CN105954446A - High-low temperature control system for gas chromatography separation - Google Patents
High-low temperature control system for gas chromatography separation Download PDFInfo
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- CN105954446A CN105954446A CN201610585263.2A CN201610585263A CN105954446A CN 105954446 A CN105954446 A CN 105954446A CN 201610585263 A CN201610585263 A CN 201610585263A CN 105954446 A CN105954446 A CN 105954446A
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- low temperature
- heating tape
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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Abstract
The invention discloses a high-low temperature control system for gas chromatography separation. The system comprises a high-low temperature column box, a chromatographic column arranged inside the high-low temperature column box, a chromatographic valve connected with the chromatographic column through a first chromatographic gas pipeline, a chromatographic detector connected with the chromatographic column through a second chromatographic gas pipeline, a self-pressurization liquid nitrogen container connected with the high-low temperature column box through a pair of liquid nitrogen conveying pipes to form a liquid nitrogen circulating loop, low temperature electromagnetic valves arranged on the liquid nitrogen conveying pipes and a temperature control device arranged on the exterior of the high-low temperature column box. Liquid nitrogen is used for controlling the chromatographic column to work under low temperature, a heating device is adopted for enabling the column box to reach the activated temperature for chromatographic column activation, high-low temperature control integration is effectively achieved, the temperature inside the column box is freely switched, and the requirement of the chromatographic column for reliably working under different temperatures is met.
Description
Technical field
The present invention relates to cryogenic gas-chromatography separation technology field, specifically, relate to a kind of high/low temperature control system separated for gas chromatogram.
Background technology
Gas chromatographic analysis is a method for separating and analyzing the most ripe, has highly important effect in fields such as pharmaceutical analysis, environmental analysis, organic and inorganic chemicals analyses.In conventional gas chromatographic analysis, chromatographic column operating temperature is 30 DEG C～450 DEG C, but the quantitative analysis for some special gas such as hydrogen isotope protium, deuterium, tritium gas needs to work at-196 DEG C～450 DEG C, wherein low temperature is for realizing gas separation on a column, and high temperature is used for pretreatment and the activation of chromatographic column.Presently commercially available gas chromatograph does not all have corollary equipment to provide the chromatographic column working environment of-196 DEG C～450 DEG C, related researcher needs generally according to experiment, produce the low temperature of-196 DEG C with liquid nitrogen when chromatographic column is in mask work state, when chromatographic column needs activation, use chromatograph to carry heat riser and carry out heat-activated.
But this method inefficiency, additional liquid nitrogen container does not matches with chromatograph, and liquid nitrogen loss amount is big.The method is unfavorable for that the pre-treatment and activation etc. of chromatographic column operates simultaneously, and chromatographic column needs often dismounting, safeguards inconvenient.Control integrated it is thus desirable to research and develop a kind of system supporting with chromatograph to realize high/low temperature, control chromatographic column at extremely low temperature (liquid nitrogen temperature) and high temperature (200-450
C) work, and freely switching and reliably working of temperature can be realized.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the present invention provides a kind of high/low temperature control system separated for gas chromatogram.
To achieve these goals, the technical solution used in the present invention is as follows:
A kind of high/low temperature control system separated for gas chromatogram, including high/low temperature post case, it is placed in the chromatographic column in high/low temperature post case, the chromatograph valve being connected with chromatographic column by the first chromatograph gas piping, the chromatographic detector being connected with chromatographic column by the second chromatograph gas piping, by a pair liquid nitrogen transfer tube and high/low temperature post case connect and compose liquid nitrogen closed circuit from supercharging liquid nitrogen container, it is arranged at the low-temperature solenoid valve on liquid nitrogen transfer tube, and is arranged at the external temperature control device outside high/low temperature post case.
Further, described high/low temperature post case includes casing and the case lid mutually fastened up and down, wherein, described casing includes shell body and the inner lining that its upper end flushes and bottom connects, it is present in the gap between shell body and each side of inner lining, it is arranged at the first heating tape of inner lining outer lower portion, the second heating tape being arranged on shell body inwall, the body thermal insulation layer that full gap between described shell body and inner lining is formed is filled by heat-barrier material, the heating tape wire hole being opened on shell body, and at least three cincture is arranged at the lower snap close of shell body side in uniform way.
Further, described case lid includes casing cover and the inner bladder cover that its lower end flushes and top connects, it is present in the gap between casing cover and each side of inner bladder cover, the lid thermal insulation layer that full gap between described casing cover and inner bladder cover is formed is filled by heat-barrier material, two pairs run through casing cover top, lid thermal insulation layer and the access opening at inner bladder cover top, and at least three cincture is arranged at the upper snap close of casing cover side in uniform way, wherein, described lower snap close and upper snap close are mutually matched；Described first chromatograph gas piping and the second chromatograph gas piping are arranged through pair of channels hole, and access opening is arranged by the pair of liquid nitrogen transfer tube through another.
In order to ensure that effect of heat insulation equalizes, the gap clearance between described shell body and each side of inner lining is equal, and the gap clearance between described casing cover and each side of inner bladder cover is equal.Further, the height that described first heating tape is arranged is not higher than the half of described inner lining.
Preferably, described shell body and the cross section of inner lining, and the cross section of described casing cover and inner bladder cover is all in concentric circles, and the size coupling of described inner lining and inner bladder cover, the size coupling of described shell body and casing cover.
Specifically, described shell body bottom interior wall is provided with body and connects post, and described inner lining bottom outer wall is provided with the body adapter sleeve being connected post coupling with described body.For the ease of installing and stable connection, described body connects post and body adapter sleeve interference fit.And the length of described body adapter sleeve is mated with the gap clearance bottom shell body and inner lining.
Further, described casing cover top inner wall is provided with lid and connects post, and described inner bladder cover top exterior walls is provided with the lid adapter sleeve being connected post coupling with described lid.For the ease of installing and stable connection, described lid connects post and lid adapter sleeve interference fit.And the described length of lid adapter sleeve is mated with the gap clearance of casing cover and inner bladder cover top.
Further, high-order liquid level sensor and low level liquid level sensor it are provided with in the inner lining of described high/low temperature post case；The nozzle position of one described liquid nitrogen transfer tube is corresponding with the position of high-order liquid level sensor, and the nozzle position of another described liquid nitrogen transfer tube is corresponding with the position of low level liquid level sensor.
More specifically, described external temperature controls the first temperature sensor that device includes being arranged on the first heating tape, the second temperature sensor being arranged on the second heating tape, the 3rd heating tape being arranged on chromatograph valve, it is arranged at the three-temperature sensor on the 3rd heating tape, it is arranged at the 4th heating tape on the first chromatograph gas piping, it is arranged at the 4th temperature sensor on the 4th heating tape, it is arranged at the 5th heating tape on the second chromatograph gas piping, it is arranged at the 5th temperature sensor on the 5th heating tape, and the temperature controller being all connected with all heating tapes and all temperature sensors.Specifically, described 3rd heating tape is coated on chromatograph valve, and described 4th heating tape is placed on the first chromatograph gas piping, and described 5th heating tape is placed on the second chromatograph gas piping.
Preferably, described first, second, third, fourth and fifth temperature sensor all uses JPt100 type platinum resistance.
For the ease of monitoring temperature, described temperature control equipment also includes that warning module, described warning module are respectively arranged between the first heating tape and temperature controller, between the second heating tape and temperature controller, between the 3rd heating tape and temperature controller, between the 4th heating tape and temperature controller, between the 5th heating tape and temperature controller.
Specifically, described warning module includes relay switch K2 and the hand switch K1 being sequentially connected in series with heating tape, and it is connected to gather between relay switch K2 and hand switch K1 the voltage transformer of switching signal, wherein, relay switch K2 and voltage transformer are all connected with temperature controller.The heating tape work when K1 and K2 switchs all Guan Bis, and the opening and closing of control signal control relay switch K2 is produced by temperature controller, and fed back to temperature controller by voltage transformer collection corresponding signal and realize early warning.
Compared with prior art, the method have the advantages that
(1) present invention utilizes liquid nitrogen control chromatographic column to work at low temperatures, coordinate heater to reach activation temperature in making post case and carry out chromatographic column activation, effectively achieve high/low temperature and control integration, and post the temperature inside the box can be made freely to switch, meet chromatographic column reliably working under condition of different temperatures, and application of the present invention is good, simple in construction, it is simple to manufacture, with low cost, it is with a wide range of applications, is suitable for popularization and application.
(2) present invention utilizes inner and outer shell and lid to build double thermal insulation system, the thermal insulation layer using heat-barrier material filling is effectively incubated in inner bladder cover, regulatable heating tape is coordinated to heat in inner bag body, contribute to the accurate control of high/low temperature post the temperature inside the box, the duct of design specialized is connected with support devices such as chromatographic detector and liquid nitrogen transfer tubes simultaneously, with strong points.
(3) present invention realizes the temperature to chromatograph pipeline control by arranging heating tape and temperature sensor on chromatograph valve and respective line, both can ensure that the steady temperature in post case, can effectively carry out again temperature regulation, it is simple to the activation temperature of chromatographic column is controlled.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of the present invention.
Fig. 2 is the structural representation of high/low temperature post case in the present invention.
Fig. 3 is the sectional view of high/low temperature post case in the present invention.
Fig. 4 is the setting principle schematic diagram of temperature control equipment in the present invention.
Fig. 5 is the schematic diagram of warning module in the present invention.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings, and embodiments of the present invention include but not limited to the following example.
Embodiment
As shown in Figures 1 to 5, this is used for the high/low temperature control system that gas chromatogram separates, including high/low temperature post case 1, it is placed in the chromatographic column 2 in high/low temperature post case, the chromatograph valve 3 being connected with chromatographic column by the first chromatograph gas piping 4, the chromatographic detector 5 being connected with chromatographic column by the second chromatograph gas piping 6, by a pair liquid nitrogen transfer tube 7 and high/low temperature post case connect and compose liquid nitrogen closed circuit from supercharging liquid nitrogen container 8, the low-temperature solenoid valve 9 being arranged on liquid nitrogen transfer tube, and it is arranged at the external temperature control device outside high/low temperature post case.
Further, described high/low temperature post case includes casing 10 and the case lid 20 mutually fastened up and down, wherein, described casing includes shell body 11 and the inner lining 12 that its upper end flushes and bottom connects, it is present in the gap between shell body and each side of inner lining, it is arranged at the first heating tape 13 of inner lining outer lower portion, the second heating tape 14 being arranged on shell body inwall, the body thermal insulation layer 15 that full gap between described shell body and inner lining is formed is filled by heat-barrier material, the heating tape wire hole 16 being opened on shell body, and at least three cincture is arranged at the lower snap close 17 of shell body side in uniform way.
Further, described case lid includes casing cover 21 and the inner bladder cover 22 that its lower end flushes and top connects, it is present in the gap between casing cover and each side of inner bladder cover, the lid thermal insulation layer 23 that full gap between described casing cover and inner bladder cover is formed is filled by heat-barrier material, two pairs of access openings 24 running through casing cover top, lid thermal insulation layer and inner bladder cover top, and at least three cincture is arranged at the upper snap close 25 of casing cover side in uniform way, wherein, described lower snap close and upper snap close are mutually matched；Described first chromatograph gas piping and the second chromatograph gas piping are arranged through pair of channels hole, and access opening is arranged by the pair of liquid nitrogen transfer tube through another.
In order to ensure that effect of heat insulation equalizes, the gap clearance between described shell body and each side of inner lining is equal, and the gap clearance between described casing cover and each side of inner bladder cover is equal.Further, the height that described first heating tape is arranged is not higher than the half of described inner lining.
Preferably, described shell body and the cross section of inner lining, and the cross section of described casing cover and inner bladder cover is all in concentric circles, and the size coupling of described inner lining and inner bladder cover, the size coupling of described shell body and casing cover.
Specifically, described shell body bottom interior wall is provided with body and connects post 18, and described inner lining bottom outer wall is provided with the body adapter sleeve 19 being connected post coupling with described body.For the ease of installing and stable connection, described body connects post and body adapter sleeve interference fit.And the length of described body adapter sleeve is mated with the gap clearance bottom shell body and inner lining.
Further, described casing cover top inner wall is provided with lid and connects post 26, and described inner bladder cover top exterior walls is provided with the lid adapter sleeve 27 being connected post coupling with described lid.For the ease of installing and stable connection, described lid connects post and lid adapter sleeve interference fit.And the described length of lid adapter sleeve is mated with the gap clearance of casing cover and inner bladder cover top.
Further, high-order liquid level sensor 28 and low level liquid level sensor 29 it are provided with in the inner lining of described high/low temperature post case；The nozzle position of one described liquid nitrogen transfer tube is corresponding with the position of high-order liquid level sensor, and the nozzle position of another described liquid nitrogen transfer tube is corresponding with the position of low level liquid level sensor.
More specifically, described external temperature controls the first temperature sensor 37 that device includes being arranged on the first heating tape, the second temperature sensor 38 being arranged on the second heating tape, the 3rd heating tape 31 being arranged on chromatograph valve, it is arranged at the three-temperature sensor 32 on the 3rd heating tape, it is arranged at the 4th heating tape 33 on the first chromatograph gas piping, it is arranged at the 4th temperature sensor 34 on the 4th heating tape, it is arranged at the 5th heating tape 35 on the second chromatograph gas piping, it is arranged at the 5th temperature sensor 36 on the 5th heating tape, and the temperature controller being all connected with all heating tapes and all temperature sensors.Specifically, described 3rd heating tape is coated on chromatograph valve, and described 4th heating tape is placed on the first chromatograph gas piping, and described 5th heating tape is placed on the second chromatograph gas piping.
Preferably, described first, second, third, fourth and fifth temperature sensor all uses JPt100 type platinum resistance.
For the ease of monitoring temperature, described temperature control equipment also includes that warning module, described warning module are respectively arranged between the first heating tape and temperature controller, between the second heating tape and temperature controller, between the 3rd heating tape and temperature controller, between the 4th heating tape and temperature controller, between the 5th heating tape and temperature controller.
Specifically, described warning module includes relay switch K2 and the hand switch K1 being sequentially connected in series with heating tape, and it is connected to gather between relay switch K2 and hand switch K1 the voltage transformer of switching signal, wherein, relay switch K2 and voltage transformer are all connected with temperature controller.The heating tape work when K1 and K2 switchs all Guan Bis, and the opening and closing of control signal control relay switch K2 is produced by temperature controller, and fed back to temperature controller by voltage transformer collection corresponding signal and realize early warning.
Low-temperature working pattern and hot operation pattern it is divided into when the present invention uses.
During low-temperature working pattern, by filling liquid nitrogen in high/low temperature post case from supercharging liquid nitrogen container, liquid nitrogen injection rate is controlled according to temperature requirements, coordinate the first and second heating tapes, can realize the demand of setting up of various low temperature environments in high/low temperature post case, minimum-196 DEG C, i.e. full liquid nitrogen environment, in the range of-196 DEG C to 0 DEG C, the first and second heating tapes that different amount of liquid nitrogen and corresponding power run reach perfect constant.
During hot operation pattern, first the amount of liquid nitrogen in detection high/low temperature post case, is emptied, is then turned on corresponding heating tape, it is achieved hot environment, and heated perimeter is that room temperature is to 450 DEG C.
The temperature control effect that the present invention can reach: realizing high/low temperature post case working range and reach-196 DEG C to 450 DEG C, wherein, when-196 DEG C to-180 DEG C, temperature control precision is ± 15 DEG C；When-180 DEG C to-150 DEG C, temperature control precision is ± 8 DEG C；When-150 DEG C to 0 DEG C, temperature control precision is ± 5 DEG C；When room temperature is to 450 DEG C, temperature control precision is ± 1 DEG C.
Above-described embodiment is only the preferred embodiments of the present invention, not limiting the scope of the invention, as long as using the design principle of the present invention, and carries out non-creativeness work on this basis and the change made, within all should belonging to protection scope of the present invention.
Claims (10)
1. the high/low temperature control system separated for gas chromatogram, it is characterized in that, including high/low temperature post case, it is placed in the chromatographic column in high/low temperature post case, the chromatograph valve being connected with chromatographic column by the first chromatograph gas piping, the chromatographic detector being connected with chromatographic column by the second chromatograph gas piping, by a pair liquid nitrogen transfer tube and high/low temperature post case connect and compose liquid nitrogen closed circuit from supercharging liquid nitrogen container, it is arranged at the low-temperature solenoid valve on liquid nitrogen transfer tube, and is arranged at the temperature control equipment outside high/low temperature post case.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 1, it is characterized in that, described high/low temperature post case includes casing and the case lid mutually fastened up and down, wherein, described casing includes shell body and the inner lining that its upper end flushes and bottom connects, it is present in the gap between shell body and each side of inner lining, it is arranged at the first heating tape of inner lining outer lower portion, the second heating tape being arranged on shell body inwall, the body thermal insulation layer that full gap between described shell body and inner lining is formed is filled by heat-barrier material, the heating tape wire hole being opened on shell body, and at least three cincture is arranged at the lower snap close of shell body side in uniform way.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 2, it is characterized in that, described case lid includes casing cover and the inner bladder cover that its lower end flushes and top connects, it is present in the gap between casing cover and each side of inner bladder cover, the lid thermal insulation layer that full gap between described casing cover and inner bladder cover is formed is filled by heat-barrier material, two pairs run through casing cover top, lid thermal insulation layer and the access opening at inner bladder cover top, and at least three cincture is arranged at the upper snap close of casing cover side in uniform way, wherein, described lower snap close and upper snap close are mutually matched；Described first chromatograph gas piping and the second chromatograph gas piping are arranged through pair of channels hole, and access opening is arranged by the pair of liquid nitrogen transfer tube through another.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 3, it is characterized in that, described shell body and the cross section of inner lining, and the cross section of described casing cover and inner bladder cover is all in concentric circles, and the size coupling of described inner lining and inner bladder cover, the size coupling of described shell body and casing cover.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 3, it is characterised in that described shell body bottom interior wall is provided with body and connects post, and described inner lining bottom outer wall is provided with the body adapter sleeve being connected post coupling with described body.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 3, it is characterised in that described casing cover top inner wall is provided with lid and connects post, described inner bladder cover top exterior walls is provided with the lid adapter sleeve being connected post coupling with described lid.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 3, it is characterised in that be provided with high-order liquid level sensor and low level liquid level sensor in the inner lining of described high/low temperature post case；The nozzle position of one described liquid nitrogen transfer tube is corresponding with the position of high-order liquid level sensor, and the nozzle position of another described liquid nitrogen transfer tube is corresponding with the position of low level liquid level sensor.
8. according to a kind of high/low temperature control system separated for gas chromatogram described in any one of claim 2～7, it is characterized in that, described temperature control equipment includes the first temperature sensor being arranged on the first heating tape, the second temperature sensor being arranged on the second heating tape, the 3rd heating tape being arranged on chromatograph valve, it is arranged at the three-temperature sensor on the 3rd heating tape, it is arranged at the 4th heating tape on the first chromatograph gas piping, it is arranged at the 4th temperature sensor on the 4th heating tape, it is arranged at the 5th heating tape on the second chromatograph gas piping, it is arranged at the 5th temperature sensor on the 5th heating tape, and the temperature controller being all connected with all heating tapes and all temperature sensors.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 8, it is characterised in that described first, second, third, fourth and fifth temperature sensor all uses JPt100 type platinum resistance.
A kind of high/low temperature control system separated for gas chromatogram the most according to claim 8, it is characterized in that, described temperature control equipment also includes that warning module, described warning module are respectively arranged between the first heating tape and temperature controller, between the second heating tape and temperature controller, between the 3rd heating tape and temperature controller, between the 4th heating tape and temperature controller, between the 5th heating tape and temperature controller.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610585263.2A CN105954446B (en) | 2016-07-25 | 2016-07-25 | A kind of height temperature control system for gas-chromatography separation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610585263.2A CN105954446B (en) | 2016-07-25 | 2016-07-25 | A kind of height temperature control system for gas-chromatography separation |
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| CN105954446A true CN105954446A (en) | 2016-09-21 |
| CN105954446B CN105954446B (en) | 2018-02-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610585263.2A Expired - Fee Related CN105954446B (en) | 2016-07-25 | 2016-07-25 | A kind of height temperature control system for gas-chromatography separation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693703A (en) * | 2017-02-15 | 2017-05-24 | 中国工程物理研究院材料研究所 | Displacement chromatography hydrogen isotope separation device |
| CN112213433A (en) * | 2020-08-04 | 2021-01-12 | 浙江中环瑞蓝科技发展有限公司 | Low-temperature gas chromatography column box |
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| CN205809012U (en) * | 2016-07-25 | 2016-12-14 | 中国工程物理研究院材料研究所 | A kind of high/low temperature control system separated for gas chromatogram |
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2016
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Patent Citations (7)
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| GB1200415A (en) * | 1967-01-30 | 1970-07-29 | Perkin Elmer Corp | Gas chromatographic instrument |
| CN1412504A (en) * | 2001-10-08 | 2003-04-23 | 中国科学院生态环境研究中心 | Semiconductor refrigerated low-temp. chromatograph enrichment and separation equipment |
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| CN106693703A (en) * | 2017-02-15 | 2017-05-24 | 中国工程物理研究院材料研究所 | Displacement chromatography hydrogen isotope separation device |
| CN112213433A (en) * | 2020-08-04 | 2021-01-12 | 浙江中环瑞蓝科技发展有限公司 | Low-temperature gas chromatography column box |
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| CN105954446B (en) | 2018-02-02 |
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Granted publication date: 20180202 Termination date: 20190725 |