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CN2798088Y - Multi-dimensional gas chromatograph for analyzing - Google Patents

Multi-dimensional gas chromatograph for analyzing Download PDF

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Publication number
CN2798088Y
CN2798088Y CN 200520042769 CN200520042769U CN2798088Y CN 2798088 Y CN2798088 Y CN 2798088Y CN 200520042769 CN200520042769 CN 200520042769 CN 200520042769 U CN200520042769 U CN 200520042769U CN 2798088 Y CN2798088 Y CN 2798088Y
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CN
China
Prior art keywords
chromatographic column
chromatographic
chromatogram
box
master control
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Expired - Fee Related
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CN 200520042769
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Chinese (zh)
Inventor
刘俊涛
钟思青
陈晓峰
王华文
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
China Petrochemical Corp
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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Abstract

The utility model relates to a multi-dimensional gas chromatogram analyzer, mainly solving the technical problem that the departed gas chromatogram device is provided with only one chromatographic column box and can not realize the control of different chromatographic columns through different temperatures simultaneously. The utility model adopts the technology schemes of adding an auxiliary chromatographic column box outside the main chromatographic column box and accurately controlling the temperature of column box by the temperature control system via the former chromatographic main board and solves the problem better, and the multi-dimensional gas chromatogram analyzer can be used in the industrial manufacture of chromatogram.

Description

The multidimensional gas chromatographic analyser
Technical field
The utility model relates to a kind of multidimensional gas chromatographic analyser, specifically, is a kind of chromatograph with double-colored chromatographic column box.
Background technology
Many problem analyses can not be resolved and maybe can not obtain fine solution in research work and the actual production process, one of its reason is exactly because existing most chromatographs have only a chromatograph box, can not realize simultaneously that different chromatographic columns are controlled in the different temperatures scope.And in the stratographic analysis of complex sample, often in the requirement at one time, the different chromatographic columns in the chromatographic analysis system preferably are controlled at different temperatures.As using the multidimensional chromatography analysis of refinery gases, a kind of four valves, five post TCD and FID dual-detector chromatographic analysis system have 5 root chromatogram columns, comprise that the capillary column of 4 packed columns and one 50 meters is placed in the same post case jointly.The maintenance that the many root chromatogram columns of one side put together to instrument brings great inconvenience, on the other hand, need be warming up to about 180 ℃ owing to analyze the hydrocarbon component capillary column, and all the other four column temperature only need rise to the 80 ℃ of compartment analysis tasks that just can finish permanent gas.But because all chromatographic columns all are placed in the same post case, four packed columns have to stand same temperature.And wherein Porapak N packed column has in various degree column bleed under higher temperature, and this not only influences the serviceable life of this post itself, simultaneously subsequent separation system is also caused harmful effect.Thereby finally have influence on the separating effect and the usability of whole analytic system.In addition as when answering in the chromatograph gasoline alkene and arene content, need to adopt ASTM D6296-98 and the described method of ASTM D6293-98 to carry out the multi-dimensional chromatograph analysis, its key is to adopt the collecting trap technology, promptly in analytic process, to a certain component in the sample, carry out selective retention as the alkene in the gasoline, by changing the chromatogram temperature it is discharged to reach the purpose of quantitative measurement again.This operation need be used chromatographic column of different nature, and as the selective retention chromatographic column, promptly the alkene collecting trap is used for the alkene reservation, and stable hydrocarbon is separated with alkene; The polarity chromatographic column is used for fractionation of fatty hydrocarbon and aromatic hydrocarbons.In the above-mentioned analytic process, require two chromatographic columns to keep different temperature, and require the alkene collecting trap in analytic process, to be warming up to different temperatures, to discharge the alkene that keeps.Therefore, require chromatograph that the chromatograph box of two independent temperature controls is arranged, to adapt to the analysis requirement.
Sonchik[American Laboratory (1985,2, P58)] the common gas chromatograph that once proposed other increase by one can independent temperature control auxilliary post case, this auxilliary post case and gas chromatograph have same design and characteristic, and have oneself sample introduction and detection system.Patent CN 2520508Y also discloses a kind of multidimensional gas chromatographic analyser, and it adopts major-minor two chromatograph boxes, and two chromatograph boxes have independently temperature control system, respectively by chromatograph master control borad and the auxilliary control of chromatograph plate control adjustment temperature.
In the above-mentioned chromatograph, has only a chromatograph box, perhaps have two chromatograph boxes but temperature control has all adopted independently two chromatograph control panels to implement temperature controlling, can't realize the control of different chromatographic column different temperatures simultaneously for the former, obviously make complexity for the latter, the cost height, complicated operation etc.
Summary of the invention
Technical problem to be solved in the utility model is having only a chromatograph box or having two chromatograph boxes but can't realize the technical matters of the control of different chromatographic column different temperatures simultaneously of existing in the conventional art, and a kind of new multidimensional gas chromatograph is provided.This chromatograph has can make full use of existing chromatograph resource, under the situation that does not increase temperature control panel, realize the independent control of major-minor post oven temperature, degree, easy for installation, simple to operate, can realize the optimization compartment analysis of refinery gas, and have chromatogram control integrated level height, making is simple, cost is low, system operation is stable, easy to maintenance, data accurately and reliably, advantage such as analysis time is short.
For solving the problems of the technologies described above, the technical solution adopted in the utility model is as follows: a kind of multidimensional gas chromatographic analyser, comprise mass-tone chromatographic column box, chromatogram sampling system, chromatographic detection system, EPC gas circuit control panel, clack box temperature controller, chromatogram master control borad and clack box heat block, wherein the chromatogram master control borad is positioned at mass-tone chromatographic column box right side, and connects with chromatogram master control operation keyboard by electronic circuit; Chromatogram master control operation keyboard top is provided with chromatogram master control operation display; The clack box heat block is positioned at mass-tone chromatographic column box top; Wherein also be provided with at least one complementary colors chromatographic column box in the multidimensional gas chromatographic analyser, the complementary colors chromatographic column box is positioned at the mass-tone chromatographic column box outside, and is connected with the carrier gas gas circuit with sample introduction by the valve associated line; The temperature control system of complementary colors chromatographic column box and clack box heat block is implemented control by the temperature controller that links to each other with the chromatogram master control borad respectively.
The clack box heat block adopts the monoblock stainless steel to make in the technique scheme, and adopts the heating of a heating plug, and can place four valve bodies simultaneously at least.
In the utility model, mainly by outside the mass-tone chromatographic column box, setting up auxilliary chromatograph box, and chromatographic column sample introduction and pipe connection system are installed in the chromatograph box, simultaneously, idle temperature control point in original chromatogram mainboard is taken out, and be used for the accurate accurately control of newly-increased complementary colors chromatographic column box temperature.Thereby realized under the condition that does not increase temperature control point, having the multidimensional gas chromatograph of two chromatograph boxes at least, obtained better technical effect.
Description of drawings
Fig. 1 is a structural representation of the present utility model.
Fig. 2 is the utility model instrument top critical piece distribution plan.
Fig. 3 is used for the valve connection layout that refinery gas is analyzed for the utility model instrument.
Among Fig. 1: 1 is that valve district, 2 is that mass-tone chromatographic column box, 3 is that auxilliary chromatograph box, 4 is that chromatogram sampling system, 5 is that chromatographic detection system, 6 is that chromatogram master control operation display, 7 is a chromatogram master control operation keyboard.
Among Fig. 2: 1 is that auxilliary chromatograph box, 2 is that chromatogram sampling system, 3 is the back injector, 4 is preceding injector, and 5 is that EPC gas circuit control panel, 6 is that transfer valve 4,7 is that transfer valve 3,8 is that clack box heat block, 9 is that transfer valve 2,10 is that transfer valve 1,11 is that thermal conductivity detector (TCD) A, 12 is that thermal conductivity detector (TCD) B, 13 is that chromatogram master control borad, 14 is that clack box temperature controller, 15 is to assist the chromatograph box temperature controller.
Among Fig. 3: 1 is carrier gas helium, and 2 is carrier gas nitrogen, and 3 is sample inlet, and 4 is that post 1,5 is that valve 4,6 is that post 3,7 is that post 2,8 is that valve 1,9 is that post 4,10 is that valve 3,11 is that post 5,12 is that valve 2,13 is thermal conductivity detector (TCD) B, and 14 is thermal conductivity detector (TCD) A.
The key problem in technology of the utility model technology is: two chromatograph boxes have independently temperature control system, by chromatogram master control borad control adjustment.Specifically be with two temperature-controlling systems in the original clack box of chromatograph, take out one and be used to control the auxilliary post case of chromatogram that another is used for operation valve oven temperature, degree.Two post oven temperature, degree can be controlled at identical or different temperature according to analyzing needs, or carry out single-stage or multi-level procedure intensification.Analysis places respectively in two post casees with chromatographic column.Analytic sample carries out the assay determination of different component through different chromatographic columns, and the conversion of analytic sample between chromatographic column controlled by transfer valve.
The utility model analyser is applicable to the separation detection of refinery gas, gasoline, rock gas, cut wet goods complex component.
Below by embodiment the utility model is further elaborated.
Embodiment
[embodiment 1]
Sample gas is a certain refinery gas standard specimen.
Concrete configuration is: HP5890II type gas chromatograph (double T CD detecting device); HP3396II type integraph
Chromatographic column: post 1 is 13X molecular sieve (1.2m*3.2mm i.d); Post 2 is sebacic dinitrile (0.6m*3.2mm i.d); Post 3 is sebacic dinitrile (9m*3.2mm i.d); Post 4 is 13X molecular sieve (3m*3.2mm i.d); Post 5 is Porpak Q (1.8m*3.2mmi.d), presses Fig. 3 and connects.
Mass-tone chromatographic column box temperature maintenance is at 90 ℃, and auxilliary post oven temperature, degree maintains 60 ℃, and the thermal conductivity detector (TCD) temperature all maintains 200 ℃.
The standard specimen analysis result is as shown in table 1:
Under above-mentioned definite chromatographic condition, we adopt same sample continuous sample introduction to investigate the reliability of this multi-dimensional chromatograph analytic sample.
Table 1 component concentration repeated experiment result (volume/volume %)
Component Experiment number Average% SD RSD/%
1 2 3 4 5 6
Hydrogene Ethane Ethylene Carbon dioxide Propane CycloPropane Propylene Oxygen Nitrogen i-Butane n-butane Methane Propadiene Carbon monoxide Acetylene 2,2-DMC3 t-2-Butene Butene-1 i-Butene c-2-Butne i-Pantane n-Pantane 1,3-Butadiene m-Acetylene c-2-Pentene 1.09 2.10 2.60 1.25 2.67 0.04 4.01 3.11 77.77 0.10 0.98 1.30 0.05 0.37 0.05 0.04 0.54 0.43 0.91 0.13 0.33 0.03 0.05 0.02 0.03 1.09 2.10 2.61 1.27 2.67 0.04 4.01 3.19 77.69 0.10 0.98 1.30 0.05 0.35 0.05 0.03 0.54 0.43 0.91 0.13 0.33 0.03 0.05 0.02 0.02 1.10 2.12 2.63 1.26 2.70 0.04 4.05 3.12 77.68 0.10 0.99 1.30 0.05 0.36 0.05 0.04 0.55 0.44 0.92 0.13 0.34 0.03 0.05 0.02 0.03 1.10 2.12 2.63 1.25 2.70 0.04 4.05 3.06 77.67 0.10 0.99 1.30 0.05 0.37 0.05 0.04 0.55 0.44 0.92 0.13 0.34 0.03 0.05 0.02 0.03 1.15 2.21 2.74 1.34 2.81 0.04 4.05 2.98 77.13 0.11 1.03 1.35 0.05 0.37 0.05 0.04 0.57 0.46 0.94 0.13 0.33 0.03 0.05 0.02 0.03 1.07 2.07 2.56 1.27 2.63 0.04 3.94 3.13 78.01 0.10 0.96 1.31 0.05 0.36 0.05 0.03 0.53 0.42 0.89 0.13 0.33 0.03 0.05 0.02 0.03 1.10 2.12 2.63 1.27 2.70 0.04 4.02 3.10 77.66 0.10 0.99 1.31 0.05 0.36 0.05 0.04 0.55 0.44 0.91 0.13 0.33 0.03 0.05 0.02 0.03 0.02 0.04 0.05 0.03 0.06 0.00 0.04 0.06 0.26 0.00 0.02 0.02 0.00 0.00 0.00 0.00 0.01 0.01 0.02 0.00 0.00 0.00 0.00 0.00 0.00 2.00 2.09 2.08 2.30 2.10 1.09 0.97 2.08 0.34 2.08 2.15 1.56 2.11 1.36 2.07 2.51 2.28 2.17 1.77 1.25 1.24 0.91 1.83 2.33 0.70
Table 1 is 6 replicate determination results, and as can be seen from Table 1, the analysis result relative standard deviation is not more than 3%, visible written or printed documents multi-dimensional chromatograph analysis result good reproducibility, precision height, accurately and reliably.

Claims (2)

1, a kind of multidimensional gas chromatographic analyser, comprise mass-tone chromatographic column box, chromatogram sampling system, chromatographic detection system, EPC gas circuit control panel, clack box temperature controller, chromatogram master control borad and clack box heat block, wherein the chromatogram master control borad is positioned at mass-tone chromatographic column box right side, and connects with chromatogram master control operation keyboard by electronic circuit; Chromatogram master control operation keyboard top is provided with chromatogram master control operation display; The clack box heat block is positioned at mass-tone chromatographic column box top; It is characterized in that also being provided with in the multidimensional gas chromatographic analyser at least one complementary colors chromatographic column box, the complementary colors chromatographic column box is positioned at the mass-tone chromatographic column box outside, and is connected with the carrier gas gas circuit with sample introduction by the valve associated line; The temperature control system of complementary colors chromatographic column box and clack box heat block is implemented control by the temperature controller that links to each other with the chromatogram master control borad respectively.
2,, it is characterized in that the clack box heat block adopts the monoblock stainless steel to make, and adopt the heating of a heating plug, and can place four valve bodies simultaneously at least according to right 1 described multidimensional gas chromatographic analyser.
CN 200520042769 2005-06-22 2005-06-22 Multi-dimensional gas chromatograph for analyzing Expired - Fee Related CN2798088Y (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102472730A (en) * 2009-07-07 2012-05-23 创控生技股份有限公司 Cascaded gas chromatograph (CGC) with individual temperature controls and gas analysis system using same
CN103604897A (en) * 2013-10-31 2014-02-26 陕西延长石油(集团)有限责任公司研究院 On-line multidimensional gas chromatographic analysis device universal for low carbon catalytic conversion reaction
CN105738548A (en) * 2016-02-14 2016-07-06 河南中分仪器股份有限公司 Portable full-automatic dielectric oil dissolved gas analytical equipment
US9658196B2 (en) 2009-07-31 2017-05-23 Tricorntech Corporation Gas collection and analysis system with front-end and back-end pre-concentrators and moisture removal
US9921192B2 (en) 2010-04-23 2018-03-20 Tricorntech Corporation Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis
CN109839468A (en) * 2017-11-24 2019-06-04 株式会社岛津制作所 Multidimensional gas chromatograph
CN110297058A (en) * 2018-03-23 2019-10-01 常志兴 A kind of multi-field gas chromatograph detector and gas chromatography
CN110927290A (en) * 2019-12-19 2020-03-27 常州磐诺仪器有限公司 Valve sample introduction three-dimensional laboratory gas chromatograph

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102472730B (en) * 2009-07-07 2016-06-22 创控生技股份有限公司 Cascaded gas chromatograph (CGC) with individual temperature controls and gas analysis system using same
CN102472730A (en) * 2009-07-07 2012-05-23 创控生技股份有限公司 Cascaded gas chromatograph (CGC) with individual temperature controls and gas analysis system using same
US9683974B2 (en) 2009-07-07 2017-06-20 Tricorntech Corporation Cascaded gas chromatographs (CGCs) with individual temperature control and gas analysis systems using same
US9658196B2 (en) 2009-07-31 2017-05-23 Tricorntech Corporation Gas collection and analysis system with front-end and back-end pre-concentrators and moisture removal
US11035834B2 (en) 2010-04-23 2021-06-15 TricornTech Taiwan Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis
US9921192B2 (en) 2010-04-23 2018-03-20 Tricorntech Corporation Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis
US12265067B2 (en) 2010-04-23 2025-04-01 Tricorntech Corporation Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis
US11796515B2 (en) 2010-04-23 2023-10-24 Tricorntech Corporation Gas analyte spectrum sharpening and separation with multi-dimensional micro-GC for gas chromatography analysis
CN103604897A (en) * 2013-10-31 2014-02-26 陕西延长石油(集团)有限责任公司研究院 On-line multidimensional gas chromatographic analysis device universal for low carbon catalytic conversion reaction
CN105738548A (en) * 2016-02-14 2016-07-06 河南中分仪器股份有限公司 Portable full-automatic dielectric oil dissolved gas analytical equipment
CN109839468A (en) * 2017-11-24 2019-06-04 株式会社岛津制作所 Multidimensional gas chromatograph
CN110297058A (en) * 2018-03-23 2019-10-01 常志兴 A kind of multi-field gas chromatograph detector and gas chromatography
CN110927290A (en) * 2019-12-19 2020-03-27 常州磐诺仪器有限公司 Valve sample introduction three-dimensional laboratory gas chromatograph

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Granted publication date: 20060719

Termination date: 20110622