CN102445498B - Automatic calibration method of process chromatograph - Google Patents
Automatic calibration method of process chromatograph Download PDFInfo
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- CN102445498B CN102445498B CN 201110304508 CN201110304508A CN102445498B CN 102445498 B CN102445498 B CN 102445498B CN 201110304508 CN201110304508 CN 201110304508 CN 201110304508 A CN201110304508 A CN 201110304508A CN 102445498 B CN102445498 B CN 102445498B
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004458 analytical method Methods 0.000 claims abstract description 21
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 84
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 abstract description 5
- 230000010354 integration Effects 0.000 abstract 3
- 238000011002 quantification Methods 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 14
- 238000003556 assay Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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Abstract
The invention discloses an automatic calibration method of a process chromatograph. The automatic calibration method is characterized by comprising the following steps of: allowing a chromatograph to drawing off a gas sample prepared by an automatic sample preparation gas flow device, controlling chromatography by a set software, storing the analysis result into a calibration database, and successively carrying out analysis and calibration according to different concentrations. The automatic sample preparation gas flow device is formed by an air inlet end module successively in series connection with a needle-valve module, a solenoid valve module, a diaphragm vacuum pump and a three-way solenoid valve. The air inlet end module is a module equipped with the integration of several air inlet pipes. The needle-valve module is a module equipped with the integration of several needle-valves. The solenoid valve module is a module equipped with the integration of several bi-pass solenoid valves. In comparison with the prior art, the invention has advantages of simple structure and convenient operation. According to the invention, automation of chromatography and sample preparation can be realized, and it is convenient to adjust and control gas amount according to the requirement of the analysis so as to carry out analysis and calibration on the prepared gas sample. In addition, quantification is accurate and sample preparation is highly precise.
Description
Technical field
The present invention relates to gas phase analysis and Instrument technology field, especially a kind of automatic calibration method of the on-stream chromatography for stratographic analysis.
Background technology
Calibration process when the stratographic analysis rock gas in well logging scene and laboratory forms in oil exploitation is extremely important.At present, no matter be well logging scene or the chromatogram commissioning staff in laboratory, generally all adopt the manual sample of syringe, then inject chromatogram and demarcate, the time-consuming effort again of this method, calibration process is very loaded down with trivial details, and each chromatogram commissioning staff's operation technique is different again, even if before and after same commissioning staff, twice operation also is not quite similar with consistent, very easily causes the inaccurate of calibration result, precision is lower, greatly affects the degree of accuracy of gas component stratographic analysis.
Summary of the invention
The automatic calibration method that the objective of the invention is a kind of on-stream chromatography of designing for the deficiencies in the prior art, the automatic sample gas circuit of its employing chromatogram extraction warp institute sample gas, analyze successively demarcation by variable concentrations, charge flow rate is controlled automatically, easy to operate, the sample precision is high, demarcates accurately, and the calibration process automaticity is high.
The object of the present invention is achieved like this: a kind of automatic calibration method of on-stream chromatography, be characterized in that chromatograph extracts after sample gas path device automatically institute sample gas the software control stratographic analysis by setting, then analysis result is stored in the nominal data storehouse, and analyzes successively demarcation by variable concentrations; Automatic sample gas path device is connected in series successively needle-valve chunk, solenoid valve chunk, diaphragm vacuum pump and three-way solenoid valve by the inlet end chunk and forms, and the inlet end chunk is to be provided with the integrated module of several draft tube; The needle-valve chunk is to be provided with the integrated module of several needle-valves; The solenoid valve chunk is to be provided with the integrated module of several two-way electromagnetic valves; Draft tube and needle-valve and two-way electromagnetic valve are corresponding and be concatenated into successively after several gas circuits with diaphragm vacuum pump entrance point and connect one by one, be connected with the three-way solenoid valve entrance point after diaphragm pump endpiece serial connection flow sensor, three-way solenoid valve one endpiece connects the gas collecting device, and another endpiece connects blow-down pipe; Chromatograph is analyzed demarcation by sample gas in chromatographic sample pump extracting gases collector, and the pipeline that the gas collecting device is connected with the chromatographic sample pump is provided with pressure transducer and sample pneumoelectric magnet valve.
Described two-way electromagnetic valve, three-way solenoid valve, diaphragm vacuum pump, sample pneumoelectric magnet valve and chromatographic sample pump are controlled by the program interlock of software set.
Described two-way electromagnetic valve and sample pneumoelectric magnet valve are controlled the break-make of each gas circuit by control signal; Diaphragm vacuum pump and chromatographic sample pump are controlled the air inlet power of sample gas by control signal; Flow sensor and pressure transducer are controlled charge flow rate and the pressure that gathers by control signal; Three-way solenoid valve is controlled the gas circuit of cleaning emptying or the collection of sample gas by control signal and is switched; Gas collector is collected respectively the sample gas of joining.
The present invention compared with prior art has simple in structure, and is easy to operate, realizes that the automaticity of stratographic analysis sample is high, can be according to the needs of the analyzing size of regulation and control tolerance easily, carry out the analysis of institute's sample gas and demarcate, quantitatively accurately, the sample precision is high.
Description of drawings
Fig. 1 is structural representation of the present invention;
Fig. 2 is the invention process illustration.
Embodiment
Consult accompanying drawing 1, automatic sample gas path device is connected in series successively needle-valve chunk 2, solenoid valve chunk 3, diaphragm vacuum pump 4 and three-way solenoid valve 6 by inlet end chunk 1 and forms, and inlet end chunk 1 is for being provided with the integrated module of several air inlet mouths of pipe 11 ~ 1n; Needle-valve chunk 2 is for being provided with the integrated module of several needle-valves 21 ~ 2n; Solenoid valve chunk 3 is for being provided with the integrated module of several two-way electromagnetic valves 31 ~ 3n; Draft tube 11 ~ 1n and needle-valve 21 ~ 2n and two-way electromagnetic valve 31 ~ 3n are corresponding and be concatenated into successively after n gas circuit with diaphragm vacuum pump 4 entrance points and connect one by one, said n=1 ~ 10, be connected with three-way solenoid valve 6 entrance points after diaphragm vacuum pump 4 endpiece serial connection flow sensors 5, three-way solenoid valve 6 one endpiece connect gas collecting device 7, and three-way solenoid valve 6 another endpiece connect blow-down pipe 8; Chromatograph 10 by the chromatographic sample pump 42 interior sample gas of extracting gases collector 7 after by the software control stratographic analysis of setting, then analysis result is stored in the nominal data storehouse, and analyzes successively demarcation by variable concentrations; The pipeline that gas collecting device 7 is connected with chromatographic sample pump 42 is provided with pressure transducer 61 and sample pneumoelectric magnet valve 9.
Above-mentioned two-way electromagnetic valve 31 ~ 3n, three-way solenoid valve 6, diaphragm vacuum pump 4, sample pneumoelectric magnet valve 9 and the chromatographic sample pump 42 stated controlled by the program interlock of software set; Two-way electromagnetic valve 31 ~ 3n and sample pneumoelectric magnet valve 9 are controlled the break-make of each gas circuit by control signal; Diaphragm vacuum pump 4 and chromatographic sample pump 42 are controlled the air inlet power of sample gas by control signal; Flow sensor 5 and pressure transducer 61 are controlled charge flow rate and the pressure that gathers by control signal; Three-way solenoid valve 6 is controlled the gas circuit of cleaning emptying or the collection of sample gas by control signal and is switched; Gas collector 7 is collected respectively the sample gas of joining; Sample pneumoelectric magnet valve 9 extracts institute's sample gas by control signal control chromatograph 10 and carries out stratographic analysis; Pressure transducer 61 is gathered the sample atmospheric pressure of gas collector 7 by control signal.
Concrete operations of the present invention are carried out in the steps below:
(1), flow regulation
Open respectively successively two-way electromagnetic valve 31 ~ 3n and the diaphragm pump 4 of each gas circuit, the flow that the needle-valve 21 ~ 2n that regulates corresponding gas circuit shows to flow sensor 5 is closed the path of all two-way electromagnetic valve 31 ~ 3n after the required flow.
(2), sample
Open the corresponding two-way electromagnetic valve 31 of draft tube 11 of the first gas circuit, gas process needle-valve 21, two-port valve 31, diaphragm vacuum pump 4, flow sensor 5 and three-way solenoid valve 6 are through blow-down pipe 8 emptying, emptying time is 2 seconds, then three-way solenoid valve 6 adds electric circuit and switches to gas collecting device 7 and collect a sample gas, until a sample gas that gathers is closed the corresponding two-way electromagnetic valve 31 of draft tube 11 to setting value; Three-way solenoid valve 6 outage gas circuits switch to blow-down pipe 8 emptying, then open the corresponding two-way electromagnetic valve 32 of draft tube 12 of the second gas circuit, gas process needle-valve 22, two-port valve 32, diaphragm vacuum pump 4, flow sensor 5 and three-way solenoid valve 6 are through blow-down pipe 8 emptying, emptying after 2 seconds three-way solenoid valve 6 add electric circuit and switch to gas collecting device 7 and collect b sample gas, until the b sample gas that gathers is to setting value.
With above-mentioned operation steps, open respectively successively the draft tube 1n of n gas circuit, until the collection of n sample gas is complete, then close the two-way electromagnetic valve 3n of n gas circuit, three-way solenoid valve 6 outage gas circuits switch to blow-down pipe 8 emptying, and diaphragm vacuum pump 4 is placed in off-position.
(3), chromatogram is demarcated
Open sample pneumoelectric magnet valve 9 and chromatographic sample pump 42, program setting by software extracts institute's sample gas and enters chromatograph 10 circumstances in which people get things ready for a trip analysis of spectrum of going forward side by side, analysis result is stored in the nominal data storehouse, then analyze demarcation by the variable concentrations point, still have sample gas to continue to sample in complete gas collecting device 7 to show that to pressure transducer 61 pressure are zero if demarcate, close sample pneumoelectric magnet valve 9 and chromatographic sample pump 42, ready for demarcate next time.
Embodiment 1
Table 1 preparation 1% methane gas assay
| Concentration | For the first time | For the second time | Precision |
| 1% | 1.0095 | 1.0031 | 0.636% |
Can be obtained by data in table 1, the error of twice experiment accuracy is analyzed the precision of demarcating high all less than 1%.
More than just the present invention is further illustrated, is not to limit this patent, and all the present invention of being equivalences are implemented, within all should being contained in the claim scope of this patent.
Claims (3)
1. the automatic calibration method of an on-stream chromatography, it is characterized in that chromatograph extracts after sample gas path device automatically institute sample gas the software control stratographic analysis by setting, then analysis result is stored in the nominal data storehouse, and analyzes successively demarcation by variable concentrations; Automatic sample gas path device is connected in series successively needle-valve chunk, solenoid valve chunk, diaphragm vacuum pump and three-way solenoid valve by the inlet end chunk and forms, and the inlet end chunk is to be provided with the integrated module of several draft tube; The needle-valve chunk is to be provided with the integrated module of several needle-valves; The solenoid valve chunk is to be provided with the integrated module of several two-way electromagnetic valves; Draft tube and needle-valve and two-way electromagnetic valve are corresponding and be concatenated into successively after several gas circuits with diaphragm vacuum pump entrance point and connect one by one, be connected with the three-way solenoid valve entrance point after diaphragm vacuum pump outlet end serial connection flow sensor, three-way solenoid valve one endpiece connects the gas collecting device, and another endpiece connects blow-down pipe; Chromatograph is analyzed demarcation by sample gas in chromatographic sample pump extracting gases collector, and the pipeline that the gas collecting device is connected with the chromatographic sample pump is provided with pressure transducer and sample pneumoelectric magnet valve.
2. the automatic calibration method of on-stream chromatography according to claim 1 is characterized in that described two-way electromagnetic valve, three-way solenoid valve, diaphragm vacuum pump, sample pneumoelectric magnet valve and chromatographic sample pump controlled by the program interlock of software set.
3. the automatic calibration method of described on-stream chromatography according to claim 1 and 2 is characterized in that described two-way electromagnetic valve and sample pneumoelectric magnet valve controlled the break-make of each gas circuit by control signal; Diaphragm vacuum pump and chromatographic sample pump are controlled the air inlet power of sample gas by control signal; Flow sensor and pressure transducer are controlled charge flow rate and the pressure that gathers by control signal; Three-way solenoid valve is controlled the gas circuit of cleaning emptying or the collection of sample gas by control signal and is switched; Gas collector is collected respectively the sample gas of joining.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110304508 CN102445498B (en) | 2011-10-10 | 2011-10-10 | Automatic calibration method of process chromatograph |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110304508 CN102445498B (en) | 2011-10-10 | 2011-10-10 | Automatic calibration method of process chromatograph |
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| CN102445498A CN102445498A (en) | 2012-05-09 |
| CN102445498B true CN102445498B (en) | 2013-06-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103529152B (en) * | 2013-10-15 | 2015-07-01 | 中国工程物理研究院化工材料研究所 | Self-feedback gasometry device based on mass spectrometer and application method thereof |
| CN105911222A (en) * | 2016-04-18 | 2016-08-31 | 中国石油化工股份有限公司 | Metrological verification device for ammonia gas detector and metrological verification method thereof |
| CN109030682A (en) * | 2018-10-16 | 2018-12-18 | 中石化石油工程技术服务有限公司 | The quick compounding device of the chromatographic hydrocarbon gas of hydrogen flame |
| CN109324145A (en) * | 2018-11-23 | 2019-02-12 | 国家电网有限公司 | Automatic calibration method and terminal equipment for online monitoring equipment |
| CN115825309A (en) * | 2022-11-18 | 2023-03-21 | 国网山东省电力公司电力科学研究院 | A fast self-test calibration device and method for transformer oil chromatographic detection |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201440135U (en) * | 2009-06-26 | 2010-04-21 | 河南省电力公司商丘供电公司 | Multifunctional gas chromatograph gas path flow |
| CN201477080U (en) * | 2009-08-20 | 2010-05-19 | 上海科油石油仪器制造有限公司 | Air Flow Control Module |
| CN102004136A (en) * | 2010-10-21 | 2011-04-06 | 上海科油石油仪器制造有限公司 | Chromatographic analysis control gas circuit device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09127074A (en) * | 1995-11-02 | 1997-05-16 | Hitachi Ltd | Carrier gas flow controller for sample inlet for gas chromatograph |
| KR20030067220A (en) * | 2002-02-07 | 2003-08-14 | (주)영린기기 | Automatic flow rate control device for use in a gas chromatograph and gas chromatography analyzing system comprising same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201440135U (en) * | 2009-06-26 | 2010-04-21 | 河南省电力公司商丘供电公司 | Multifunctional gas chromatograph gas path flow |
| CN201477080U (en) * | 2009-08-20 | 2010-05-19 | 上海科油石油仪器制造有限公司 | Air Flow Control Module |
| CN102004136A (en) * | 2010-10-21 | 2011-04-06 | 上海科油石油仪器制造有限公司 | Chromatographic analysis control gas circuit device |
Non-Patent Citations (5)
| Title |
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| JP特开平9-127074A 1997.05.16 |
| 于世林.国外二维气相色谱仪的现状.《分析仪器》.1985,(第04期),1-6. |
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