CN103163013B - 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 PDFInfo
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- CN103163013B CN103163013B CN201110419901.0A CN201110419901A CN103163013B CN 103163013 B CN103163013 B CN 103163013B CN 201110419901 A CN201110419901 A CN 201110419901A CN 103163013 B CN103163013 B CN 103163013B
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- 239000012528 membrane Substances 0.000 title claims abstract description 71
- 238000002076 thermal analysis method Methods 0.000 title claims abstract description 59
- 239000007788 liquid Substances 0.000 title claims abstract description 23
- 239000007787 solid Substances 0.000 title claims abstract description 21
- 150000001875 compounds Chemical class 0.000 title claims abstract description 10
- 238000002347 injection Methods 0.000 title 1
- 239000007924 injection Substances 0.000 title 1
- 238000005070 sampling Methods 0.000 claims abstract description 37
- 239000004744 fabric Substances 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 239000000523 sample Substances 0.000 claims description 15
- 238000000197 pyrolysis Methods 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 2
- 229920002379 silicone rubber Polymers 0.000 claims description 2
- 239000004945 silicone rubber Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 16
- 238000004458 analytical method Methods 0.000 abstract description 12
- 239000012159 carrier gas Substances 0.000 abstract description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- 230000003204 osmotic effect Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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。
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.
Description
技术领域 technical field
本发明属于化学分析领域的固体液体的分析技术，具体是一种固体液体进样热解析与渗透膜的复合装置。The invention belongs to the analysis technology of solid liquid in the field of chemical analysis, in particular to a composite device of solid liquid sampling thermal analysis and permeable membrane.
背景技术 Background technique
在采用气体分析技术进行分析的时候，通常需要首先将固体、液体样品加热热解析形成相应的气体样品，然后对该气体样品进行分析，例如专利申请号ZL 200610088949.7所发明的一种固体、液体样品的进样装置。When using gas analysis technology for analysis, it is usually necessary to heat and thermally analyze solid and liquid samples to form corresponding gas samples, and then analyze the gas samples, such as a solid and liquid sample invented by patent application number ZL 200610088949.7 sampling device.
同时，由于固体、液体样品往往是混合物，在加热形成气体时除了化合物本身，还包括水蒸气和其它气体杂质，干扰分析的准确度和灵敏度，因此可以采用渗透膜技术，来阻止水蒸气的透过膜、保证待分析的固体液体化合物透过膜，得到准确的分析。At the same time, since solid and liquid samples are often mixtures, in addition to the compound itself, water vapor and other gas impurities are included when heating to form gas, which interferes with the accuracy and sensitivity of the analysis. Therefore, permeable membrane technology can be used to prevent the penetration of water vapor. Through the membrane to ensure that the solid and liquid compounds to be analyzed pass through the membrane to obtain accurate analysis.
分别采用将固体液体加热热解析的装置，和渗透膜的装置，对样品加热汽化、气体样品透过膜、再进行分析，增加了连接管路、增加了气体样品所在的体积、还需要增加保温措施，最终影响了分析的准确性。The device that heats the solid liquid and the thermal analysis device, and the device that permeates the membrane are respectively used to heat and vaporize the sample, and then analyze the gas sample through the membrane, which increases the connecting pipeline, increases the volume of the gas sample, and also needs to increase the heat preservation. measures, ultimately affecting the accuracy of the analysis.
因此本发明设计了固体液体进样热解析与渗透膜的复合装置，以解决上述问题。Therefore, the present invention designs a composite device of solid liquid sampling thermal analysis and permeable membrane to solve the above problems.
发明内容 Contents of the invention
本发明的目的在于提供一种气固体液体进样热解析与渗透膜的复合装置。The object of the present invention is to provide a composite device for gas-solid-liquid sampling thermal analysis and permeable membrane.
为实现上述目的，本发明采用的技术方案为：To achieve the above object, the technical solution adopted in the present invention is:
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，A compound device for thermal analysis and permeable membrane of solid liquid sampling, including upper cover body, 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.
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.
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.
嵌入式膜支撑体为多孔的金属板。The embedded membrane support is a porous metal plate.
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.
渗透膜是耐温的硅橡胶膜，渗透膜的厚度为25-500微米。The permeable membrane is a temperature-resistant silicone rubber membrane, and the thickness of the permeable membrane is 25-500 microns.
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.
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。This composite device of thermal analysis and osmotic membrane for solid liquid sampling has a compact structure and small dead volume, which can realize thermal analysis of samples, efficiently pass through the osmotic membrane, and rapid analysis.
附图说明 Description of drawings
下面结合附图进一步详细描述。Further detailed description below in conjunction with accompanying drawings.
图1为固体液体进样热解析与渗透膜的复合装置的示意图。Fig. 1 is a schematic diagram of a composite device of solid-liquid sampling thermal analysis and permeable membrane.
具体实施方式 Detailed ways
一种固体液体进样热解析与渗透膜的复合装置，由上盖体1、渗透膜3、热解析体4、采样布5、螺栓15和开关电磁阀6组成，上盖体1和热解析体4之间安装有渗透膜3，上盖体1和热解析体4通过螺栓15紧固在一起。A compound device for thermal analysis and permeable membrane of solid liquid sampling, which is composed of upper cover body 1, permeable membrane 3, thermal analysis body 4, sampling cloth 5, bolts 15 and switch solenoid valve 6, upper cover body 1 and thermal analysis unit A permeable membrane 3 is installed between the bodies 4 , and the upper cover body 1 and the thermal analysis body 4 are fastened together by bolts 15 .
其中上盖体1上有膜后端腔11、嵌入式膜支撑体2、膜后端进气口9、膜后端出气口13、螺栓孔10。Wherein the upper cover body 1 has a membrane rear cavity 11 , an embedded membrane support 2 , a membrane rear air inlet 9 , a membrane rear air outlet 13 , and bolt holes 10 .
热解析体4上有热解析腔12、嵌入式膜支撑体2、膜前端进气口16、膜前端出气口17、采样布腔14、加热棒孔8、温度传感器孔7、螺栓孔10。The thermal analysis body 4 has a thermal analysis chamber 12, an embedded membrane support body 2, an air inlet 16 at the front end of the membrane, an air outlet 17 at the front end of the membrane, a sampling cloth chamber 14, a heating rod hole 8, a temperature sensor hole 7, and a bolt hole 10.
将载有固体液体样品的采样布5，插入到采样布腔14、用开关电磁阀6的阀芯压紧在热解析体4上进行加热，得到的样品气体，透过渗透膜3扩散到膜后端腔11，由流过膜后端进气口9、膜后端出气口13的载气带走进行分析。Insert the sampling cloth 5 loaded with solid and liquid samples into the sampling cloth cavity 14, press the valve core of the switching solenoid valve 6 on the thermal analysis body 4 for heating, and the obtained sample gas diffuses through the permeable membrane 3 to the membrane The rear cavity 11 is carried away by the carrier gas flowing through the membrane rear inlet 9 and the membrane rear gas outlet 13 for analysis.
残留在热解析腔12的样品，由流过膜前端进气口16、膜前端出气口17的载气进行吹扫和清洗。The sample remaining in the thermal analysis chamber 12 is purged and cleaned by the carrier gas flowing through the inlet 16 at the front end of the membrane and the gas outlet 17 at the front end of the membrane.
当采样布腔没有采样布、用开关电磁阀的阀芯压紧在热解析体上的热解析腔时，由流过膜前端进气口、膜前端出气口的气体样品直接进样，可以实现气体样品的分析。When there is no sampling cloth in the sampling cloth chamber, and the valve core of the switching solenoid valve is used to press the thermal analysis chamber on the thermal analysis body, the gas sample flowing through the inlet port at the front end of the membrane and the gas outlet port at the front end of the membrane can be directly injected into the thermal analysis chamber, which can realize Analysis of gas samples.
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。This composite device of thermal analysis and osmotic membrane for solid liquid sampling has a compact structure and small dead volume, which can realize thermal analysis of samples, efficiently pass through the osmotic membrane, and rapid analysis.
实施例1：Example 1:
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。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.
将载有100纳克TNT固体样品的采样布，插入到采样布腔进行50度热解析，渗透膜厚度为25微米，TNT气体样品透过渗透膜扩散后，由流过膜后端进气口、膜后端出气口的载气带走，送入到离子迁移谱中、采用负离子模式进行分析，可以得到TNT的检测信号。Insert the sampling cloth containing 100 nanograms of TNT solid sample into the sampling cloth cavity for thermal analysis at 50 degrees. The thickness of the permeable membrane is 25 microns. After the TNT gas sample diffuses through the permeable membrane, it flows through the air inlet at the back of the membrane. , The carrier gas at the gas outlet at the back end of the membrane is taken away, sent to the ion mobility spectrometer, and analyzed in negative ion mode, the detection signal of TNT can be obtained.
实施例2：Example 2:
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。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.
将载有10微升二甲基亚砜液体样品的采样布，插入到采样布腔进行200度热解析，渗透膜厚度为500微米，二甲基亚砜气体样品透过渗透膜扩散后，由流过膜后端进气口、膜后端出气口的载气带走，送入到离子迁移谱中、采用正离子模式进行分析，可以得到二甲基亚砜的检测信号。Insert the sampling cloth containing 10 microliters of dimethyl sulfoxide liquid sample into the sampling cloth cavity for thermal analysis at 200 degrees. The thickness of the permeable membrane is 500 microns. After the dimethyl sulfoxide gas sample diffuses through the permeable membrane, The carrier gas flowing through the inlet and outlet of the rear end of the membrane is taken away, sent to the ion mobility spectrometer, and analyzed in the positive ion mode, and the detection signal of dimethyl sulfoxide can be obtained.
Claims (7)
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| CN201110419901.0A CN103163013B (en) | 2011-12-15 | 2011-12-15 | Thermal analysis and permeable membrane compound device for solid and liquid sample injection |
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| CN201110419901.0A CN103163013B (en) | 2011-12-15 | 2011-12-15 | Thermal analysis and permeable membrane compound device for solid and liquid sample injection |
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| CN103163013B true CN103163013B (en) | 2015-04-08 |
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| CN105717188B (en) * | 2014-12-05 | 2018-03-20 | 中国科学院大连化学物理研究所 | A kind of device of quick heating fluid sample |
| CN108226267B (en) * | 2017-06-15 | 2023-09-12 | 深圳市天和时代电子设备有限公司 | Split type thermal analysis sampling device |
| 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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| US5988002A (en) * | 1996-04-03 | 1999-11-23 | Barringer Research Limited | Method of collecting trace samples for analysis |
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