CN113252716A - Method for measuring crystallinity of igneous rock - Google Patents
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- 239000011435 rock Substances 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims abstract description 66
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 77
- 239000010431 corundum Substances 0.000 claims abstract description 77
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 16
- 238000001228 spectrum Methods 0.000 claims abstract description 12
- 238000004364 calculation method Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 27
- 238000012360 testing method Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 23
- 239000002734 clay mineral Substances 0.000 claims description 12
- 150000001875 compounds Chemical class 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- 238000002050 diffraction method Methods 0.000 claims description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000006004 Quartz sand Substances 0.000 description 5
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
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Abstract
The invention discloses a method for measuring crystallinity of igneous rock, and relates to the technical field of petroleum exploration and development. The method is mainly based on an X-ray diffraction analysis technology, an external standard method is applied, a crystallinity calculation model is established by an XRD crystal calculation method on the basis of a full spectrum fitting method and a K value method by means of the advantage that pure corundum has good stability, so that the problem of analysis of the crystallinity of the igneous rock is solved, and quantitative measurement of the crystallinity of the igneous rock is realized.
Description
Technical Field
The invention relates to the technical field of petroleum exploration and development, in particular to a method for measuring crystallinity of igneous rock.
Background
Igneous rock is also called magma rock, a geological term, one of the three major rocks, and refers to a rock formed after cooling of magma (either injected in the earth's crust or melted existing rock).
The two-cascade volcaniclastic lava in the Sichuan basin has excellent storage conditions, good pore development and physical properties, is a high-quality porous reservoir, can form a structural-lithologic composite trap, and has an outburst-spray phase distribution area of 7000km in the region from Jianyang to three regions2The resource amount is large, the source storage is well matched and the storage condition is excellent close to the hydrocarbon generation center of the Hanwu system, and the method becomes a new field for exploration, development, storage increase and production promotion of the Sichuan basin.
Volcanic belongs to the eruption rock class of igneous rock, in order to promote the exploration and development of volcanic oil gas in Sichuan basin, the attack and customs research in igneous rock foundation field needs to be increased, wherein the research on the crystallinity of igneous rock has very important significance for reservoir evaluation, reservoir transformation, well logging explanation, next well location deployment and the like.
Igneous rocks are influenced by factors such as different volcanic eruption types, multi-period eruption, rapid accumulation and the like, the rock component structure is complex, more unstable minerals are contained, the rock crystallinity difference is large, the rock crystallinity difference can be divided into a full-crystalline structure, a cryptocrystalline structure and a glassy structure according to the crystallinity degree of the rock, wherein the glassy structure belongs to an amorphous substance, and in addition, the rock crystallinity analysis is very difficult due to the influence of other amorphous substances such as organic matters and the like. Therefore, an effective igneous rock crystallinity measuring method is urgently needed to be researched to solve the technical problem and provide accurate and scientific technical support for igneous rock oil and gas reservoir exploration and development and basic geological research.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides a method for measuring the crystallinity of igneous rock. The invention aims to provide a igneous rock crystallinity measuring method, which aims to solve the problem of difficulty in analyzing and researching the igneous rock reservoir rock crystallinity and provide accurate and scientific technical support for exploration and development of igneous rock oil and gas reservoirs and basic geological research. The invention is based on the traditional XRD quantitative analysis technology, fully considers the characteristics of crystalline substances and amorphous substances contained in igneous rocks, and accurately measures the crystallinity of the igneous rocks by analyzing and measuring the content of the crystalline substances and the content of the amorphous substances contained in the igneous rocks.
The method is mainly based on an X-ray diffraction analysis technology, an external standard method is applied, a crystallinity calculation model is established by an XRD crystal calculation method on the basis of a full spectrum fitting method and a K value method by means of the advantage that pure corundum has good stability, so that the problem of analysis of the crystallinity of the igneous rock is solved, and quantitative measurement of the crystallinity of the igneous rock is realized.
In order to solve the problems in the prior art, the invention is realized by the following technical scheme:
a method for measuring the crystallinity of igneous rock is characterized by comprising the following steps:
s1, selecting a igneous rock sample, washing oil and drying the rock sample, crushing and grinding the rock sample until the particle size of the rock sample is less than 40 mu m, and fully mixing the rock sample and the oil and the drying;
s2, selecting a part of ground samples in the S1 step to perform X-ray diffraction full spectrum fitting analysis, judging whether diffraction peaks of corundum appear or not, and determining that the original samples do not contain corundum;
s3, selecting a sample partially ground in the step S1 as an analysis sample, and then weighing corundum powder with a certain mass as an external standard;
s4, fully mixing the corundum powder obtained in the step S3 with the igneous rock analysis sample to form a mixture, and calculating the total mass of the mixture;
s5, measuring the relative mass fraction of corundum in the mixture in the step S4 by adopting an X-ray diffraction K value method;
s6, calculating the mass fraction of the crystalline part in the igneous rock according to the relative mass fraction of the corundum obtained in the step S5;
s7, calculating the total mass of the crystalline part of the igneous rock according to the relative mass fraction and mass of the corundum obtained in the S5 step and the mass fraction of the crystalline part of the igneous rock obtained in the S6 step;
s8, calculating the total mass of the amorphous part of the igneous rock according to the total mass of the crystalline part of the igneous rock in the step S7;
and S9, calculating the crystallinity of the igneous rock according to the total mass of the crystalline part and the total mass of the amorphous part of the igneous rock in S7 and S8.
Further, in the step S3, the corundum powder has a total particle size of less than 40 μm and a purity of more than 99.9%.
Further, in the step S3, the quality of the igneous rock analysis sample is selected to beM(ii) a The corundum powder has the mass of
。
In the step S2, the X-ray diffraction full-spectrum fitting method is an X-ray diffraction full-spectrum fitting method in the industry standard SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks.
In the step S5, an X-ray K value method is adopted as a K value method in an industry standard SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks.
In the step S5, the calculation formula of the relative mass fraction of corundum is as follows:
In the step S6, the mass fraction of the crystalline part of igneous rock
Is shown as
The total mass of the igneous rock crystalline fraction in the step S7 is calculated as follows:
in the formula (I), the compound is shown in the specification,
is the total mass of crystalline fractions in igneous rocks in the mixture;
is the mass of corundum in the mixture.
Total mass of amorphous portion of igneous rock in the step S8
It can be expressed as:
in the formula (I), the compound is shown in the specification,
is the quality of igneous rock (crystalline phase + amorphous phase) in the mixture;
is the total mass of the amorphous portion of igneous rock in the mixture;
is the total mass of crystalline fractions in igneous rocks in the mixture;
is the mass of corundum in the mixture;
to test the mass fraction of the amorphous phase of the sample.
Crystallinity of igneous rock in the step S9
It can be expressed as:
compared with the prior art, the beneficial technical effects brought by the invention are as follows:
1. the method has important reference significance for researching the action of the igneous rock, the petrophysical characteristics of the igneous rock reservoir and the like.
2. In the invention, the corundum is specifically selected as an external standard, the X-ray diffraction intensity of the corundum is high, the separation condition of the corundum from the diffraction lines of all components in igneous rock is good, and the influence of the change of external environmental conditions is small. The measurement error can be effectively reduced. Pure corundum powder (alpha-Al)2O3) The separation condition of the peak angle and other substances is good, the crystal structure is stable, the igneous rock does not contain corundum, and the substance can not interfere the experiment due to crystal minerals contained in the sample, and the error of pure corundum powder is smaller than that of pure quartz powder through experimental comparison.
3. In X-ray diffraction phase analysis, an external standard method is an extremely important method, an external standard which is irrelevant to various minerals in igneous rock is introduced, and the relation between each mineral in igneous rock and the quality can be found according to the relation between the diffraction intensity and the quality, so that the method is the key for realizing quantitative analysis of crystalline phase and amorphous phase in igneous rock.
4. The invention provides a method for analyzing by comprehensively using an X-ray diffraction full-spectrum fitting method and a K value method, has higher precision and reliability, can effectively avoid the problem of final result error caused by inaccurate reference standard sample quality, and has more accurate calculated amorphous phase content.
5. The traditional X-ray diffraction method needs to search a diffraction peak of an amorphous substance and a diffraction peak of a crystalline substance, then calculates the relative crystallinity of the rock according to the proportional relation of the diffraction peak areas of the amorphous substance and the crystalline substance, and the diffraction peak of the amorphous substance is easily interfered by the diffraction peak of the crystalline substance and the complex superposition condition exists between the two, so that the determination of the diffraction peak area of the amorphous phase is extremely inaccurate.
Drawings
FIG. 1 is a flow chart of the method for measuring the crystallinity of igneous rock according to the present invention.
Detailed Description
The technical scheme of the invention is further elaborated in the following by combining the drawings in the specification.
Example 1
Referring to the attached fig. 1, this embodiment discloses:
a method for measuring the crystallinity of igneous rock comprises the following steps:
s1, selecting a igneous rock sample, washing oil and drying the rock sample, crushing and grinding the rock sample until the particle size of the rock sample is less than 40 mu m, and fully mixing the rock sample and the oil and the drying;
s2, selecting a part of ground samples in the S1 to perform X-ray diffraction full spectrum fitting analysis, judging whether diffraction peaks of corundum appear or not, and determining that the original samples do not contain corundum;
s3, selecting a partially ground sample in S1 as an analysis sample, and then weighing corundum powder (the whole grain diameter is less than 40 mu m, and the purity is more than 99.9%) with a certain mass as an external standard;
s4, fully mixing the corundum powder obtained in the step S3 with the igneous rock analysis sample to form a mixture, and calculating the total mass of the mixture;
s5, measuring the relative mass fraction of corundum in the mixture in the step S4 by adopting an X-ray diffraction K value method;
s6, calculating the mass fraction of the crystalline part in the igneous rock according to the relative mass fraction of the corundum obtained in the step S5;
s7, calculating the total mass of the crystalline part of the igneous rock according to the relative mass fraction and mass of the corundum obtained in the S5 step and the mass fraction of the crystalline part of the igneous rock obtained in the S6 step;
s8, calculating the total mass of the amorphous part of the igneous rock according to the total mass of the crystalline part of the igneous rock in the step S7;
and S9, calculating the crystallinity of the igneous rock according to the total mass of the crystalline part and the total mass of the amorphous part of the igneous rock in the steps S7 and S8.
Further, in the step S3, the quality of the igneous rock analysis sample is selected to beM(ii) a The corundum powder has the mass of
。
In the step S2, the X-ray diffraction full-spectrum fitting method is an X-ray diffraction full-spectrum fitting method in an industry standard SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks. In the step S5, the X-ray K value method is the K value method in the industry standard SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks.
In the step S5, the calculation formula of the relative mass fraction of corundum is as follows:
in the step S6, the mass fraction of the crystalline part of igneous rock
Is shown as
the total mass of the crystalline fraction of igneous rock in step S7 is calculated as follows:
in the formula (I), the compound is shown in the specification,
is the total mass of crystalline fractions in igneous rocks in the mixture;
is the mass of corundum in the mixture;
total mass of amorphous portion of igneous rock in step S8
It can be expressed as:
in the formula (I), the compound is shown in the specification,
is the quality of igneous rock (crystalline phase + amorphous phase) in the mixture;
is the total mass of the amorphous portion of igneous rock in the mixture;
is the total mass of crystalline fractions in igneous rocks in the mixture;
is the mass of corundum in the mixture;W amor to test the mass fraction of the amorphous phase of the sample.
Crystallinity of igneous rock in step S9D crystal It can be expressed as:
example 2
As another preferred embodiment of the present invention, this example was conducted by using corundum and quartz sand powders as comparative experiments. The specific process is as follows:
weighing a proper amount of analytically pure corundum and analytically pure quartz sand powder, grinding the analytically pure corundum and analytically pure quartz sand powder, fully mixing the powder to meet experimental requirements, respectively placing the powder in two glass slides, performing spectrogram test by using an XRD method, calculating by using a peak height method or a diffraction integral intensity method, and comparing the difference between the actually weighed mass fraction and the mass fraction of a spectrogram test result to judge the XRD method test error in a multiphase system.
Table 1 analytical error table for mixed sample of pure corundum and quartz.
From table 1 above, the test error for analyzing pure quartz is: 3.76 percent; the test error of analytical pure corundum is: 1.76 percent.
The specific experimental procedures and results are as follows:
experimental principle error:
weighing a proper amount of analytically pure corundum and analytically pure quartz sand powder, grinding the analytically pure corundum and analytically pure quartz sand powder, fully mixing the powder to meet experimental requirements, respectively placing the powder in two glass slides, performing spectrogram test by using an XRD method, calculating by using a peak height method or a diffraction integral intensity method, and comparing the difference between the actual weighed mass fraction and the mass fraction of a spectrogram test result so as to judge the XRD method test error in a multiphase system.
Table 2 analytical error table for mixed sample of pure corundum and quartz.
From the above table 2, the test error for analyzing pure quartz is: 3.76 percent; the test error of analytical pure corundum is: 1.76 percent. Both errors meet the quality requirements of SY/T5163-.
And (3) calculating the crystallinity:
the experimental thought is as follows: adding a proper amount of analytical pure corundum into a sample, measuring the mass percentage of the crystalline substance in the mixed sample, comparing the mass percentage measured by the corundum with the actual weighed mass when the corundum is added to obtain the total mass of the crystalline substance in the sample, and subtracting the total mass of the crystalline substance from the original mass to obtain the total mass of the amorphous substance.
Because the actual mass and the test mass fraction of the corundum are known, the ratio of the actual mass to the test mass fraction of the crystalline substance in the test sample is the ratio of the actual mass to the test mass fraction of the crystalline substance. The test mass fraction of the crystalline substance can be calculated according to the test mass fraction of the corundum, the actual mass of the crystalline substance can be calculated, the total mass of the amorphous phase can be calculated according to the total mass of the test sample, and the crystallinity is finally obtained, wherein the calculation formula is deduced as follows, and the result is shown in table 3;
in the formula:
X corundum is the mass fraction of corundum,%;
I corundum is the integrated intensity of diffraction peaks of corundum;
K corundum is the reference intensity of corundum;
m is the total mass of the test sample, g;
M corundum to analyze the mass of a pure corundum sample, g;
M crystal to test the total mass of the crystalline part of the sample, g;
M amor to test the total mass of the amorphous part of the sample, g;
D crystal for test sample crystallinity,%;
table 3N 230 well and TF2 well amorphous phase content calculation results table.
Claims (10)
1. A method for measuring the crystallinity of igneous rock is characterized by comprising the following steps: the method comprises the following steps:
s1, selecting a igneous rock sample, washing oil and drying the rock sample, crushing and grinding the rock sample until the particle size of the rock sample is less than 40 mu m, and fully mixing the rock sample and the oil and the drying;
s2, selecting a part of ground samples in the S1 step to perform X-ray diffraction full spectrum fitting analysis, judging whether diffraction peaks of corundum appear or not, and determining that the original samples do not contain corundum;
s3, selecting a sample partially ground in the step S1 as an analysis sample, and then weighing corundum powder with a certain mass as an external standard;
s4, fully mixing the corundum powder obtained in the step S3 with the igneous rock analysis sample to form a mixture, and calculating the total mass of the mixture;
s5, measuring the relative mass fraction of corundum in the mixture in the step S4 by adopting an X-ray diffraction K value method;
s6, calculating the mass fraction of the crystalline part in the igneous rock according to the relative mass fraction of the corundum obtained in the step S5;
s7, calculating the total mass of the crystalline part of the igneous rock according to the relative mass fraction and mass of the corundum obtained in the S5 step and the mass fraction of the crystalline part of the igneous rock obtained in the S6 step;
s8, calculating the total mass of the amorphous part of the igneous rock according to the total mass of the crystalline part of the igneous rock in the step S7;
and S9, calculating the crystallinity of the igneous rock according to the total mass of the crystalline part and the total mass of the amorphous part of the igneous rock in S7 and S8.
2. A igneous rock crystallinity measuring method as defined in claim 1, wherein: in the step S3, the total grain diameter of the corundum powder is less than 40 μm, and the purity is more than 99.9%.
3. A method of measuring crystallinity of igneous rock as claimed in claim 1 or 2, wherein: in the step S3, the quality of the selected igneous rock analysis sample isM(ii) a The corundum powder has the mass of
。
4. A method of measuring crystallinity of igneous rock as defined in claim 1 or 2, wherein: in the step S2, the X-ray diffraction full-spectrum fitting method is an X-ray diffraction full-spectrum fitting method in the industry standard SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks.
5. The method of measuring crystallinity of igneous rock as defined in claim 4, wherein: in the step S5, an X-ray K value method is adopted as a K value method in an industry standard SY/T5163-2018X-ray diffraction analysis method for clay minerals and common non-clay minerals in sedimentary rocks.
6. A igneous rock crystallinity measuring method as defined in claim 3, wherein: in the step S5, the calculation formula of the relative mass fraction of corundum is as follows:
7. A process as claimed in claim 6A method for measuring the crystallinity of igneous rock is characterized by comprising the following steps: in the step S6, the mass fraction of the crystalline part of igneous rock
Is shown as
8. A igneous rock crystallinity measuring method as defined in claim 7, wherein: the total mass of the igneous rock crystalline fraction in the step S7 is calculated as follows:
in the formula (I), the compound is shown in the specification,
is the total mass of crystalline fractions in igneous rocks in the mixture;
is the mass of corundum in the mixture.
9. A igneous rock crystallinity measuring method as defined in claim 8, wherein: what is needed isThe total mass of the amorphous portion of igneous rock in the step S8
It can be expressed as:
in the formula (I), the compound is shown in the specification,
is the quality of igneous rock (crystalline phase + amorphous phase) in the mixture;
is the total mass of the amorphous portion of igneous rock in the mixture;
is the total mass of crystalline fractions in igneous rocks in the mixture;
is the mass of corundum in the mixture;
to test the mass fraction of the amorphous phase of the sample.
10. A igneous rock crystallinity measuring method as defined in claim 9, wherein: crystallinity of igneous rock in the step S9
Expressed as:
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| Title |
|---|
| 伍月等: "X射线粉晶衍射基体清洗法在矿物定量分析中的应用", 《地质与资源》 * |
| 吕海波 等: "广西红黏土矿物成分分析", 《工程地质学报》 * |
| 黄清明等: "复合材料结晶度的测定", 《山东陶瓷》 * |
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| CN113252716B (en) | 2023-02-24 |
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