CN1308678C - Soil adsorbed hydrocarbon low-temperature desorption apparatus and method - Google Patents
Soil adsorbed hydrocarbon low-temperature desorption apparatus and method Download PDFInfo
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- CN1308678C CN1308678C CNB2005100647582A CN200510064758A CN1308678C CN 1308678 C CN1308678 C CN 1308678C CN B2005100647582 A CNB2005100647582 A CN B2005100647582A CN 200510064758 A CN200510064758 A CN 200510064758A CN 1308678 C CN1308678 C CN 1308678C
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Abstract
The present invention relates to a soil adsorbed hydrocarbon low-temperature desorption device and a method thereof. The soil adsorbed hydrocarbon low-temperature desorption method comprises the steps that a purpose-made device is used; firstly, water which does not contain gas is added into soil, the soil is stirred and is made into slurry which is sucked into the device, the device can avoid atmospheric mixture in a slurry sucking process, and adsorbed gaseous hydrocarbon is desorbed under a vacuum condition; then, the water which does not contain gas is filled into the device to regulate the temperature and the pressure in the device into normal temperature and normal pressure. A desorbed gas sample is collected and is tested by a gas-phrase color spectrum. The adsorbed hydrocarbon desorption device and the method provided by the present invention can realize the quantitative desorption under a low-temperature condition; consequently, the predicted successful rate of oil and gas exploration is increased, and the present invention can reach the purposes of little investment and high oil and gas exploration rate.
Description
Technical field
The present invention relates to the new technology of oil and gas geochemistry in reconnoitring, particularly relate to a kind of partial extraction apparatus and method that soil adsorbed hydrocarbon is measured that are used for.
Technical background
Hydrocarbon geochemical exploration is a kind ofly to survey the cheapness of descending the hydrocarbon-bearing pool position definitely and exploration means fast by the face of land, belongs to a kind of unconventional method of exploration.Lighter hydrocarbons (CH in the soil
4~ C
4H
10) be of paramount importance index in the hydrocarbon geochemical exploration prediction, also be the important foundation of the indirect index of further research and development simultaneously.
Lighter hydrocarbons in the soil have three kinds of existence forms: the free hydrocarbon in the earth gas, soil adsorbed hydrocarbon and soil occlusion hydrocarbon.Acidolysis hydrocarbon methods analyst be soil occlusion hydrocarbon, its test data is subjected to strong interference because of the variation of carbonate mineral content in the soil, and also can't use in the obsolete area of soil carbon hydrochlorate, its effect and range of application all are subjected to bigger restriction.The test of earth gas free hydrocarbon can overcome these shortcomings.But gather in the process of gaseous sample, the ratio that atmosphere is sneaked into is difficult to but determine that its test result also is subjected to the strong influence of the water saturation and the water table change in depth of weather conditions, soil.Gather the method for free hydrocarbon and also come with some shortcomings by burying artificial adsorbent underground, for example cost is higher, and the engineering time is long, receives the destruction of human and livestock activity easily, and its result also is subjected to the influence of water table change in depth etc.The soil adsorbed hydrocarbon method does not possess the shortcoming of above-mentioned two class methods, and has their advantage, if test condition is suitable, adsorbed hydrocarbons can become more importantly geochemical exploration index.The head space gas method is the method that is most widely used in the adsorbed hydrocarbons test.Its major defect is desorption efficient, if temperature is lower, the gas of deviating under can't condition of stirring seldom, and repeatability is relatively poor; If pyrolysis can take place again in the rising temperature.Though hydrogen stripping technology has realized the stirring under the lower temperature condition, but can only measure the high strength relevant usually and ooze ease unusually with tomography, its reason is that the desorption efficient under the normal pressure (1atm) is lower, and it is unusual to measure the little ease of oozing of low-intensity, thereby has influence on the prediction of hydrocarbon occurrence.
Above-mentioned the analysis showed that, soil adsorbed hydrocarbon are the most important things in the hydrocarbon geochemical exploration work, but the partial extraction device and method of soil adsorbed hydrocarbon exists bigger problem.
Summary of the invention
It is unusual and along tomography upwards migration and form ooze ease unusual soil adsorbed hydrocarbon low-temperature desorption apparatus and method to the purpose of this invention is to provide a kind of little ease of oozing of differentiating oil reservoir top at an easy rate, realize the quantitative desorption under the vacuum and low temperature condition, thereby improve the success rate prediction of hydrocarbon geochemical exploration, reach the purpose of few many oil prospectings of input gas.
The key of soil adsorbed hydrocarbon method of testing is how solid-state pedotheque to be added among the vacuum plant, guarantees also that simultaneously atmosphere can not leak into vacuum plant.For overcoming this difficult point, the invention provides a kind of soil adsorbed hydrocarbon low-temperature desorption apparatus and method.Wherein,
Described soil adsorbed hydrocarbon low-temperature desorption apparatus is made up of condenser pipe 13, flask 17, funnel 19, vacuum pump 12, water-bath 16 and glass pipe 25 and first to the 5th valve 1-5, wherein, condenser pipe 13 is connected with graduated tube 6, vacuum pump 12 by threeway, and described threeway and vacuum pump 12 links are provided with the 5th valve 5; By interpolation pipe threeway 18, condenser pipe 13, flask 17 and glass pipe 25 are connected, glass pipe 25 has four outlets, all be provided with a valve at each endpiece, funnel 19 lower ends are connected with glass pipe 25 by second valve 2, air free water case 7 is connected with glass pipe 25 and the 3rd valve 3 by emulsion tube 21, described graduated tube 6 upper ends are the gas sampling mouth, this thief hatch is tight with plug 10 lids, and condenser pipe 13, flask 17, funnel 19, vacuum pump 12, water-bath 16, glass pipe 25 and air free water case 7 are fixed on the support 24 by fixture.
Soil adsorbed hydrocarbon low-temperature desorption method step of the present invention is as follows:
A, in flask, add the NaOH of 10-30mL10-25%, flask is installed on the device tighten then, guarantee not reveal air;
B, close first valve 1, second valve 2 and the 4th valve 4, open the 3rd valve 3 and the 5th valve 5, connect vacuum pump;
C, when vacuum pump is worked, open first valve 1 gently, when air free water slowly flows to first valve 1, close first valve 1; Open second valve 2 then, when air free water flows to second valve 2, close second valve 2 and the 3rd valve 3; Air in the glass pipe between the valve can be extracted out by these operations;
D, in funnel, add the air free water of 20-50mL, add 15-30g dry screen or wet screening pedotheque then; Stir with glass bar, make it form mud, air come-up liquid level wherein; When vacuum tightness reaches 0.0005atm when following, close the 5th valve 5, open second valve 2;
E, open first valve 1 gently, allow mud flow in the flask; When liquid level arrives second valve 2, close first valve 1;
F, clean funnel with air free water, and repeating step e, up to all pedotheque accesss to plant;
G, open the 3rd valve 3 and first valve 1 successively, make that the sample in the glass tube enters flask, close first valve 1 then;
H, under vacuum condition mud by water-bath heating back boiling, boiling time 5-15 minute, open first valve 1, make pressure go back up to normal pressure; The volume of gas deviate from record, uses the syringe gas bleeding, and inject gas chromatograph is tested.
Wherein, the temperature in the water-bath is 67-72 ℃.The pedotheque particle diameter is the 40-200 order that sieves.Boiling time is 8-10 minute.
Above-mentioned showing, what the soil adsorbed hydrocarbon low-temperature desorption method was used is a kind of special device.At first add the water that does not contain gas, soil is made mud by stirring.Mud is inhaled into described device, can avoid the air access to plant in this process.Adsorptive gaseous hydrocarbon is desorption under vacuum condition, adds the water that does not contain gas subsequently, and the temperature and pressure in the device are transferred to normal temperature and pressure.The gaseous sample that desorption goes out is separated in collection, tests with gas chromatography.
The soil adsorbed hydrocarbon low-temperature desorption method is compared with traditional acidolysis hydrocarbon analytical approach, owing to do not destroy carbonate and clay mineral in the operation, the occlusion hydrocarbon is still stayed in the sample, and soil adsorbed hydrocarbon is measured more effective than the hydro carbons of other existence forms in the soil.Therefore, the data signal to noise ratio (S/N ratio) that is obtained is higher, guaranteed higher desorption rate, background and unusual deviation are bigger in the test result, help oozing unusual and little unusual identification of ease of oozing of escaping, can differentiate oil reservoir top at an easy rate little ooze ease unusual and along tomography upwards migration and form to ooze ease unusual, the unusual and oil field and the tomography of acquisition match.This method is compared with classic method, and is cheap more, quick, is suitable for large-area exploration.
Description of drawings
Fig. 1 is the soil adsorbed hydrocarbon low-temperature desorption apparatus synoptic diagram;
Fig. 2 is second kind of valve synoptic diagram in the soil adsorbed hydrocarbon low-temperature desorption apparatus;
Fig. 3 is the synoptic diagram of the water-bath pot cover among Fig. 1.
Embodiment
Fig. 1-3 is the soil adsorbed hydrocarbon low-temperature desorption apparatus synoptic diagram, this device can be under lower temperature and pressure condition quantitative desorb soil adsorbed hydrocarbon.It is made of condenser pipe 13, flask 17, funnel 19, vacuum pump 12 and water-bath 16.Wherein, condenser pipe 13 is connected with graduated tube 6, vacuum pump 12 by threeway, and described threeway and vacuum pump 12 links are provided with the 5th valve 5; By interpolation pipe threeway 18, condenser pipe 13, flask 17 and glass pipe 25 are connected, glass pipe 25 has four outlets, all is provided with a valve first valve 1, second valve 2, the 3rd valve 3 and the 4th valve 4 at each endpiece; Funnel 19 lower ends are connected with glass pipe 25 by second valve 2, and air free water case 7 is connected with the 3rd valve 3 and glass pipe 25 by emulsion tube 21; Described graduated tube 6 upper ends are the gas sampling mouth, and this thief hatch is tight with plug 10 lids, and condenser pipe 13, flask 17, funnel 19, glass pipe 25 and air free water case 7 are fixed on the support 24 by fixture.The inner, an end inner passage that described threeway 8 is connected with vacuum pump 12 is hydraucone or flat-shaped hydraucone.Described water-bath 16 pot covers are formed by cover plate 28 butt joints of two symmetries.Described first valve 1, second valve 2, the 3rd valve 3, the 4th valve 4 and the 5th valve 5 are ground vacuum valve or the valve that is made of emulsion tube 26 and hemostatic forceps 27.Described interpolation pipe threeway 18 lower ends are by ground and the socket of flask ground, and interpolation pipe threeway 18 upper ends are connected with condenser pipe 13 lower ends by emulsion tube, and its transverse end is connected with glass pipe 25 by emulsion tube.
Its principle of work is at first a certain amount of NaOH to be put into flask 17, so that can reach the purpose of further step-down with the sour gas reaction of deviating from.Drive air (this water is treated, and its solution gas is discharged from) in the glass pipe 25 out of with air free water.Then, be evacuated to below the 0.0001atm.In funnel 19, add the air free water of 40mL and the 20g sample (wet screening or dry screen) that sieves, stir into mud with glass bar, and make bubble floating to the water surface.Open valve, allow mud slowly suck flask 17.Clean funnel 19 with air free water again, and sample is all sucked flask 17.The consumption of air free water will remain unchanged, as is 60mL.Mud in the flask 17 heats under vacuum condition, because the low very fast boiling of pressure, even in the time of 50 ℃, also be like this.When the lighter hydrocarbons of water vapour reconciliation sucking-off enter condenser pipe 13, water vapour will become water and flow back to flask 17, and lighter hydrocarbons can continue to move up, and enter the graduated tube 6 above the condenser pipe 13.Boiling can not make pressure significantly increase, and the stirring of sample is helped desorption, and adsorbed hydrocarbons are played the effect of stripping.After desorb is finished, add air free water and make pressure return to normal pressure, the volume of gas deviate from record, and use the syringe gas bleeding, and inject gas chromatograph is tested.
The soil adsorbed hydrocarbon desorption method, its desorption procedure comprises: (a) with distilled water to going in the water-bath 16 and opening power; When temperature reaches 70 ℃, connect condenser pipe 13 and tap water; In flask 17, add the NaOH of 15mL20%, flask 17 is installed on the device tighten then, guarantee not reveal air; (b) with the tight gas sampling mouth of inorganic plug 10 (as silicon rubber) lid; Close first valve 1, second valve 2 and the 4th valve 4, open the 3rd valve 3 and the 5th valve 5; Connect vacuum pump 12; (c) when vacuum pump 12 is being worked, open first valve 1 gently, when air free water (boiling the chilled saturated aqueous common salt in back) when slowly flowing to first valve 1, is closed first valve 1; Open second valve 2 then, when air free water flows to second valve 2, close second valve 2 and the 3rd valve 3; Air in the glass pipe between the valve 25 can be discharged by these operations; (d) air free water of adding 40mL in funnel adds 20g sieved soil sample (dry screen or wet screening) then; Stir with glass bar, make it form mud, the liquid level that also floats of air wherein; When vacuum tightness reaches 0.0001atm when following, close the 5th valve 5, open second valve 2; (e) open first valve 1 gently, allow mud flow into vacuum plant; When liquid level arrives second valve 2, close first valve 1; (f) clean funnel with air free water, and repetitive operation (e), up to all pedotheque accesss to plant; (g) open the 3rd valve 3 and first valve 1 successively, make that the sample liquid in the glass pipe 25 enters flask 17, close first valve 1 then; (h) mud can seethe with excitement under vacuum condition, when the gas rising of steam reconciliation sucking-off reaches condenser pipe 13, steam can become water and flow back to flask 17, the gas of separating sucking-off can continue to rise, so boiling can not increase intrasystem pressure, on the contrary, boiling has beating action to sample, and adsorbed hydrocarbons are had the stripping effect.The mud boiling was opened first valve 1 after 9 minutes, made pressure go back up to normal pressure; The volume of gas deviate from record, uses the syringe gas bleeding, and inject gas chromatograph is tested.
Above-mentioned desorption process is finished under the low-temp low-pressure condition, does not also have the loss of adsorbed hydrocarbons in the process of sample being inserted vacuum.This technology can be guaranteed higher desorption efficient and can prevent the generation of pyrolysis.Mainly, in the process of sample being inserted vacuum, also can avoid the loss of adsorbed hydrocarbons under low temperature, low pressure condition because desorption process is to carry out.In said method, the addition of bath temperature, desorption time, soil grades, NaOH is important.
The present invention optimizes above-mentioned four factors by experiment, and wherein, the span of NaOH can be 10-30mL, and concentration is 10-25%; Vacuum degree control is below 0.0005atm; Dry screen or wet screening pedotheque are 15-30g, and the pedotheque particle diameter is the 40-200 order that sieves; Boiling time was controlled at 5-15 minute; Controllable Temperature in the water-bath is built in 50～80 ℃.The NaOH of 70 ℃ of its best bath temperatures, 15mL20%, desorption time 9 minutes, washing 200 orders that sieve.
Claims (10)
1, a kind of device that is used for the soil adsorbed hydrocarbon desorption method, it is characterized in that this device comprises condenser pipe, flask, funnel, vacuum pump, water-bath and glass pipe and valve, wherein, condenser pipe is connected with graduated tube, vacuum pump by threeway, and described threeway and vacuum pump link are provided with the 5th valve (5); The interpolation pipe threeway respectively with condenser pipe, flask and glass pipe are connected, glass pipe has four outlets, all be provided with a valve at each endpiece, it is respectively first valve (1), second valve (2), the 3rd valve (3), the 4th valve (4), the funnel lower end is connected with glass pipe by second valve (2), the air free water case is connected with glass pipe by emulsion tube, described glass pipe is connected with the 3rd valve (3), described graduated tube upper end is the gas sampling mouth, this thief hatch is tight with the plug lid, condenser pipe, flask, funnel, glass pipe and air free water case are fixed on the support by fixture.
2, the device that is used for the soil adsorbed hydrocarbon desorption method according to claim 1 is characterized in that the inner of the end inner passage that described threeway is connected with vacuum pump is hydraucone or flat-shaped hydraucone.
3, the device that is used for the soil adsorbed hydrocarbon desorption method according to claim 1 and 2 is characterized in that described water-bath pot cover is formed by the cover plate butt joint of two symmetries.
4, the device that is used for the soil adsorbed hydrocarbon desorption method according to claim 3 is characterized in that described valve is ground vacuum valve or the valve that is made of emulsion tube and hemostatic forceps.
5, according to claim 3 or the 4 described devices that are used for the soil adsorbed hydrocarbon desorption method, it is characterized in that interpolation pipe threeway lower end is by ground and the socket of flask ground, interpolation pipe threeway upper end is connected with the condenser pipe lower end by emulsion tube, and its transverse end is connected with glass pipe by emulsion tube.
6, a kind of soil adsorbed hydrocarbon desorption method, its desorption procedure comprises:
A, in flask, add the NaOH of 10-30mL10-25%, flask is installed to according to claim 1 tighten on the device then, guarantee not reveal air;
B, close first valve (1), second valve (2) and the 4th valve (4), open the 3rd valve (3) and the 5th valve (5), connect vacuum pump;
C, when vacuum pump is worked, open first valve (1) gently, when air free water slowly flows to first valve (1), close first valve (1); Open second valve (2) then, when air free water flows to second valve (2), close second valve (2) and the 3rd valve (3); Air in the glass pipe between the valve can be extracted out by these operations;
D, in funnel, add the air free water of 20-50mL, add 15-30g dry screen or wet screening pedotheque then; Stir with glass bar, make it form mud, the liquid level that also floats of air wherein; When vacuum tightness reaches 0.0005atm when following, close the 5th valve (5), open second valve (2);
E, open first valve (1) gently, allow mud flow in the flask; When liquid level arrives second valve (2), close first valve (1);
F, clean funnel with air free water, and repeating step e, up to all pedotheque accesss to plant;
G, open the 3rd valve (3) and first valve (1) successively, make that the sample in the glass tube enters flask, close first valve (1) then;
H, under vacuum condition, mud is by water-bath heating back boiling, boiling time 5-15 minute, open first valve (1), make pressure go back up to normal pressure; The volume of gas deviate from record, uses the syringe gas bleeding, and inject gas chromatograph is tested.
7, desorption method according to claim 6 is characterized in that the temperature in the water-bath is 50～80 ℃.
8,, it is characterized in that the temperature in the water-bath is 67-72 ℃ according to claim 6 or 7 described desorption methods.
9,, it is characterized in that the pedotheque particle diameter is the 40-200 order that sieves according to claim 6 or 7 described desorption methods.
10, desorption method according to claim 6 is characterized in that boiling time is 8-10 minute.
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| CN101837367A (en) * | 2009-03-17 | 2010-09-22 | Dec股份有限公司 | Operation method of thermal desorption equipment |
| CN106289891A (en) * | 2015-05-18 | 2017-01-04 | 中国辐射防护研究院 | A kind of assay device in polonium auto-deposition source |
| CN106680029B (en) * | 2015-11-11 | 2020-04-17 | 中国石油化工股份有限公司 | Portable vacuum sampling bottle and application method thereof |
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| CN1450349A (en) * | 2002-04-10 | 2003-10-22 | 中国石油天然气总公司石油勘探开发科学研究院 | Quick petroleum hydrocarbon distribution analysis instrument |
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| US5390529A (en) * | 1993-03-19 | 1995-02-21 | Agip S.P.A. | Method for determining heavy hydrocarbons in rock matrices and the apparatus for the purpose |
| RU2102742C1 (en) * | 1995-10-31 | 1998-01-20 | Маковская Нелли Владимировна | Method of gas-chromatography mixture analysis |
| WO1999001739A1 (en) * | 1997-07-03 | 1999-01-14 | Environmental Compliance Consulting, Inc. | Soil sampling for oil and gas exploration |
| CN2479504Y (en) * | 2001-06-08 | 2002-02-27 | 南京化工大学 | Concentration and desorption device of micro hydrocarbon matter in mine atmosphere |
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Owner name: INST OF GEOLOGY AND GEOPHYSICS, CHINESE ACADEMY O Free format text: FORMER OWNER: ZHANG LIUPING Effective date: 20071207 |
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Effective date of registration: 20071207 Address after: Beijing city Chaoyang District Beitucheng West Road No. 19 Patentee after: Institute of Geology and Geophysics, Chinese Academy of Sciences Address before: Floor 8, building 3-902, Chaoyang District North Beach, Beijing Patentee before: Zhang Liuping |
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Assignee: Shanghai Zhongke Mining Co., Ltd. Assignor: Institute of Geology and Geophysics, Chinese Academy of Sciences Contract record no.: 2010210000113 Denomination of invention: Soil adsorbed hydrocarbon low-temperature desorption apparatus and method Granted publication date: 20070404 License type: Exclusive License Open date: 20050914 Record date: 20100706 |