CN115639040B - Method for manufacturing superfine powder pressed cake standard sample for carbonate rock in-situ micro-area - Google Patents
Method for manufacturing superfine powder pressed cake standard sample for carbonate rock in-situ micro-area Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 35
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 22
- 239000011435 rock Substances 0.000 title claims abstract description 15
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 title claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 29
- 238000005516 engineering process Methods 0.000 claims abstract description 17
- 239000004809 Teflon Substances 0.000 claims abstract description 10
- 229920006362 Teflon® Polymers 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 238000006467 substitution reaction Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 239000010419 fine particle Substances 0.000 claims description 7
- 238000004062 sedimentation Methods 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 229910021532 Calcite Inorganic materials 0.000 claims description 4
- 238000011161 development Methods 0.000 claims description 4
- 229910000514 dolomite Inorganic materials 0.000 claims description 4
- 239000010459 dolomite Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 3
- 238000005111 flow chemistry technique Methods 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 41
- 238000004458 analytical method Methods 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 235000013619 trace mineral Nutrition 0.000 description 4
- 239000011573 trace mineral Substances 0.000 description 4
- 238000012795 verification Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 238000000608 laser ablation Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000007542 hardness measurement Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000010902 jet-milling Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910001748 carbonate mineral Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010249 in-situ analysis Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000513 principal component analysis Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention provides a method for manufacturing a carbonate rock in-situ micro-region ultra-fine powder pressed cake standard sample, which comprises the following steps: (1) sample environment substitution; reducing pollution by a sample environment substitution technology, replacing grinding equipment possibly having pollution after introducing raw materials for processing for a plurality of times, and introducing a large amount of samples for grinding and collecting after sample replacement and discarding processes; the Teflon tank body and the grinding ball are selected for grinding, and the Teflon material is removed from the grinding ball by extracting and cleaning for many times by utilizing the characteristics of extremely low friction coefficient, stability, density difference of the grinding ball and the like; (3) testing the optimal hardness of the standard sample. By adopting the three main technologies and the related processes, a whole set of standardized flow processing method is formed, and a better technical effect can be achieved when the carbonate standard sample is manufactured. The method can improve the uniformity and high purity of the standard sample, and has better scientific research and economic value.
Description
Technical Field
The invention relates to the field of the earth science, in particular to a method for manufacturing a carbonate rock in-situ micro-area ultrafine powder pressed cake standard sample, which is used for geology, geochemistry, petrology and mineralogy.
Background
An important method for testing the content of mineral elements, the isotope ratio and the like on a microscopic scale by utilizing a laser ablation system and an inductively coupled plasma mass spectrometer or other in-situ micro-area analysis technology. In order to accurately test the element content of minerals and specific structures in a micro-area environment, calibration is mainly performed at home and abroad at present by using standard samples with components and chemical properties which are relatively close to those of samples to be tested. At present, the international standard sample and method for internal standard correction of most rock types are mature, but the development of the standard sample for carbonate rock samples is still in a preliminary stage. This is because the major elements in carbonates (mainly calcite CaCO 3 and dolomite CaMg (CO 3)2 minerals) are Ca and Mg, and some trace elements, especially rare earth elements, are very low in content, for example, the total rare earth element content in carbonate powder is less than 2 micrograms in a modern marine environment of 1 gram, whereas the total rare earth element content in existing standard (MACS-3) is about 150 micrograms.
Disclosure of Invention
The invention provides a method for manufacturing a carbonate rock in-situ micro-area ultrafine powder pressed cake standard sample, which aims to obtain a carbonate rock standard sample with extremely low pollution and extremely high component uniformity degree and realize high-precision in-situ analysis of carbonate rock.
The invention is realized by the following technical scheme:
A method for manufacturing a carbonate rock in-situ micro-region ultra-fine powder pressed cake standard sample comprises the following steps of
(1) Sample environment substitution technology
Three different analytical methods were used for the milling step of the carbonate raw material, respectively jet milling, planetary ball milling+sedimentation fine particle collection, and high-speed milling;
The pollution is reduced by a sample environment replacement technology, grinding equipment possibly polluted is replaced after raw materials are introduced for processing for a plurality of times, and a large-dose sample (70%) is introduced for grinding and collecting after at least 3 sample replacement and discarding processes (about 10% of the total amount of each time), so that the background influence is greatly reduced.
(2) Separation technology of low-pollution grinding ball and sample
The planetary ball milling and sedimentation method is used for collecting fine particles, a Teflon material (polytetrafluoroethylene) tank body and a grinding ball are selected for grinding, and the pollution risk is obviously reduced by utilizing the characteristics of extremely low friction coefficient, stability, grinding ball density difference and the like, and the Teflon material is removed after repeated extraction and cleaning.
(3) Optimal hardness testing technology for standard sample
Pressing the standard sample by high pressure (50 tons-200 tons); after the surface hardness of the calcite and dolomite geological samples manufactured into sheets is measured by a sclerometer and compared with the surface hardness of the standard samples manufactured under different pressures, the pressure conditions corresponding to the standard samples with basically consistent hardness are selected for subsequent standard sample development, the conditions with basically consistent hardness of the sample to be tested and the standard samples are achieved, and the pressure selection of the standard samples is optimized.
In the step (3), the consistency of the hardness of the standard sample and the hardness of the actual material is defined, and the test precision is improved.
By adopting the three main technologies and the related processes, a whole set of standardized flow processing method is formed, and a better technical effect can be achieved when the carbonate standard sample is manufactured. The method can improve the uniformity and high purity of the standard sample, and has better scientific research and economic value.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The specific technical scheme of the invention is described by combining the embodiments.
The invention provides a method for manufacturing a carbonate rock in-situ micro-region ultra-fine powder pressed cake standard sample, which is formed by a raw material processing method, optimization conditions, technical flow and the like which are not involved in an application patent (application number 202210066350.2) of a preamble standard sample.
As shown in fig. 1, the method for manufacturing the superfine powder pressed cake standard sample for the carbonate rock in-situ micro-region comprises the following steps:
(1) Sample environment substitution technology
The invention explores three different analysis methods for grinding steps of carbonate raw materials, namely jet milling, planetary ball milling and sedimentation method fine particle collection, and high-speed grinding, wherein the three methods can obtain processed ultrafine particles. However, both techniques involve prolonged contact of the feedstock with the inner walls of the machine and the abrasive, and may involve analysis of other highly contaminated samples for residual impurities. The invention reduces pollution as much as possible through a sample environment substitution technology. The technology is characterized in that grinding equipment possibly polluted is replaced after the raw material is introduced for processing for a plurality of times, and a large-dose sample (70%) is introduced for grinding and collecting after at least 3 sample replacement and discarding processes (about 10% of the total amount of each time).
(2) Separation technology of low-pollution grinding ball and sample
The planetary ball milling and sedimentation method fine particle collecting technology is a raw material grinding technology commonly used at present, but at present, grinding balls are mainly made of aluminum-silicon materials, metal materials and the like, and collision and abrasion among the grinding balls possibly introduce some components with high rare earth element content to cause certain pollution. The technology can effectively reduce pollution by selecting the Teflon material (polytetrafluoroethylene) tank body and the grinding ball for grinding. The Teflon is a high molecular polymer, has stable chemical property, no metal element pollution, abrasion temperature resistance and extremely low friction coefficient. The samples were ground by planetary ball mill with almost no metal contamination. Although the grinding balls are also worn slightly due to high-intensity abrasion, when the ultra-pure water is used for cleaning, teflon abradant has density difference with carbonate grinding fine particles, and the Teflon abradant can be removed from mixing after being extracted and cleaned for many times in the sedimentation process.
(3) Optimal hardness testing technology for standard sample
If the pressure is insufficient during the manufacture of the standard sample, the laser ablation objects are different in size, and fractionation effect is easy to generate, so that the test precision is affected. The denuded cavity of the pressed standard sample is smoother by high pressure (50 tons-200 tons). However, too high a hardness of the standard may cause a difference between the amount of degradation of the sample and the amount of degradation of the standard. According to the method, after the surface hardness of the calcite and dolomite geological samples are measured through a durometer and are manufactured into thin slices, and the surface hardness of the standard samples manufactured under different pressures is compared, the pressure conditions corresponding to the standard samples with basically consistent hardness are selected for subsequent standard sample development, so that the conditions with basically consistent hardness of the sample to be measured and the standard sample are achieved, and the pressure selection of the standard samples is optimized.
The prepared standard sample is verified by a test for a plurality of months in a laboratory, and the prepared standard sample is found to be stable in performance in the laser ablation process, and the effect is very similar to that of other actually measured carbonate rock samples, so that the whole preparation process and the quality of finished products are considered to be reliable, and the method can be used for in-situ original content calibration of carbonate minerals and specific compositions.
The standard sample is subjected to comparative analysis of main trace element content in a laboratory for a plurality of times, and the results are shown in tables 1 and 2 (the main trace element verification is carried out by an electronic probe method; the trace element verification uses an international carbonate standard sample MACS-3 as an external standard and uses an element Ca as an internal standard).
TABLE 1 microelement analysis results and uniformity verification
TABLE 2 principal component analysis results and uniformity verification
| Elemental oxide | SrO | MgO | Na2O | CaO | P2O5 | SiO2 |
| Average (%) | 0.841 | 0.12 | 0.226 | 51.912 | 0.368 | 0 |
| Elemental oxide | Al2O3 | FeO | MnO | CO2 | CaCO3 | Al2O3 |
| Average (%) | 0 | 0 | 0.008 | 41.963 | 95.438 | 0 |
Through a large number of repeatability tests of the instrument, the embodiment finds that the prepared standard sample has good uniformity and reproducibility, and achieves the test analysis effect of the in-situ micro-area carbonate sample.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (1)
1. The method for manufacturing the superfine powder pressed cake standard sample in the carbonate rock in-situ micro-area is characterized by comprising the following steps of:
(1) Sample environment substitution
The method for treating the carbonate rock raw material comprises the steps of planetary ball milling and fine particle collection by a sedimentation method;
the pollution is reduced by a sample environment substitution technology, samples possibly polluted in grinding equipment are replaced after raw materials are introduced for a plurality of times, and the samples are introduced for grinding and collection after the sample replacement and discarding processes; at least 3 sample substitutions, 10% of the total mass was discarded each time during the discarding process; the reintroduced samples amounted to 70% of the total mass;
(2) Separation of low-pollution grinding balls from sample
Fine particles are collected by a planetary ball milling and sedimentation method, a Teflon material tank body and a grinding ball are selected for grinding, and the Teflon material is removed after multiple times of extraction and cleaning;
(3) Optimal hardness test for standard sample
Pressing a standard sample by high pressure; after the surface hardness of the calcite and dolomite geological samples manufactured into sheets is measured by a sclerometer and compared with the surface hardness of the standard samples manufactured under different pressures, the pressure conditions corresponding to the standard samples with basically consistent hardness are selected for subsequent standard sample development, the conditions with basically consistent hardness of the sample to be tested and the standard samples are achieved, and the pressure selection of the standard samples is optimized.
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