CN100573144C - Acidolysis hydrocarbon reference material - Google Patents
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- CN100573144C CN100573144C CNB2007100628769A CN200710062876A CN100573144C CN 100573144 C CN100573144 C CN 100573144C CN B2007100628769 A CNB2007100628769 A CN B2007100628769A CN 200710062876 A CN200710062876 A CN 200710062876A CN 100573144 C CN100573144 C CN 100573144C
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Abstract
Acidolysis hydrocarbon reference material disclosed by the invention belongs to the technical field of measuring transmission of quantity value, in order to satisfy present eager needs to acidolysis hydrocarbon reference material, proposition is used for the acidolysis hydrocarbon reference material with accurate definite value of geochemical analysis test, it has less than 40 purpose uniform particle sizes, the acidolysis hydrocarbon content is in the scope of 8.97～280.9 μ l/kg, be by taking from basin, Hefei sieve collection block, depression Xiakou, Jiyang block, the soil of Jiyang depression buttress stone bridge block or Tongxu, basin, Zhoukou City block is smart broken, grind, mixing is made, analyze through a cover analytical approach, carry out many families cooperation definite value simultaneously, adopt the series of standards rule to provide optimum value and uncertainty at last.Standard substance of the present invention makes many can't dealing with problems at present obtain solution as material standard, has filled up the development blank of domestic and international acidolysis hydrocarbon standard model.
Description
Technical field
The present invention relates to the technical field of metrology and measurement standard transmission of quantity value, more particularly, the present invention relates to a kind of all kinds of geochemical analyses test that is used for, can be used as that oil and gas geochemistry is reconnoitred, the standard substance during the acidolysis hydrocarbon is measured in the soil investigation, environmental surveys.
Background technology
Acidolysis hydrocarbon method is one of method the most frequently used in the oil and gas geochemical exploration.The ultimate principle of this method is by decompression, heating and chemical treatment means such as (adding acid), after existing hydro carbons (based on the occlusion hydrocarbon) in pedotheque carbonate mineral lattice and the cementing matter thereof to isolate the tax, utilize gas chromatograph that its content is analyzed again.Long-term exploration practices explanation, acidolysis hydrocarbon method good stability has obtained to use widely in hydrocarbon geochemical exploration.
For standard is carried out in the application to each hydrocarbon geochemical exploration method of comprising the acidolysis hydrocarbon, successively worked out and issued and implemented " oil and gas geochemistry exploration technique standard and rules ", " oil and gas geochemistry exploration technique standard ", " petroleum gas face of land geochemical exploration sample analyzing method " and a series of hydrocarbon geochemical exploration industry standards such as " hydrocarbon geochemical exploration sample assay methods " from 1987, this is basic premise and guarantee that acidolysis hydrocarbon method is able to widespread use.
" hydrocarbon geochemical exploration sample assay method part 1: the acidolysis hydrocarbon is measured vapor-phase chromatography " made specified in more detail from aspects such as specimen preparation, specimen preparation, determination step, result's calculating and precision to acidolysis hydrocarbon samples test process.Some other standard then retrains the application process of each hydrocarbon geochemical exploration method of comprising the acidolysis hydrocarbon.In specific survey district, different exploration main bodys adopt above-mentioned standard can successfully implement acidolysis hydrocarbon method surveying work, but these literal standards have just been carried out standard from the mensuration and the application point of method itself, do not consider different exploration main bodys, different regions acidolysis hydrocarbon standardization of data problem.And the practice of long-term hydrocarbon geochemical exploration, different exploration main bodys have obtained a large amount of acidolysis hydrocarbon data in the survey district of different geologic backgrounds.Owing to do not develop acidolysis hydrocarbon standard model as yet so far, make acidolysis hydrocarbon method some occur and be difficult to deal with problems, the main performance in the following areas: the data that (1) different regions are obtained are difficult to contrast, are unfavorable for large tracts of land one-tenth figure; (2) be difficult to suspicious data is arbitrated, be difficult to measurement result is monitored; (3) owing to there is not acidolysis hydrocarbon reference material to can be used as reference, be difficult to each exploration different measuring instrument that main body adopted is accurately demarcated; (4) can't comprehensive assessment with estimate the measuring method that different exploration main bodys are adopted.
At present, the domestic precedent of still not developing acidolysis hydrocarbon standard model does not see that abroad the development of such standard model reports that the development work of acidolysis hydrocarbon standard model is in space state yet.The acidolysis hydrocarbon data that this situation causes the different exploration of hydrocarbon geochemical exploration industry main body, different exploratory area to obtain are difficult to contrast, can't accurately demarcate the different measuring instrument, are difficult to measurement result is monitored.This also is unfavorable for standard hydrocarbon geochemical exploration market object not only bad for the development of oil and gas geochemical exploration technique itself.And domestic some other industry has all been developed standard substance separately as environmental protection industry, nuclear industry, aerospace, geology mining industry, metallurgical industry, commerce and hygiene department etc., has developed up to ten thousand country-level standard substances.
At above-mentioned condition, for ease of acidolysis hydrocarbon measurement result in the hydrocarbon geochemical exploration of different regions is compared, surveying instrument is accurately demarcated, measurement result is monitored, provide foundation for standard hydrocarbon geochemical exploration object market access condition and race condition simultaneously, need a kind of acidolysis hydrocarbon reference material of research in a hurry.
Summary of the invention
The present invention proposes the acidolysis hydrocarbon reference material with accurate definite value in order to satisfy present eager needs to acidolysis hydrocarbon reference material.
Concrete technical scheme is as follows.
The acidolysis hydrocarbon reference material that is used for the geochemical analysis test that the present invention proposes, have less than 40 purpose uniform particle sizes, the acidolysis hydrocarbon content has definite value accurately, the acidolysis hydrocarbon content is 8.97 μ l/kg, 51.6 μ l/kg, 111.7 μ l/kg or 280.9 μ l/kg, uncertainty is respectively ± 0.34 μ l/kg, ± 3.0 μ l/kg, ± 10.6 μ l/kg and ± 11.5 μ l/kg use the soil of basin, Hefei sieve collection block respectively, the mixed soil of basin, Hefei sieve collection block and Tongxu, basin, Zhoukou City block, the soil of the soil of Tongxu, basin, Zhoukou City block and depression Xiakou, Jiyang block is made.
When described acidolysis hydrocarbon reference material was made with the soil of basin, Hefei sieve collection block, the acidolysis hydrocarbon content was 8.97 μ l/kg, and uncertainty is ± 0.34 μ l/kg.
When described acidolysis hydrocarbon reference material was made with the mixed soil of basin, Hefei sieve collection block and Tongxu, basin, Zhoukou City block, the acidolysis hydrocarbon content was 51.6 μ l/kg, and uncertainty is ± 3.0 μ l/kg.
When described acidolysis hydrocarbon reference material was made with the soil of Tongxu, basin, Zhoukou City block, the acidolysis hydrocarbon content was 111.7 μ l/kg, and uncertainty is ± 10.6 μ l/kg.
When described acidolysis hydrocarbon reference material was made with the soil of depression Xiakou, Jiyang block, the acidolysis hydrocarbon content was 280.9 μ l/kg, and uncertainty is ± 11.5 μ l/kg.
Because the uncertainty in the unevenness of sample, the analysis to measure process, Stability of Substance or the like many-sided reason, the analysis data that all may cause inconsistent, the purpose that provides hydrocarbon geochemical exploration standard sample uncertainty is, when analyzing data within the data variation scope that given standard value and uncertainty are formed the time, think that then analyzing data is reliably, otherwise think that then the analysis data are unreliable.
Described acidolysis hydrocarbon reference material is made by following steps:
(1) coarse crushing: under the condition of natural air drying or artificial draft, the soil natural of gathering is dried; Drying the back is broken to below 20 orders with the hardwood hammering;
(2) in small, broken bits: that soil further is crushed to below 40 orders;
(3) mixing: whole soil heap awls in small, broken bits are mixed after 5 times, move in the cylindrical mixed model machine of diameter 1m, degree of depth 1m, move 8～12h continuously, carry out the homogeneity initial survey, treat the qualified back discharging of homogeneity in the upper, middle and lower, the left and right sampling that mix model machine;
(4) packing: the soil of mixing is divided in polyethylene bottle, Clear glass bottles and jars or the Brown Glass Brown glass bottles and jars only.
There is family more than 60 in domestic unit and the troop that is engaged in hydrocarbon geochemical exploration, obtains a large amount of hydrocarbon geochemical exploration data in China.Owing to there is not standard model, cause each tame data to compare, whether data correctly also can't arbitrate.The constituent parts data differ bigger, at double in addition tens times ground poor.
Whether standard substance has accurately that definite value is an index of the most important thing of research standard material, is whether a standard substance can obtain the prerequisite that everybody generally acknowledges, is the basis of metering transmission of quantity value.In order to make acidolysis hydrocarbon reference material of the present invention have definite value accurately, the following definite value of preferred described acidolysis hydrocarbon reference material: adopt electronic balance to take by weighing sample 50.0g ± 0.2g, place sealing in the ground flask, receive on the degas system, be evacuated to-0.1MPa～-0.05MPa, continue to take out 5min; The ground flask that sample will be housed then places 40 ℃ water-bath to heat, and slowly dripping hydrochloric acid solution outgases, after reacting completely, and balance 20 minutes; Change under the condition that is no more than 2 ℃ in room temperature, slowly extract the gas of deviating from, analyze with gas chromatograph with glass syringe; Adopt chromatographic peak retention index, retention time, experiment to carry out qualitative to deviating from gas with the qualitative, quantitative calibrating gas; The component concentration computing formula is carried out quantitative Analysis to deviating from gas in employing response factor computing formula, the sample.
The present invention at first processes processing by the pedotheque to specified particle size, prepares the pedotheque that meets the development of acidolysis hydrocarbon standard model; Adopt the degassing, analysis and calculation procedure that acidolysis hydrocarbon standard model is carried out definite value again.Adopt method of analysis of variance, mean value consistency-checking method that the homogeneity and the stability of acidolysis hydrocarbon standard sample concentration value are tested.Adopt the industry standard assay method, select a plurality of by the qualified hydrocarbon geochemical exploration project analysis laboratory of national China Metrology Accreditation, to the acidolysis hydrocarbon standard model definite value of cooperating.Utilizing Grubbs method, Rod Dixon method, normal distribution statistics, Cochran rule etc. that the acidolysis hydrocarbon that is obtained is measured numerical value adds up, calculates and handle, according to standard sample definite value principle, finally determine the optimum value and the uncertainty of acidolysis hydrocarbon standard model content.
The granularity of acidolysis hydrocarbon reference material of the present invention has the greatest impact to the definite value analysis result, and the fine fraction sample is obviously higher than the acidolysis hydrocarbon methane content of coarse fraction sample, and performance is particularly outstanding in the low content sample; This is relevant with the easier adsorbs hydrocarbons material of fine fraction sample.And fine fraction sample analysis result's stability is relatively poor relatively.Therefore granularity is controlled at below 40 orders is in demand in the present invention, otherwise, different people uses this standard substance to analyze this standard substance, yet the carbonate content of standard substance has different results in different analyses, thereby can not reach the purpose of transmission of quantity value.The present invention is limited to granularity can guarantee below 40 orders that people obtain stable result in use, thereby can proofread and correct oneself analytical instrument or method according to standard substance of the present invention institute specified value, reaches the purpose of transmission of quantity value.
The inventor discovers that the content of low content acidolysis hydrocarbon standard sample also changes with the variation of granularity, sample weighting amount, and at first the acidolysis hydrocarbon methane content of 25 gram sample weighting amounts, 80 purpose samples is apparently higher than other samples, and content is comparatively stable; The acidolysis hydrocarbon methane content of 50 gram sample weighting amounts, 40 purpose samples is starkly lower than other samples, and content is also comparatively stable; And the methane content amplitude of variation of the acidolysis hydrocarbon samples of the acidolysis hydrocarbon samples of 25 gram sample weighting amounts, 40 purpose samples and 50 gram sample weighting amounts, 80 purpose samples is bigger.
Granularity 80 purpose sample methane contents obviously increase than granularity 40 purpose sample methane contents, and 80 purpose samples are along with the increase of sample methane content, and error becomes big in the analysis.Analyzing reason is owing to fine-graded part in the sample has bigger specific surface area, easier adsorbs hydrocarbons material, and in the more coarsely graded relatively sample, more be quartz particles, it is less to be rich in hydrocarbons.So acidolysis hydrocarbon standard model is advisable to be processed into 40 orders.Sample weighting amount is not obvious to the analysis result influence.
The inventor also studies the influence of temperature of reaction.The rising temperature of reaction, slightly influential to the not obviously influence of the acidolysis hydrocarbon standard model of lower content for the analysis of the acidolysis hydrocarbon standard model of high-load, show as analysis result and slightly reduce.When finding that after deliberation temperature of reaction is 60 ℃, exist: (1) amount of gas evolved is bigger than normal; (2) analysis is dangerous increases (because the bath temperature height reacts acutely, absorption tube is awfully hot, and with the crack sound in the Pi); (3) sample easily is bonded at easy cleaning not on the flask walls of degassing usefulness, has reduced efficient.So acidolysis hydrocarbon analytical test temperature of reaction is chosen as 40 ℃.
Also determined the save set of acidolysis hydrocarbon standard model among the present invention simultaneously.By selecting wrappage such as polyethylene bottle, Clear glass bottles and jars, Brown Glass Brown glass bottles and jars only to compare test, through after the preservation of one-year age, the analyzing test data of various save sets does not have significant change, from the angle of transportation and long preservation, more preferably polyethylene bottle is as the save set of acidolysis hydrocarbon standard standard substance.
Utilize acidolysis hydrocarbon reference material, can accurately demarcate acidolysis hydrocarbon surveying instrument; The measuring method of comprehensive assessment and evaluation acidolysis hydrocarbon samples; Transmit the hydrocarbon geochemical exploration industry and respectively explore the test value of main body acidolysis hydrocarbon, be convenient to the data that difference exploration main body obtains are compared, make large tracts of land become figure to become possibility; Be convenient to suspicious data is arbitrated.
Acidolysis hydrocarbon reference material is the necessary complement of hydrocarbon geochemical exploration rules and standard as material standard, with the effect of literal standard in combination, is expected further to improve the confidence level of hydrocarbon geochemical exploration data, promotes the hydrocarbon geochemical exploration subject energetically and develops healthy and orderlyly.
Acidolysis hydrocarbon system row standard model succeed in developing the research blank of not only having filled up acidolysis hydrocarbon reference material field in China's hydrocarbon geochemical exploration, and make China's acidolysis hydrocarbon reference material development work reach international most advanced level.
Embodiment
Embodiment 1
Select basin, Hefei sieve collection block, gather the near surface pedotheque, sampling quantity is 200kg, sampling depth 1.5～1.8m.Sample is prepared the pedotheque that meets acidolysis hydrocarbon standard sample test needs through operations such as fragmentation, grinding, mixings.The sample of preparing proves its homogeneity and has good stability through variance analysis method (F method of inspection) and mean value consistency-checking method (T method of inspection) check.
Relevant regulations according to " hydrocarbon geochemical exploration sample assay method part 1: acidolysis hydrocarbon mensuration---vapor-phase chromatography (SY/T6009.1-2003) " are analyzed the acidolysis hydrocarbon samples.Get 40 order sample 50g, slowly splash into concentration and be 1: 6 dilute hydrochloric acid solution, react under 40 ℃ of temperature, when no longer bubble occurring, balance 20 minutes is gathered gas air feed analysis of hplc, determines the content value of acidolysis hydrocarbon samples.Simultaneously, select a plurality ofly, carried out the cooperation definite value by the qualified hydrocarbon geochemical exploration project analysis laboratory of national China Metrology Accreditation; Utilize test results such as Grubbs method, Rod Dixon method, normal distribution statistics, Cochran rule to carry out statistics, calculate and handled, determine that finally the optimum value of acidolysis hydrocarbon standard model content is 8.97 μ l/kg, uncertainty is ± 0.34 μ l/kg.
Embodiment 2
Respectively gather near surface pedotheque 100kg at basin, Hefei sieve collection block and Tongxu, basin, Zhoukou City block, total sampling quantity is 200kg, and sampling depth is 1.5～1.8m.Sample is prepared the pedotheque that meets acidolysis hydrocarbon standard sample test needs through operations such as fragmentation, grinding, mixings.The sample of preparing proves its homogeneity and has good stability through variance analysis method (F method of inspection) and mean value consistency-checking method (T method of inspection) check.
Relevant regulations according to " hydrocarbon geochemical exploration sample assay method part 1: acidolysis hydrocarbon mensuration---vapor-phase chromatography (SY/T6009.1-2003) " are analyzed the acidolysis hydrocarbon samples.Get 40 order sample 50g, slowly splash into concentration and be 1: 6 dilute hydrochloric acid solution, react under 40 ℃ of temperature, when no longer bubble occurring, balance 20 minutes is gathered gas air feed analysis of hplc, determines the content value of acidolysis hydrocarbon samples.Simultaneously, select a plurality ofly, carried out the cooperation definite value by the qualified hydrocarbon geochemical exploration project analysis laboratory of national China Metrology Accreditation; Utilize Grubbs method, Rod Dixon method, normal distribution statistics, Cochran rule etc. that test result has been carried out statistics, calculates and handled, the optimum value of final acidolysis hydrocarbon standard model content is 51.6 μ l/kg, and uncertainty is ± 3.0 μ l/kg.
Embodiment 3
Gather near surface pedotheque 200kg at Tongxu, basin, Zhoukou City block, sampling depth is 1.5～1.8m.Sample is prepared the pedotheque that meets acidolysis hydrocarbon standard sample test needs through operations such as fragmentation, grinding, mixings.The sample of preparing proves its homogeneity and has good stability through variance analysis method (F method of inspection) and mean value consistency-checking method (T method of inspection) check.
Relevant regulations according to " hydrocarbon geochemical exploration sample assay method part 1: acidolysis hydrocarbon mensuration---vapor-phase chromatography (SY/T6009.1-2003) " are analyzed the acidolysis hydrocarbon samples.Get 40 order sample 50g, slowly splash into concentration and be 1: 6 dilute hydrochloric acid solution, react under 40 ℃ of temperature, when no longer bubble occurring, balance 20 minutes is gathered gas air feed analysis of hplc, determines the content value of acidolysis hydrocarbon samples.Simultaneously, select a plurality ofly, carried out the cooperation definite value by the qualified hydrocarbon geochemical exploration project analysis laboratory of national China Metrology Accreditation; Utilize Grubbs method, Rod Dixon method, normal distribution statistics, Cochran rule etc. that test result has been carried out statistics, calculates and handled, the optimum value of final acidolysis hydrocarbon standard model content is 111.7 μ l/kg, and uncertainty is ± 10.6 μ l/kg.
Embodiment 4
Block is gathered near surface pedotheque 200kg in depression Xiakou, Jiyang, and sampling depth is 1.5～1.8m.Sample is prepared the pedotheque that meets acidolysis hydrocarbon standard sample test needs through operations such as fragmentation, grinding, mixings.The sample of preparing proves its homogeneity and has good stability through variance analysis method (F method of inspection) and mean value consistency-checking method (T method of inspection) check.
Relevant regulations according to " hydrocarbon geochemical exploration sample assay method part 1: acidolysis hydrocarbon mensuration---vapor-phase chromatography (SY/T6009.1-2003) " are analyzed the acidolysis hydrocarbon samples.Get 40 order sample 50g, slowly splash into concentration and be 1: 6 dilute hydrochloric acid solution, react under 40 ℃ of temperature, when no longer bubble occurring, balance 20 minutes is gathered gas air feed analysis of hplc, determines the content value of acidolysis hydrocarbon samples.Simultaneously, select a plurality ofly, carried out the cooperation definite value by the qualified hydrocarbon geochemical exploration project analysis laboratory of national China Metrology Accreditation; Utilize Grubbs method, Rod Dixon method, normal distribution statistics, Cochran rule etc. that test result has been carried out statistics, calculates and handled, the optimum value of final acidolysis hydrocarbon standard model content is 280.9 μ l/kg, and uncertainty is ± 11.5 μ l/kg.
Claims (1)
1. one kind is used for the acidolysis hydrocarbon reference material that geochemical analysis is tested, it is characterized in that, described acidolysis hydrocarbon reference material has less than 40 purpose granularities, the acidolysis hydrocarbon content has definite value accurately, the acidolysis hydrocarbon content is 8.97 μ l/kg, 51.6 μ l/kg, 111.7 μ l/kg or 280.9 μ l/kg, uncertainty is respectively ± 0.34 μ l/kg, ± 3.0 μ l/kg, ± 10.6 μ l/kg and ± 11.5 μ l/kg use the soil of basin, Hefei sieve collection block respectively, the mixed soil of basin, Hefei sieve collection block and Tongxu, basin, Zhoukou City block, the soil of the soil of Tongxu, basin, Zhoukou City block and depression Xiakou, Jiyang block is made;
Described acidolysis hydrocarbon reference material is made by following steps:
(1) coarse crushing: under the condition of natural air drying or artificial draft, the soil natural of gathering is dried; Drying the back is broken to below 20 orders with the hardwood hammering;
(2) in small, broken bits: that soil further is crushed to below 40 orders;
(3) mixing: whole soil heap awls in small, broken bits are mixed after 5 times, move in the cylindrical mixed model machine of diameter 1m, degree of depth 1m, move 8～12h continuously, carry out the homogeneity initial survey, treat the qualified back discharging of homogeneity in the upper, middle and lower, the left and right sampling that mix model machine;
(4) packing: the soil of mixing is divided in polyethylene bottle, Clear glass bottles and jars or the Brown Glass Brown glass bottles and jars only;
The following definite value of described acidolysis hydrocarbon reference material: adopt electronic balance to take by weighing sample 50.0g ± 0.2g, place sealing in the ground flask, receive on the degas system, be evacuated to-0.1MPa～-0.05MPa, continue to take out 5min; The ground flask that sample will be housed then places 40 ℃ water-bath to heat, and slowly dripping hydrochloric acid solution outgases, after reacting completely, and balance 20 minutes; Change under the condition that is no more than 2 ℃ in room temperature, slowly extract the gas of deviating from, analyze with gas chromatograph with glass syringe; Adopt chromatographic peak retention index, retention time, experiment to carry out qualitative to deviating from gas with the qualitative, quantitative calibrating gas; The component concentration computing formula is carried out quantitative Analysis to deviating from gas in employing response factor computing formula, the sample.
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| CN101907613B (en) * | 2010-06-04 | 2012-10-17 | 中国科学院广州地球化学研究所 | Acid-hydrolyzable hydrocarbon preparation device and acid-hydrolyzable hydrocarbon measuring method by using same |
| CN104075926B (en) * | 2014-07-24 | 2018-03-06 | 云南健牛生物科技有限公司 | A kind of preparation method and application using soil as benzo [a] pyrene detection standard sample of matrix |
| CN110389056A (en) * | 2018-04-18 | 2019-10-29 | 中国石油化工股份有限公司 | A kind of production method of oil-contaminated soil sample |
| CN110736800A (en) * | 2019-11-07 | 2020-01-31 | 济南海关技术中心 | pentachlorophenol standard sample in soil and preparation method thereof |
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Non-Patent Citations (4)
| Title |
|---|
| 中国主要含油气盆地区域地球化学场参数特征及其成因研究. 汤玉平等.石油勘探与开发，第28卷第3期. 2001 |
| 中国主要含油气盆地区域地球化学场参数特征及其成因研究. 汤玉平等.石油勘探与开发，第28卷第3期. 2001 * |
| 酸解烃技术在油气勘探中的应用. 缪九军等.物 探 与 化 探，第29卷第3期. 2005 |
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