CN114428094A - Analysis method and application of rock core mineral composition - Google Patents
Analysis method and application of rock core mineral composition Download PDFInfo
- Publication number
- CN114428094A CN114428094A CN202011022580.6A CN202011022580A CN114428094A CN 114428094 A CN114428094 A CN 114428094A CN 202011022580 A CN202011022580 A CN 202011022580A CN 114428094 A CN114428094 A CN 114428094A
- Authority
- CN
- China
- Prior art keywords
- rock core
- analysis
- detection
- core
- mineral
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/616—Specific applications or type of materials earth materials
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses an analysis method and application of a rock core mineral composition. The analysis method comprises the following steps: step A, establishing analysis test conditions based on X-ray fluorescence analysis; b, selecting an element analysis method suitable for the rock core, and detecting the rock core to be detected; and step C, obtaining element composition information of the rock core and calculating according to a mathematical model to obtain the mineral composition of the rock core. The method can quickly identify the composition and the type of minerals in the rock core, and can quickly identify the lithology and the minerals on the premise of not losing a rock core sample.
Description
Technical Field
The invention relates to an analysis method and application of a rock core mineral composition.
Background
Mineral composition analysis is one of the important fundamental research efforts in the field of oil and gas exploration research. Through mineral analysis, the types, causes, distribution and enrichment rules and the like of minerals can be effectively identified, and the results of the mineral analysis in the field of oil and gas exploration can reveal the distribution rules of the lithology of strata and indicate the mineral composition of strata (hydrocarbon source strata, reservoirs, cap layers and the like) of different types. The work has important significance for finding favorable crude oil reservoirs and distribution rules thereof in oil and gas exploration.
There are currently two methods of mineral composition analysis: the first method is based on the laboratory X-ray diffraction analysis technique (abbreviated as XRD in english), which obtains the main components in the rock by analyzing the diffraction pattern of the rock by X-ray diffraction. The method can analyze the contents of the whole rock mineral components and the clay minerals aiming at rocks with different lithologies, and further obtain the rock names of the test samples according to the mineral combination. However, this method has various disadvantages: 1) the equipment belongs to large-scale equipment, has high experimental analysis environmental requirements, and cannot meet the requirements of field and oil-gas exploration field operation; 2) the sample can be damaged in the analysis and test process, the rock sample needs to be ground into powder, and the analysis can be carried out after tabletting and forming; 3) the analysis and test speed is slow, a large amount of time and energy are consumed, and accurate lithology information cannot be provided for field geologists quickly. The second method is a portable element analyzer based on X-ray fluorescence analysis (abbreviated as XRF in english), which obtains element information in a sample by irradiating X-rays on the sample to be measured. It has effectually solved some technical application limitations in the XRD technique: 1) the equipment is small and exquisite and convenient to carry, and can meet the working requirements of the field and the oil-gas exploration field; 2) the nondestructive testing can be carried out on the sample, namely, the equipment is directly contacted with the surface of the sample to be tested, and then the related analysis test can be carried out; 3) the analysis speed is relatively fast, can help the on-the-spot staff to obtain the elemental information of rock sample. It also suffers from two disadvantages: 1) the detection result based on the XRF method is only element information, and mineral composition information in the rock core cannot be directly obtained; 2) the portable XRF analyzers manufactured by different types and instrument manufacturers have different detection modes, detection time and analysis conditions, so that the detection results have larger differences. Aiming at the defects of XRF in field work, no documents and patent reports of related technical methods or research ideas are found at present, so that a rapid core mineral composition analysis method which can effectively solve the problems and is suitable for the field needs to be established.
The instrument and analytical test methods for XRF that have been disclosed so far are as follows:
CN102735705B discloses a portable analyzer and XRF analysis method, the portable analyzer includes: an x-ray source configured to emit x-rays to a specimen; a detector subsystem responsive to x-rays emitted by the specimen and outputting intensities of detected x-rays having different energy levels; an air pressure measuring device configured to measure ambient air pressure; a processing subsystem responsive to the detector subsystem and the air pressure measurement device and configured to: calculating a content of at least one low atomic number element within the sample based on an intensity of x-rays detected by the detector subsystem at an energy level corresponding to the element, wherein the calculating comprises correcting the intensity based on the ambient air pressure. However, the analytical method disclosed in this patent application must be based on this analyzer and therefore does not have broad spectrum.
CN109239115A discloses an XRF detector, which redesigns the relevant components of XRF, and focuses on real-time detection and analysis of the content of heavy metal elements in soil. CN109358081A discloses a soil detection device based on XRF. Both are suitable for soil and cannot detect core samples.
CN107367520A discloses a method for identifying lithology of fine grained sedimentary rock based on XRF, which calculates mineral content of fine grained sedimentary rock based on XRF element detection results. The method can only carry out analysis and test on the fine-grained sedimentary rock and has certain limitation.
Therefore, in the prior art, the existing element detection method has no universality and applicability for most lithologic types encountered in field and field work.
Disclosure of Invention
The invention provides a novel analysis method for rock core mineral composition, which can be used for rapidly identifying mineral composition and type in a rock core and rapidly identifying lithology and minerals on the premise of not losing a rock core sample.
The invention provides a method for analyzing the mineral composition of a rock core in a first aspect, which comprises the following steps:
step A, establishing analysis test conditions based on X-ray fluorescence analysis (XRF);
b, selecting an element analysis method suitable for the rock core, and detecting the rock core to be detected;
and step C, obtaining element composition information of the rock core and calculating according to a mathematical model to obtain the mineral composition of the rock core.
According to some embodiments of the vector of the present invention, the step of establishing analytical test conditions comprises:
step A1: evaluating the repeatability of the detection result, determining the minimum detection time and evaluating the humidity detection result under different detection modes;
step A2: and integrating the evaluation results of the step A1.
According to some embodiments of the vector of the present invention, the number of repetitions is 3 to 5.
According to some embodiments of the support of the present invention, the reproducibility evaluation criterion has an error of not more than 20%, preferably not more than 15%.
In the present invention, the error is calculated by the formula
Wherein: a is the first measurement of the checkpoint and B is the second measurement of the checkpoint.
According to some embodiments of the vector of the present invention, the method of determining a minimum detection time comprises: the error is not more than 20%, preferably not more than 15%, at different detection times.
According to some embodiments of the carrier of the present invention, the method of evaluating detection humidity comprises: under the condition that the humidity difference is not less than 30%, the error is not more than 20%, and preferably not more than 15%. In the present invention, the difference of the humidities of not less than 30% means that the difference of the two humidities of not less than 30%. For example, when the humidity in the first measurement is 20%, the humidity in the second measurement is not less than 50%.
According to some embodiments of the vector of the present invention, the method of calculating the mathematical model comprises: the mineral type, and optionally the content, is obtained by conversion based on the molecular weight relationship of the element to the mineral.
According to some embodiments of the carrier of the present disclosure, prior to step a, the method further comprises preparing a core to be tested.
According to some embodiments of the vector of the invention, the method of preparing comprises: core arrangement and homing, detection point positioning and characteristic sample labeling.
In a second aspect, the invention provides the use of an analysis method as described above in oil and gas exploration.
The invention has the beneficial effects that:
the traditional mineral composition analysis is mainly completed in a laboratory, and the method is restricted by a plurality of factors such as huge analysis equipment, high analysis environment requirement, complex pretreatment process of a sample to be tested, long test analysis time and the like, so that the method provides rapid lithology analysis and identification for geological field workers. By combining XRF technology, the invention provides a rapid core mineral composition analysis method suitable for the field. The method can realize the rapid identification of lithology and minerals on the premise of not damaging the core sample.
Drawings
Fig. 1 is a schematic diagram of an analysis process of a core mineral composition provided in example 1 of the present invention;
FIG. 2a shows Al detected multiple times in the Gengram mode provided in example 1 of the present invention2O3A repetitive result graph;
FIG. 2b is a graph of the results of multiple measurements in the Gengram mode provided in example 1 of the present invention;
FIG. 2c shows multiple SiO assays in the Gengram mode provided in example 1 of the present invention2A repetitive result graph;
FIG. 2d is a diagram showing the CaO repeated results of multiple detections in the Gengram mode provided in example 1 of the present invention;
FIG. 3a is a graph showing the results of MgO analysis at different detection times, which is provided in example 1 of the present invention;
FIG. 3b shows Al at different detection times according to example 1 of the present invention2O3Analyzing the result graph;
FIG. 3c is a diagram of SiO at different detection times according to example 1 of the present invention2Analyzing the result graph;
FIG. 3d shows K at different detection times according to embodiment 1 of the present invention2O, analyzing a result graph;
FIG. 3e is a diagram showing CaO analysis results at different detection times, which are provided in example 1 of the present invention;
FIG. 3f shows Fe at different detection times according to example 1 of the present invention2O3Analyzing the result graph;
fig. 4 is a triangular diagram of the types of main minerals in mudstone and the distribution of the contents thereof, which is provided in example 1 of the present invention.
Detailed Description
In order that the present invention may be more readily understood, the following detailed description of the invention is given by way of example only, and is not intended to limit the scope of the invention.
[ example 1 ]
The schematic diagram of the analysis process is shown in fig. 1.
The first step is as follows: preparing a sample, including arranging and homing the rock core, calibrating detection points, and finally selecting 25 detection points;
the second step is that: establishing analysis test conditions, wherein the following work is included:
(1) determination of detection mode: an XRF model S1 TITAN 600 from Bruker was used, with three detection modes, General, Concentrate and Trace.
(2.1) evaluation of reproducibility of test results: in General mode, three parallel experiments were performed on 25 spots, Al2O3、S、SiO2The CaO detection results are shown in FIG. 2a, FIG. 2b, FIG. 2c and FIG. 2d, and it can be seen from the graphs that the results are stable, the repeatability is good, and the error is 8%;
then, three parallel experiments are respectively carried out on 25 detection points in a concentrative mode and a Trace mode, and Al2O3、S、SiO2The CaO repeatability error is 12% in the Concentrate mode and 15% in the Trace mode.
(2.2) determining a minimum detection time: in a General mode, the first point of 25 detection points is detected, under different detection time, the detection results of 1min, 2 mm and 3min are basically the same, and the detection result of 6min has an error. MgO and Al2O3、SiO2、K2O, CaO and Fe2O3The analysis results of (a) are shown in FIGS. 3a to 3 f. May be related to the decay of the excitation detection energy. The MgO detection error is large. Under the condition that the errors of the detection results of 1min, 2mim and 3min are all less than 20%, determining the minimum detection time to be 1 min;
and then detecting the detection points detected in the General mode under the control mode and the Trace mode respectively, wherein the result is similar to that of the General mode, the detection results of 1min, 2 mm and 3min are basically the same, and the detection result of 6min has an error, so that the minimum detection time is determined to be 1 min.
(2.3) comparing analysis results under different dry and wet conditions: under the condition of selecting a General mode and under the conditions of humidity of 10% and humidity of 60%, three parallel experiments are carried out, the detection results are basically the same, and the error is 10%;
then, the detection points detected in the General mode were detected in the central mode and the Trace mode, respectively, with a result display error of 11% in the central mode and 14% in the Trace mode.
(2.4) the results of the evaluations (2.1) to (2.3) were combined to determine that the detection mode was the General mode.
(3) After a quick identification method suitable for elements in the rock core is established, 25 detection points are detected to obtain rock core detection data.
(4) Conversion is carried out according to the molecular weight relationship of the elements and the minerals (clastic rock system, Brumsack molecular weight calculation model: SiO2-Al2O3CaO x 2, calculated for the relative content of minerals) the mineral type, carbonate, and its content can be determined, as shown in fig. 4.
What has been described above is merely a preferred example of the present invention. It should be noted that other equivalent variations and modifications can be made by those skilled in the art based on the technical teaching provided by the present invention, and the protection scope of the present invention should be considered.
Claims (10)
1. A method of analyzing the mineral composition of a core, comprising the steps of:
step A, establishing analysis test conditions based on X-ray fluorescence analysis;
b, selecting an element analysis method suitable for the rock core, and detecting the rock core to be detected;
and step C, obtaining element composition information of the rock core and calculating according to a mathematical model to obtain the mineral composition of the rock core.
2. The analytical method of claim 1, wherein the step of establishing analytical test conditions comprises:
step A1: evaluating the repeatability of the detection result, determining the minimum detection time and evaluating the humidity detection result under different detection modes;
step A2: and integrating the evaluation results of the step A1.
3. The assay of claim 2, wherein the number of repetitions is from 3 to 5.
4. An assay method according to claim 3, wherein the criterion for the assessment of reproducibility is an error of no more than 20%, preferably no more than 15%.
5. The analytical method of claim 2, wherein the method of determining a minimum detection time comprises: the error is not more than 20%, preferably not more than 15%, at different detection times.
6. The analytical method of claim 2, wherein the method of evaluating the detected humidity comprises: under the condition that the humidity difference is not less than 30%, the error is not more than 20%, and preferably not more than 15%.
7. The analytical method of any one of claims 1 to 6, wherein the mathematical model is calculated by a method comprising: and obtaining the mineral type through conversion based on the relationship between the elements and the molecular weight of the mineral.
8. The method of any one of claims 1-7, wherein prior to step a, the method further comprises preparing a core under test.
9. The analytical method of claim 8, wherein the method of preparing comprises: core arrangement and homing, detection point positioning and characteristic sample labeling.
10. Use of the analytical method of any one of claims 1 to 9 in oil and gas exploration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011022580.6A CN114428094A (en) | 2020-09-25 | 2020-09-25 | Analysis method and application of rock core mineral composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011022580.6A CN114428094A (en) | 2020-09-25 | 2020-09-25 | Analysis method and application of rock core mineral composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114428094A true CN114428094A (en) | 2022-05-03 |
Family
ID=81310108
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011022580.6A Pending CN114428094A (en) | 2020-09-25 | 2020-09-25 | Analysis method and application of rock core mineral composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114428094A (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101354362A (en) * | 2008-07-21 | 2009-01-28 | 中国石化集团华北石油局 | Method for analyzing x-ray fluorescence shale content in petroleum well drilling |
| CN104122283A (en) * | 2014-08-01 | 2014-10-29 | 桂林理工大学 | Total-rock component testing method based on in-situ electronic probe analysis |
| CN104989392A (en) * | 2015-07-10 | 2015-10-21 | 中国石油天然气股份有限公司 | Lithology identification method |
| CN105372298A (en) * | 2014-08-24 | 2016-03-02 | 中国石油集团渤海钻探工程有限公司 | Analysis method for formation rock mineral constituents |
| CN106885815A (en) * | 2017-03-22 | 2017-06-23 | 中国石油大学(华东) | A kind of method that depositional environment is differentiated based on element XRF methods in sandstone |
| CN107367520A (en) * | 2017-06-27 | 2017-11-21 | 中国石油天然气股份有限公司 | A kind of method based on XRF identification pulveryte lithology |
| CN108535303A (en) * | 2018-05-28 | 2018-09-14 | 中石化石油工程技术服务有限公司 | A kind of XRF instruments of detection core sample element |
| CN109490266A (en) * | 2018-11-15 | 2019-03-19 | 中国石油化工股份有限公司江汉油田分公司勘探开发研究院 | A kind of rock sample sampling without damage method |
| US20190351804A1 (en) * | 2016-09-09 | 2019-11-21 | Bly Ip Inc. | Systems and methods for analyzing core using x-ray fluorescence |
| CN210604460U (en) * | 2019-04-17 | 2020-05-22 | 中国石油化工股份有限公司 | XRF automatic testing device suitable for rock core test |
| CN111458363A (en) * | 2020-04-21 | 2020-07-28 | 中国地质大学（武汉） | Method for rapidly delineating titanium deposit based on handheld X-ray fluorescence analyzer |
-
2020
- 2020-09-25 CN CN202011022580.6A patent/CN114428094A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101354362A (en) * | 2008-07-21 | 2009-01-28 | 中国石化集团华北石油局 | Method for analyzing x-ray fluorescence shale content in petroleum well drilling |
| CN104122283A (en) * | 2014-08-01 | 2014-10-29 | 桂林理工大学 | Total-rock component testing method based on in-situ electronic probe analysis |
| CN105372298A (en) * | 2014-08-24 | 2016-03-02 | 中国石油集团渤海钻探工程有限公司 | Analysis method for formation rock mineral constituents |
| CN104989392A (en) * | 2015-07-10 | 2015-10-21 | 中国石油天然气股份有限公司 | Lithology identification method |
| US20190351804A1 (en) * | 2016-09-09 | 2019-11-21 | Bly Ip Inc. | Systems and methods for analyzing core using x-ray fluorescence |
| CN106885815A (en) * | 2017-03-22 | 2017-06-23 | 中国石油大学(华东) | A kind of method that depositional environment is differentiated based on element XRF methods in sandstone |
| CN107367520A (en) * | 2017-06-27 | 2017-11-21 | 中国石油天然气股份有限公司 | A kind of method based on XRF identification pulveryte lithology |
| CN108535303A (en) * | 2018-05-28 | 2018-09-14 | 中石化石油工程技术服务有限公司 | A kind of XRF instruments of detection core sample element |
| CN109490266A (en) * | 2018-11-15 | 2019-03-19 | 中国石油化工股份有限公司江汉油田分公司勘探开发研究院 | A kind of rock sample sampling without damage method |
| CN210604460U (en) * | 2019-04-17 | 2020-05-22 | 中国石油化工股份有限公司 | XRF automatic testing device suitable for rock core test |
| CN111458363A (en) * | 2020-04-21 | 2020-07-28 | 中国地质大学（武汉） | Method for rapidly delineating titanium deposit based on handheld X-ray fluorescence analyzer |
Non-Patent Citations (1)
| Title |
|---|
| 张广玉等: ""手持式X 射线荧光光谱多点测试技术在地质岩心和岩石标本预研究中的应用"", 《岩矿测试》, vol. 36, no. 5, pages 501 - 509 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sharma et al. | Characterizing soils via portable X-ray fluorescence spectrometer: 3. Soil reaction (pH) | |
| Carvajal-Ortiz et al. | Critical considerations when assessing hydrocarbon plays using Rock-Eval pyrolysis and organic petrology data: Data quality revisited | |
| US6140643A (en) | Method for identification of unknown substances | |
| CN104251846A (en) | Discriminant analysis combined laser-induced breakdown spectroscopy quantitative analysis method | |
| CN104458693A (en) | Raman spectrum measuring method for drug detection | |
| EA027574B1 (en) | Method for determining volume of organic matter in reservoir rock | |
| CN110274925A (en) | Method based on the gold in energy-dispersion X-ray fluorescence spectrometry measurement ore | |
| CN115128247A (en) | Novel method for distinguishing prospecting type based on chlorite indication element change | |
| Mohamed et al. | Chemical and Mineralogical Mapping of Platinum‐Group Element Ore Samples Using Laser‐Induced Breakdown Spectroscopy and Micro‐X‐Ray Fluorescence | |
| CN110530961B (en) | Method and device for determining control factors of carbonate mineral cathode luminous intensity | |
| CN106442474A (en) | Cement raw meal three moduli measuring method based on partial least squares | |
| Folco et al. | In situ identification, pairing, and classification of meteorites from Antarctica through magnetic susceptibility measurements | |
| CN104212804A (en) | Aptamer sequence for quantitatively and rapidly detecting lead ions and method for detecting lead ions by utilizing same | |
| CN109490266B (en) | Nondestructive rock sample sampling method | |
| Liebmann et al. | Strategies towards robust interpretations of in situ zircon oxygen isotopes | |
| CN201034951Y (en) | X fluorescent measuring sulphur instrument used for petroleum crude and oil products | |
| CN105807330A (en) | Method for rapidly recognizing mineral volume content of shale formation | |
| CN101984351A (en) | Measuring method of grade of magnetic iron made of fine iron powder and measuring device thereof | |
| CN114428094A (en) | Analysis method and application of rock core mineral composition | |
| CN102330553B (en) | Method for identifying dynamic spectrum fluid for MDI (Manual Data Input) test | |
| Ingle et al. | Difficulties with determining the detection limit with nonlinear calibration curves in spectrometry | |
| CN111458363A (en) | Method for rapidly delineating titanium deposit based on handheld X-ray fluorescence analyzer | |
| CN114894829B (en) | Electronic probe analysis method for testing F and Cl of olivine trace elements | |
| CN110907379A (en) | Method for measuring components and content of Anshan type iron ore based on random forest algorithm | |
| CN108507923A (en) | Rock core magnetic nuclear resonance analyzer porosity measurement precision is examined and bearing calibration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |