CN103698166A - Rock analysis gas high-vacuum degassing and gas-collecting device - Google Patents
Rock analysis gas high-vacuum degassing and gas-collecting device Download PDFInfo
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- CN103698166A CN103698166A CN201210365450.1A CN201210365450A CN103698166A CN 103698166 A CN103698166 A CN 103698166A CN 201210365450 A CN201210365450 A CN 201210365450A CN 103698166 A CN103698166 A CN 103698166A
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Abstract
The invention relates to a rock analysis gas high-vacuum degassing and gas-collecting device. The device comprises a degassing device and a gas collecting device. The degassing device comprises a stainless steel tank body and a gas pressure detector. Stainless steel balls are disposed in the stainless steel tank body. A stainless steel sealed cap is disposed on the upper portion of the stainless steel tank body. An analysis gas collecting port, a vacuum pump connecting port and the gas pressure detector are respectively disposed on the stainless steel sealed cap. The gas collecting device comprises a glass tank body, a push rod and a needle tube, wherein a sealed piston is arranged on the end portion of the push rod. The push rod is disposed at one end of the glass tank body and the needle tube is disposed at the other end of the glass tank body. The sealed piston is disposed in the glass tank body. The rock analysis gas high-vacuum degassing and gas-collecting device is wide in application range, large in the amount of obtained analysis gas, short in vacuum broken time and low in temperature, and effectively improves the precision and reliability of component data of the analysis gas and isotope composition data.
Description
Technical field
The present invention relates to the degassed gas extractor of resolution gas in oil and gas geochemistry field, relate in particular to rock resolution gas high vacuum degassing gas extractor.
Background technology
There is the residual valence field of force in the atom on blowhole surface or ion, the ability with adsorbed gas or liquid, rock gas is in diffusion And Movement process, constantly be adsorbed, form rock adsorbed gas, by means of various physical methods, make it be converted into free state and collected from rock ADSORPTION STATE, in oil and gas geochemistry field, be referred to as resolution gas.The research of resolution gas is sentenced knowledge, Gas Source Correlation, Migration, hydrocarbon source rock and evaluating reservoir for Natural Gas Origin, and the unconventional rock gas hot research field such as coal-seam gas, shale gas, compact sandstone gas, all has very important theoretical and practical significance.
At present, the degassed gas extractor of domestic resolution gas is mainly divided into two classes, and a class is for take the degassed gas extractor system that water is airtight medium, and another kind of is the apparatus system of vacuum outgas additional drainage gas collection.All there is following shortcoming in this two classes device: the (1) restriction of the volume of degasser, and sample size is limited in below 50 grams, causes retrievable resolution gas narrow-minded; (2) due to the existence of aqueous medium, two class devices are low vacuum, high background, high leak rate system, and in the resolution gas obtaining, hydro carbons concentration is low, cannot use conventional means to carry out test analysis to the component of resolution gas and isotopics.Generally need to carry out enrichment to resolution gas could form and test its component, has increased difficulty of test and cost.Particularly, the isotopics of resolution gas test is difficult to realize on existing apparatus basis; (3) gas extractor all be take water as airtight medium, and because retrievable rock resolution gas quantity is little, the water in gas extractor can, on the component of resolution gas and isotopics impact, affect research and the application of rock resolution gas in gas geochemistry field; (4) existing vacuum degasser in long operational process, the rock temperature that is impacted raises rapidly, make rock decomposes produce a certain amount of pyrolysis gas, thereby affected resolution gas component and isotopics, covered the original looks of rock resolution gas; (5) existing apparatus cannot accurately carry out measurements and calculations to the resolution gas tolerance of desorption.
Above-mentioned shortcoming has directly affected accuracy and the reliability of resolution gas component and isotopics data.In addition, the degassed gas extractor report of external resolution gas is few, has no way of using for reference and reference, has seriously restricted the application and research of resolution gas in gas geochemistry field.Therefore; must design research and develop the more scientific and reasonable degassed gas extractor of resolution gas; component and the isotopics of guaranteeing the resolution gas that obtains are unaffected; for the reliable experiment basis of science is laid in research and the application of resolution gas; fill up the blank of domestic resolution gas gas collection degasser design research and development, thereby change resolution gas in the situation relatively lagging behind of gas geochemistry research field.
Summary of the invention
Technical matters to be solved by this invention is to provide the rock resolution gas high vacuum degassing gas extractor of a kind of component of effective raising resolution gas and the accuracy of isotopics data and reliability.
For addressing the above problem, rock resolution gas high vacuum degassing gas extractor of the present invention, is characterized in that: this device is comprised of degasser and gas extractor two parts; Described degasser comprises stainless steel tank body and the gas pressure detection unit of built-in stainless steel ball; Described stainless steel tank body top is provided with stainless steel gland bonnet, is respectively equipped with resolution gas acquisition port, vacuum pump connector and described gas pressure detection unit on this stainless steel gland bonnet; Described gas extractor comprises that glass tank body, end are provided with push rod and the needle tubing of packed-piston; One end of described glass tank body is provided with described push rod, and its other end is provided with described needle tubing; Described packed-piston is placed in described glass tank body.
Big up and small down cylindrical of described stainless steel tank body.
Between described stainless steel tank body and described stainless steel gland bonnet, be provided with concavo-convex vacuum flange and be connected, this concavo-convex vacuum flange connects and is evenly equipped with several holding screws, and its joint is provided with vacuum flange sealing.
On described resolution gas acquisition port and described vacuum pump connector, stainless-steel vacuum valve is all installed.
Between described glass tank body and described needle tubing, be provided with packoff.
The present invention compared with prior art has the following advantages:
1, sample of the present invention is applied widely, rock core, landwaste and the surface occurence of hydrocarbon source rock (comprising mud stone, coal petrography, shale, carbonatite etc.), and the resolution gas of three class samples extracts experiment and has all obtained good effect.
2, the resolution gas obtaining is large-minded.
Matching requirements sample of the prior art, between 20 ~ 50g, and need be pulverized as particle in advance, to pack closed container into, tests, and has artificially reduced the resolution gas tolerance that can collect.And sample size of the present invention is larger, be generally 100g ~ 200g, bulk sample directly packs parsing tank into tests, and without precomminution, processes, and has avoided to the full extent the artificial loss of resolution gas.
3, good leak tightness, vacuum tightness is high.
Device of the prior art generally has the shortcoming of low vacuum, high background, high leak rate, and the resolution gas obtaining is mixed with the air of a greater number and hydrocarbon gas relative content is reduced, thereby does not reach the requirement that proper testing is analyzed.And the present invention has fabulous leakproofness, vacuum tightness is high, and sample is all the time in the experimental situation in high vacuum, low background, less leakage rate.Generally, device vacuum tightness is between 10
-4~ 10
-5standard atmospheric pressure, the atmospheric level in the present invention only has 0.0001% ~ 0.00001%, and the resolution gas obtaining is subject to the impact of atmospheric pollution completely negligible.
4, the vacuum breaking time short, temperature is low.
Resolution gas vacuum degasser of the prior art, in the process of vacuum breaking sample, unit temp raises rapidly, likely makes sample decomposes produce a certain amount of pyrolysis gas, causes the resolution gas test data distortion of obtaining.And 3 ~ 5 minutes sample vacuum breaking time of the present invention, broken rear sample temperature is between 40 ℃ ~ 50 ℃, and the resolution gas obtaining is not subject to the impact of " pyrolysis gas ", has guaranteed accuracy and the representativeness of test data.
5, adopt anhydrous gas extractor.
No matter device of the prior art is to take the degassed gas extractor system that water is airtight medium, or the apparatus system of vacuum outgas additional drainage gas collection, all with draining water gathering of gas law, collect resolution gas, cannot avoid the impact of water on resolution gas component and isotopics, and the present invention adopts anhydrous gas extractor to collect resolution gas, avoided to the full extent the interference of draining water gathering of gas law to resolution gas component and isotopics.Utilize the resolution gas tolerance that anhydrous gas extractor obtains to reach as high as 3ml left and right, met the requirement of correlation analysis test completely.
6, by different core samples being carried out to resolution gas, extract experiment, in order to verify science of the present invention and reliability.Result shows: (1) as shown in table 1, the resolution gas obtaining mainly be take hydrocarbon gas and carbon dioxide as main, and the relative percentage composition of hydrocarbon gas can reach more than 80%, can stable detection go out δ
13c
1~ δ
13c
3data, sample segment detects δ
13c
4~ δ
13c
5data are changed abundant information containedly, have met the needs of resolution gas geochemical investigation and application completely, have filled up the blank of domestic resolution gas device research and development; (2) as shown in Figure 4, in conjunction with actual Analysis On The Geological Background, show, hydrocarbon gas carbon isotope value in resolution gas is sentenced knowledge result to its Type of hydrocarbon source rock and degree of ripeness, with using organic geochemistry and petrology, the knowledge result of sentencing of the type of same hydrocarbon source rock and degree of ripeness is had to fabulous consistance, show that resolution gas and corresponding source rock have fabulous sibship; The also strong newly-established method feasibility of counterevidence and science from another point of view simultaneously; (3) the δ surveying with exploration area natural source rock sample product resolution gas for the first time as shown in Figure 5,
13c
1the R of value and the actual measurement of same source rock
othe lgR that value returns
ovs δ
13c
1expression formula, this is highly significant to earth science research.That is to say, by newly-established apparatus and method, by the means of experimental geology, set up the pattern of the meticulous oil-gas-source contrast of a workspace, and as insertion point, expand to deeper some oil gas of research and learn critical problem, as the potentiality of oil gas in the accurate identification of the genetic type of oil gas, hydrocarbon migration, region hydrocarbon source rock, region and even oil-gas exploration direction etc. all can provide extremely valuable scientific information.
table 1 rock resolution gas test data complete list
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is degasser schematic diagram of the present invention.
Fig. 2 is gas extractor schematic diagram of the present invention.
Fig. 3 is degasser work schematic diagram of the present invention.
Fig. 4 is for utilizing resolution gas
δ 13c
1value with
δ 13c
2value is divided source rock/Natural Gas Type figure.
Fig. 5 is humic type source rock
r ovs
δ 13c
1correlationship figure.
In figure: 1-stainless steel tank body, 2-stainless steel ball, 3-vacuum flange sealing, 4-stainless steel gland bonnet, 5-holding screw, 6-resolution gas acquisition port, 7-vacuum pump connector, 8-gas pressure detection unit, 9-stainless-steel vacuum valve, 10-sample, 11-glass tank body, 12-packed-piston, 13-push rod, 14-packoff, 15-needle tubing, 16-planetary ball mill rotating disk.
Embodiment
Rock resolution gas high vacuum degassing gas extractor, this device is comprised of degasser and gas extractor two parts.
Degasser comprises that the stainless steel tank body 1 of built-in stainless steel ball 2 and gas pressure detection unit 8(are referring to Fig. 1).Stainless steel tank body 1 top is provided with stainless steel gland bonnet 4, on this stainless steel gland bonnet 4, be respectively equipped with resolution gas acquisition port 6, vacuum pump connector 7 and gas pressure detection unit 8, realize that resolution gas extracts, sealed shell of tank vacuumizes, and the function that detects resolution gas pressure.
Wherein: big up and small down cylindrical of stainless steel tank body 1.
Between stainless steel tank body 1 and stainless steel gland bonnet 4, be provided with concavo-convex vacuum flange and be connected, this concavo-convex vacuum flange connects and is evenly equipped with several holding screws 5, and its joint is provided with vacuum flange sealing 3.
On resolution gas acquisition port 6 and vacuum pump connector 7, stainless-steel vacuum valve 9 is all installed.
Gas extractor comprises that glass tank body 11, end are provided with the push rod 13 of packed-piston 12 and needle tubing 15(referring to Fig. 2).One end of glass tank body 11 is provided with push rod 13, and its other end is provided with needle tubing 15; Packed-piston 12 is placed in glass tank body 11.Between glass tank body 11 and needle tubing 15, be provided with packoff 14.
Gas extractor, by the resolution gas acquisition port 6 of degasser, is directly collected resolution gas in order to carry out the test of its component and isotopics.
During work, first 100 ~ 200g large rock mass sample 10 and 8 ~ 10 stainless steel balls 2 are positioned in stainless steel tank body 1, by 7 pairs of stainless steel tank bodies 1 of vacuum pump connector, seal and vacuumize, vacuum tightness to 10
-4~ 10
-5after standard atmospheric pressure, stainless steel tank body 1 is fixed on planetary ball mill; Then switch on power, stainless steel tank body 1 is (Fig. 3) in the process of High Rotation Speed and rotation, and the stainless steel ball 2 in tank body smashes sample 10 to Powdered, the adsorbed gas of rock sample 10 desorption in high vacuum environment, stainless steel tank body 1 rotation, after 4 ~ 5 minutes, stops and taking off; The test analysis that the adsorbed gas that finally adopts gas extractor to extract 1ml left and right carries out component and isotopics.
Claims (5)
1. rock resolution gas high vacuum degassing gas extractor, is characterized in that: this device is comprised of degasser and gas extractor two parts; Described degasser comprises stainless steel tank body (1) and the gas pressure detection unit (8) of built-in stainless steel ball (2); Described stainless steel tank body (1) top is provided with stainless steel gland bonnet (4), is respectively equipped with resolution gas acquisition port (6), vacuum pump connector (7) and described gas pressure detection unit (8) on this stainless steel gland bonnet (4); Described gas extractor comprises that glass tank body (11), end are provided with push rod (13) and the needle tubing (15) of packed-piston (12); One end of described glass tank body (11) is provided with described push rod (13), and its other end is provided with described needle tubing (15); Described packed-piston (12) is placed in described glass tank body (11).
2. rock resolution gas high vacuum degassing gas extractor as claimed in claim 1, is characterized in that: big up and small down cylindrical of described stainless steel tank body (1).
3. rock resolution gas high vacuum degassing gas extractor as claimed in claim 1, it is characterized in that: between described stainless steel tank body (1) and described stainless steel gland bonnet (4), be provided with concavo-convex vacuum flange and be connected, in this concavo-convex vacuum flange connection, be evenly equipped with several holding screws (5), its joint is provided with vacuum flange sealing (3).
4. rock resolution gas high vacuum degassing gas extractor as claimed in claim 1, is characterized in that: on described resolution gas acquisition port (6) and described vacuum pump connector (7), stainless-steel vacuum valve (9) is all installed.
5. rock resolution gas high vacuum degassing gas extractor as claimed in claim 1, is characterized in that: between described glass tank body (11) and described needle tubing (15), be provided with packoff (14).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104407089A (en) * | 2014-12-09 | 2015-03-11 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Rock degassing high-sensitivity gas chromatography-mass spectrometry coupling analysis system and use method thereof |
| CN104777073A (en) * | 2015-04-22 | 2015-07-15 | 中国石油大学(北京) | Device and method for measuring remnant gas amount |
| CN104833787A (en) * | 2015-05-29 | 2015-08-12 | 沈阳煤层甲烷气开发中心 | Shale sample smashing desorption device |
| CN106153374A (en) * | 2015-04-21 | 2016-11-23 | 中国石油化工股份有限公司 | A kind of sealing crushes degasser |
| CN106680029A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Portable vacuum sampling bottle and application method thereof |
| CN109230023A (en) * | 2018-09-18 | 2019-01-18 | 安徽宁磁电子科技有限公司 | Ultra-fine powder collecting device |
| CN109813580A (en) * | 2018-12-25 | 2019-05-28 | 核工业北京地质研究院 | A kind of closed crush method extracts the device and method of volatile organic constituents in rock |
| CN113181838A (en) * | 2021-06-04 | 2021-07-30 | 河北华运鸿业化工有限公司 | Ball-milling drying vacuum reaction kettle |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104407089A (en) * | 2014-12-09 | 2015-03-11 | 中国科学院地质与地球物理研究所兰州油气资源研究中心 | Rock degassing high-sensitivity gas chromatography-mass spectrometry coupling analysis system and use method thereof |
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| CN104777073A (en) * | 2015-04-22 | 2015-07-15 | 中国石油大学(北京) | Device and method for measuring remnant gas amount |
| CN104833787A (en) * | 2015-05-29 | 2015-08-12 | 沈阳煤层甲烷气开发中心 | Shale sample smashing desorption device |
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| CN109230023A (en) * | 2018-09-18 | 2019-01-18 | 安徽宁磁电子科技有限公司 | Ultra-fine powder collecting device |
| CN109813580A (en) * | 2018-12-25 | 2019-05-28 | 核工业北京地质研究院 | A kind of closed crush method extracts the device and method of volatile organic constituents in rock |
| CN113181838A (en) * | 2021-06-04 | 2021-07-30 | 河北华运鸿业化工有限公司 | Ball-milling drying vacuum reaction kettle |
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Application publication date: 20140402 |