CN104849427A - Determination method for content of organic carbon in mud shale strata series - Google Patents

Determination method for content of organic carbon in mud shale strata series Download PDF

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CN104849427A
CN104849427A CN 201510204490 CN201510204490A CN104849427A CN 104849427 A CN104849427 A CN 104849427A CN 201510204490 CN201510204490 CN 201510204490 CN 201510204490 A CN201510204490 A CN 201510204490A CN 104849427 A CN104849427 A CN 104849427A
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organic carbon
oil
solvent
step
result
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CN 201510204490
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邹才能
侯连华
罗霞
赵忠英
杨智
林森虎
吴松涛
张丽君
张昕
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中国石油天然气股份有限公司
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Abstract

The invention provides a determination method for the content of organic carbon in a mud shale strata series. The method comprises the following steps: preparing a to-be-determined mud-shale core sample; weighing a part of the to-be-determined mud shale core and carrying out primary organic carbon analysis; cleaning oil on the rest of the to-be-determined mud shale core with a solvent capable of cleaning organic matters; weighing a part of oil-cleaned mud shale core, carrying out secondary organic carbon analysis, and comparing the result of the secondary organic carbon analysis with the result of the primary organic carbon analysis, wherein the result of the secondary organic carbon analysis is taken as a final determined value if the result is within an error range, or oil cleaning treatment with a multi-component solvent is carried out if the result is beyond the error range; and weighing a part of mud shale core having undergone oil cleaning with the multi-component solvent, then carrying out tertiary organic carbon analysis, and comparing the result of the tertiary organic carbon analysis with the result of the secondary organic carbon analysis, wherein the content of the organic carbon determined by the secondary organic carbon analysis is taken as the final determined value and the oil-cleaning solvent for the area is determined to be the solvent capable of cleaning the organic matters if the result is within the error range, or if the result is beyond the error range, the oil-cleaning solvent is the multi-component solvent, the result of the tertiary organic carbon analysis is taken as the final value of organic carbon and the oil-cleaning solvent for the area is determined to be the multi-component solvent.

Description

一种泥页岩层系有机碳含量的测定方法 Determination of a content of organic carbon-based mud shale

技术领域 FIELD

[0001] 本发明涉及石油勘探技术领域,特别涉及一种泥页岩层系有机碳含量的测定方法。 [0001] The present invention relates to a technical field of oil exploration, particularly relates to a method for measuring a content of organic carbon-based mud shale.

背景技术 Background technique

[0002] 大型体积压裂技术的成功应用,不仅使非生油层系但极为致密的储层中原油得以成功地进行商业开发,2013年,中国鄂尔多斯盆地致密储层原油产量超过了2000万吨;美国致密储层原油产量达到了9700万吨。 [0002] The successful application of large volume fracturing technology, not only the non-oil-based raw but extremely dense reservoir of crude oil to the successful commercial development, in 2013, tight reservoirs in the Ordos Basin crude oil production in China exceeded 20 million tons; American tight reservoir crude oil production reached 97 million tons. 大型体积压裂技术的成功应用,同样也使储集于烃源岩层系中的原油得以商业开发变为可能,如美国Eagle ford页岩油的成功开发就得益于工厂化的大型体积压裂技术。 Successful application of large volume fracturing technology also makes reservoirs in source rock in the oil-based commercial exploitation is made possible, such as the American Eagle ford successful development of shale oil to benefit from a large volume fracturing factory technology. 世界上常规石油资源量约为4878亿吨,页岩油的资源量达到470亿吨,勘探开发的潜力很大。 The world's conventional oil resources of about 487.8 billion tons, oil shale resources of 470 million tons, great potential for exploration and development.

[0003] 有机碳含量通常是指岩石中含有机碳元素的含量,是烃源岩层系有机质评价的重要指标,常用于评价烃源岩层系有机质丰度高低,因此,也常作为计算油气资源的重要参数。 [0003] The organic carbon content generally refers to rock content containing elemental carbon, is an important indicator organic evaluate source rock-based, used to evaluate source rocks based organic abundance level, therefore, often as computing gas resources Important parameters. 通常按GB/T19145-2003标准进行岩石中总有机碳含量分析,方法原理是用稀盐酸去除样品中的无机碳后,在高温氧气流中燃烧,使总有机碳转化为二氧化碳,经红外检测器检测并给出总有机碳的含量。 After the rock is generally carried out by analyzing total organic carbon content GB / T19145-2003 standard, principle of the method is the removal of inorganic carbon in the sample with dilute hydrochloric acid, in a high temperature stream of oxygen combustion, the total organic carbon to carbon dioxide by infrared detector detecting and gives total organic carbon. 烃源岩中有机碳包括三个部分,干酪根、液态有机物及气态烃,而在常规分析有机碳过程中,在岩样粉碎和酸处理时,已使气态烃和部分液态有机质散失掉,因此,对烃源岩而言,总有机碳包括两个部分,一是岩石中还未演化成油的干酪根中有机碳含量,二是液态有机质(包括干酪根已生成的原油但仍滞留于岩石中未排出和原始液态有机质)中有机碳的含量。 Organic carbon source rock consists of three parts, kerogen, organic liquid and gaseous hydrocarbons, and organic carbon analysis in the conventional process, when the rock sample grinding and acid treatment has partially liquid hydrocarbons and gaseous organic dissipated, so , source rocks, the TOC comprising two parts, one has not evolved rock kerogen in the oil content of organic carbon, the second is a liquid organic matter (kerogen including crude oil generated in the rock but still retained and discharging liquid are not the original organic matter) content of organic carbon. 虽该方法中测得的有机碳既不代表岩石中原始有机碳含量,也不代表岩石中固态的干酪根中有机碳含量。 Although the method of organic carbon measured do not represent the original organic carbon content in the rock, it does not mean solid rock kerogen in the organic carbon content. 但该方法拟定的背景是针对常规石油聚集而制定的,常规石油聚集背景是烃源岩与储集层常常不是同一层位,原油从烃源岩中排出至储集岩中聚集通常需要一定的运移距离,能用其它方法清楚辨别烃源岩与储集层。 However, the method proposed is the background for conventional petroleum accumulations enacted, conventional oil accumulation BACKGROUND source rock and reservoir are often not, the crude oil is discharged from the source rocks same layer to the reservoir rock aggregate usually requires some migration distance, other methods can clearly identify the source rock and reservoir. 因此,只需要测定烃源岩中有机碳含量,在同一条件下有机碳含量的高低代表烃源岩中有机质丰度的高低;储集层则为非生油层,不需要进行有机碳分析。 Therefore, only the measurement of organic carbon source rock content, the level of rock under the same conditions in organic abundance hydrocarbon source level represents an organic carbon content; non-biomass was reservoir oil, and organic carbon analysis is not required. 而在泥页岩层系中,烃源岩与储集岩常常共生,岩性大多为混合的中间岩性,如粉砂质泥岩或白云质泥岩,泥质粉砂岩或泥质白云岩等,在肉眼或显微镜下进行岩石定名有一定难度,烃源岩与储层常常分辨不清,储层也可能具有一定生烃能力,而烃源岩在一定条件下也可能成为储层。 In the mud shale lines, source rock and reservoir rock is often symbiotic, lithology mostly intermediate mixed lithologies, such as silty or dolomitic shale, shale or argillaceous dolomite, etc., for the naked eye or under a microscope has some difficulties named rock, source rocks often confusion and reservoir, the reservoir may also have certain hydrocarbon capacity, and source rocks, under certain conditions may become reservoirs. 在这种情况下,岩石中液态有机质对总有机碳贡献大小对该地区烃源岩评价、原油资源量计算均具有较大的影响。 In this case, the liquid rock evaluate the contribution of organic matter in the area of ​​total organic carbon source rock, crude oil resource calculation have a greater impact. 若岩石中液态有机质贡献远远大于干酪根的贡献,则岩石可能主要作为储集层,若液态有机质贡献远远小于干酪根的贡献,则岩石可能主要作为烃源层,若液态有机质和干酪根的贡献均占有一定比例,则在岩石中可能有页岩油聚集。 If the rock is much larger than the contribution of organic matter in the liquid kerogen contribution, the rock may be used as the main reservoir, when the organic liquid contribution is far less than the contribution of kerogen, may be mainly used as the hydrocarbon source rock layer, if the organic liquid kerogen and the contribution is a certain proportion of the rock shale oil may have gathered.

[0004] 基于上述分析可知,目前对于有机碳测定的方法主要是基于常规石油聚集背景制定的,这些方法仅适用于常规石油勘探评价。 [0004] Based on the above analysis, the determination of organic carbon present method is mainly based on conventional petroleum accumulations BACKGROUND developed, these methods are only applicable to the evaluation of conventional oil exploration. 然而,由于液态有机质对总有机碳贡献的部分不能有效地区分开,从而不适合于可以作为储层的泥页岩层系的有机碳测定与有机质丰度评价。 However, since the organic part of the liquid can not be separated effectively contribute TOC area, so as not suitable for the determination of organic carbon and organic matter can be evaluated as an abundance of clay shale reservoir system.

[0005] 针对上述问题,目前尚未提出可以适应于泥页岩层系有机碳含量的测定方法。 [0005] In view of the above problems, it has not yet proposed method can be adapted to determination of organic carbon content in shale-based mud.

发明内容 SUMMARY

[0006] 本发明的一个目的在于提供一种泥页岩层系有机碳含量的测定方法。 [0006] An object of the present invention to provide a method for measuring a content of organic carbon-based mud shale. 该方法至少能够解决相关技术中无法区分液态有机质和干酪根中有机碳含量而导致的无法准确识别与评价泥页岩层系有机质丰度的技术问题。 This method can solve at least the problems in the related art technology can not distinguish between liquid organic and organic carbon kerogen result of evaluation of the mud can not be accurately identify page-based organic abundance formation.

[0007] 为达上述目的,一方面,本发明提供了一种泥页岩层系有机碳含量的测定方法,所述方法包括: [0007] To achieve the above object, in one aspect, the present invention provides a method for measuring a content of organic carbon-based mud shale, the method comprising:

[0008] (I)制作待测岩心样品; [0008] (I) Production of core samples to be tested;

[0009] (2)取部分待测岩心进行第一次有机碳分析; [0009] (2) A portion of the core for the first test and organic carbon analysis;

[0010] (3)剩余待测岩心用能洗净吸附于岩石中的有机质的溶剂洗净油; [0010] (3) The remaining core can be measured by washing the organic matter adsorbed on the rock oil cleaning solvent;

[0011] (4)取部分步骤(3)洗净油后的岩心进行第二次有机碳分析,结果与步骤(2)的第一次有机碳分析结果进行对比,如果结果在误差范围内,则该结果即为有机碳含量最终测定值;如果结果超出误差范围,则继续步骤(5)的洗净油处理; [0011] (4) A portion of step (3) after washing the oil core a second organic carbon analysis, the first organic carbon analysis result of step (2) comparison of the results, if the results in the error range, the organic carbon content in the final result is the value measured; if the result is out of tolerance range, proceed to step (5) washing the oil-treated;

[0012] (5)如果步骤⑷和步骤(2)的结果超出误差范围,则用能洗出岩石晶格中有机质的多元溶剂进行洗净油处理; [0012] (5) If the result of step ⑷ step (2) exceeds the error range, it can be washed with an organic polyol solvent in the crystal lattice of the rock is cleaned oil treatment;

[0013] (6)取部分步骤(5)洗净油后的岩心进行第三次有机碳分析,结果与步骤(4)的第二次有机碳分析结果进行对比,如果结果在误差范围内,则步骤(4)中测定有机碳含量为最终测定值,并确定该地区的洗净油溶剂为步骤(3)的所述能洗净吸附于岩石中的有机质的溶剂;如果结果超出误差范围,则洗油溶剂为步骤(5)的所述能洗出岩石晶格中有机质的多元溶剂,第三次检测的结果为最终有机碳值,并确定该地区的洗净油溶剂为步骤(5)的所述能洗出岩石晶格中有机质的多元溶剂。 [0013] (6) A portion of step (5) after washing the core oil third organic carbon analysis, the result of step (4) a second organic carbon analysis results are compared, if the result in the error range, the step (4) the organic carbon content of the final measurement value, and determines an oil solvent washing step of the region (3) washing the organic solvent can be adsorbed on the rock; if the result is out of tolerance, the step of washing the oil solvent (5) can be washed out of the polyhydric organic solvent in the crystal lattice of the rock, the detection results of the third organic carbon as a final value, and determines an oil solvent washing step of the area (5) wash out the polyhydric solvent can rock crystal lattice organic matter.

[0014] 一般来说,由于不同地区泥页岩层系岩石成分差异大,孔隙结构差异大,因此,对液态有机质吸附能力差异也很大,不能用固定溶剂洗油,对尚未进行该项分析工作的地区来说,首先需要选择适合研宄地区的洗油溶剂。 [0014] In general, due to the large different regions based mud shale rock composition differences, differences in the structure of large pores, and therefore, the adsorption capacity of organic liquid also a great difference, fixed oil can not wash solvents, the analysis has not been speaking area, we first need to select the appropriate wash oil solvent in a Subsidiary area. 一般来说,优先选用极性弱的溶剂将岩心样品洗净如三氯甲烷或二氯甲烷,极性越强的溶剂,对人体危害和环境污染越大。 In general, the preferred core would weakly polar solvent such as chloroform or methylene chloride wash sample, the more polar solvent, greater harm to human body and environmental pollution. 具体地,将剩余待测岩心样品(5〜1g)用滤纸包裹,放于抽提容器中,为保证充分洗净油,每个抽提容器最多装10个样品,用洗油溶剂对岩心样品进行循环淋滤,直至检测滤出溶剂中荧光级别小于3级,证明洗油完毕,样品经自然烘干后,在烘箱中低于100°C继续烘干,供测定总有机碳时用。 Specifically, the remaining core samples tested (5~1g) wrapped with filter paper, placed in the extraction vessel, washed in order to ensure adequate oil, each extracted sample containers up to 10, with a solvent wash oil core samples leaching is circulated, the solvent was filtered off until it detects the fluorescence level is less than level 3, wash oil proof is completed, the sample was naturally dried, below 100 ° C in an oven to continue drying for measuring total organic carbon using.

[0015] 根据本发明所述的测定方法,其中步骤(3)所述的能洗净吸附于岩石中的有机质的溶剂可以为本领域常规的溶剂;其中本发明优选采用的是极性在3-5的不溶于水的溶剂;其中更进一步优选为二氯甲烷或三氯甲烷。 [0015] The measuring method according to the present invention, wherein in step (3) can be adsorbed on the rock washed organic solvent may be the conventional solvent-based art; preferably wherein the present invention uses a polarity 3 water-insoluble solvent -5; wherein further preferably dichloromethane or trichloromethane.

[0016] 根据本发明所述的测定方法,其中洗净油的标准可以参照现有技术标准,本发明优选的是洗油后溶剂荧光减弱至荧光3级以下。 [0016] The measuring method according to the present invention, wherein a standard reference oil may wash prior art standards, the present invention is preferably a solvent decrease in fluorescence to the fluorescence after wash oil grade 3 or less.

[0017] 根据本发明所述的测定方法,其中步骤(5)的所述能洗出岩石晶格中有机质的多元溶剂极性为3-7。 [0017] The measuring method according to the present invention, wherein said step (5) can be washed out of the polyhydric organic solvent polarity rock lattice is 3-7.

[0018] 其中更优选所述多元溶剂易溶于水。 [0018] More preferably wherein said polyol solvent is soluble in water.

[0019] 根据本发明所述的测定方法,其中优选步骤(5)的多元溶剂为至少三种溶剂的混入口O [0019] The measuring method according to the present invention, preferably wherein the step (5) is a polyhydric solvent mixed solvent of at least three inlet O

[0020] 根据本发明所述的测定方法,其中更优选步骤(5)的多元溶剂为苯、甲醇和丙酮的混合。 [0020] The measuring method according to the present invention, wherein the polyol solvent is more preferably in step (5) is mixed benzene, methanol and acetone.

[0021] 根据本发明所述的测定方法,其中更优选所述苯、甲醇和丙酮的体积比为50-70 ;25-15 ;25-15。 [0021] The measuring method according to the present invention, wherein said benzene and more preferably, methanol and acetone in a volume ratio of 50-70; 25-15; 25-15.

[0022] 根据本发明所述的测定方法,所述洗净油处理是按SYT 5118-2005中7.2方法进行。 [0022] The measuring method according to the present invention, the cleaning process is carried out in oil in 7.2 Method SYT 5118-2005.

[0023] 根据本发明任意一项所述的测定方法,步骤(I)是按照GB/T19145-2003标准制作待测岩心样品。 [0023] The measurement method according to any one of the present invention, the step (I) is to produce a core sample to be tested according to GB / T19145-2003 standard.

[0024] 根据本发明任意一项所述的测定方法,步骤(2)、(4)和(6)的有机碳分析是按照GB/T19145-2003标准进行分析。 [0024] The measurement method according to any one of the present invention, the organic carbon analysis step (2), (4) and (6) is analyzed in accordance with GB / T19145-2003 standard.

[0025] 根据本发明任意一项所述的测定方法,步骤(4)和(6)的结果比对和误差是按照GB/T19145-2003 标准执行。 [0025] The measuring method according to the present invention, the results of step (4) and (6) and the alignment error is performed according to GB / T19145-2003 standard.

[0026] 在本发明一个实施方式中,洗净油后的岩心样品取出部分按GB/T19145-2003标准进行总有机碳分析。 [0026] In one embodiment of the present invention, the core samples taken after washing the oil part TOC analysis by GB / T19145-2003 standard. 分析结果与未洗油总有机碳进行对比分析,若误差在GB/T19145-2003标准范围内,则样品中液态有机质含量极低,可以按GB/T19145-2003标准直接进行岩石样品总有机碳含量分析测定。 Unwashed oil analysis results were analyzed TOC, if the error in the GB / T19145-2003 standard range, the liquid sample is very low organic matter content, total organic carbon content can be performed directly by the rock samples GB / T19145-2003 standard analysis. 若误差很大,则样品中液态有机质含量高,需分别进行洗油前后有机碳测定。 If the error is large, the sample liquid high organic matter content, for an organic carbon was measured before and after the wash oil, respectively. 为确保所选溶剂能完全洗净油,建议在一个没有分析数据的研宄地区先进行几个不同岩性样品的试验,对洗油溶剂的筛选按权利I要求进行,选择在误差范围内的极性小的溶剂进行洗油。 To ensure that the selected solvent is completely cleaned of oil, it recommended study based on analysis of the data area without a prior test for several different rock samples, screening solvent wash oil as claimed in claim I for accommodation within an error range small polar solvent wash oil.

[0027] 根据本发明任意一项所述的测定方法,所述泥页岩层系是含原油的(原油储层发育在其中的泥页岩层系),岩性包括含有有机质的页岩及不含有机质的其它岩石。 [0027] According to the present invention, any one of the measuring method, the system is mud shale (oil shale reservoir development system in which the mud) containing crude oil, including lithological and free of organic matter in shales other rock organic matter.

[0028] 综上所述,本发明提供了一种泥页岩层系有机碳含量的测定方法。 [0028] In summary, the present invention provides a method for measuring a content of organic carbon-based mud shale. 即将岩石中游离的烃类与岩石本身所含有的有机碳分别测定的方法。 The method of rock coming free of organic carbon and hydrocarbons contained in the rocks themselves were measured. 本发明的测定方法解决了现有技术中无法准确确定含油的过渡岩性如泥质砂岩或砂质泥岩中有机碳含量。 Method of the present invention solves the transition can not be accurately determined lithology of oil carbon content as the prior art sandy shales or shaly sands organic. 从而导致的页岩油资源量无法准确评价的技术问题,达到了有效确定页岩固态有机碳和液态有机碳含量,为准确计算页岩油资源量提供可靠依据。 Thereby resulting oil shale resources can not be an accurate assessment of technical problems and achieve the efficient determination of organic carbon shale solid and liquid organic carbon content, provide a reliable basis for accurate calculation of the amount of oil shale resources.

附图说明 BRIEF DESCRIPTION

[0029] 图1是根据本发明实施例1的一种泥页岩层系有机碳含量的测定方法的流程图; [0029] FIG. 1 is a flowchart of a method of determining one of mud-based shale organic carbon content in accordance with an embodiment of the present invention;

[0030] 图2是根据本发明实施例1的确定岩石样品可以应用三氯甲烷溶剂洗油后测定有机碳值的结果分析图; [0030] FIG. 2 is an embodiment of the present invention determines rock sample analysis results of Example 1 may FIG organic carbon values ​​measured after application of wash oil chloroform solvent;

[0031] 图3是根据本发明实施例1的在泥页岩层系中夹的薄层储层洗油前后的有机碳值的结果分析图; [0031] FIG. 3 is a result of the analysis of organic carbon values ​​before and after a thin layer of an oil reservoir in the mud washing shale clip system 1 of the embodiment according to the present embodiment of the invention;

[0032] 图4是根据本发明实施例1的确定岩石样品可以应用多元溶剂洗油后测定有机碳值的结果分析图。 [0032] FIG. 4 is an embodiment of the present invention determines the rock sample can be applied in Example 1 the analysis results of FIG polyhydric solvent of organic carbon values ​​measured after wash oil.

具体实施方式 detailed description

[0033] 以下通过具体实施例详细说明本发明的实施过程和产生的有益效果,旨在帮助阅读者更好地理解本发明的实质和特点,不作为对本案可实施范围的限定。 [0033] Example embodiments described below in detail by way of specific embodiment of the process of the present invention and advantageous effects produced, is intended to aid the reader in better understanding of the nature and features of the present invention is not intended to limit the scope of the instant case.

[0034] 实施例1 [0034] Example 1

[0035] 如图1所示,包括以下步骤: [0035] As shown in FIG 1, comprising the steps of:

[0036] 步骤SlOl:取30块新鲜岩心样品,每个样品按GB/T 19145-2003碎样,碎至粒径小于0.2mm的,碎好的样品量约在20克左右,碎好的样品按四等分法分成2份; [0036] Step SlOl: fresh core samples taken 30, each sample according to GB / T 19145-2003 broken sample, crushed to a particle size of less than 0.2mm, crushed in a good sample of about 20 grams, broken good sample They were divided into four quarters by two parts;

[0037] 步骤S102:其中一份待测岩心按国家标准GB/T19145-2003进行有机碳分析,记录下样品的第一次有机碳分析值; [0037] the step S102: A test core wherein organic carbon analysis of the national standard GB / T19145-2003, the recording time of the organic carbon analysis of the sample values;

[0038] 步骤S103:另一份待测样品应用三氯甲烷按SYT 5118-2005中7.2方法进行,洗净油,洗净油的标准是洗油溶剂荧光弱至荧光3组以下; [0038] Step S103: chloroform another test sample application by SYT 5118-2005 7.2 methods, standard washing oil, wash oil are washed oil solvent to the weak fluorescent phosphor 3 groups;

[0039] 步骤S104:洗净油后岩心按四等分法分成2份,其中一份按国家标准GB/T19145-2003进行第二次有机碳分析,记录样品第二次有机碳分析结果。 [0039] Step S104: after the wash oil were divided into four quarters by the core parts 2, wherein one national standard GB / T19145-2003 a second organic carbon analysis, the second recording and organic carbon analysis results of the samples.

[0040] 步骤S105:与第一次测定值对比,如果两次测定值的误差在GB/T 19145-2003要求的误差范围内则说明该样品不需洗油可以直接测定样品总有机碳含量;反之,则应用剩下的另一份样品用“三元溶剂”即苯、甲醇和丙酮的混合溶剂,苯、甲醇和丙酮的比例为70:15:15洗净油,洗净油的标准如步骤S103。 [0040] Step S105: the first measurement value and the comparison, if the measured value is twice the error within an error range GB / T 19145-2003 requirements it indicates that the oil sample can be measured directly without washing the sample TOC; On the contrary, the rest of the application with another sample "ternary solvent" i.e., the ratio of benzene, a mixed solvent of methanol and acetone, benzene, methanol and acetone washed to 70:15:15 oil, wash oil, such as standard step S103.

[0041] 步骤S106:洗净油后岩心按四等分法分成2份,其中一份按国家标准GB/T19145-2003进行第三次有机碳分析,并与第二次有机碳测定值对比,如果两次测定值的误差在GB/T 19145-2003要求的误差范围内确定该种类型样品洗油溶剂为三氯甲烷,反之为“三元溶剂”,洗油后测定有机碳值为最终测定值。 [0041] Step S106: after the wash oil were divided into four quarters by the core parts 2, wherein one national standard GB / T19145-2003 third organic carbon analysis, and compared with the measured value of the second organic carbon, If the error type of the sample measured values ​​within an error range is determined twice GB / T 19145-2003 claim wash oil solvent is chloroform, and vice versa for "ternary solvent", after washing the oil is final assay organic carbon value.

[0042] 通过本实施方式的上述方法对准噶尔盆地吉木萨尔凹陷芦草沟组吉174井泥页岩层段有机碳含量进行了测定。 [0042] The organic carbon content of clay shale interval well Lucaogou guitar 174 by the above method of the present embodiment of the depressions were measured Jimusaer Junggar Basin.

[0043] 具体地,选取了吉174井泥页岩层系的29块岩心样品,按GB/T19145-2003标准制作了待测岩心样品。 [0043] Specifically, a core sample 29 selected guitar 174 wells shale clay-based, according to GB / T19145-2003 standard test core sample was produced. 首先按GB/T19145-2003标准测定了30块样品的有机碳值(泥质粉砂岩值为3.73%,黑色泥岩值为6.71% ),然后应用三氯甲烷进行洗净油;洗净油后按GB/T19145-2003标准进行第二次有机碳分析(泥质粉砂岩值为0.20%,黑色泥岩值为6.49%,泥质粉砂岩两次测定值误差为3.53%,与误差允许值0.64%差异大,黑色泥岩两次测定值误差为0.22%,与误差允许值1.24%差异小),统计发现,第二次测定结果与第一次测定结果进行对比,其中有6块样品的两次结果差值能够满足GB/T19145-2003标准要求的误差范围,如图2所示,该6块样品是较好的烃源岩,有机碳含量较高,平均有机质含量可达7.10%,而且其中液态有机质含量有限,洗油前后有机碳含量值差别不大,该类样品直接按GB/T19145-2003标准进行有机碳含量测定即可。 First, according to GB / T19145-2003 standard assay of organic carbon values ​​of 30 samples (argillaceous value of 3.73%, 6.71% black mudstone value), then the application is cleaned oil chloroform; washed oil press GB / T19145-2003 second standard organic carbon analysis (argillaceous value of 0.20%, 6.49% is black mudstone, argillaceous two measurement error is 3.53%, with 0.64% error tolerance differences large, black mudstone two measurement error of 0.22%, 1.24% and less error tolerance differences), statistics showed that the second measurement result and the comparison result of the first measurement, the results of which difference between the two samples 6 value can satisfy the error range GB / T19145-2003 requirements of the standard, FIG. 2, the sample 6 is preferred source rocks, high organic carbon content, organic matter content of up to 7.10% on average, and wherein the liquid organic limited content, carbon content before and after washing the organic oil is not very different, such samples were GB / T19145-2003 standard organic carbon content can be measured directly. 图3所示的14块样品按GB/T19145-2003标准进有机碳含量测定的结果显示为较好的烃源岩,有机碳含量平均为2.65%,但经过三氯甲烷洗净油后,在测定的有机碳含量值明显下降,每个样品的有机碳含量值均降低到烃源岩界限(0.5%)以下,该类样品在泥页岩层系中应作为储集岩,在烃源岩评价的过程中应该被剔除。 14 samples shown in FIG. 3 by GB / T19145-2003 standard in the organic carbon content measured results are shown as the preferred source rocks, organic carbon content of 2.65% on average, but after chloroform wash oil, in organic carbon content value measured decreased, the organic carbon content of each sample was reduced to limit source rocks (0.5%) or less, such samples in the mud system should be as shale reservoir rock, source rocks evaluation the process should be removed. 图4所示的9块样品的第二次用三氯甲烷进行洗净油后测定的有机碳值(典型值为2.15% )与第一次按GB/T19145-2003标准测定的值(典型值为3.07% )差别较大,误差为0.92%,不能满足GB/T19145-2003标准要求的误差范围,因此对样品进行了“三元溶剂”继续洗净油,洗净油后的样品进行第三次有机碳测定(典型值为2.09% ),第三次与第二次有机碳测定的误差值0.07%,能够满足GB/T19145-2003标准要求的误差范围。 Organic carbon value (typically 2.15%) 4 9 samples shown in the second measurement after washing the oil with chloroform and the first value (typically a value measured by GB / T19145-2003 standard 3.07%) vary greatly, 0.92% error, the error range can not meet the GB / T19145-2003 standards, so the samples were "ternary solvent" continue clean oil, the oil sample after washing third organic carbon measuring times (typically 2.09%), the third error value of 0.07% was measured with a second organic carbon, can satisfy the error range GB / T19145-2003 standard requirements. 该9块样品是一般的径源岩,有机碳含量较低,平均有机碳含量为1.55%,其中液态有机质含量较高,洗油前后有机碳含量值差别较大,该类样品需要首先进行三氯甲烷洗净油,然后按GB/T19145-2003标准进行有机碳含量测定。 9 The diameter of the sample is a general source rock, lower total organic carbon, organic carbon content of an average 1.55%, wherein the high liquid content of organic matter, organic carbon content before and after washing the oil values ​​vary greatly, three such samples need to be washed oil methyl chloride, and then press GB / T19145-2003 standard organic carbon content was measured.

[0044] 本发明解决了现有技术中无法准确确定富含油的过渡岩性如泥质砂岩或砂质泥岩中有机碳含量。 [0044] The present invention solves the prior art can not determine the exact transition lithology oil rich organic carbon content, such as sandy shales or shaly sands. 从而导致的页岩油资源量无法准确评价的技术问题,达到了有效确定页岩固态有机碳和液态有机碳含量,为准确计算页岩油资源量提供可靠依据。 Thereby resulting oil shale resources can not be an accurate assessment of technical problems and achieve the efficient determination of organic carbon shale solid and liquid organic carbon content, provide a reliable basis for accurate calculation of the amount of oil shale resources.

[0045] 可以理解的是,以上描述的一种泥页岩层系有机碳含量的测定方法也可以应用于常规油气聚集地区的泥页岩层系。 [0045] It will be appreciated that the method for measuring a content of organic carbon-based mud shale described above may also be applied to conventional oil-based mud shale accumulation region. 但是,考虑到洗油后测定岩石总有机碳的成本增加,且烃源岩与储集层能显而易见地分开,再者洗油溶剂对人体有一定的危害,对环境造成一定的污染,在洗油过程中更需要重视安全等因素,常规油气聚集区泥岩总有机碳测定不必要进行洗油分析。 However, considering the cost of the measurement of total organic carbon rock wash oil increases, and the source rock and reservoir can be apparent separated, wash oil solvent addition on the human body were damaged, cause some environmental pollution, wash oil process requires more emphasis on safety and other factors, conventional oil and gas gathering area measuring total organic carbon mudstone were unnecessary wash oil analysis. 而当原油储层发育在泥页岩层系时,烃源岩与储层常常分辨不清,洗油前后有机碳对比分析则使它们的区别一目了然,且对烃源岩评价和资源量计算更趋客观和真实。 When the reservoir development in oil-based mud shales, source rocks and reservoir often confusion, comparative organic carbon analysis of the oil before and after washing to make clear the difference between them, and the evaluation of Rocks and become more source computing resource objective and true. 因此,本实施方式所提供的方法优选地适用于原油储层发育于泥页岩层系中,解决了现有技术中无法有效确定烃源岩中固态有机碳含量的难题。 Thus, the method according to the present embodiment is preferably applied to provide oil shale reservoir development in the mud system, it solves the prior art can not effectively determine the source rocks solid organic carbon content of the problem.

Claims (10)

  1. 1.一种泥页岩层系有机碳含量的测定方法,其特征在于,所述方法包括: (1)制作待测岩心样品; (2)取部分待测岩心进行第一次有机碳分析; (3)剩余待测岩心用能洗净吸附于岩石中的有机质的溶剂洗净油; (4)取部分步骤(3)洗净油后的岩心进行第二次有机碳分析,结果与步骤(2)的第一次有机碳分析结果进行对比,如果结果在误差范围内,则该结果即为有机碳含量最终测定值;如果结果超出误差范围,则继续步骤(5)的洗净油处理; (5)如果步骤⑷和步骤(2)的结果超出误差范围,则用能洗出岩石晶格中有机质的多元溶剂进行洗净油处理; (6)取部分步骤(5)洗净油后的岩心进行第三次有机碳分析,结果与步骤(4)的第二次有机碳分析结果进行对比,如果结果在误差范围内,则步骤(4)中测定有机碳含量为最终测定值,并确定该地区的洗净油溶剂为步骤(3)的所述能洗 1. A method of determining the organic carbon content of the shale-based mud, characterized in that the method comprises: (1) Production of core samples to be tested; (2) A portion of the core to be tested for the first organic carbon analysis; ( 3) the remaining core can be measured by washing the organic matter adsorbed on the rock oil cleaning solvent; (4) a portion of step (3) after washing the oil core organic carbon analysis of the second, the result of step (2 ) and organic carbon analysis of the first results of comparison, if the result is within an error range, then the organic carbon content in the final result is the value measured; if the result is out of tolerance range, proceed to step (5) of the washing process oil; ( after the core (6) a portion of step (5) washing oil; 5) if the result of step ⑷ step (2) exceeds the error range, can be washed with an organic polyol solvent in the crystal lattice of the rock is cleaned oil treatment third organic carbon analysis, the result of step (4) of the second comparison organic carbon analysis results, if the results are within an error range, then in step (4) Determination of content of organic carbon in the final measurement value, and determining the the oil solvent washing step of the region (3) can be washed 吸附于岩石中的有机质的溶剂;如果结果超出误差范围,则洗油溶剂为步骤(5)的所述能洗出岩石晶格中有机质的多元溶剂,第三次检测的结果为最终有机碳值,并确定该地区的洗净油溶剂为所述多元溶剂。 Organic matter adsorbed in the rock of the solvent; if the result is out of tolerance, then the step of washing the oil solvent (5) can be washed out of the polyhydric organic solvent in the crystal lattice of the rock, the detection results of the third organic carbon values ​​of the final and an oil solvent wash to determine the area of ​​the polyhydric solvent.
  2. 2.根据权利要求1所述的测定方法,其特征在于,所述洗净油处理过程按SYT5118-2005 中7.2 方法进行。 2. The measuring method according to claim 1, wherein the oil cleaning process performed in 7.2 SYT5118-2005 method.
  3. 3.根据权利要求1或2所述的测定方法,其特征在于,步骤(I)是按照GB/T19145-2003标准制作待测岩心样品。 3. The assay method according to claim 12, wherein step (I) is to produce a core sample to be tested according to GB / T19145-2003 standard.
  4. 4.根据权利要求1或2所述的测定方法,其特征在于,步骤(2)、(4)和(6)的有机碳分析是按照GB/T19145-2003标准进行分析。 The measurement method of claim 1 or claim 2, wherein the organic carbon analysis step (2), (4) and (6) is analyzed in accordance with GB / T19145-2003 standard.
  5. 5.根据权利要求1或2所述的测定方法,其特征在于,步骤(4)和(6)的结果比对和误差是按照GB/T19145-2003标准执行。 The measuring method according to claim 1, wherein (4) and the result of step (6) and the alignment error is performed according to GB / T19145-2003 standard.
  6. 6.根据权利要求1或2所述的测定方法,其特征在于,所述泥页岩层系是含原油的、岩性包括含有有机质的页岩及不含有机质的其它岩石。 The measurement method of claim 1 or claim 2, wherein said lines containing clay shale oil, lithologies including shales containing organic matter and other rock-free organic matter.
  7. 7.根据权利要求1或2所述的测定方法,其特征在于,步骤(3)所述能洗净吸附于岩石中的有机质的溶剂为极性在3-5的不溶于水的溶剂。 The measurement method of claim 1 or claim 2, wherein the step (3) can be washed with the organic solvent adsorbed in the rock to the water-insoluble polar solvent 3-5.
  8. 8.根据权利要求7所述的测定方法,其特征在于,步骤(3)所述能洗净吸附于岩石中的有机质的溶剂为二氯甲烷或三氯甲烷。 8. A measuring method according to claim 7, wherein the step (3) can be adsorbed on the rock washing organic solvent is dichloromethane or trichloromethane.
  9. 9.根据权利要求1或2所述的测定方法,其特征在于,步骤(5)所述多元溶剂极性为3-7,优选所述多元溶剂易溶于水。 9. The assay method according to claim 1, wherein the step (5) said polar solvent is polyvalent 3-7, the polyhydric solvent is preferably soluble in water.
  10. 10.根据权利要求9所述的测定方法,其特征在于,步骤(5)所述多元溶剂为至少三种溶剂的混合;优选所述多元溶剂为苯、甲醇和丙酮的混合;更优选所述苯、甲醇和丙酮的体积比为50-70 ;25-15 ;25-15。 10. The measuring method according to claim 9, wherein the step (5) the polyol solvent is a mixed solvent of at least three; preferably the solvent is a polyol mixture of benzene, methanol and acetone; more preferably the benzene, methanol and acetone volume ratio of 50-70; 25-15; 25-15.
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