CN102004134A - Automatic thermal desorption instrument based on thermal gas desorption - Google Patents
Automatic thermal desorption instrument based on thermal gas desorption Download PDFInfo
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- CN102004134A CN102004134A CN 201010580637 CN201010580637A CN102004134A CN 102004134 A CN102004134 A CN 102004134A CN 201010580637 CN201010580637 CN 201010580637 CN 201010580637 A CN201010580637 A CN 201010580637A CN 102004134 A CN102004134 A CN 102004134A
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Abstract
The invention relates to an automatic thermal desorption instrument based on thermal gas desorption. The auotomatic thermal desorption instrument comprises a sample pipe provided with a first desorption sample outlet and a condensing adsorption pipe which is provided with a desorption sample inlet, an adsorption/desorption inlet/outlet and a second desorption sample outlet and is filled with adsorbent, wherein a first end of a first sample output pipe is communicated with the desorption sample outlets, and a second end of the first sample output pipe extends out of the end surface of the adsorbent after penetrating through the condensing adsorption tube and the adsorbent; a first end of a second sample output pipe is communicated with the second desorption sample outlet; a preheated carrier gas conveyer pipe the first end of which is communicated with the adsorption/desorption inlet/outlet is provided with a heater, and a second end of the preheated carrier gas conveyer pipe is provided with a first control valve; a desorption exhaust pipe connected with the first control valve is provided with a second control valve; and a second carrier gas conveyer pipe is connected with the first control valve. Besides, the desorption instrument also comprises a first carrier gas conveyer pipe, a transfer pipe the first end of which is communicated with a gas chromatograph and a changeover valve. By adopting the invention, the secondary desorption rate can be improved, the chromatographic peak is sharpened and simultaneously the desorption efficiency is improved.
Description
Technical field:
What the present invention relates to is a kind of analytical instrument sample pre-treatments device, particularly be a kind of automatic thermal desorption desorption instrument that adopts the hot gas desorb.
Background technology:
Sample pre-treatments unit as a kind of analytical instrument, one-level thermal desorption (thermal desorption is called thermal desorption again) is exactly that ready sample hose is delivered to gas chromatograph analysis by heating the direct desorb in back, because sample hose generally all bigger (pipe when industrial standard is external diameter 1/4) can cause the excessive broadening of chromatographic peak.
Traditional two-stage desorb is sample hose to be separated be drawn onto in the cryogenic condensation adsorption tube, and then to the condensation adsorption tube carry out Fast Heating by carrier gas with the vaporization the sample blowback to gas chromatograph.The speed that temperature rises in the condensation adsorption tube directly influences the width and the desorption efficiency of chromatographic peak, under the certain situation of other condition, the width of component chromatographic peak is the speed decision that is broken away from the cold-trap adsorbent by component, under the same conditions, the heat that passes to carrier gas by the condensation adsorption tube speed that the carrier gas temperature is raise has just determined the width of component chromatographic peak.Because carrier gas is flowed, it can constantly take away heat, its the true temperature temperature more indicated than the well heater on the condensation adsorption tube is low, and be subjected to the influence of factors such as condensation adsorption tube size, material, carrier gas type, flow velocity by the speed that the condensation adsorption tube passes to its heat, will bring the broadening problem of component chromatographic peak like this.In order to overcome the influence of this factor, analyzed narrower helping of component chromatographic peak.
Summary of the invention:
The objective of the invention is to make chromatographic peak more sharp-pointed, improve the automatic thermal desorption desorption instrument of the employing hot gas desorb of desorption efficiency simultaneously for second level desorption rate in the desorb of a kind of raising two-stage is provided.
The object of the present invention is achieved like this:
The present invention adopts the automatic thermal desorption desorption instrument of hot gas desorb, include the sample hose that sample and adsorbent are housed of the carrier gas input port and the first desorb sample export, be positioned at the condensation adsorption tube that adsorbent is housed that the second desorb sample inlet and the adsorption-desorption import and export and the second desorb sample export are arranged at sample hose top, first end of the first sample efferent duct is communicated with the first desorb sample export on the sample hose and second end stretches out the adsorbent end face after passing desorb sample inlet on the condensation adsorption tube and adsorbent, first end of the second sample efferent duct is communicated with the second desorb sample export on the condensation adsorption tube, first end and adsorption-desorption are imported and exported preheating of being communicated with and on the carrier gas delivery pipe well heater are housed and first operation valve is housed on second end, with on the desorb gas outlet that first operation valve is connected second operation valve is housed, the second carrier gas delivery pipe is connected with first operation valve, the first carrier gas delivery pipe that also has first end to be communicated with in the described desorption instrument with carrier gas source, the transfer tube that first end is communicated with gas chromatograph, second end at the first carrier gas delivery pipe, control second sample efferent duct and the transfer tube arranged between second end of second end of transfer tube and the second sample efferent duct, the first carrier gas delivery pipe and transfer tube are logical, disconnected transfer valve, adorn well heater preheating on the carrier gas delivery pipe, be to enter the carrier gas temperature of condensation adsorption tube when the desorb of the second level in order to improve, first operation valve is controlled the second carrier gas delivery pipe and is preheated the carrier gas delivery pipe, desorb gas outlet and preheat logical between the carrier gas delivery pipe, disconnected.
The recovery gas outlet that contains the 3rd operation valve is housed on the exhausr port on the above-mentioned sample hose, realizes the recovery again of sample, recovery sample can be analyzed once more, improve the utilization factor of rare sample.
First isocon with the 4th operation valve is housed on the first above-mentioned sample efferent duct, second isocon with the 5th operation valve is housed on the second sample efferent duct, regulate first, second bypass flow respectively.
When the present invention works, first, second operation valve is opened, transfer valve and other operation valve are closed, sample hose is discharged into the condensation adsorption tube by heating with sample gas, sample gas is passed second end of the first sample efferent duct on the condensation adsorption tube and the agent that begins to be condensed of turning back is adsorbed once more, carrier gas is imported and exported reconciliation suction tracheae by adsorption-desorption and is flowed out from second operation valve, and sample is focused once more; When first operation valve, transfer valve are opened, well heater is heated to design temperature to preheating the carrier gas delivery pipe, carrier gas by the second carrier gas delivery pipe, first operation valve, preheat carrier gas delivery pipe heater via and add the thermosetting thermal current and enter the condensation adsorption tube and make the sample instant vaporization be transferred to gas chromatograph through transfer tube again to finish sample introduction through transfer valve outlet.
The present invention adopts the pre-warmed method of desorb carrier gas when the desorb of the second level, effectively improved desorption effect.The present invention can improve second level desorption rate (can reach more than 20%), makes chromatographic peak more sharp-pointed, has improved desorption efficiency simultaneously greatly.
Description of drawings:
Fig. 1 is a structural representation of the present invention.
Fig. 2 working state figure of the present invention that is second carrier gas channel when the condensation adsorption tube is carried carrier gas through heating.
Working state figure of the present invention when Fig. 3 is the disconnection of second carrier gas channel.
Working state figure of the present invention when Fig. 4 opens for reclaiming gas outlet.
Embodiment:
Referring to Fig. 1, present embodiment adopts the automatic thermal desorption desorption instrument of hot gas desorb, include the sample hose that sample and adsorbent are housed 4 of the carrier gas input port 1 and the first desorb sample export 3, have desorb sample inlet 5 and the adsorption-desorption that are positioned at the sample hose top are imported and exported the condensation adsorption tube 9 that adsorbent 8 is housed of the 6 and second desorb sample export 7.First end of the first sample efferent duct 10 is communicated with the first desorb sample export on the sample hose and second end stretches out adsorbent end face A after passing desorb sample inlet on the condensation adsorption tube and adsorbent.First end of the second sample efferent duct 11 is communicated with the second desorb sample export on the condensation adsorption tube.First end and adsorption-desorption are imported and exported preheating of being communicated with and on the carrier gas delivery pipe 25 well heater 26 are housed and first operation valve 13 is housed on second end.With on the desorb gas outlet that first operation valve is connected second operation valve 14 is housed.The second carrier gas delivery pipe 19 is connected with first operation valve.With on the desorb gas outlet that first operation valve is connected second operation valve 14 is housed.The transfer tube 16 that the first carrier gas delivery pipe, 15, the first ends that also have first end to be communicated with carrier gas source in this desorption instrument are communicated with gas chromatograph.At second end of the first carrier gas delivery pipe, the transfer valve 18 of the control second sample efferent duct and transfer tube, the first carrier gas delivery pipe and transfer tube switching is arranged between second end of second end of transfer tube and the second sample efferent duct.
Be connected with the recovery gas outlet 21 that the 3rd operation valve 20 is housed on the exhausr port 2 on the sample hose.
When sample hose is heated, the sample that is adsorbed on the sample hose 4 interior adsorbents will come out by desorption (desorb), if all valves all are in position among Fig. 1, bring the sample that desorbs into condensation adsorption tube 9 from the carrier gas meeting that carrier gas input port 1 enters, passed adsorbent owing to enter the pipeline of condensation adsorption tube 9 from sample hose 4, sample gas will from then on turn back and the adsorption tube that begins to be condensed in adsorbent adsorb once more, carrier gas is flowed out from second operation valve 14, because the adsorption efficiency height of condensation adsorption tube, sample is focused on once more.When wanting the sample of desorb condensation adsorption tube 9, enter Fig. 2 state, carrier gas inlet 1 sealing, 26 pairs of well heaters preheat the carrier gas delivery pipe and are heated to design temperature, open first operation valve 13, carrier gas makes sample produce instantaneous vaporization through first operation valve 13 after heater heats formation thermal current enters condensation adsorption tube 9 by the second carrier gas delivery pipe 19, is transferred to gas chromatograph through transfer tube 16 again through the transfer valve outlet and finishes sample introduction.The adsorption tube of condensation simultaneously 9 Fast Heating.
The present invention also has sample and reclaims function, as Fig. 4, opens the 3rd operation valve 20 in to the desorb of condensation adsorption tube, and the sample that desorbs like this part is brought into sample hose 4 by carrier gas and reclaimed, and what of recovery can be by 20 controls of the 3rd operation valve.
The present invention can directly send into gas chromatograph by carrier gas after the sample desorb with sample hose 4, as Fig. 3, operation valve 14,17,20 and 22 is all closed, and transfer valve 15 switchings couple together b and c, and the sample that sample hose 4 desorbs is directly sent into gas chromatograph by carrier gas.
The foregoing description is that foregoing of the present invention is further described, but this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to the foregoing description.All technology that realizes based on foregoing all belong to scope of the present invention.
Claims (3)
1. adopt the automatic thermal desorption desorption instrument of hot gas desorb, include the sample hose that sample and adsorbent are housed (4) of the carrier gas input port (1) and the first desorb sample export (3), have desorb sample inlet (5) and the adsorption-desorption that are positioned at the sample hose top are imported and exported the condensation adsorption tube (9) that adsorbent (8) is housed of (6) and the second desorb sample export (7), first end of the first sample efferent duct (10) is communicated with the first desorb sample export on the sample hose and second end stretches out the adsorbent end face after passing desorb sample inlet on the condensation adsorption tube and adsorbent, first end of the second sample efferent duct (11) is communicated with the second desorb sample export on the condensation adsorption tube, first end and adsorption-desorption are imported and exported preheating of being communicated with and on the carrier gas delivery pipe (25) well heater (26) are housed and first operation valve (13) is housed on second end, with on the desorb gas outlet that first operation valve is connected second operation valve (14) is housed, the second carrier gas delivery pipe (19) is connected with first operation valve, the first carrier gas delivery pipe (15) that also has first end to be communicated with in the described desorption instrument with carrier gas source, the transfer tube that first end is communicated with gas chromatograph (16) is at second end of the first carrier gas delivery pipe, control second sample efferent duct and the transfer tube arranged between second end of second end of transfer tube and the second sample efferent duct, the first carrier gas delivery pipe and transfer tube are logical, disconnected transfer valve (18).
2. the automatic thermal desorption desorption instrument of employing hot gas as claimed in claim 1 desorb is characterized in that being equipped with on the exhausr port (2) on the sample hose recovery gas outlet (21) that contains the 3rd operation valve (20).
3. the automatic thermal desorption desorption instrument of employing hot gas as claimed in claim 1 or 2 desorb, it is characterized in that being equipped with on the first sample efferent duct first isocon (23), second isocon (24) with the 5th operation valve (17) is housed on the second sample efferent duct with the 4th operation valve (22).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010580637 CN102004134A (en) | 2010-12-09 | 2010-12-09 | Automatic thermal desorption instrument based on thermal gas desorption |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010580637 CN102004134A (en) | 2010-12-09 | 2010-12-09 | Automatic thermal desorption instrument based on thermal gas desorption |
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| CN102004134A true CN102004134A (en) | 2011-04-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108508113A (en) * | 2018-04-19 | 2018-09-07 | 成都科林分析技术有限公司 | single-stage thermal desorption desorption system |
| CN109030679A (en) * | 2018-07-19 | 2018-12-18 | 浙江赛鹭鑫仪器有限公司 | A kind of second level pyrolysis analysis system |
| CN110346490A (en) * | 2019-08-07 | 2019-10-18 | 常州磐宇仪器有限公司 | A kind of multi-functional second level thermal desorption air-channel system |
| CN115479999A (en) * | 2021-06-16 | 2022-12-16 | 中国石油天然气股份有限公司 | A detection system and method for sulfur-free odorant |
| US11846575B2 (en) | 2018-12-31 | 2023-12-19 | Teknologian Tutkimuskeskus Vtt Oy | Sampling arrangement |
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| US20060016245A1 (en) * | 2004-07-26 | 2006-01-26 | Perkinelmer Las, Inc. | System for regulating fluid flowing through chromatographic column |
| US20070151326A1 (en) * | 2004-11-03 | 2007-07-05 | Kim Jo C | Sample collection apparatus for analysis of air pollution comprising moisture pretreatment means |
| CN101639468A (en) * | 2009-08-25 | 2010-02-03 | 成都科林分析技术有限公司 | Automatic thermal desorption analyzer |
| CN201518018U (en) * | 2009-10-23 | 2010-06-30 | 河南省建筑科学研究院有限公司 | Freely-pluggable type thermal desorbing instrument |
| CN201876443U (en) * | 2010-12-09 | 2011-06-22 | 成都科林分析技术有限公司 | Automatic thermal desorption instrument capable of using thermal gas for desorption |
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2010
- 2010-12-09 CN CN 201010580637 patent/CN102004134A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060016245A1 (en) * | 2004-07-26 | 2006-01-26 | Perkinelmer Las, Inc. | System for regulating fluid flowing through chromatographic column |
| US20070151326A1 (en) * | 2004-11-03 | 2007-07-05 | Kim Jo C | Sample collection apparatus for analysis of air pollution comprising moisture pretreatment means |
| CN101639468A (en) * | 2009-08-25 | 2010-02-03 | 成都科林分析技术有限公司 | Automatic thermal desorption analyzer |
| CN201518018U (en) * | 2009-10-23 | 2010-06-30 | 河南省建筑科学研究院有限公司 | Freely-pluggable type thermal desorbing instrument |
| CN201876443U (en) * | 2010-12-09 | 2011-06-22 | 成都科林分析技术有限公司 | Automatic thermal desorption instrument capable of using thermal gas for desorption |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108508113A (en) * | 2018-04-19 | 2018-09-07 | 成都科林分析技术有限公司 | single-stage thermal desorption desorption system |
| CN109030679A (en) * | 2018-07-19 | 2018-12-18 | 浙江赛鹭鑫仪器有限公司 | A kind of second level pyrolysis analysis system |
| US11846575B2 (en) | 2018-12-31 | 2023-12-19 | Teknologian Tutkimuskeskus Vtt Oy | Sampling arrangement |
| CN110346490A (en) * | 2019-08-07 | 2019-10-18 | 常州磐宇仪器有限公司 | A kind of multi-functional second level thermal desorption air-channel system |
| CN110346490B (en) * | 2019-08-07 | 2022-05-24 | 常州磐宇仪器有限公司 | Multifunctional two-stage thermal desorption gas path system |
| CN115479999A (en) * | 2021-06-16 | 2022-12-16 | 中国石油天然气股份有限公司 | A detection system and method for sulfur-free odorant |
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Application publication date: 20110406 |