CN113295666B - Quantitative analysis method for As element in pyrite by utilizing mineral Raman parameters - Google Patents
Quantitative analysis method for As element in pyrite by utilizing mineral Raman parameters Download PDFInfo
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
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Abstract
The invention discloses a quantitative analysis method for the As content in pyrite by utilizing mineral Raman parameters, which comprises the following steps: s1, performing pyrite Raman spectrum imaging scanning; s2, carrying out peak-splitting fitting on the Raman image, and making an accurate imaging distribution diagram of the sample about the Ag Raman displacement value; s3, measuring a Raman imaging diagram of the As content in the same area of the sample; s4, performing Photoshop calibration and anastomosis on an accurate imaging distribution diagram and an As content Raman imaging diagram of the Ag Raman displacement value, and converting the accurate imaging distribution diagram and the As content Raman imaging diagram into a data diagram; s5, making a scatter diagram of a Cartesian coordinate system through an electronic probe and a Raman imaging data diagram, analyzing the quantitative relation between Ag Raman displacement and the As content in pyrite, and fitting an equation. According to the invention, quantitative analysis is carried out on the content of As in pyrite by utilizing the mineral Raman parameters, the operation is simple, and the test speed is high; the Raman spectrum characteristic signal is strong, the signal-to-noise ratio is high, the specificity is strong, the recognition accuracy can be improved, and the false recognition is reduced.
Description
Technical Field
The invention relates to a quantitative analysis method for the As content in pyrite by utilizing mineral Raman parameters.
Background
Pyrite is a common sulfide of iron, often mistaken for gold due to its pale brass color and bright metallic luster. Pyrite is an important gold-carrying mineral in a gold ore bed, and a large amount of gold ore causes and prospecting information can be provided by measuring the As content in pyrite, so that the method has very important practical application value for rapidly measuring the As content in pyrite.
As element content test in pyrite is mainly based on electron probe or laser ablation plasma mass spectrometry at present, and has the defects of complex preparation work, complex instrument operation, sample damage and the like. There is therefore a need for a new technical way which can be rapidly characterized and results reliable.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a method for quantitatively analyzing the As content in pyrite by utilizing mineral Raman parameters, which has the advantages of simple operation, less sample preparation time and high test speed; the quantitative analysis method for the As content in pyrite by utilizing the mineral Raman parameters can improve the identification accuracy.
The aim of the invention is realized by the following technical scheme: the quantitative analysis method for the As content in pyrite by utilizing the mineral Raman parameters comprises the following steps:
s1, performing pyrite Raman spectrum imaging scanning: scanning the pyrite sample to be detected by adopting an incident light source with the wavelength of 556nm to obtain a Raman image of the pyrite sample to be detected;
s2, carrying out peak-splitting fitting on the Raman image, fitting out Ag Raman displacement values of each point on the image, and making an accurate imaging distribution diagram of the sample about the Ag Raman displacement values;
s3, carrying out an electronic probe scanning test on the pyrite sample to be tested, and measuring a Raman imaging image of the As content in the same area of the sample;
s4, performing image processing and data conversion: firstly, performing Photoshop calibration and matching on an accurate imaging distribution diagram about Ag Raman shift value and an As content Raman imaging diagram, and then converting the two images into data diagrams by using origin data processing software;
s5, a scatter diagram of a Cartesian coordinate system is made through an electronic probe and a Raman imaging data diagram, the quantitative relation between Ag Raman displacement and the As content in pyrite is analyzed, and an equation is fitted.
Further, in the step S1, a LabRAM HR Evolution laser confocal micro-raman spectrometer manufactured by the company HORIBA JOBIN YVON in france is adopted to scan the mineral sample to be detected, and the spectral resolution is 0.65cm -1 The focal length of the spectrometer is 800mm, ar with 556nm is adopted + Laser, 10 times Leica objective lens, scanning range is 300-400 -1 cm。
Further, the pyrite sample to be tested needs to meet the following three characteristic peak bands identified by pyrite: at 343cm -1 On displacement of Fe- [ S 2 ] 2- Deformation vibration, eg for short; at 379cm -1 On displacement of Fe- [ S 2 ] 2- Stretching vibration, abbreviated as Ag; at 430cm -1 S-S stretching vibration on displacement, namely Tg; and the lithology and microscopy observations did not show any phase change process and oxidation.
Further, in the step S1, the number of the points of the x and y axes of the mineral Raman scanning area are 7.4 μm and 6.8 μm respectively, and the length and width of the mineral Raman scanning area are 806.5 μm and 472.38 μm respectively.
Further, in the step S2, the software used for determining the Ag shift value of each point by peak-by-peak fitting is the peak clipping method in labspec6 of HORIBA JOBIN YVON in france.
Further, in the step S3, an electron probe is scanned by using a JEOL-JXA-8230 micro-area X-ray spectrum analyzer manufactured by Japan electronics company and a 10-time objective lens under the conditions of 20KV and 20nA, and the number step sizes of the X-axis point and the y-axis point of the scanning area are respectively 2.5 mu m and 2.5 mu m.
Further, in the step S4, the sizes of the two imaging images are the same, and the numbers of data points converted from the two imaging images are the same. The two imaging images are converted into data points according to gray images and the black-white brightness of the pixel points, and are converted into real data according to the legends of the original images.
The beneficial effects of the invention are as follows: according to the invention, quantitative analysis is carried out on the As content in pyrite by utilizing the mineral Raman parameters, and only the region where the sample is located is needed to be found out, so that the operation is simple; the data is rich, the sample preparation time is short, and the test speed is high; the Raman spectrum characteristic signal is strong, the signal-to-noise ratio is high, the specificity is strong, the recognition accuracy can be improved, and the false recognition is reduced.
Drawings
FIG. 1 is a flow chart of a method for quantitative analysis of the As content of pyrite using mineral Raman parameters;
FIG. 2 is a graph showing the effect of quantitative analysis of the As content in pyrite by Raman shift in the present example;
fig. 3 is a graph of As and Ag shifts divided and fitted with respect to the median of pixel values.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
As shown in fig. 1, the quantitative analysis method for the As content in pyrite by utilizing the mineral raman parameters, disclosed by the invention, comprises the following steps:
s1, performing pyrite Raman spectrum imaging scanning: scanning the pyrite sample to be detected by adopting an incident light source with the wavelength of 556nm to obtain a Raman image of the pyrite sample to be detected; in the step, a LabRAM HR Evolution laser confocal microscopic Raman spectrometer manufactured by French HORIBA JOBIN YVON company is adopted to scan a mineral sample to be detected, and the spectral resolution is 0.65cm -1 The focal length of the spectrometer is 800mm, ar with 556nm is adopted + Laser, 10 times Leica objective lens, scanning range is 300-400 -1 cm。
The pyrite sample to be tested needs to meet the following three characteristic wave peak sections identified by pyrite: at 343cm -1 On displacement of Fe- [ S 2 ] 2- Deformation vibration, eg for short; at 379cm -1 On displacement of Fe- [ S 2 ] 2- Stretching vibration, abbreviated as Ag; at 430cm -1 S-S stretching vibration on displacement, namely Tg; and the lithology and microscopy observations did not show any phase change process and oxidation.
The number of the points of the X-axis and the y-axis of the mineral Raman scanning area are 7.4 mu m and 6.8 mu m respectively, the length and the width of the mineral Raman scanning area are 806.5 mu m and 472.38 mu m respectively, and the total number of the mineral Raman scanning area is 7800 points (including useless background areas).
S2, carrying out peak-splitting fitting on the Raman image, fitting out Ag Raman displacement values of each point on the image, and making an accurate imaging distribution diagram of the sample about the Ag Raman displacement values;
in this step, the software used for determining the Ag displacement value of each point by peak-by-peak fitting is the peak clipping method in labspec6 of HORIBA JOBIN YVON, france, and the obtained imaging image should be a mosaic gray scale image with mosaic points of 2 μm by 2 μm.
S3, carrying out an electronic probe scanning test on the pyrite sample to be tested, and measuring a Raman imaging image of the As content in the same area of the sample;
in this step, an electron probe was scanned by using a JEOL-JXA-8230 micro field X-ray spectrometer produced by Japanese electronics company and a 10-fold objective lens under the conditions of 20KV and 20nA, the number of scanning points in the scanning area X and y axes were 2.5 μm and 2.5 μm, respectively, and the number of scanning points was 201930 (including useless background areas).
The As content of the invention comprises the common As content in pyrite such As Co, ni, au, as, and the sample in the test result needs to have only one As content in the main influence such As Co, ni or As, and the other As content should be lower or not.
S4, performing image processing and data conversion: firstly, performing Photoshop calibration and matching on an accurate imaging distribution diagram about Ag Raman shift value and an As content Raman imaging diagram, and then converting the two images into data diagrams by using origin data processing software;
in this step, firstly, the useless background area in the two images is deleted, then the sizes of the two images are adjusted to be the same, and the number of data points converted by the two imaging images is kept the same (scanning points which cannot correspond to the positions in the two images can be deleted). The two imaging images are converted into data points according to gray images and the black-white brightness of the pixel points, and are converted into real data according to the legends of the original images.
S5, a scatter diagram of a Cartesian coordinate system is made through an electronic probe and a Raman imaging data diagram, the quantitative relation between Ag Raman displacement and the As content in pyrite is analyzed, and an equation is fitted.
The recognition effect of the present invention is further verified by experiments as follows.
Control group: elemental analysis testing was performed on As in pyrite samples using an electron probe. The sample sources of the control group and the experimental group are the same region of the same sample.
According to the analysis of the imaging data of the electronic probe, the sample is selected to test the As content, which is common As content in pyrite such As Co, ni, au, as and the like, and the sample in the test result needs to have only one As content which has a dominant influence such As Co, ni or As, and other As content should have lower or no content.
Experimental group: a 556nm laser light source is selected, a lens with a focal length of 10 times is adopted as an objective lens, and Raman scanning is performed on the same sample and the same region after a target field of view is found.
The pyrite sample wafer, which has been tested for electronic probes, is placed under the field of view of the objective lens of the stage and the same area is tested.
Measuring a Raman imaging diagram of the region, wherein the Raman shift scanning range is 300-400 cm -1 Scanning is performed.
After the test is completed, the data is processed by using a peak clipping method in labspec6 of HORIBA JOBIN YVON company, and the obtained mosaic gray scale Ag displacement imaging graph has a peak clipping range of 378cm -1 ～380cm -1 。
The method comprises the steps of performing image processing and data conversion by using software such as Photoshop and origin, firstly performing Photoshop calibration and matching on two imaging images of a region, and then performing image data conversion operation on the two imaging images by using origin data processing software.
Quantitative analysis of raman Ag peak shift for the As content in pyrite was analyzed by making a scatter plot of cartesian coordinates with electron probe and raman imaging map scan data of mineral samples.
The detection of the Raman shift of pyrite Fe-S stretching vibration 379cm-1 (Ag) in the area of 300-4000-1 cm can indicate the change of the As content in the pyrite. In pyrite, changes in As content tend to cause changes in mineral structure, such As bond length, bond energy changes.
As enters the pyrite lattice in a similar form to form an arsenic-rich pyrite and an arsenic-rich girdle. The position of arsenic-substituted sulfur in the lattice is [ S-As ] when sulfur is combined in the lattice] 3- Its bond [ S-S] 2- The vibration frequency shifts to low frequency, and for diatomic molecules, the Raman shift is present(c is the speed of light, k is the bond force constant, μ is the folded mass) when As and S are gradually combined to form [ S-As] 3- And before [ S-S] 2- In contrast, electronegativity is increased, covalent bonds transition to ionic bonds, so that the value of the bond force constant k becomes smaller, and on the other hand, as the relative atomic mass of As is far greater than S, the folded mass mu thereof is increased, so that the vibration frequency is reduced, and the vibration frequency moves to low frequency.
Therefore, when the Ag Raman shift increases, it is indicated that the As content in pyrite at the point or region increases.
Therefore, the quantitative relation between the Raman shift and the As content can be found out by analyzing the Raman shift and big data fitting of the electronic probe imaging, and the change condition of the As content is further indicated.
Fig. 2 is a plot of As and Ag displacements versus pixel values, and because of the large data volume, it is necessary to further integrate the data, divide the data by median (fig. 3), fit the equation one-dimensional multiple times, and fit the quantitative equation negative correlation of raman displacement versus As content. From this, it can be seen that the raman shift of pyrite (x-axis) and the As content in pyrite measured by the electron probe (y-axis) overall exhibit a clear inverse relationship, suggesting that the raman shift is approximately coincident with the electron probe for the indication of As content.
Then we can estimate the As content by Raman Ag displacement, first test the Raman Ag displacement value at a certain point of pyrite, and convert the obtained Ag displacement value into pixel value to be brought into the equation of FIG. 3, and obtain the pixel value of As with respect to the content. And then converting the pixel value by using a formula, and finally estimating the As content of the pyrite at the position. Therefore, the quantitative analysis result of the invention for the As content in pyrite by utilizing the mineral Raman parameter is reliable.
Those of ordinary skill in the art will recognize that the embodiments described herein are for the purpose of aiding the reader in understanding the principles of the present invention and should be understood that the scope of the invention is not limited to such specific statements and embodiments. Those of ordinary skill in the art can make various other specific modifications and combinations from the teachings of the present disclosure without departing from the spirit thereof, and such modifications and combinations remain within the scope of the present disclosure.
Claims (7)
1. The quantitative analysis method for the As content in pyrite by utilizing the mineral Raman parameters is characterized by comprising the following steps:
s1, performing pyrite Raman spectrum imaging scanning: scanning the pyrite sample to be detected by adopting an incident light source with the wavelength of 556nm to obtain a Raman image of the pyrite sample to be detected; the pyrite sample to be tested needs to meet the following three characteristic wave peak sections identified by pyrite: at 343cm -1 On displacement Fe- [ S2] 2 Deformation vibration, eg; at 379cm -1 On displacement Fe- [ S2] 2 -stretching vibration, ag for short; at 430cm -1 S-S stretching vibration on displacement, namely Tg; and the lithology and microscope observation do not show any phase change process and oxidation;
s2, carrying out peak-splitting fitting on the Raman image, fitting out Ag Raman displacement values of each point on the image, and making an accurate imaging distribution diagram of the sample about the Ag Raman displacement values;
s3, carrying out an electronic probe scanning test on the pyrite sample to be tested, and measuring a Raman imaging image of the As content in the same area of the sample;
s4, performing image processing and data conversion: firstly, performing Photoshop calibration and matching on an accurate imaging distribution diagram about Ag Raman shift value and an As content Raman imaging diagram, and then converting the two images into data diagrams by using origin data processing software;
s5, making a scatter diagram of a Cartesian coordinate system through an electronic probe and a Raman imaging data diagram, analyzing the quantitative relation between Ag Raman displacement and the As content in pyrite, and fitting an equation.
2. The quantitative analysis method for As content in pyrite by utilizing mineral Raman parameters according to claim 1, wherein in the step S1, a LabRAM HR Evolution laser confocal micro Raman spectrometer manufactured by French HORIBA JOBIN YVON company is adopted to scan a mineral sample to be detected, and the spectral resolution is 0.65cm -1 The focal length of the spectrometer is 800mm, ar with 556nm is adopted + Laser, 10 times Leica objective lens, scanning range is 300-400 -1 cm。
3. The quantitative analysis method for As content in pyrite by utilizing the Raman parameters of minerals according to claim 1, wherein in the step S1, the number of steps of the x-axis and the y-axis points of the Raman scanning area of minerals are 7.4 μm and 6.8 μm respectively, and the length and the width of the steps are 806.5 μm and 472.38 μm respectively.
4. The quantitative analysis method for the As content in pyrite by utilizing the mineral Raman parameters according to claim 1, wherein in the step S2, the software adopted for determining the Ag displacement value of each point by peak-by-peak fitting is a peak clipping method in labspec6 of the company HORIBA JOBIN YVON in France.
5. The quantitative analysis method for As content in pyrite by utilizing mineral Raman parameters according to claim 1, wherein in the step S3, a JEOL-JXA-8230 micro-area X-ray spectrum analyzer manufactured by Japanese electronics company is adopted, an objective lens of 10 times is adopted, an electronic probe is adopted to conduct surface scanning under the conditions of 20KV and 20nA, and the number step sizes of the X-axis point and the y-axis point of a scanning area are respectively 2.5 μm and 2.5 μm.
6. The quantitative analysis method for the As content in pyrite using the mineral Raman parameters according to claim 1, wherein in the step S4, two imaging images are processed into gray-scale mosaic images with the same size and consistent pixel points.
7. The quantitative analysis method for the As content in pyrite by utilizing the mineral Raman parameters according to claim 1, wherein in the step S4, two imaging images are converted into data points according to gray level images and the size of black-white brightness of pixel points, and are converted into real data according to the legend of each original image.
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