CN1885031A - 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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- CN1885031A CN1885031A CN 200510027030 CN200510027030A CN1885031A CN 1885031 A CN1885031 A CN 1885031A CN 200510027030 CN200510027030 CN 200510027030 CN 200510027030 A CN200510027030 A CN 200510027030A CN 1885031 A CN1885031 A CN 1885031A
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Abstract
The invention relates to a device for analyzing the mixed gas of O2, N2, and H2, for solving the defects of present analysis which needs at least two color spectrums with complex operation and large error, wherein the invention uses one gas switch valve to realize different carrier gas switch, to use nitrogen gas or argon gas as carrier gas when testing hydrogen gas, and use hydrogen gas or argon gas as carrier gas when testing other gas, while the detections of all components are processed on single thermal conductive detector, to analyze the mixed gas with single machine. The invention can be used in the industrial production of color spectrum analyze 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, quantity tube 1 and quantity tube 2, thermal conductivity detector (TCD), chromatographic column 1, chromatographic column 2, chromatographic column 3 and chromatographic work station, wherein, chromatographic column 3, 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, orifice valve and chromatographic column 1 are connected on the isolation valve, be connected by chromatographic column 2 between isolation valve and the gas sampling valve, chromatographic work station links to each other with the thermal conductivity detector (TCD) series connection, and 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 chromatographic column 3, 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 B inlet that is connected with isolation valve, the carrier gas inlet that is connected with the thermal conductivity detector (TCD) carrier gas reaches the outlet with chromatographic column 3.
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 chromatographic column 3 to finish, and does carrier gas with nitrogen or argon gas, and the separation of all the other components is adopted chromatographic column 1, chromatographic column 2 to switch and finished, and does carrier gas with hydrogen or helium.
Among the present invention owing to adopted the gas transfer valve, chromatographic column 3 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 chromatographic column 3 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 post 1; 6 is post 2; 7 is gas sampling valve; 8 is quantity tube 1; 9 is quantity tube 2; 10 is the gas transfer valve; 11 is post 3; 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 for reference gas and the carrier gas that required carrier gas of analytic system and thermal conductivity detector (TCD) 12 are provided.The fluctuation of system pressure when orifice valve 3 is used for 4 switchings of balance isolation valve.Isolation valve 4 is used to isolate O
2, N
2, CH
4, CO component and bypass CO
2And hydrocarbon gas component; Chromatographic column 1 is used for separating mixed gas O
2, N
2, the CO component, chromatographic column 2 is used for the initial gross separation blending ingredients, mainly is with component 1 (O
2, N
2, CO) and CO
2And the hydrocarbon gas component separately.Chromatographic column 3 is exclusively used in the blowback of separating hydrogen gas and all the other components.Sampling valve 7, quantity tube 1 (8), quantity tube 2 (9) are used for the chromatogram sample introduction of piece-rate system.Gas transfer valve 1) bears the blowing function of thermal conductivity detector (TCD) 12 carrier gas switchings and chromatographic column 3.Component detects and adopts single thermal conductivity detector (TCD) 12 to finish, and data processing is carried out on chromatographic work station 13.Gas transfer valve 10 all adopts capillary line to be connected with all associated lines between the thermal conductivity detector (TCD) 12.
Concrete analysis techniqueflow of the present invention is (state of three valves is defaulted as the OFF state in the diagram 1, is the ON state on the contrary): 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, samples in this moment quantity tube 2 (9) are brought chromatographic column 3 (11) into by nitrogen carrier gas and are separated, hydrogen after to be separated enters that the TCD detecting device detects and all the other components when not leaving chromatographic column 3 (11), gas transfer valve 10 switches, and this moment, all the other components were by blowback.And the carrier gas of detecting device and reference gas all switch to hydrogen.
When sampling valve 7 switched, the sample in the quantity tube 1 (8) was introduced into chromatographic column 2 (6) under hydrogen carrier gas simultaneously, and post 2 (6), chromatographic column 1 (5), TCD detecting device 12 are in series connection at this moment.Component is worked as O in the sample after carrying out initial gross separation on the chromatographic column 2 (6)
2, N
2, CO enters chromatographic column 1 (5), and CO
2Enter before this post, isolation valve 4 switches to the ON state, at this moment O
2, N
2, CO closed in chromatographic column 1 (5) CO
2, hydrocarbon component enters TCD detecting device 12 through orifice valve 3 and detects.After treating that all components all leaves chromatographic column 2 (6), isolation valve 4 switches to the OFF state, at this moment the component O in the chromatographic column 1 (5)
2, N
2, CO separates successively and enters TCD detecting device 12 and 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: chromatographic column 2 is a Porapak N packed column, and post 3 is a 13-x moleculer sieve post; Chromatographic column 1 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
| Time | Type | State | Action Specification |
| 0 | Back detector | (-)Polarity on | The negate of TCD negative pole is used to measure hydrogen |
| 0.02 0.7 0.8 1.8 2.0 6.0 13.0 13.0 13.0 | Valve 1 Valve 2 Back detector Valve 3 Valve 1 Valve 3 Valve 3 Valve 2 Valve 3 | ON OFF (-)Polarity on ON OFF OFF ON OFF OFF | The sample introduction carrier gas is switched TCD and is recovered polarity and get and just survey permanent gas and close permanent gas and recover valve position and emit post 3 interior permanent gases and recover valve position and recover valve position and recover valve position |
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
| To sample long run test number of times | ||||||||||||
| The component title | Standard specimen is formed | 1 | 2 | 3 | 4 | 5 | 6 | 7 | Mean value | Relative error % | Standard deviation | Relative standard deviation |
| H2 C2H6 C2H4 CO2 O2 N2 CH4 CO | 8.11 0.02 0.04 1.42 1.15 36.68 52.16 0.42 | 8.35 0.02 0.04 1.43 1.13 36.62 52.02 0.40 | 8.15 0.02 0.04 1.42 1.15 36.64 52.16 0.42 | 8.06 0.02 0.04 1.41 1.15 36.68 52.22 0.43 | 8.11 0.02 0.04 1.42 1.16 36.66 52.16 0.43 | 8.21 0.02 0.04 1.42 1.15 36.67 52.10 0.40 | 8.26 0.02 0.04 1.40 1.23 36.59 52.03 0.43 | 8.08 0.02 0.04 1.41 1.23 36.70 52.12 0.40 | 8.17 0.02 0.04 1.42 1.17 36.65 52.12 0.41 | -0.78 -1.09 -0.99 -0.10 -1.56 0.09 0.09 1.70 | 0.10 0.00 0.00 0.01 0.04 0.04 0.07 0.01 | 1.19 1.20 1.15 0.69 3.24 0.10 0.13 3.24 |
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, 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, quantity tube 1 and quantity tube 2, thermal conductivity detector (TCD), chromatographic column 1, chromatographic column 2, chromatographic column 3 and chromatographic work station, wherein, chromatographic column 3, 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, orifice valve and chromatographic column 1 are connected on the isolation valve, be connected by chromatographic column 2 between isolation valve and the gas sampling valve, chromatographic work station links to each other with the thermal conductivity detector (TCD) series connection, it 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 chromatographic column 3, 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 B inlet that is connected with isolation valve, the carrier gas inlet that is connected with the thermal conductivity detector (TCD) carrier gas reaches the outlet with chromatographic column 3.
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 chromatographic column 3 to finish, and does carrier gas with nitrogen or argon gas that the separation of all the other components is adopted chromatographic column 1, chromatographic column 2 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1885031A true CN1885031A (en) | 2006-12-27 |
| CN100409009C CN100409009C (en) | 2008-08-06 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100270302A Expired - Fee Related CN100409009C (en) | 2005-06-22 | 2005-06-22 | Analyzer for mixed gas containing O2, N2 and H2 |
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| Country | Link |
|---|---|
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