CN100409009C - Analyzer for mixed gas containing O2, N2 and H2 - Google Patents
Analyzer for mixed gas containing O2, N2 and H2 Download PDFInfo
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- CN100409009C CN100409009C CNB2005100270302A CN200510027030A CN100409009C CN 100409009 C CN100409009 C CN 100409009C CN B2005100270302 A CNB2005100270302 A CN B2005100270302A CN 200510027030 A CN200510027030 A CN 200510027030A CN 100409009 C CN100409009 C CN 100409009C
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Abstract
The present invention relates to an analysis device for mixture gas containing O2, N2 and H2, which mainly solves the technical problems that at least two chromatograms carry out analysis, operation is complex, data processing work is complex, error is large, etc. in a previous analysis method. The present invention adopts a gas switch valve to realize the switch of different carrier gas, when hydrogen is measured, nitrogen or argon is used as the carrier gas, when other kinds of gas is measured, hydrogen gas or helium is used as carrier gas, and all detection of ingredients is carried out on a single thermal conductivity detector; thereby, the single analysis device completing the analysis of the mixture gas containing O2, N2 and H2 is realized. The problem is solved better, and the present invention can be used for the industrial production of a chromatographic analysis device.
Description
Technical field
The present invention relates to a kind of O of containing
2, N
2And H
2The analytical equipment of mixed gas.
Background technology
In petrochemical complex, coal processing and a lot of production run, run into H through regular meeting
2, O
2, N
2, CO, CO
2And the compartment analysis work of hydro carbons mixed gas.Analytical work person has made extensive work both at home and abroad in this respect.Pertinent literature is to said mixture or remove the outer mixed gas of hydro carbons and many reports [Shi Mingyu, Li Yuqing, Nanjing Chemical Engineering College's journal, 12 (12), 67～70,1990 have occurred; 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.Chen Hejun, Yin Zongling, analysis and testing technology and instrument, 9 (1) 14～16,2003] totally conclude to get up above-mentioned permanent mixed gas is had following several analytical approach:
1) adopt two chromatographs to finish the compartment analysis of above-mentioned mixed gas.Wherein a chromatograph disposes the separation detection that thermal conductivity detector (TCD) (TCD) is exclusively used in hydrogen, and an other chromatograph disposes the separation detection that a thermal conductivity detector (TCD) (TCD) is finished residual gas at least.
2) adopt the separate unit chromatograph to finish the compartment analysis of above-mentioned mixed gas.This chromatograph disposes double T CD detecting device, and one of them detector-specific is in detecting hydrogen component, and the another one detecting device is used to detect all the other components outside the hydrogen.
3) adopt the separate unit chromatograph.This chromatograph disposes single thermal conductivity detector (TCD) (TCD), but must adopt helium or argon gas to realize the separation detection of permanent mixed gas do carrier gas.
For method 1, adopt two chromatographs to finish the separation detection of above-mentioned mixed gas, obviously there is the cost height, complex operation, data processing complex, shortcoming such as error is big.Though method 2 has realized the chromatographic separation detection of separate unit, but gas chromatograph must dispose two thermal conductivity detector (TCD)s (TCD), there is the cost height equally, expensive shortcoming, simultaneously, the configuration of two thermal conductivity detector (TCD)s of separate unit chromatograph makes the expansion of its analytic function be greatly limited.For scheme 3, need to adopt helium or argon gas to do carrier gas.As everyone knows, for thermal conductivity detector (TCD), 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, it is also still bigger that it detects error, can't meet the demands.And adopt argon gas to do carrier gas, and for the compartment analysis of a large amount of samples of routine,, and costing an arm and a leg 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.It is also lower to the sensitivity of permanent gases that the while argon gas is done carrier gas.
Summary of the invention
Technical matters to be solved by this invention is the manufacturing cost height that exists in the conventional art, complex operation, and data processing complex, error is big, and shortcoming such as sensitivity is low, and a kind of O of containing is provided
2, N
2And H
2The analytical equipment of mixed gas, this analytical equipment 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 used in the present invention is as follows: a kind of O that contains
2, N
2And H
2The analytical equipment of mixed gas, comprise gas sampling valve, the gas transfer valve, isolation valve, orifice valve, first quantity tube and second quantity tube, thermal conductivity detector (TCD), first chromatographic column, second chromatographic column, the 3rd chromatographic column and chromatographic work station, wherein, the 3rd chromatographic column, the carrier gas A channel all links to each other with the gas transfer valve with carrier gas B passage and thermal conductivity detector (TCD), two quantity tubes all are connected on the gas sampling valve, the orifice valve and first chromatographic column are connected on the isolation valve, be connected by second chromatographic column between isolation valve and the gas sampling valve, chromatographic work station links to each other with the thermal conductivity detector (TCD) series connection, six interfaces of isolation valve are followed successively by with the extraneous order that is connected: the outlet of second chromatographic column, the inlet of first chromatographic column, the outlet of first chromatographic column, the carrier gas A interface that is connected with the gas transfer valve, the a interface of orifice valve and the b interface of orifice valve, ten interfaces of gas sampling valve are followed successively by with the extraneous order that is connected: carrier gas A inlet, the inlet of second chromatographic column, the a interface of first quantity tube, the a interface of second quantity tube, connector with the gas transfer valve, carrier gas B inlet, the b interface of second quantity tube, the sample gas drain, the b interface of the sample gas inlet and first quantity tube, wherein ten of the gas transfer valve interfaces are followed successively by with the extraneous order that is connected: from the sample introduction gas interface of gas sampling valve, the inlet of the 3rd chromatographic column, carrier gas A drain, carrier gas A inlet, the inlet that is connected with thermal conductivity detector (TCD) reference gas, the reference gas interface that is connected with the carrier gas source of the gas, carrier gas B drain, the carrier gas A inlet that is connected with isolation valve, the carrier gas inlet that is connected with the thermal conductivity detector (TCD) carrier gas and the outlet of the 3rd chromatographic column.
Piece-rate system is to be finished by three root chromatogram columns in the technique scheme, and gas sampling valve, gas transfer valve and isolation valve method are formed the gas circuit switched system, and component detects and adopts single TCD detecting device to detect; The switching of thermal conductivity detector (TCD), carrier gas and reference gas is switched realization by the gas transfer valve, and all pipelines that the gas transfer valve links to each other with detecting device all adopt capillary line to link to each other; The compartment analysis of hydrogen adopts the 3rd chromatographic column to finish, and does carrier gas with nitrogen or argon gas, and the separation of all the other components is adopted first chromatographic column, second chromatographic column to switch and finished, and does carrier gas with hydrogen or helium.
Among the present invention owing to adopted the gas transfer valve, the 3rd chromatographic column and thermal conductivity detector (TCD), do carrier gas with nitrogen when making in the specimen hydrogen, pass through the switching of gas transfer valve when testing all the other components, finishing carrier gas changes, the setting of the 3rd chromatographic column can make hydrogen effectively separate with all the other components, thereby ensure hydrogen and O simultaneously
2, N
2All under the high sensitivity condition, operate with the hydro carbons blending ingredients, and ensured that the component outside the hydrogen had realized blowback when carrier gas was switched, finally reach the separation detection that above-mentioned all components is all realized ideal under the high sensitivity condition by single thermal conductivity detector (TCD), obtained better technical effect.
Description of drawings
Accompanying drawing 1 is a kind of O that contains
2, N
2, CO, CO
2, hydro carbons and H
2The chromatographic process figure of the analytical equipment of mixed gas.
In the accompanying drawing 1: 1 is hydrogen gas cylinder; 2 is the high pure nitrogen steel cylinder; 3 is orifice valve; 4 is isolation valve; 5 is first chromatographic column; 6 is second chromatographic column; 7 is gas sampling valve; 8 is first quantity tube; 9 is second quantity tube; 10 is the gas transfer valve; 11 is the 3rd chromatographic column; 12 is thermal conductivity detector (TCD); 13 is chromatographic work station;
The objective of the invention is to be achieved through the following technical solutions.
Hydrogen gas cylinder 1, high pure nitrogen steel cylinder 2 are respectively applied to provide the reference of the required carrier gas of analytical system and thermal conductivity detector (TCD) 12 Gas and carrier gas. The fluctuation of system pressure when orifice valve 3 is used for 4 switching of balance isolating valve. Isolating valve 4 is used for isolation O2、
N
2、CH
4, CO component and bypass CO2And hydrocarbon gas component; First chromatographic column is for separating of O in the mist2、
N
2, the CO component, second chromatographic column is used for the initial gross separation blending ingredients, mainly is with component O2、N
2, CO and CO2And The hydrocarbon gas component separately. The 3rd chromatographic column is exclusively used in the blowback of separating hydrogen gas and all the other components. Sampling valve 7, first quantitative Pipe 8, second quantity tube 9 is for separating of the chromatogram sample introduction of system. Gas transfer valve 10 is born thermal conductivity detector (TCD) 12 carrier gas and is cut Change and the blowing function of the 3rd chromatographic column. Component detects and adopts single thermal conductivity detector (TCD) 12 to finish, and data are processed the chromatogram worker Do to carry out on the station 13. All connecting lines between gas transfer valve 10 and the thermal conductivity detector (TCD) 12 all adopt capillary line to connect Connect.
Concrete analysis techniqueflow of the present invention is for (state of three valves is defaulted as the OFF state in the diagram 1, is on the contrary ON State): after all parts of analytical equipment are stable, start the start key, device beginning sample analysis. At first, sampling valve 7 switches To the ON state, the samples in this moment second quantity tube 9 are brought the 3rd chromatographic column 11 into by nitrogen carrier gas and are separated, and treat Hydrogen after the separation enters that the TCD detector detects and all the other components when not leaving the 3rd chromatographic column 11, gas transfer valve 10 Switch, this moment, all the other components were by blowback. And the carrier gas of detector and reference gas all switch to hydrogen.
When sampling valve 7 switched, the sample in first quantity tube 8 was introduced into second chromatographic column under hydrogen carrier gas simultaneously 6, second chromatographic column 6, first chromatographic column 5, TCD detector 12 are in series connection at this moment. Component is second in the sample After carrying out initial gross separation on the chromatographic column 6, work as O2、N
2, CO enters first chromatographic column 5, and CO2Enter before this post, isolating valve 4 switches to the ON state, at this moment O2、N
2, CO closed in first chromatographic column 5 CO2, the hydrocarbon component warp Orifice valve 3 enters TCD detector 12 and detects. After treating that all components all leaves second chromatographic column 6, isolating valve 4 is cut Change the state to OFF, at this moment the component O in first chromatographic column 52、N
2, CO separates successively and enters TCD detector 12 Finish detection, chromatographic work station 13 provides data processed result.
The inventive method has following advantage:
(1) the chromatogram configuration is simple, convenient data processing, good reproducibility, accuracy height.
(2) to stratographic analysis component detection sensitivity height, sensing range is wide.
(3) stratographic analysis regular job expense is low, is convenient to popularize.
(4) chromatograph can a tractor serves several purposes, can greatly expand chromatographic range of application, the extensive diagnostic space.
The invention will be further elaborated below by embodiment.
Embodiment
[embodiment 1]
Analytical instrument: HP-6890, U.S. Agilent company disposes a six-way valve, two ten-way valves, a TCD detecting device.Data processing adopts chromatographic work station HP 2070A to handle.
Chromatographic column: second chromatographic column is a Porapak N packed column, and the 3rd chromatographic column is a 13-x moleculer sieve post; First chromatographic column is a 613-x moleculer sieve packed column;
Chromatographic condition: temperature programme: 50 ℃ of furnace temperature, stopped 3 minutes, rise to 80 ℃ with 5 ℃ of/minute clock rate then and stopped 5.5 minutes; The TCD detecting device, 250 ℃ of temperature, carrier gas begins to do carrier gas (being used to survey hydrogen) for nitrogen, does carrier gas with hydrogen after 0.7 minute; The post flow is 18 ml/min.
Working time, control program saw Table 1.
Table 1 combination gas is analyzed and is controlled switching table working time
Valve 1 refers to sampling valve-7, and Valve 2 refers to gas transfer valve-10, and Valve 3 refers to isolation valve-4;
Sample precision and accuracy are investigated:
Under above-mentioned chromatographic condition, to a certain standard specimen analyze continuously 7 this, result such as table 2 are investigated in its stratographic analysis precision and accuracy.
Result (volume/volume %) is investigated in table 2 standard model precision and accuracy
Data precision and good reproducibility as can be seen from Table 2, the accuracy height.Relative standard deviation is no more than 4%, and relative error can satisfy testing requirements fully less than 2%.
This analytical plan enlarges the stratographic analysis space and has earthshaking meaning for expanding stratographic analysis sample scope.
Claims (4)
1. one kind contains O
2, N
2And H
2The analytical equipment of mixed gas, comprise gas sampling valve, the gas transfer valve, isolation valve, orifice valve, first quantity tube and second quantity tube, thermal conductivity detector (TCD), first chromatographic column, second chromatographic column, the 3rd chromatographic column and chromatographic work station, wherein, the 3rd chromatographic column, the carrier gas A channel all links to each other with the gas transfer valve with carrier gas B passage and thermal conductivity detector (TCD), two quantity tubes all are connected on the gas sampling valve, the orifice valve and first chromatographic column are connected on the isolation valve, be connected by second chromatographic column between isolation valve and the gas sampling valve, chromatographic work station links to each other with the thermal conductivity detector (TCD) series connection, six interfaces of isolation valve are followed successively by with the extraneous order that is connected: the outlet of second chromatographic column, the inlet of first chromatographic column, the outlet of first chromatographic column, the carrier gas A interface that is connected with the gas transfer valve, the a interface of orifice valve and the b interface of orifice valve, ten interfaces of gas sampling valve are followed successively by with the extraneous order that is connected: carrier gas A inlet, the inlet of second chromatographic column, the a interface of first quantity tube, the a interface of second quantity tube, connector with the gas transfer valve, carrier gas B inlet, the b interface of second quantity tube, the sample gas drain, the b interface of the sample gas inlet and first quantity tube is characterized in that ten interfaces of gas transfer valve are followed successively by with the extraneous order that is connected: from the sample introduction gas interface of gas sampling valve, the inlet of the 3rd chromatographic column, carrier gas A drain, carrier gas A inlet, the inlet that is connected with thermal conductivity detector (TCD) reference gas, the reference gas interface that is connected with the carrier gas source of the gas, carrier gas B drain, the carrier gas A inlet that is connected with isolation valve, the carrier gas inlet that is connected with the thermal conductivity detector (TCD) carrier gas and the outlet of the 3rd chromatographic column.
2. according to the right 1 described O that contains
2, N
2And H
2The analytical equipment of mixed gas is characterized in that piece-rate system is to be finished by three root chromatogram columns, and gas sampling valve, gas transfer valve and isolation valve are formed the gas circuit switched system, and component detects and adopts single TCD detecting device to detect.
3. according to the right 1 described O that contains
2, N
2And H
2The analytical equipment of mixed gas is characterized in that the switching of thermal conductivity detector (TCD), carrier gas and reference gas is switched realization by the gas transfer valve, and all pipelines that the gas transfer valve links to each other with detecting device all adopt capillary line to link to each other.
4. according to the right 1 described O that contains
2, N
2And H
2The analytical equipment of mixed gas is characterized in that the compartment analysis of hydrogen adopts the 3rd chromatographic column to finish, and does carrier gas with nitrogen or argon gas, and the separation of all the other components is adopted first chromatographic column, second chromatographic column to switch and finished, and does carrier gas with hydrogen or helium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100270302A CN100409009C (en) | 2005-06-22 | 2005-06-22 | Analyzer for mixed gas containing O2, N2 and H2 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100270302A CN100409009C (en) | 2005-06-22 | 2005-06-22 | Analyzer for mixed gas containing O2, N2 and H2 |
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| Publication Number | Publication Date |
|---|---|
| CN1885031A CN1885031A (en) | 2006-12-27 |
| CN100409009C true CN100409009C (en) | 2008-08-06 |
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Cited By (1)
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|---|---|---|---|---|
| CN103123341A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Method for determining mixed gas content |
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| Publication number | Publication date |
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| CN1885031A (en) | 2006-12-27 |
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