合装置,其特征在于:4. The composite device according to claim 3, characterized in that: 嵌入式膜支撑体为多孔的金属板。The embedded membrane support is a porous metal plate. 5.根据权利要求1所述复合装置,其特征在于:5. The compound device according to claim 1, characterized in that: 采样布通过采样布取放口置入通孔内。The sampling cloth is put into the through hole through the sampling cloth opening. 6.根据权利要求1所述复合装置,其特征在于:渗透膜是耐温的硅橡胶膜,渗透膜的厚度为25-500微米。6. The composite device according to claim 1, characterized in that the permeable membrane is a temperature-resistant silicone rubber membrane, and the thickness of the permeable membrane is 25-500 microns. 7.根据权利要求1所述复合装置,其特征在于:7. The composite device according to claim 1, characterized in that: 热解析体内设有温度传感器探头;温度传感器探头通过导线与温度控制器相连;热解析体的加热温度在50-200度。The thermal analysis body is provided with a temperature sensor probe; the temperature sensor probe is connected to the temperature controller through a wire; the heating temperature of the thermal analysis body is 50-200 degrees.
CN201110419901.0A 2011-12-15 2011-12-15 Thermal analysis and permeable membrane compound device for solid and liquid sample injection Expired - Fee Related CN103163013B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105717188A (en) * 2014-12-05 2016-06-29 中国科学院大连化学物理研究所 Device capable of quickly heating liquid sample
CN108226267A (en) * 2017-06-15 2018-06-29 深圳市天和时代电子设备有限公司 A kind of split type thermal desorption sampling device
CN112683987A (en) * 2020-12-30 2021-04-20 上海新漫传感科技有限公司 Gas circuit working system of multifunctional ion mobility spectrometry

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CN102033098A (en) * 2009-09-29 2011-04-27 中国科学院大连化学物理研究所 Tray type thermal analysis multi-path sample introduction device
CN202433239U (en) * 2011-12-15 2012-09-12 中国科学院大连化学物理研究所 Solid and liquid sampling thermal analysis and osmotic membrane compounding device

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US5988002A (en) * 1996-04-03 1999-11-23 Barringer Research Limited Method of collecting trace samples for analysis
US5741984A (en) * 1996-10-21 1998-04-21 Barringer Technologies Inc. Method and apparatus for sample collection by a token
CN1707259A (en) * 2004-06-04 2005-12-14 中国科学院大连化学物理研究所 A device for solid-state adsorption stirring rod thermal desorber
CN1721850A (en) * 2004-07-14 2006-01-18 中国科学院大连化学物理研究所 A solid phase extraction sample bottle and thermal desorption device
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105717188A (en) * 2014-12-05 2016-06-29 中国科学院大连化学物理研究所 Device capable of quickly heating liquid sample
CN108226267A (en) * 2017-06-15 2018-06-29 深圳市天和时代电子设备有限公司 A kind of split type thermal desorption sampling device
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CN112683987A (en) * 2020-12-30 2021-04-20 上海新漫传感科技有限公司 Gas circuit working system of multifunctional ion mobility spectrometry
CN112683987B (en) * 2020-12-30 2023-01-06 上海新漫传感科技有限公司 Gas circuit working system of multifunctional ion mobility spectrometry

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