CN2840034Y - Carrier gas switching device - Google Patents

Carrier gas switching device Download PDF

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Publication number
CN2840034Y
CN2840034Y CN 200520042767 CN200520042767U CN2840034Y CN 2840034 Y CN2840034 Y CN 2840034Y CN 200520042767 CN200520042767 CN 200520042767 CN 200520042767 U CN200520042767 U CN 200520042767U CN 2840034 Y CN2840034 Y CN 2840034Y
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CN
China
Prior art keywords
carrier gas
gas
tcd
transfer valve
thermal conductivity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN 200520042767
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Chinese (zh)
Inventor
刘俊涛
钟思青
刘国强
唐健芬
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
China Petrochemical Corp
Original Assignee
China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Priority to CN 200520042767 priority Critical patent/CN2840034Y/en
Application granted granted Critical
Publication of CN2840034Y publication Critical patent/CN2840034Y/en
Anticipated expiration legal-status Critical
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Abstract

The utility model relates to a carrier gas switching device. It mainly solves the technical problems that the departed chromatographic analyzer can not switch the carrier gas so as to lead to poor detecting sensitivity and linearity of partial components caused by using a single carrier gas in the course of simultaneous detection of all the complicated sample components containing hydrogen gas, oxygen gas and nitrogen gas. The invention adopts the technical scheme that a switching valve and a carrier gas type controller are equipped inside the carrier gas analyzer, which preferably solves the problems, and the invention can be used in the process of the industrial manufacture of chromatogram.

Description

The carrier gas switching device shifter
Technical field
The utility model relates to a kind of carrier gas switching device shifter, specifically, is a kind of chromatograph that has the carrier gas switching device shifter.
Background technology
As everyone knows, the ultimate principle of gas chromatographic analysis is: sample separates in chromatographic column by carrier gas, and the component after the separation detects by detecting device.No matter be to separate or testing process, carrier gas all plays a part very important.For thermal conductivity detector (TCD), the prerequisite of input is that sample component has difference carrier gas thermal conductivity, and therefore selecting suitable carrier gas type is the key of accurate or high-sensitivity detection.At present, Chang Yong carrier gas type has H 2, N 2, He, Ar etc.But in petrochemical complex, coal processing and a lot of production or process of experimental, run into H through regular meeting 2, O 2, N 2, CO, CO 2Compartment analysis work Deng mixed gas.Obvious H 2And N 2In time, occur and need to detect bringing great difficulty for the selection of carrier gas.Though work that forefathers do (Chen Hejun, Yin Zongling, analysis and testing technology and instrument, 9 (1) 14~16,2003; Shi Mingyu, Li Yuqing, Nanjing Chemical Engineering College's journal, 12 (12), 67~70,1990; Chen Guanrong, south refining science and technology, 7 (4) 50~53,2000; Yang Haiying, Ren Sumei, Lu Wanzhen, chromatogram, 10 (1) 1992,9~13.Wang Yamin, Yang Haiying, analytical instrument, the 4th phase in 41~46,2003.) certain reference and reference value arranged.But prior art is summarized, or adopts H respectively 2And N 2Do carrier gas with double T CD detecting device (separate unit chromatogram configuration double T CD detecting device or two chromatograms respectively dispose a thermal conductivity detector (TCD)), or can only in other gases such as He, Ar, carry out the selection of carrier gas.Obviously there is the cost height in the former, complex operation, data processing complex, shortcoming such as error is big.The latter, if adopt helium to do carrier gas, hydrogen is relatively poor with respect to the detection linearity of helium, especially in the sample hydrogen content lower (<%5) time, even if adopt the multiple spot correction method to come hydrogen content is carried out quantitatively, its detection error is also still bigger, can't meet the demands.And adopt argon gas to do carrier gas, though for the compartment analysis of a large amount of samples of routine, then because the consumption of argon gas is big, the regular job cost height that makes stratographic analysis obviously is unfavorable for popularizing of this scheme.Also exist simultaneously O 2, N 2Shortcomings such as detection sensitivity is low.
Simultaneously, along with the increase of people, or, be badly in need of the analysis of some complex samples of solution, and the analysis of some complex sample needs usually a plurality of detecting devices to work simultaneously to the raising that the Automation of Manufacturing Process controlled target requires to the research object breadth and depth.And the existing domestic and international chromatograph overwhelming majority can only dispose two detecting devices, and this brings great difficulty for the solution of some complex sample problem analysis.
Summary of the invention
Technical problem to be solved in the utility model is the manufacturing cost height that exists in the conventional art, complex operation, and data processing complex, error is big, and sensitivity is low and instrumental function is expanded shortcomings such as limited, and a kind of carrier gas switching device shifter is provided.This device has can realize that single thermal conductivity detector (TCD) is equivalent to the function of dual-detector, if chromatograph disposes other detecting device (as FID, ECD, FPD, HECD) again, then chromatograph is equivalent to dispose three detecting devices, can greatly widen the stratographic analysis function, and has low cost of manufacture, easy to operate, good reproducibility, accuracy height, advantages such as sensitivity height.
For solving the problems of the technologies described above, the technical solution adopted in the utility model is as follows: a kind of carrier gas switching device shifter, comprise electronic flow control valve, flow valve controller, transfer valve, transfer valve controller, reference gas transfer valve, chromatographic work station, thermal conductivity detector (TCD) and carrier gas type controllers, wherein the two-way carrier gas is all earlier by linking to each other with thermal conductivity detector (TCD) behind chromatographic column, the transfer valve, simultaneously thermal conductivity detector (TCD) and another terminal of switching are provided with reference gas transfer valve in propping up and being connected, and associated line all adopts capillary line; The carrier gas type controllers links to each other with chromatographic work station and thermal conductivity detector (TCD) by signal wire; The flow of the flow of two-way carrier gas and reference gas is controlled by the flow valve controller, and links to each other with chromatographic work station; Be provided with the transfer valve controller between transfer valve and the chromatographic work station, and switch by its control.
Chromatographic work station has carrier gas type selecting programmed control function in the technique scheme, and implements control by the carrier gas type controllers.All be provided with electronic flow control valve in carrier gas, thermal conductivity detector (TCD) and the reference air pipe and be used for accurate pilot-gas flow.
In the utility model, electronic flow control valve and flow valve controller are used for the accurate control of device gas flow; The collaborative handoff functionality of finishing the different carrier gas of thermal conductivity detector (TCD) of transfer valve controller and transfer valve; All associated lines all adopt the capillary line connection to reduce the adverse effect that system's dead volume brings sample analysis simultaneously.The selection of carrier gas type controllers different carrier gas types of synchronization implementation when the transfer valve controller is implemented control to transfer valve changes.Thereby ensured the switching of carrier gas type when different sample component are analyzed, and the problem of switching the flow rate test distortion that brings owing to carrier gas, reached chromatographiccondition and be in optimum state always, and single detecting device finishes the analysis of complex sample, obtained better technical effect.
The utlity model has following obvious advantage:
(1) to stratographic analysis component detection sensitivity height, sensing range is wide.
(2) stratographic analysis regular job expense is low, is convenient to popularize.
(3) can be by can realizing to the existing simple transformation of chromatogram, and convenient data processing, good reproducibility, accuracy height.
(4) but improved chromatograph a tractor serves several purposes is greatly expanded chromatographic range of application, the extensive diagnostic space.
Description of drawings
Fig. 1 is a kind of carrier gas switching device shifter synoptic diagram.
Among Fig. 1: 1,2,3,4 be electronic flow control valve; 5 is the flow valve controller; 6 is the transfer valve controller; 7 is transfer valve; 8 is the reference transfer valve; 9 is chromatographic work station; 10 is thermal conductivity detector (TCD); 11 are the carrier gas type controllers; 12 is that carrier gas 1,12 is that chromatographic column 1,14 is a chromatographic column 2 for carrier gas 2,13.
The workflow of the utility model technology is: acquiescence transfer valve shown position is the OFF state, and inverse state is the ON state.Carrier gas 1 is divided into two-way, and one the road earlier after the back emptying of the b of transfer valve 7 end a end, another road after electronic flow control valve 2 Control Flow, emptying behind the f of chromatographic column 2, transfer valve 7 end e end.This this state of road gas circuit only is in the separation component state.Carrier gas 2 also is divided into two-way, and one the road earlier after divide two-way to be connected with make-up gas electronic flow control valve 4 with the sub-flowrate control valve 3 of thermal conductivity detector (TCD) 10 reference pneumoelectrics respectively again behind the d of the transfer valve 7 end c end; Reference gas through entering TCD detecting device 10 behind electronic flow control valve 3 and the reference transfer valve 8, is used to provide the reference gas of detecting device operate as normal needs successively.Make-up gas is used for replenishing the deficiency that has the carrier gas flux of sample from chromatographic column.Another road of carrier gas 2 enters thermal conductivity detector (TCD) 10 injection ports behind the i of chromatographic column 1, transfer valve 7 end j end h end g end after electronic flow control valve 1 Control Flow, enter thermal conductivity detector (TCD) 10 together with make-up gas and detect.After carrier gas 2 gas circuits are finished the detection task, chromatographic work station 9 is implemented transfer valve 7 state transformations (ON state) by transfer valve 7 controllers 6, this moment, reference gas, make-up gas and the chromatographic column carrier gas of thermal conductivity detector (TCD) 10 were all identical with carrier gas 1, and thermal conductivity detector (TCD) 10 is also worked under carrier gas 1 state thereupon.In transfer valve 7 actions, chromatographic work station 9 is realized thermal conductivity detector (TCD) 10 corresponding carrier gas type selecting switchings synchronously by carrier gas type controllers 11, thereby ensure the stable of chromatographic system analysis state, thermal conductivity detector (TCD) 10 is worked under the reasonable flow state.Two states can repeatedly switch according to analyzing needs, and implements dynamic routine control by chromatographic work station 9.All electronic flow control valves of whole process are by spectrum workstation 9) implement to control.In addition, system's chromatographic column can connect flexibly according to concrete condition, and diagram only is a kind of of connection.
Below will the utility model is described in further detail by embodiment.
Embodiment
[embodiment 1]
Adopt the utility model to compare with the analysis of general analytical equipment
The utility model
Analytical instrument: HP-6890, U.S. Agilent company disposes above-mentioned carrier gas switching device shifter and a TCD detecting device.Data processing adopts chromatographic work station HP 2070A to handle.
Sample gas is the potpourri of oxygen, nitrogen and hydrogen.
Chromatographic column: post 1 post 2 is, 13-x moleculer sieve packed column;
Chromatographic condition: temperature programme: 50 ℃ of furnace temperature, the TCD detecting device, 250 ℃ of temperature, carrier gas 1 is a nitrogen, carrier gas 2 is a hydrogen; The post flow is 18ml/min.
The general analysis device does not have the carrier gas switching device shifter, and does carrier gas with helium.The same the utility model of all the other chromatographic conditions.
Sample precision and accuracy are investigated relatively:
Under above-mentioned chromatographic condition, a certain standard specimen is analyzed 7 times continuously, novel and its stratographic analysis precision of general analysis device of this uses and accuracy investigation result are respectively shown in table 1 and 2.
The result is investigated in table 1 general device standard model precision and accuracy:
To sample long run test number of times
The component title Standard specimen is formed 1 2 3 4 5 6 7 Relative error % Standard deviation Relative standard deviation
H 2 O 2 N 2 4.11 10.15 86.68 4.01 10.16 85.82 3.05 10.26 86.68 4.68 10.08 85.23 4.3 10.13 85.56 3.56 10.21 86.22 3.67 10.29 86.03 4.2 10.21 85.58 1.855 -0.356 -0.047 0.501 0.067 0.447 12.768 0.661 0.520
The result is investigated in table 2 the utility model standard model precision and accuracy:
To sample long run test number of times
The component title Standard specimen is formed 1 2 3 4 5 6 7 Relative error % Standard deviation Relative standard deviation
H 2 O 2 N 2 4.11 10.15 86.68 4.35 10.13 86.62 4.15 10.15 86.64 4.06 10.15 86.68 4.11 10.16 36.66 4.21 10.15 36.67 4.26 10.23 36.59 4.08 10.23 36.70 -1.551 -0.209 0.099 0.0972 0.0379 0.097 2.32 0.373 0.113
Can find out obviously that from table 1 and 2 the utility model data precision and repeatability apparently higher than the general analysis device, can satisfy testing requirements fully.
This analytical plan enlarges the stratographic analysis space and has earthshaking meaning for expanding stratographic analysis sample scope.

Claims (2)

1, a kind of carrier gas switching device shifter, comprise electronic flow control valve, flow valve controller, transfer valve, transfer valve controller, reference gas transfer valve, chromatographic work station, thermal conductivity detector (TCD) and carrier gas type controllers, it is characterized in that the two-way carrier gas is all earlier by linking to each other with thermal conductivity detector (TCD) behind chromatographic column, the transfer valve, simultaneously thermal conductivity detector (TCD) and another terminal of switching are provided with reference gas transfer valve in propping up and being connected, and associated line all adopts capillary line; The carrier gas type controllers links to each other with chromatographic work station and thermal conductivity detector (TCD) by signal wire; The flow of the flow of two-way carrier gas and reference gas is controlled by the flow valve controller, and links to each other with chromatographic work station; Be provided with the transfer valve controller between transfer valve and the chromatographic work station, and switch by its control.
2, carrier gas switching device shifter according to claim 1 is characterized in that all being provided with in carrier gas, thermal conductivity detector (TCD) and the reference air pipe electronic flow control valve and is used for accurate pilot-gas flow.
CN 200520042767 2005-06-22 2005-06-22 Carrier gas switching device Expired - Fee Related CN2840034Y (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102749391A (en) * 2011-04-20 2012-10-24 中国石油化工股份有限公司 Method for determining content of monomer aromatic hydrocarbons in gasoline through gas chromatography
JP2019082434A (en) * 2017-10-31 2019-05-30 株式会社島津製作所 Analysis method and analysis device
CN114509525A (en) * 2021-12-29 2022-05-17 聚光科技(杭州)股份有限公司 Apparatus and method for chromatographic analysis of hydrogen and hydrocarbons

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102749391A (en) * 2011-04-20 2012-10-24 中国石油化工股份有限公司 Method for determining content of monomer aromatic hydrocarbons in gasoline through gas chromatography
CN102749391B (en) * 2011-04-20 2014-07-23 中国石油化工股份有限公司 Method for determining content of monomer aromatic hydrocarbons in gasoline through gas chromatography
JP2019082434A (en) * 2017-10-31 2019-05-30 株式会社島津製作所 Analysis method and analysis device
CN114509525A (en) * 2021-12-29 2022-05-17 聚光科技(杭州)股份有限公司 Apparatus and method for chromatographic analysis of hydrogen and hydrocarbons
CN114509525B (en) * 2021-12-29 2023-12-01 聚光科技(杭州)股份有限公司 Chromatographic analysis device and method for hydrogen and hydrocarbon

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Granted publication date: 20061122

Termination date: 20110622