CN102445498A - Automatic calibration method of process chromatograph - Google Patents
Automatic calibration method of process chromatograph Download PDFInfo
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- CN102445498A CN102445498A CN2011103045087A CN201110304508A CN102445498A CN 102445498 A CN102445498 A CN 102445498A CN 2011103045087 A CN2011103045087 A CN 2011103045087A CN 201110304508 A CN201110304508 A CN 201110304508A CN 102445498 A CN102445498 A CN 102445498A
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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 that is used for the on-stream chromatography of stratographic analysis.
Background technology
Calibration process when the on-the-spot and breadboard stratographic analysis rock gas of well logging is formed in oil exploitation is extremely important.At present, no matter be well logging scene or breadboard chromatogram commissioning staff, generally all adopt syringe manually to join appearance; Inject chromatogram then 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 twice operation also is not quite similar with consistent before and after the same commissioning staff, very easily causes the inaccurate of calibration result; Precision is lower, influences the degree of accuracy of gas component stratographic analysis greatly.
Summary of the invention
The automatic calibration method of a kind of on-stream chromatography that the objective of the invention is to be directed against the deficiency of prior art and design; It adopts the chromatogram extraction to join a kind gas through joining a kind gas circuit automatically, analyzes demarcation successively by variable concentrations, and charge flow rate is controlled automatically; Easy to operate; Join a kind precision height, demarcate accurately, the calibration process automaticity is high.
The objective of the invention is to realize like this: a kind of automatic calibration method of on-stream chromatography; Be characterized in chromatograph extraction software control stratographic analysis by setting after joining kind gas path device automatically to join kind gas; Then analysis result is stored in the nominal data storehouse, and analyzes demarcation successively by variable concentrations; Automatically join kind gas path device and be connected in series needle-valve chunk, solenoid valve chunk, diaphragm vacuum pump and three-way solenoid valve successively by the inlet end chunk and form, 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 one by one and be concatenated into after several gas circuits with diaphragm vacuum pump entrance point successively and connect; Be connected with the three-way solenoid valve entrance point behind the 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 appearance gas in the 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 appearance pneumoelectric magnet valve.
Said two-way electromagnetic valve, three-way solenoid valve, diaphragm vacuum pump, appearance pneumoelectric magnet valve and chromatographic sample pump are by the program interlock control of software set.
Said two-way electromagnetic valve and the break-make of appearance pneumoelectric magnet valve by each gas circuit of control signal control; Diaphragm vacuum pump and chromatographic sample pump are by the air inlet power of control signal control appearance gas; Charge flow rate and pressure that flow sensor and pressure transducer are gathered by control signal control; Three-way solenoid valve is switched by the gas circuit that emptying or the collection of appearance gas are cleaned in control signal control; Gas collector is collected the appearance gas of being joined respectively.
The present invention compared with prior art has simple in structure, and is easy to operate, and the automaticity that appearance is joined in the realization stratographic analysis is high; Can regulate and control the size of tolerance according to the needs of analyzing easily; Carry out join kind gas analysis demarcate, quantitatively accurately, join a kind precision height.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is embodiment of the invention figure.
Embodiment
Consult accompanying drawing 1, join kind gas path device automatically and be connected in series needle-valve chunk 2, solenoid valve chunk 3, diaphragm vacuum pump 4 and three-way solenoid valve 6 successively by inlet end chunk 1 and form, 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 one by one and be concatenated into after n the gas circuit with diaphragm vacuum pump 4 entrance points successively and connect; Said n=1 ~ 10; Diaphragm vacuum pump 4 endpiece serial connection flow sensor 5 backs are connected with three-way solenoid valve 6 entrance points; 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 kind gas in the chromatographic sample pump 42 extracting gases collectors 7 after by the software control stratographic analysis of setting, then analysis result is stored in the nominal data storehouse, and analyzes demarcation successively by variable concentrations; The pipeline that gas collecting device 7 is connected with chromatographic sample pump 42 is provided with pressure transducer 61 and appearance pneumoelectric magnet valve 9.
The above-mentioned program interlock control of stating two-way electromagnetic valve 31 ~ 3n, three-way solenoid valve 6, diaphragm vacuum pump 4, appearance pneumoelectric magnet valve 9 and chromatographic sample pump 42 by software set; Two-way electromagnetic valve 31 ~ 3n and the break-make of appearance pneumoelectric magnet valve 9 by each gas circuit of control signal control; Diaphragm vacuum pump 4 and the air inlet power of chromatographic sample pump 42 by control signal control appearance gas; Flow sensor 5 and charge flow rate and the pressure of pressure transducer 61 by control signal control collection; Three-way solenoid valve 6 is switched by the gas circuit that emptying or the collection of appearance gas are cleaned in control signal control; Gas collector 7 is collected the appearance gas of being joined respectively; Appearance pneumoelectric magnet valve 9 is joined kind gas by control signal control chromatograph 10 extraction institutes and is carried out stratographic analysis; Pressure transducer 61 is gathered the appearance atmospheric pressure of gas collector 7 by control signal.
Concrete operations of the present invention are undertaken by following step:
(1), flow regulation
Open the two-way electromagnetic valve 31 ~ 3n and the diaphragm pump 4 of each gas circuit successively respectively, 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 behind the required flow.
(2), join appearance
Open the draft tube 11 pairing two-way electromagnetic valves 31 of 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; Three-way solenoid valve 6 powers up gas circuit and switches to gas collecting device 7 collection a appearance gas then, after a appearance gas to the setting value of gathering, closes draft tube 11 pairing two-way electromagnetic valves 31; Three-way solenoid valve 6 outage gas circuits switch to blow-down pipe 8 emptying; Open the draft tube 12 pairing two-way electromagnetic valves 32 of second gas circuit then; 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 power up gas circuit and switch to gas collecting device 7 and collect b appearance gas, until the b appearance gas of gathering to setting value.
With above-mentioned operation steps, open the draft tube 1n of n gas circuit successively respectively, finish until the collection of n appearance gas, close the two-way electromagnetic valve 3n of n gas circuit then, three-way solenoid valve 6 outage gas circuits switch to blow-down pipe 8 emptying, and diaphragm vacuum pump 4 places off-position.
(3), chromatogram is demarcated
Open kind pneumoelectric magnet valve 9 and chromatographic sample pump 42; Program setting through software with join kind gas extract and get into a 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, analyzes demarcation by the variable concentrations point then, demarcating finishes shows that to pressure transducer 61 pressure is zero if still have kind gas then to continue to sample in the gas collecting device 7; Close kind pneumoelectric magnet valve 9 and chromatographic sample pump 42, ready for demarcate next time.
Embodiment 1
Consulting accompanying drawing 2, is 1% methane and Air mixing gas with dose volume concentration, and the present invention is done further elaboration, and its operation steps is following:
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 the table 1, the error of twice experiment accuracy is all less than 1%, and it is high to analyze the precision of demarcating.
More than just the present invention being further described, is not in order to the restriction this patent, all for the present invention's equivalence enforcement, all should be contained within the claim scope of this patent.
Claims (3)
1. the automatic calibration method of an on-stream chromatography; It is characterized in that chromatograph extraction software control stratographic analysis by setting after joining kind gas path device automatically to join kind gas; Then analysis result is stored in the nominal data storehouse, and analyzes demarcation successively by variable concentrations; Automatically join kind gas path device and be connected in series needle-valve chunk, solenoid valve chunk, diaphragm vacuum pump and three-way solenoid valve successively by the inlet end chunk and form, 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 one by one and be concatenated into after several gas circuits with diaphragm vacuum pump entrance point successively and connect; Be connected with the three-way solenoid valve entrance point behind the 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 appearance gas in the 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 appearance pneumoelectric magnet valve.
2. according to the automatic calibration method of the said on-stream chromatography of claim 1, it is characterized in that the program interlock control of said two-way electromagnetic valve, three-way solenoid valve, diaphragm vacuum pump, appearance pneumoelectric magnet valve and sample pump by software set.
3. according to the automatic calibration method of claim 1 or 2 said on-stream chromatographies, it is characterized in that said two-way electromagnetic valve and the break-make of appearance pneumoelectric magnet valve by each gas circuit of control signal control; Diaphragm vacuum pump and chromatographic sample pump are by the air inlet power of control signal control appearance gas; Charge flow rate and pressure that flow sensor and pressure transducer are gathered by control signal control; Three-way solenoid valve is switched by the gas circuit that emptying or the collection of appearance gas are cleaned in control signal control; Gas collector is collected the appearance gas of being joined respectively.
Priority Applications (1)
| 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 |
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| CN 201110304508 CN102445498B (en) | 2011-10-10 | 2011-10-10 | Automatic calibration method of process chromatograph |
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| CN102445498A true CN102445498A (en) | 2012-05-09 |
| CN102445498B CN102445498B (en) | 2013-06-05 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103529152A (en) * | 2013-10-15 | 2014-01-22 | 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 | On-line monitoring equipment automatic calibration method and terminal device |
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| JPH09127074A (en) * | 1995-11-02 | 1997-05-16 | Hitachi Ltd | Adjusting device for flow rate of carrier gas at sample injection port for gas chromatograph |
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| 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 | Gas circuit 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 |
-
2011
- 2011-10-10 CN CN 201110304508 patent/CN102445498B/en active Active
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| JPH09127074A (en) * | 1995-11-02 | 1997-05-16 | Hitachi Ltd | Adjusting device for flow rate of carrier gas at sample injection port 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 |
| 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 | Gas circuit flow control module |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103529152A (en) * | 2013-10-15 | 2014-01-22 | 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 | On-line monitoring equipment automatic calibration method and terminal device |
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| CN102445498B (en) | 2013-06-05 |
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