CN104713967B - Chromatography column feed materials two-stage thermal desorption device and method - Google Patents
Chromatography column feed materials two-stage thermal desorption device and method Download PDFInfo
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- CN104713967B CN104713967B CN201510049372.8A CN201510049372A CN104713967B CN 104713967 B CN104713967 B CN 104713967B CN 201510049372 A CN201510049372 A CN 201510049372A CN 104713967 B CN104713967 B CN 104713967B
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Abstract
The invention discloses a kind of chromatography column feed materials two-stage thermal desorption device, first flow stabilizing valve and the first electromagnetic valve connect, first electromagnetic valve is connected with first heater, first heater is connected with secondary heating mechanism, secondary heating mechanism and the 3rd electromagnetic valve connect, 3rd electromagnetic valve is connected with chromatographic analysis device, 3rd electromagnetic valve is additionally provided with the first emptying passage, a Tenax pipe it is provided with in secondary heating mechanism, gas passage m and the second pressure maintaining valve connect, second pressure maintaining valve and the second electromagnetic valve connect, second electromagnetic valve and the 4th electromagnetic valve connect, 4th electromagnetic valve with add thermal refrigerating device and be connected, add thermal refrigerating device and the 3rd electromagnetic valve connects；Described first heater is provided with sampling device, is provided with the 2nd Tenax pipe in adding thermal refrigerating device.First heater when invention increases two-stage thermal desorption air path part and do standard series pipe so that testing sample, through twice thermal desorption process, improves concentration during testing sample entrance chromatographic analysis device.
Description
Technical field
The invention belongs to technical field of chromatographic analysis, particularly relate to a kind of chromatography column feed materials two-stage thermal desorption device and method.
Background technology
Chromatography column feed materials device of the prior art is generally a thermal desorption device, shunting can be used and do not shunt two kinds of sample introduction patterns, split sampling is usually used in trace or constant sample feeding, and Splitless injecting samples is mainly used in the sample feeding of low concentration, primarily to improve the sensitivity of sample introduction.
But, when the most conventional shunting Splitless injecting samples mouth carries out Splitless injecting samples, have the disadvantage in that
(1) in sample, main component is solvent, and when therefore carrying out Splitless injecting samples, a large amount of solvents enter chromatographic column, cause solvent peak broadening the most severe, such as boiling point or character and the close material of solvent, then it is easy to be affected by solvent peak, it is difficult with Splitless injecting samples pattern and be analyzed.
(2) chromatographic column is entered in a large number because of solvent, chromatographic column is caused to be transshipped, especially with the chromatographic column period of the day from 11 p.m. to 1 a.m of below 0.25mm internal diameter, the phenomenon that chromatographic column overload causes chromatographic peak broadening, peak lopsided is even more serious, may cause worse situation under remolding sensitivity draining conditions.
So, the sample introduction analysis result of a most conventional thermal desorption device is the most unsatisfactory, and when gas chromatograph detects, chromatographic peak hangover is serious, appearance time is the most early, peak shape more hangover, the later chromatographic peak peak area of appearance time is less than normal, and adjacent two nearer peak separating degrees are on the low side.
Summary of the invention
The technical problem to be solved in the present invention is that the sample introduction analysis result of a most conventional thermal desorption device is the most unsatisfactory, when gas chromatograph detects, chromatographic peak hangover is serious, appearance time is the most early, peak shape more hangover, the later chromatographic peak peak area of appearance time is less than normal, adjacent two nearer peak separating degrees are on the low side, and for solving the problems referred to above, the present invention provides a kind of chromatography column feed materials two-stage thermal desorption device and method.
It is an object of the invention to realize in the following manner:
nullChromatography column feed materials two-stage thermal desorption device，Including the first flow stabilizing valve，First gas passage a and the first flow stabilizing valve connect，First flow stabilizing valve is connected by the second gas passage b and the first electromagnetic valve，First electromagnetic valve is connected with first heater by the 3rd gas passage c，First heater is connected with secondary heating mechanism by the 4th gas passage d，Secondary heating mechanism is connected by the 5th gas passage e and the 3rd electromagnetic valve，3rd electromagnetic valve is connected with chromatographic analysis device by the 6th gas passage g，3rd electromagnetic valve is additionally provided with the first emptying passage f，A Tenax pipe it is provided with in secondary heating mechanism，Also include the 11st gas passage m，11st gas passage m and the second pressure maintaining valve connect，Second pressure maintaining valve is connected by the tenth gas passage and the second electromagnetic valve，Second electromagnetic valve is connected by the 9th gas passage k and the 4th electromagnetic valve，4th electromagnetic valve is connected with heating-refrigerating plant by the 8th gas passage i，Heating-refrigerating plant is connected by the 7th gas passage h and the 3rd electromagnetic valve；Described first heater is provided with sampling device, and described 4th electromagnetic valve is additionally provided with the second emptying passage j, is provided with the 2nd Tenax pipe in heating-refrigerating plant.
Described 2nd Tenax pipe is the internal stainless steel tube equipped with 50-100mg Tenax-TA organic adsorbent.
Described gas passage uses stainless steel tube.
Described heating-refrigerating plant is thermoelectric refrigerator.
Being provided with heater on described 3rd electromagnetic valve, the outside of the 5th gas passage e and the 7th gas passage h is enclosed with heating mantle.
Specifically comprise the following steps that
(1) standard series pipe is done: first heater heats, secondary heating mechanism does not heats, 7th gas passage h and the 6th gas passage g closes, first gas passage a, second gas passage b, 3rd gas passage c, 4th gas passage d, 5th gas passage e and first emptying passage f opens, testing sample is injected from the sampling device of first heater, at high temperature ensure that sample quickly gasifies, then by the high pure nitrogen entered from the first gas passage a by testing sample band to secondary heating mechanism, and adsorbed by Tenax-TA organic adsorbent, thus make standard series pipe；
(2) thermal desorptions: secondary heating mechanism is heated to 280-300 DEG C, and heating-refrigerating plant freezes, temperature is adjusted to less than 4 DEG C, and to keep constant；First gas passage a, the second gas passage b, the 3rd gas passage c, the 4th gas passage d, the 5th gas passage e and the 7th gas passage h keep unimpeded, second emptying passage j opens, first emptying passage f, the 6th gas passage g and the second closed electromagnetic valve, 5th gas passage e, the 7th gas passage h and the 3rd electromagnetic valve heat, and prevent testing sample from condensing；After secondary heating mechanism heating 5-15min, the testing sample of the Tenax-TA organic adsorbent absorption in the oneth Tenax pipe is desorbed out, by the high pure nitrogen entered from the first gas passage a by testing sample band to heating-refrigerating plant, and adsorbed by the Tenax-TA organic adsorbent in the 2nd Tenax pipe；
(3) two-stage thermal desorption: after a thermal desorption, heating-refrigerating plant is heated, open the second electromagnetic valve, second emptying passage j closes, 9th gas passage k and the 8th gas passage i keeps unimpeded, 7th gas passage h and the 6th gas passage g keeps unimpeded, first emptying passage f and the 5th gas passage e closes, heating-refrigerating plant is through heating, the testing sample of the Tenax-TA organic adsorbent absorption in the 2nd Tenax pipe is desorbed out, by the high pure nitrogen entered from the 11st gas passage m, testing sample band is analyzed to chromatographic analysis device.
Relative to prior art, the present invention provides a kind of chromatography column feed materials two-stage thermal desorption device, compared with a thermal desorption device, first heater when adding two-stage thermal desorption air path part and do standard series pipe, make testing sample through twice thermal desorption process, improve concentration during testing sample entrance chromatographic analysis device.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention.
Wherein, 1 is the first flow stabilizing valve；2 is the first electromagnetic valve；3 is first heater；4 is secondary heating mechanism；5 is the 3rd electromagnetic valve；6 is heating-refrigerating plant；7 is the 4th electromagnetic valve；8 is the second electromagnetic valve；9 is the second pressure maintaining valve；10 is chromatographic analysis device.
Detailed description of the invention
nullAs shown in Figure 1，Chromatography column feed materials two-stage thermal desorption device，Including the first flow stabilizing valve 1，First gas passage a and the first flow stabilizing valve 1 connect，First flow stabilizing valve 1 is connected by the second gas passage b and the first electromagnetic valve 2，First electromagnetic valve 2 is connected with first heater 3 by the 3rd gas passage c，First heater 3 is connected with secondary heating mechanism 4 by the 4th gas passage d，Secondary heating mechanism 4 is connected by the 5th gas passage e and the 3rd electromagnetic valve 5，3rd electromagnetic valve 5 is connected with chromatographic analysis device 10 by the 6th gas passage g，3rd electromagnetic valve 5 is additionally provided with the first emptying passage f，A Tenax pipe it is provided with in secondary heating mechanism 4，Also include the 11st gas passage m，11st gas passage m and the second pressure maintaining valve 9 connect，Second pressure maintaining valve 9 is connected by the tenth gas passage l and the second electromagnetic valve 8，Second electromagnetic valve 8 is connected by the 9th gas passage k and the 4th electromagnetic valve 7，4th electromagnetic valve 7 is connected with heating-refrigerating plant 6 by the 8th gas passage i，Heating-refrigerating plant 6 is connected by the 7th gas passage h and the 3rd electromagnetic valve 5；Described first heater 3 is provided with sampling device, and described 4th electromagnetic valve 7 is additionally provided with the second emptying passage j, is provided with the 2nd Tenax pipe in heating-refrigerating plant 6.
A described Tenax pipe meets the requirement of GB50325-2010 (version in 2013), and the 2nd Tenax pipe is the internal stainless steel tube equipped with 50-100mg Tenax-TA organic adsorbent.
Described gas passage uses stainless steel tube.
Described heating-refrigerating plant 6 is thermoelectric refrigerator.
Being provided with heater on described 3rd electromagnetic valve 5, the outside of the 5th gas passage e and the 7th gas passage h is enclosed with heating mantle.
The present invention specifically comprises the following steps that
(1) standard series pipe is done: first heater heats, secondary heating mechanism does not heats, 7th gas passage h and the 6th gas passage g closes, first gas passage a, second gas passage b, 3rd gas passage c, 4th gas passage d, 5th gas passage e and first emptying passage f opens, testing sample is injected from the sampling device of first heater, at high temperature ensure that sample quickly gasifies, then by the high pure nitrogen entered from the first gas passage a by testing sample band to secondary heating mechanism, and adsorbed by Tenax-TA organic adsorbent, thus make standard series pipe；
(2) thermal desorptions: secondary heating mechanism is heated to 280-300 DEG C, and heating-refrigerating plant freezes, temperature is adjusted to less than 4 DEG C, and to keep constant；First gas passage a, the second gas passage b, the 3rd gas passage c, the 4th gas passage d, the 5th gas passage e and the 7th gas passage h keep unimpeded, second emptying passage j opens, first emptying passage f, the 6th gas passage g and the second closed electromagnetic valve, 5th gas passage e, the 7th gas passage h and the 3rd electromagnetic valve heat, and prevent testing sample from condensing；After secondary heating mechanism heating 5-15min, the testing sample of the Tenax-TA organic adsorbent absorption in the oneth Tenax pipe is desorbed out, by the high pure nitrogen entered from the first gas passage a by testing sample band to heating-refrigerating plant, and adsorbed by the Tenax-TA organic adsorbent in the 2nd Tenax pipe；
(3) two-stage thermal desorption: after a thermal desorption, heating-refrigerating plant is heated, open the second electromagnetic valve (8), second emptying passage j closes, 9th gas passage k and the 8th gas passage i keeps unimpeded, 7th gas passage h and the 6th gas passage g keeps unimpeded, first emptying passage f and the 5th gas passage e closes, heating-refrigerating plant is through heating, the testing sample of the Tenax-TA organic adsorbent absorption in the 2nd Tenax pipe is desorbed out, by the high pure nitrogen entered from the 11st gas passage m, testing sample band is analyzed to chromatographic analysis device.
Relative to prior art, the present invention provides a kind of chromatography column feed materials two-stage thermal desorption device, compared with a thermal desorption device, first heater when adding two-stage thermal desorption air path part and do standard series pipe, make testing sample through twice thermal desorption process, improve concentration during testing sample entrance chromatographic analysis device.
Above-described is only the preferred embodiment of the present invention, it is noted that for a person skilled in the art, without departing under general idea premise of the present invention, it is also possible to making some changes and improvements, these also should be considered as protection scope of the present invention.
Claims (6)
- null1. chromatography column feed materials two-stage thermal desorption device，Including the first flow stabilizing valve (1)，First gas passage (a) is connected with the first flow stabilizing valve (1)，First flow stabilizing valve (1) is connected with the first electromagnetic valve (2) by the second gas passage (b)，First electromagnetic valve (2) is connected with first heater (3) by the 3rd gas passage (c)，First heater (3) is connected with secondary heating mechanism (4) by the 4th gas passage (d)，Secondary heating mechanism (4) is connected with the 3rd electromagnetic valve (5) by the 5th gas passage (e)，3rd electromagnetic valve (5) is connected with chromatographic analysis device (10) by the 6th gas passage (g)，3rd electromagnetic valve (5) is additionally provided with the first emptying passage (f)，A Tenax pipe it is provided with in secondary heating mechanism (4)，It is characterized in that: also include the 11st gas passage (m)，11st gas passage (m) is connected with the second pressure maintaining valve (9)，Second pressure maintaining valve (9) is connected with the second electromagnetic valve (8) by the tenth gas passage (l)，Second electromagnetic valve (8) is connected with the 4th electromagnetic valve (7) by the 9th gas passage (k)，4th electromagnetic valve (7) is (i) connected with heating-refrigerating plant (6) by the 8th gas passage，Heating-refrigerating plant (6) is connected with the 3rd electromagnetic valve (5) by the 7th gas passage (h)；Described first heater (3) is provided with sampling device, and described 4th electromagnetic valve (7) is additionally provided with the second emptying passage (j), is provided with the 2nd Tenax pipe in heating-refrigerating plant (6).
- Chromatography column feed materials two-stage thermal desorption device the most according to claim 1, it is characterised in that: described 2nd Tenax pipe is the internal stainless steel tube equipped with 50-100mg Tenax-TA organic adsorbent.
- Chromatography column feed materials two-stage thermal desorption device the most according to claim 1, it is characterised in that: described gas passage uses stainless steel tube.
- Chromatography column feed materials two-stage thermal desorption device the most according to claim 1, it is characterised in that: described heating-refrigerating plant (6) is thermoelectric refrigerator.
- Chromatography column feed materials two-stage thermal desorption device the most according to claim 1, it is characterised in that: being provided with heater on described 3rd electromagnetic valve (5), the outside of the 5th gas passage (e) and the 7th gas passage (h) is enclosed with heating mantle.
- 6. according to the sample injection method of the arbitrary described chromatography column feed materials two-stage thermal desorption device of claim 1-5, it is characterised in that: specifically comprise the following steps that(1) standard series pipe is done: first heater (3) heats, secondary heating mechanism (4) does not heats, 7th gas passage (h) and the 6th gas passage (g) are closed, first gas passage (a), second gas passage (b), 3rd gas passage (c), 4th gas passage (d), 5th gas passage (e) and the first emptying passage (f) are opened, testing sample is injected from the sampling device of first heater (3), at high temperature ensure that sample quickly gasifies, then by the high pure nitrogen entered from the first gas passage (a) by testing sample band to secondary heating mechanism (4), and adsorbed by Tenax-TA organic adsorbent, thus make standard series pipe；(2) thermal desorptions: secondary heating mechanism (4) is heated to 280-300 DEG C, heating-refrigerating plant (6) freezes, and temperature is adjusted to less than 4 DEG C, and to keep constant；First gas passage (a), the second gas passage (b), the 3rd gas passage (c), the 4th gas passage (d), the 5th gas passage (e) and the 7th gas passage (h) keep unimpeded, second emptying passage (j) is opened, first emptying passage (f), the 6th gas passage (g) and the second electromagnetic valve (8) are closed, 5th gas passage (e), the 7th gas passage (h) and the 3rd electromagnetic valve (5) heat, and prevent testing sample from condensing；After secondary heating mechanism (4) heating 5-15min, the testing sample of the Tenax-TA organic adsorbent absorption in the oneth Tenax pipe is desorbed out, by the high pure nitrogen entered from the first gas passage (a) by testing sample band to heating-refrigerating plant (6), and adsorbed by the Tenax-TA organic adsorbent in the 2nd Tenax pipe；(3) two-stage thermal desorption: after a thermal desorption, heating-refrigerating plant (6) is heated, open the second electromagnetic valve (8), second emptying passage (j) is closed, 9th gas passage (k) and the 8th gas passage (i) keep unimpeded, 7th gas passage (h) and the 6th gas passage (g) keep unimpeded, first emptying passage (f) and the 5th gas passage (e) are closed, heating-refrigerating plant (6) is through heating, the testing sample of the Tenax-TA organic adsorbent absorption in the 2nd Tenax pipe is desorbed out, by the high pure nitrogen entered from the 11st gas passage (m), testing sample band to chromatographic analysis device (10) is analyzed.
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| CN101294936B (en) * | 2007-04-25 | 2011-08-10 | 中国科学院沈阳应用生态研究所 | Plant source volatile organic matter test method |
| CN101639468B (en) * | 2009-08-25 | 2011-11-16 | 成都科林分析技术有限公司 | Automatic thermal desorption analyzer |
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Inventor after: Han Linzeng Inventor after: Wu Yunhui Inventor after: Wang Jinghua Inventor after: Zhu Dengbiao Inventor after: Li Baoqi Inventor after: Wang Huaigang Inventor after: Xu Dongliang Inventor after: Wang Xianming Inventor after: Zhao Qianfeng Inventor after: Qiao Rui Inventor after: Li Renhu Inventor after: Zhao Xinran Inventor after: Xu Yanxi Inventor after: Yuan Dawei Inventor after: Fu Siwei Inventor after: Zhang Qiaoyun Inventor after: Yu Huiliang Inventor after: Tosugi Toshiko Inventor after: Lu Limin Inventor after: Ding Huifu Inventor after: Meng Supin Inventor after: Guo Ying Inventor before: Han Linzeng Inventor before: Wang Jinghua Inventor before: Zhu Dengbiao Inventor before: Li Baoqi Inventor before: Wang Huaigang Inventor before: Xu Dongliang Inventor before: Wang Xianming Inventor before: Zhao Qianfeng Inventor before: Qiao Rui Inventor before: Li Renhu Inventor before: Xu Yanxi Inventor before: Zhao Xinran Inventor before: Yuan Dawei Inventor before: Fu Siwei Inventor before: Yu Huiliang Inventor before: Tosugi Toshiko Inventor before: Lu Limin Inventor before: Ding Huifu Inventor before: Meng Supin Inventor before: Guo Ying Inventor before: Wu Yunhui |