CN113866197B - Method for determining main quantity elements of sample with non-uniform mineral composition - Google Patents
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Abstract
The invention provides a method for determining main quantity elements of a sample with non-uniform mineral composition, which comprises five steps of processing a single-particle sample with non-uniform mineral composition, processing a homologous sample, obtaining mineral phase composition, obtaining main quantity element characteristics of each mineral and calculating integral main quantity elements, the method for determining the main quantity elements of the sample with the inhomogeneous mineral composition nondestructively determines the main quantity element characteristics of a tiny sample with the inhomogeneous mineral composition in the interior by combining the electron computer tomography technology, the sample does not need to be crushed, and the advantages of the CT technology, the electronic probe technology and the XRD technology are combined, so that the main quantity element characteristics of the tiny single-particle sample can be nondestructively determined, the method is suitable for the sample with tiny mass, for example, basalt detritus in lunar soil and a certain part of detritus in precious meteorite are subjected to lossless principal element determination.
Description
Technical Field
The invention relates to the technical field of geochemistry, in particular to a method for determining main quantity elements of a sample with inhomogeneous mineral composition.
Background
The existing means for measuring the major elements of a sample mainly include an Electron Probe (EPMA), an X-Ray Fluorescence Spectroscopy (XRF) and Energy Dispersive X-Ray Spectroscopy (EDS) analysis technologies, the Electron probe technology needs to polish and plate carbon on the sample after target preparation, and then can judge the components of an object by exciting X-rays, the result is usually very accurate, the detection line is low, but the sample can be damaged, and the major elements of the sample can be obtained by the EPMA, and are significantly influenced by the heterogeneity of the minerals in the sample in space, and different major element characteristics of the sample can be obtained in different sections of the same sample; the X-ray fluorescence spectrum analysis (XRF) technology can identify the main amount elements of a sample without damage, but the detection line is high and poor in precision, the measurement result is mainly controlled by the distribution of the main amount elements on the surface of the sample and does not represent the characteristics of the main amount elements of the whole sample, the mass of a single-particle sample is required to be large enough (gram level), the ground sample powder is required to be uniform enough to represent the components of the whole rock, otherwise, the powder is not uniform, so that the main amount element analysis results of the powder of the same sample are different; the EDS (Electron emission spectroscopy) energy spectrum analysis technology is usually combined with a Scanning Electron Microscope (SEM), can quickly identify minerals, but also needs to manufacture a sample target, destroys a sample and controls the measured main quantity elements by the distribution of the main quantity elements of a sample section, and is similar to the defects of EPMA (Electron beam emission spectroscopy), and meanwhile, the defects that the original sample must be destroyed, the quality requirement is high (gram level), the mineral distribution in the sample is not uniform and the like exist in the conventional method for obtaining the main quantity elements of the sample, so the invention provides a method for determining the main quantity elements of the sample with the nonuniform mineral composition to solve the problems in the prior art.
Disclosure of Invention
In view of the above problems, the present invention is directed to a method for determining a main amount of elements in a sample having a non-uniform mineral composition, which can solve the problems of the prior art by non-destructively determining the main amount of elements characteristic of a sample having a small size (< 1 mg) and a non-uniform internal mineral composition (single particle) by combining with Computed Tomography (CT), without pulverizing the sample.
In order to realize the purpose of the invention, the invention is realized by the following technical scheme: a method of determining the principal amount of elements in a sample having a non-uniform mineral composition, comprising the steps of:
step one, processing single-particle samples with non-uniform mineral composition
Fixing a single-particle sample on the surface of a test tube by using a conductive adhesive tape, then carrying out CT scanning to obtain a three-dimensional gray image of the sample, and then carrying out gray resolution and identification on the three-dimensional image according to the structure of minerals in the sample to obtain the volume of each mineral in the sample;
step two, processing the homologous sample
Performing lithology work on other samples which are homologous or in the same area with the single-particle sample in the step one, and giving the mineral phase composition and the main quantity element characteristics of each mineral of the other samples in the homologous or in the same area;
step three, obtaining mineral phase composition
Selecting powder samples of other samples in the same source or the same region in the step two, thoroughly stirring the powder samples, scraping the samples onto a flat surface by using a quartz glass sheet, and analyzing by using XRD (X-ray diffraction), so as to obtain the mineral phase composition of other samples in the same source or the same region in the step two;
step four, obtaining the main quantity element characteristics of each mineral
EPMA analyzing other samples in the same source or the same area in the second step, and measuring the main quantity element characteristics of each mineral of the selected samples by using EPMA equipped with an energy dispersion spectrometer;
step five, calculating the integral principal elements
Combining the volume obtained by CT scanning with the density obtained by other parts of the sample, which are homologous or in the same region, the mass M of the mineral in different parts can be calculatedmineralAnd total mass M of the sampletotalElement based on the mass of the mineral and the content of the principal Element of the mineralmineral(wt.%) and the mass M of the elements of the main quantities contained in the different minerals are calculatedmineral-elementAnd recalculating the sum M of the mass of each principal quantity element in the sampleelement totalAnd then recalculating the Element proportion of each main quantity Element in the sample in the whole sampletotal（wt%）。
The further improvement lies in that: in the first step, the volume of the same gray level unit is counted, and the volume V of each mineral is represented by the volume of the same gray level unitmineral。
The further improvement lies in that: in the second step, in order to eliminate the interference of abnormal values, the main quantity elements of each mineral are represented by the arithmetic mean value of the main quantity elements, and the mineral category is represented by the mineral phase with the highest proportion.
The further improvement lies in that: in the third step, after each measurement, the sample is stirred again, the sample is scraped again to a flat surface by using a quartz glass sheet, and the sample is reanalyzed by using XRD, and the analysis by using XRD is repeated for 10-20 times for each sample.
The further improvement lies in that: in the fourth step, the mineral was analyzed at an acceleration voltage of 15kV and an electron beam current of 10nA, the spot diameter was 5 μm, the peak count time of each element was 20s, and the background time was 10 s.
The further improvement lies in that: in the fifth step, the mass M of different part mineralsmineralThe calculation formula is as follows:
in the formula, ρmineralIs mineral density, VmineralIs the mineral volume.
The further improvement lies in that: in the fifth step, the total mass M of the sampletotalThe calculation formula is as follows:
in the formula, MmineralThe quality of different part of minerals.
The further improvement lies in that: in the fifth step, the mass M of each main element contained in different mineralsmineral-elementThe calculation formula is as follows:
in the formula, Elementmineral(wt%) is based on the mass of the mineral and the content of the major elements of the mineral.
The further improvement lies in that: in the fifth step, the sum M of the mass of each main quantity element in the sampleelement totalThe calculation formula is as follows:
in the formula, Mmineral-elementThe mass of each main element contained in different minerals.
The further improvement lies in that: in the fifth step, the Element accounts for the proportion of the major Element in the sample in the whole sampletotal(wt%) the calculation formula is as follows:
the invention has the beneficial effects that: the method for determining the major element of the sample with the inhomogeneous mineral composition can be used for nondestructively determining the major element characteristics of a certain tiny (< 1 mg) sample with the inhomogeneous mineral composition (single particle) by combining the Computed Tomography (CT) technology without crushing the sample, and combining the advantages of the CT technology, the electronic probe technology and the XRD technology, so that the major element characteristics of the tiny single particle sample can be nondestructively determined, and the method is suitable for nondestructively determining the major element characteristics of a certain part of rock debris in samples with tiny mass (< 1 mg), such as basalt rock debris in lunar soil and precious meteorite (mars and lunar meteorite).
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic flow diagram of the present invention.
FIG. 2 is a schematic diagram showing the basic elements of the principal elements of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
According to the present example, as shown in fig. 1-2, a method for determining a major amount of elements in a sample having a non-uniform mineral composition is provided, comprising the steps of:
step one, processing a single particle sample
Fixing a single-particle sample on the surface of a resin tube with the diameter of 1mm by using a conductive adhesive tape, then carrying out CT scanning to obtain a three-dimensional gray scale image of the sample, carrying out gray scale splitting and identification on the three-dimensional image according to the structure of minerals in the sample to obtain the volume of each mineral in the sample, counting the volume of the same gray scale unit, and representing the volume V of each mineral by using the volume of the same gray scale unitmineralThereby obtaining the volume of each mineral in the single particle sample;
step two, processing the homologous sample
Performing lithology work on other samples which are homologous or homologous to the single-particle sample in the first step, giving the mineral phase composition of the other samples which are homologous or homologous and giving the principal element characteristics of each mineral, wherein the principal element characteristics and the categories of main minerals contained in the samples are similar as the samples are homologous, for example, feldspar is anorthite, pyroxene is common pyroxene and olivine is fayalite, in order to eliminate the interference of abnormal values, the principal element of each mineral is represented by the arithmetic mean value (n data are added and then divided by n), the mineral phase with the highest proportion represents the mineral category, and for example, the anorthite is the highest proportion in all feldsps, anorthite is used for representing the feldspars and participating in the search of subsequent densities;
step three, obtaining mineral phase composition
Selecting 100mg of powder sample from other samples in the same source or the same area in the second step, thoroughly stirring the powder sample for at least one hour, and scraping the sample to a flat surface by using a quartz glass sheetAnd then using XRD to make analysis, then obtaining mineral phase composition of other samples of same source or same region in step two, after every measurement, stirring sample again, using quartz glass sheet to scrape sample on flat surface, using XRD to make analysis again, for every sample using XRD (X-ray diffraction) analysis must repeat 10-20 times, the whole analysis process of every sample is continued for one hour, then obtaining specific correspondent mineral, and the standard diffraction pattern of every mineral phase is come from international diffraction centre data, then making mineral density search, density rhomineralThe density of the corresponding category of minerals can be obtained by searching a mineral density database;
step four, obtaining the main quantity element characteristics of each mineral
EPMA analysis is carried out on other samples of the same source or the same region in the second step, EPMA equipped with an energy dispersion spectrometer is used for measuring the main quantity element characteristics of each mineral of the selected sample, the minerals are analyzed under the acceleration voltage of 15kV and the electron beam current of 10nA, the light spot diameter is 5 μm, the peak counting time of each element is 20s, the background time is 10s, natural minerals and synthetic glass are used as standard products, the detection limit of most elements is 0.01 wt.% to 0.03 wt.%, and then the data are corrected by atomic number (Z), X-ray absorption (A) and fluorescence (F) effects;
step five, calculating the integral principal elements
Combining the volume obtained by CT with the density obtained by other parts of the sample, which are homologous or in the same region, the mass M of the mineral in different parts can be calculatedmineralAnd total mass M of the sampletotalBased on the mass of the mineral and the content E of the principal elements of the minerallementmineral(wt.%) and the mass M of the elements of the main quantities contained in the different minerals are calculatedmineral-elementAnd recalculating the sum M of the mass of each principal quantity element in the sampleelement totalAnd then the proportion E of each main quantity element in the sample in the whole sample is recalculatedlementtotal(wt.%) of different part of the mineral mass MmineralThe calculation formula is as follows:
in the formula, ρmineralIs mineral density, VmineralTotal mass M of sample as mineral volumetotalThe calculation formula is as follows:
in the formula, MmineralThe mass M of each main element contained in different minerals is the mass of different mineralsmineral-elementThe calculation formula is as follows:
in the formula, Mmineral-elementThe sum M of the mass of each main quantity element in the sample is the mass of each main quantity element contained in different mineralselement totalThe calculation formula is as follows:
in the formula, Mmineral-elementThe mass of each main Element contained in different minerals is the proportion of the main Element in the sample in the Elementtotal(wt%) the calculation formula is as follows:
wherein, mineral = Anorthite (Anorthite), enstatite (enstatite) … …
Wherein element = calcium (Ca), iron (Fe), magnesium (Mg) … …
Example two
In this embodiment, taking the calculation of the principal component element of the basalt rock debris as an example, the method includes the following steps:
step one, fixing the sample on the surface of a glass rod with the diameter of 1mm by using conductive adhesive, vertically placing the sample on a CT sample table, carrying out CT scanning to obtain a three-dimensional gray scale image, carrying out gray scale identification and splitting according to different minerals in basalt to respectively obtain the volume of main minerals in basalt chips, wherein V isFeldspar= 2.10E+07 μm3；VPyroxene= 1.62E+07 μm3；VOlivine stone= 5.10E+06 μm3；VIlmenite= 2.10E+06 μm3；
Step two, the main element data of each mineral of basalt which is homologous with the basalt detritus and analyzed by EPMA is published, wherein the main element result of feldspar is SiO2（Wt%）=49.03%；TiO2（Wt%）=0.08% ；Al2O3（Wt%）=31.73% FeO（Wt%）=0.79% ；MnO（Wt%）=0.02%； MgO（Wt%）=0.10%； CaO（Wt%）=15.69%； Na2O（Wt%）=1.47% ；K2O（Wt%）=0.22% ；Cr2O3（Wt%）=0%；P2O5(Wt%) = 0.02%; the predominant elemental result for pyroxene is SiO2（Wt%）=47.83%；TiO2（Wt%）=1.40% ；Al2O3（Wt%）=1.70% ；FeO（Wt%）=25.87% ；MnO（Wt%）=0.41%； MgO（Wt%）=7.56%； CaO（Wt%）=13.73%； Na2O（Wt%）=0.03% ；K2O（Wt%）=0% ；Cr2O3（Wt%）=0.18%；P2O5(Wt%) = 0.02%; the result of the major element of olivine is SiO2（Wt%）=30.92%；TiO2（Wt%）=0.24% ；Al2O3（Wt%）=0.01% FeO（Wt%）=58.17% ；MnO（Wt%）=0.65%； MgO（Wt%）=8.26%； CaO（Wt%）=0.52%； Na2O（Wt%）=0% ；K2O（Wt%）=0；Cr2O3（Wt%）=0.02%；P2O5(Wt%) = 0.12%; the major elemental result of ilmenite was SiO2（Wt%）=0.02%；TiO2（Wt%）=52.5% ；Al2O3（Wt%）=0% FeO（Wt%）=45.61% ；MnO（Wt%）=0.38%； MgO（Wt%）=0.35%；
Thirdly, the analysis data of the species of the mineral phase homologous with the basalt chips identified by XRD are published, and the feldspar is mainly Bytownite (Bytownite); pyroxenes are mainly common pyroxenes (Augite); olivine is between fayalite and forsterite; ilmenite is not distinguished. Corresponding the above mineral phases to a mineral density database to obtain rhoBytownite=2.71 g/cm3；ρaugite=3.4 g/cm3 ；ρfayalite=3.83 g/cm3 ；ρilmenite=4.72 g/cm3；
Step four and all the data meet the calculation requirements (density, volume and main element of each mineral), and the calculation requirements are substituted into the formula in the first embodiment to obtain the main element component SiO of the basalt chips2（Wt%）=44.47%；TiO2（Wt%）=4.62% ；Al2O3（Wt%）=10.93% FeO（Wt%）=21.33% ；MnO（Wt%）=0.30%； MgO（Wt%）=4.82%； CaO（Wt%）=12.85%； Na2O（Wt%）=0.48% ；K2O（Wt%）=0.07% ；Cr2O3（Wt%）=0.11%；P2O5（Wt%）=0.02%。
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A method of determining the principal quantity of elements in a sample having a non-uniform mineral composition, the method comprising: the method comprises the following steps:
step one, processing a single-particle sample with non-uniform mineral composition, fixing the single-particle sample on the surface of a test tube by using a conductive adhesive tape, then performing CT scanning to obtain a three-dimensional gray image of the sample, and performing gray resolution and identification of the three-dimensional image according to the structure of minerals in the sample to obtain the volume of each mineral in the sample;
step two, processing the homologous sample
Performing lithology work on other samples which are homologous or in the same area with the single-particle sample in the step one, giving the mineral phase composition of other samples in the homologous or in the same area and the main quantity element characteristics of each mineral, representing the main quantity element of each mineral by the arithmetic mean value (n data are added and then divided by n) of each main quantity element in order to eliminate the interference of abnormal values, representing the mineral category by the mineral phase with the highest proportion, and participating in the subsequent density search;
step three, obtaining mineral phase composition
Selecting powder samples of other samples of the same source or the same region in the step two, thoroughly stirring the powder samples, scraping the samples onto a flat surface by using a quartz glass sheet, analyzing by using XRD, further obtaining the mineral phase composition of other samples of the same source or the same region in the step two, after each measurement, re-stirring the samples, scraping the samples onto the flat surface by using the quartz glass sheet again, re-analyzing by using XRD, repeating the XRD analysis for 10-20 times for each sample to obtain specific corresponding minerals, wherein the standard diffraction pattern of each mineral phase is from international diffraction center data, and then searching the mineral density, wherein the density rho ismineralObtaining the density of the corresponding category of minerals by searching a mineral density database;
step four, obtaining the main quantity element characteristics of each mineral
EPMA analyzing other samples in the same source or the same area in the second step, and measuring the main quantity element characteristics of each mineral of the selected samples by using EPMA equipped with an energy dispersion spectrometer;
step five, calculating the integral principal elements
Combining the volume obtained by CT scanning with the density ρ obtained by other parts of the sample that are homologous or in the same regionmineralThe mass M of different partial minerals can be calculatedmineralAnd total mass M of the sampletotalBased on the quality of the mineral and the oreElement content of principal componentmineral(wt.%) and the mass M of the elements of the main quantities contained in the different minerals are calculatedmineral-elementAnd recalculating the sum M of the mass of each principal quantity element in the sampleelement totalAnd then recalculating the Element proportion of each main quantity Element in the sample in the whole sampletotal（wt%）。
2. The method according to claim 1, wherein the method comprises the steps of: in the first step, the volume of the same gray level unit is counted, and the volume V of each mineral is represented by the volume of the same gray level unitmineral。
3. The method according to claim 1, wherein the method comprises the steps of: in the fourth step, the mineral was analyzed at an acceleration voltage of 15kV and an electron beam current of 10nA, the spot diameter was 5 μm, the peak count time of each element was 20s, and the background time was 10 s.
4. The method according to claim 1, wherein the method comprises the steps of: in the fifth step, the mass M of different part mineralsmineralThe calculation formula is as follows:
Mmineral=ρmineral×Vmineral
in the formula, ρmineralIs mineral density, VmineralIs the mineral volume.
5. The method according to claim 1, wherein the method comprises the steps of: in the fifth step, the total mass M of the sampletotalThe calculation formula is as follows:
Mtotal=∑Mmineral
in the formula, MmineralThe quality of different part of minerals.
6. The method according to claim 1, wherein the method comprises the steps of: in the fifth step, the mass M of each main element contained in different mineralsmineral-elementThe calculation formula is as follows:
Mmineral-element=Mmineral×Elementtotal（wt%）
in the formula, Elementtotal(wt%) is based on the mass of the mineral and the content of the major elements of the mineral.
7. The method according to claim 1, wherein the method comprises the steps of: in the fifth step, the sum M of the mass of each main quantity element in the sampleelement totalThe calculation formula is as follows:
Melement total=∑Mmineral-element
in the formula, Mmineral-elementThe mass of each main element contained in different minerals.
8. The method according to claim 1, wherein the method comprises the steps of: in the fifth step, the Element accounts for the proportion of the major Element in the sample in the whole sampletotal(wt%) the calculation formula is as follows:
Elementtotal（wt%）=Melement total/Mtotal。
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