CN1141574C - Gas chromatography for rock pyrolysis - Google Patents
Gas chromatography for rock pyrolysis Download PDFInfo
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- CN1141574C CN1141574C CNB011063416A CN01106341A CN1141574C CN 1141574 C CN1141574 C CN 1141574C CN B011063416 A CNB011063416 A CN B011063416A CN 01106341 A CN01106341 A CN 01106341A CN 1141574 C CN1141574 C CN 1141574C
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- feeding rod
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Abstract
The present invention relates to a gas chromatograph for rock pyrolysis, which belongs to the comprehensive analytical instrument field of petroleum exploration and the rock pyrolysis. A method for directly heating a rock sample is adopted, a thermal evaporation hydrocarbon component is subdivided, and each detection data can be completely reflected. The gas chromatograph for rock pyrolysis comprises an electromagnetic valve 1, a stabilizing pressure valve 2, a four-way 3, a pressure gauge 4, a flow stabilizing valve 5, a switching valve 6, a pyrolysis oven 7, a pyrolysis oven cavity 8, a filter 9, a multiple-way valve 10, a back pressure shunt valve 11, a pre-column pressure gauge 12, a chromatographic column 13, a detector 14, a sampling bar 15, a sealed sliding block 16, a copple 17, an air resistor 18 and a three-way 19. The gas chromatograph can be widely applied to a rock pyrolysis exploring and detecting field, and the gas chromatograph has the advantages of high detection efficiency, accurate data, high stability, good repeatability, etc.
Description
(1) technical field: the invention belongs to petroleum prospecting rock pyrolysis composite analyser field.
(2) background technology: at present, chloroform bitumen " A " gas chromatographic analysis device that petroleum prospecting, developing department's stable hydrocarbon analysis are generally adopted, analysis result hydrocarbon component relative content is low, the analytic process sample will pass through multiple working procedures such as grind away, weighing, organic reagent extracting, transfer, filtration, sense cycle is long, hydrocarbon component in the sample is very easily lost, has influenced the accuracy of sample monitoring data.
(3) summary of the invention: gas chromatography for rock pyrolysis has adopted the direct-fired method of rock sample, and thermal evaporation hydrocarbon component is segmented, can the every detection data of complete reflection.
Its principle of work is as follows: sample is not taked multiprogrammings such as grind away, weighing, organic reagent extracting, transfer, filtration, and the heating furnace that the graininess rock sample is directly sent into temperature programme is heated, the pyrolysis gas that produces is carried by carrier gas, after the filtrator filtration, carry out the gas chromatographic detection analysis again.In the system of the present invention, tensimeter 12, chromatographic column 13, detecting device 14, crucible 17, vapour lock 18, the threeway 19, transfer valve 6, filtrator 9, multiport valve 10, back pressure diverting valve 11, sample feeding rod 15 and sealing slide block 16 have also been set up before the transfer valve 1 that in comprising common gas chromatograph, has, pressure maintaining valve 5, pyrolysis oven 7, pyrolysis furnace chamber 8, the post.
In detecting the rock sample data procedures, two kinds of duties are arranged, duty I inserts the carrier gas state, and duty II is that the pyrolysis gaseity is carried in carrier gas.Transfer valve 6 is responsible for two kinds of conversion of operation state.The inlet end C of transfer valve 6 connects the output terminal of flow stabilizing valve 5, and outlet side L connects pyrolysis furnace chamber 8, and outlet side F connects sample feeding rod 15.Filtrator 9 can cushion tested component, the impurity such as dust that elimination need not detect.Filtrator 9 one termination pyrolysis furnace chambers 8, the input end of another termination multiport valve 10, other 2 outlet one termination chromatographic columns 13 of multiport valve 10, the other end connects the input end of back pressure diverting valve 11 through tensimeter 12 before the post.Multiport valve 10 guarantees that a large amount of gases enter back pressure diverting valve 11, and a small amount of gas enters chromatographic column 13.Reach the pressure of setting when back pressure diverting valve 11 after, begin to discharge gas, and keep constant pressure, the carrier gas flux that keeps entering chromatographic column 13 is constant relatively.Sealing slide block 16 is enclosed within on the sample feeding rod 15, and sealing also can move axially separately or jointly mutually.Sample feeding rod 15 is a hollow tubular, and front end is equipped with the crucible 17 of built-in rock sample, and hollow tubular communicates with crucible 17.Carrier gas is carried away the component that heats rock sample in the crucible 17 by sample feeding rod 15, and a small amount of gas enters chromatographic column 13, and a large amount of gases are through 11 emptying of back pressure diverting valve.
The present invention can be widely used in rock pyrolysis exploration detection range, has advantages such as detection efficiency height, accurate, the stable height of data, good reproducibility.
(4) description of drawings: figure one is the gas chromatography for rock pyrolysis principle schematic.Among the figure: the 1st, solenoid valve, the 2nd, pressure maintaining valve, the 3rd, four-way, the 4th, tensimeter, the 5th, flow stabilizing valve, the 6th, transfer valve, the 7th, pyrolysis oven, the 8th, pyrolysis furnace chamber, the 9th, filtrator, the 10th, multiport valve, the 11st, tensimeter, the 13rd before the back pressure diverting valve, the 12nd, post, chromatographic column, the 14th, detecting device, the 15th, sample feeding rod, the 16th, sealing slide block, the 17th, crucible, the 18th, vapour lock, the 19th, threeway.
(5) embodiment:
Carrier gas enters four-way 3 through solenoid valve 1 and pressure maintaining valve 2, and one tunnel carrier gas enters transfer valve 6 through flow stabilizing valve 5, and tensimeter 4 indications enter the pressure of carrier gas.During I, CF cuts off transfer valve 6 in working order, CL connects.At this moment, sealing slide block 16 squeezes with pyrolysis oven 7 and closes, and sample feeding rod 15 does not push in the pyrolysis oven 7, and carrier gas enters the pyrolysis furnace chamber 8 of sealing, and enters multiport valve 10 by the gas outlet of pyrolysis oven 7 through filtrator 9.Pressure before the post before the tensimeter 12 indication chromatographic columns.A small amount of gas enters chromatographic column 13, and a large amount of gases enter back pressure diverting valve 11.After the carrier gas flux that enters chromatographic column 13 kept stablizing, transfer valve 6 entered duty II, and CL cuts off, CF connects.At this moment, sample feeding rod 15 pushes in the pyrolysis oven 7.Carrier gas is carried away by the component that sample feeding rod 15, crucible 17 will heat rock sample, and a large amount of gases make a small amount of gas enter chromatographic column 13 through 11 emptying of back pressure diverting valve.Enter the carrier gas of chromatographic column 13 and the combination gas of sample component, after chromatographic column 13 is separated, enter detecting device 14 and detect.In order to guarantee to detect the authenticity of thermal evaporation hydrocarbon component, transfer valve 6 is got back to duty I after II worked about 3 minutes in working order automatically, and CF cuts off, CL connects.Another road make-up gas of four-way 3 through vapour lock 18, carries gas that chromatographic column 13 comes out and enters detecting device 14 by threeway 19 and detect.After detecting end, sample feeding rod 15 is released pyrolysis oven 7 together with sealing slide block 16, takes out the rock sample in the crucible 17.
Transfer valve 6 models are KXD23; Filtrator 9 specifications are 8 * 100 millimeters of Φ, and interior dress filters reagent; Multiport valve 10 is threeway; Back pressure diverting valve 11 models are DL-1, and pressure is 0.08 MPa; Hollow specification is 10 * 100 millimeters of Φ in the sample feeding rod 15; The carrier gas flux that enters transfer valve 6 is 50 milliliters of per minutes; Pyrolysis oven 7 cavity temperatures are 300 degrees centigrade.Sample: the sample of Liaohe Oil Field well; Detection time: February 2 calendar year 2001;
Detection site: laboratory, our factory;
Testing result:
| Technical indicator | The method of inspection | The instruments of inspection | Specifications and models | The component title | Massfraction | Mean value | Relative deviation (%) | ||||
| 1 | 2 | 3 | 1 | 2 | 3 | ||||||
| Same sample analysis precision: massfraction scope: 1.＞10%, relative deviation≤10%; 2.＞5%-10% relative deviation≤15%; 3.＞1%-5% relative deviation≤20%; 4.＞0.5%-1% relative deviation≤30%; 5.＜0.5%, do not stipulate | With the verification of work mass transfer sample | Balance | FX- 40C | nC13 | 3.651 | 3.951 | 3.853 | 3.818 | 4.4 | 3.5 | 0.9 |
| nC14 | 5.121 | 5.423 | 6.123 | 5.556 | 7.8 | 2.4 | 10.2 | ||||
| nC15 | 6.110 | 6.217 | 6.504 | 6.227 | 2.7 | 1.0 | 3.6 | ||||
| nC16 | 6.755 | 6.770 | 6.550 | 6.692 | 0.9 | 1.2 | 2.1 | ||||
| nC17 | 6.828 | 6.854 | 6.959 | 6.880 | 0.8 | 0.4 | 1.1 | ||||
| Pr | 3.441 | 3.353 | 3.326 | 3.373 | 2.0 | 0.6 | 1.4 | ||||
| nC18 | 6.648 | 6.191 | 6.339 | 6.393 | 4.0 | 3.2 | 0.8 | ||||
| Ph | 1.816 | 1.700 | 1.747 | 1.754 | 4 | 3.1 | 0.4 | ||||
| nC19 | 7.487 | 7.287 | 6.779 | 7.184 | 4.2 | 1.4 | 5.6 | ||||
| nC20 | 7.740 | 7.420 | 7.486 | 7.549 | 2.5 | 1.7 | 0.8 | ||||
| nC21 | 8.512 | 8.021 | 8.326 | 8.286 | 2.7 | 3.2 | 0.5 | ||||
| nC22 | 7.971 | 7.808 | 7.860 | 7.880 | 1.2 | 0.9 | 0.2 | ||||
| nC23 | 8.184 | 8.307 | 8.300 | 8.264 | 1.0 | 0.5 | 0.4 | ||||
| nC24 | 5.894 | 6.071 | 6.016 | 5.994 | 1.7 | 1.3 | 0.4 | ||||
| nC25 | 4.968 | 5.567 | 5.353 | 5.296 | 6.2 | 5.1 | 1.1 | ||||
| nC26 | 3.492 | 3.553 | 3.357 | 3.467 | 0.7 | 2.5 | 3.2 | ||||
| nC27 | 2.785 | 2.691 | 2.584 | 2.687 | 3.7 | 0.2 | 3.8 | ||||
| nC28 | 1.575 | 1.734 | 1.586 | 1.626 | 3.1 | 6.7 | 3.5 | ||||
| nC29 | 1.021 | 1.082 | 0.967 | 1.024 | 0.2 | 5.7 | 5.5 | ||||
Claims (1)
1, a kind of gas chromatography for rock pyrolysis, transfer valve (1), pressure maintaining valve (2), four-way (3), tensimeter (4), flow stabilizing valve (5), pyrolysis oven (7), pyrolysis furnace chamber (8), the preceding tensimeter (12) of post, chromatographic column (13), detecting device (14), crucible (17), vapour lock (18), threeway (19) are arranged, it is characterized in that transfer valve (6), filtrator (9), multiport valve (10), back pressure diverting valve (11), sample feeding rod (15), sealing slide block (16) in addition; The inlet end C of transfer valve (6) connects the output terminal of flow stabilizing valve (5), outlet side L connects pyrolysis furnace chamber (8), outlet side F connects sample feeding rod (15), sealing slide block (16) is enclosed within on the sample feeding rod (15), sealing mutually, and can move axially separately or jointly, sample feeding rod (15) is a hollow tubular, front end is equipped with the crucible (17) of built-in rock sample, and hollow tubular communicates with crucible (17); One termination pyrolysis furnace chamber (8) of filtrator (9), the input end of another termination multiport valve (10), other 2 outlet one termination chromatographic columns (13) of multiport valve (10), the other end connects the input end of back pressure diverting valve (11) through tensimeter (12) before the post.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011063416A CN1141574C (en) | 2001-03-22 | 2001-03-22 | Gas chromatography for rock pyrolysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011063416A CN1141574C (en) | 2001-03-22 | 2001-03-22 | Gas chromatography for rock pyrolysis |
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| CN1376918A CN1376918A (en) | 2002-10-30 |
| CN1141574C true CN1141574C (en) | 2004-03-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB011063416A Expired - Lifetime CN1141574C (en) | 2001-03-22 | 2001-03-22 | Gas chromatography for rock pyrolysis |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004102156A2 (en) * | 2003-05-07 | 2004-11-25 | Saudi Arabian Oil Company | Compositional modeling and pyrolysis data analysis methods |
| US7258132B2 (en) * | 2004-06-18 | 2007-08-21 | Agilent Technologies, Inc. | Electronically controlled back pressure regulator |
| CN104090052B (en) * | 2013-12-18 | 2017-11-03 | 力合科技（湖南）股份有限公司 | Gas chromatograph and its multichannel carrier gas stream, gas path control method |
| CN103994917B (en) * | 2014-05-06 | 2016-04-06 | 中国科学院广州地球化学研究所 | A kind of heating arrangement on rock pyrolysis instrument |
| CN105651912A (en) * | 2015-12-30 | 2016-06-08 | 海城市石油化工仪器厂 | Rock pyrologger and pyrolytic analysis method |
| CN109115824A (en) * | 2017-06-26 | 2019-01-01 | 中国石油化工股份有限公司 | Sample feeding rod for rock pyrolysis analysis |
| CN109374810B (en) * | 2018-12-05 | 2020-12-04 | 中国科学院西北生态环境资源研究院 | Method for rapidly analyzing soluble organic light hydrocarbon components of source rock |
| CN113640400A (en) * | 2021-06-25 | 2021-11-12 | 中国科学院紫金山天文台 | Method for detecting organic matters in solar system asteroid rock soil |
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2001
- 2001-03-22 CN CNB011063416A patent/CN1141574C/en not_active Expired - Lifetime
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