Method, system, equipment and medium for determining impurity components in graphite ore

Abstract

The invention discloses a method, a system, equipment and a medium for determining impurity components in graphite ore, and relates to the technical field of component determination. The method comprises the following steps: preparing a standardized sample; respectively measuring a to-be-measured sample and the standardized sample by using an X-ray fluorescence spectrophotometer, and determining the elemental analysis line intensity of the to-be-measured sample and the elemental analysis line intensity of the standardized sample; performing regression analysis on the elemental analysis line intensity of the standardized sample by using a mathematical correction mode, and determining related parameters; the related parameters comprise a calibration curve constant and a spectral line overlapping interference correction coefficient; and content calculation is carried out based on the elemental analysis line strength of the sample piece to be detected and the related parameters, and the impurity components in the target graphite ore are obtained. The method provided by the invention can improve the determination precision of impurity components in graphite ore.

Description

Technical Field

[0001] The present invention relates to the technical field of component determination, and in particular to a method, system, equipment and medium for determining impurity components in graphite ore. Background Art

[0002] In the current booming graphite industry, graphite ore, a key raw material for the production of numerous graphite products, has a quality that directly determines the performance and application range of the final product. The content of impurities in graphite ore is one of the core indicators of its quality. Accurately measuring these impurities is crucial for graphite ore grading and pricing, production process optimization, and strict product quality control.

[0003] Currently, numerous methods exist for determining impurity components in graphite ore. Traditional methods, such as chemical analysis, while highly accurate, suffer from numerous drawbacks, including cumbersome and complex procedures, lengthy analysis cycles, high technical requirements for laboratory personnel, and potential environmental pollution during analysis. With the continuous advancement of modern analytical technology, X-ray fluorescence spectrometry, with its significant advantages such as rapidity, non-destructiveness, simultaneous analysis of multiple elements, and relative ease of operation, has become increasingly widely used in the field of elemental analysis.

[0004] However, the actual application of X-ray fluorescence spectrometry for impurity component analysis in graphite ore presents numerous technical challenges. On the one hand, due to the influence of the graphite ore matrix effect, complex interactions occur between different elements and between elements and the matrix, resulting in a non-linear relationship between the measured elemental analysis line intensity and the actual element content. This poses significant difficulties in accurately determining the impurity component content. On the other hand, during X-ray fluorescence spectrometry analysis, spectral line overlap interference often occurs, meaning that the characteristic X-ray spectral lines of certain elements overlap, making it difficult to accurately measure the spectral line intensity of the target element, which in turn affects the accuracy of the impurity component analysis results. Summary of the Invention

[0005] The purpose of the present invention is to provide a method, system, equipment and medium for determining impurity components in graphite ore, which can improve the determination accuracy of impurity components in graphite ore.

[0006] To achieve the above object, the present invention provides the following solutions:

[0007] A method for determining impurity components in graphite ore, comprising:

[0008] Preparation of standardized samples;

[0009] Using an X-ray fluorescence spectrometer to measure the sample to be tested and the standardized sample respectively, and determining the elemental analysis line intensity of the sample to be tested and the elemental analysis line intensity of the standardized sample;

[0010] Performing regression analysis on the elemental analysis line intensity of the standardized sample using a mathematical correction model to determine relevant parameters; the relevant parameters include a calibration curve constant and a spectral line overlap interference correction coefficient;

[0011] The content is calculated based on the element analysis line intensity of the sample to be tested and the relevant parameters to obtain the impurity components in the target graphite ore.

[0012] Optionally, the preparation process of the standardized sample is:

[0013] The sample was first ashed and then melted at 1150°C on an automatic flame melting machine using a melting method to prepare a standardized sample; wherein, in the melting method, anhydrous lithium tetraborate was used as a flux, ammonium nitrate was used as an oxidant, lithium bromide was used as a release agent, and the mass ratio of the sample to the flux was 1:7.

[0014] Optionally, the sample is first ashed and then melted at 1150° C. on an automatic flame melting machine by a melting method to prepare a standardized sample. Specifically, the process is as follows:

[0015] Weigh 0.7 g of sample into a magnetic crucible, place it in the center of a muffle furnace, gradually heat it from low temperature to 800°C, and burn it for 30 minutes. Take it out, cool it slightly, and move it into a desiccator to room temperature. Add 7.0 g of anhydrous lithium tetraborate-lithium metaborate mixed flux, stir it evenly, and move it into a platinum-gold alloy crucible. Add 8 drops of saturated ammonium nitrate solution as an oxidant and 2 drops of lithium bromide solution as a release agent. Place it on an automatic flame melting machine and melt and mold it at 1150°C. After the molding is completed, remove the sample, label it, and store it in a desiccator.

[0016] Optionally, the mass ratio of the anhydrous lithium tetraborate-lithium metaborate mixed flux is 67:33.

[0017] Optionally, the setting parameters of the automatic flame melting machine are: sample melting time 240s, mixing time 840s, pouring time 30s, and cooling time 120s.

[0018] Optionally, the mathematical correction mode includes background correction, drift correction and calibration correction.

[0019] Optionally, the content calculation formula is:

[0020] W i =(aI 2 i +bI i +c)(1+∑α ij W j )+∑B ik W k

[0021] Among them, W i represents the content of the analytical element i in the unknown sample after matrix correction; a, b, c represent the calibration curve constants of the analytical element i; I i represents the X-ray intensity of the analyzed element i in the unknown sample; α ij W represents the influence coefficient of coexisting element j on analysis element i; j Indicates the content of coexisting element j; B ik W represents the interference correction coefficient of the spectral line overlap of the interfering element k on the analyzed element i; k Indicates the content of interfering element K.

[0022] The present invention also provides a system for measuring impurity components in graphite ore, comprising:

[0023] Sample preparation unit, used for preparing standardized samples;

[0024] A sample measuring unit, configured to measure the sample to be tested and the standardized sample respectively using an X-ray fluorescence spectrometer, and determine the elemental analysis line intensity of the sample to be tested and the elemental analysis line intensity of the standardized sample;

[0025] A regression analysis unit, configured to perform regression analysis on the elemental analysis line intensity of the standardized sample using a mathematical correction model to determine relevant parameters; the relevant parameters include a calibration curve constant and a spectral line overlap interference correction coefficient;

[0026] The component determination unit is used to calculate the content based on the element analysis line intensity of the sample to be tested and the related parameters to obtain the impurity components in the target graphite ore.

[0027] The present invention also provides an electronic device, comprising a memory and a processor, wherein the memory is used to store a computer program, and the processor runs the computer program to enable the electronic device to execute the above-mentioned method for determining impurity components in graphite ore.

[0028] The present invention also provides a computer-readable storage medium storing a computer program, wherein the computer program, when executed by a processor, implements the above-mentioned method for determining impurity components in graphite ore.

[0029] According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects:

[0030] The present invention discloses a method, system, device, and medium for determining impurity components in graphite ore. The method comprises: preparing a standardized sample; measuring the sample to be tested and the standardized sample separately using an X-ray fluorescence spectrometer, and determining the elemental analysis line intensity of the sample to be tested and the elemental analysis line intensity of the standardized sample; performing regression analysis on the elemental analysis line intensity of the standardized sample using a mathematical correction model to determine relevant parameters; the relevant parameters include a calibration curve constant and a spectral line overlap interference correction coefficient; and calculating the content based on the elemental analysis line intensity of the sample to be tested and the relevant parameters to obtain the impurity components in the target graphite ore. The present invention can improve the accuracy of determining impurity components in graphite ore. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0032] Figure 1 The figure is a schematic flow chart of the method for determining impurity components in graphite ore according to the present invention. DETAILED DESCRIPTION

[0033] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0034] The purpose of the present invention is to provide a method, system, equipment and medium for determining impurity components in graphite ore, which can improve the determination accuracy of impurity components in graphite ore.

[0035] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0036] like Figure 1 As shown, the present invention provides a method for determining impurity components in graphite ore, comprising:

[0037] Step 100: Prepare standardized samples.

[0038] Step 200: Use an X-ray fluorescence spectrometer to measure the sample to be tested and the standardized sample respectively, and determine the elemental analysis line intensity of the sample to be tested and the elemental analysis line intensity of the standardized sample.

[0039] Step 300: Perform regression analysis on the elemental analysis line intensity of the standardized sample using a mathematical correction model to determine relevant parameters; the relevant parameters include a calibration curve constant and a spectral line overlap interference correction coefficient.

[0040] Step 400: Calculate the content based on the element analysis line intensity of the sample to be tested and the relevant parameters to obtain the impurity components in the target graphite ore.

[0041] As a specific implementation method, the specific process shown below is provided.

[0042] Principle: The sample is first ashed. Then, using a fusion method, anhydrous lithium tetraborate is used as a flux, ammonium nitrate as an oxidant, and lithium bromide as a release agent. The mass ratio of sample to flux is 1:7. The sample is melted at 1150°C in a fusion machine to produce a glass sample, which is then measured using an X-ray fluorescence spectrometer.

[0043] The reagents used were a Li₂B₄Oₐ-LiBO₂ mixed flux with a mass ratio of 67:33. Ammonium nitrate and lithium bromide were analytical grade. Instrumentation included an X-ray fluorescence spectrometer, a muffle furnace, and a sample fusion machine. The sample was pre-dried at 105°C for 2 hours, placed in a desiccator, and cooled to room temperature.

[0044] Analysis steps:

[0045] 1. Sample Preparation

[0046] Weigh 0.7g of sample (accurate to 0.1mg) into a magnetic crucible and place it in the center of a muffle furnace. Gradually heat from low temperature to 800°C and ignite for 30 minutes. Remove, cool slightly, and transfer to a desiccator to room temperature. Add 7.0g (accurate to 0.1mg) of anhydrous lithium tetraborate (67%)-lithium metaborate (33%) mixed flux. Stir thoroughly and transfer to a platinum-gold alloy crucible. Add 8 drops of saturated ammonium nitrate solution (oxidant) and 2 drops of lithium bromide solution (10%) (release agent). Place the sample in an automatic flame melting machine with the following parameters: sample melting time 240s, mixing time 840s, pouring time 30s, and cooling time 120s. After molding, remove the sample, label it, and store it in a desiccator to prevent moisture absorption and contamination.

[0047] 2X-ray fluorescence spectrometry analysis

[0048] 2.1 Measurement conditions: The measurement conditions of the elements analyzed are shown in Table 1.

[0049] 2.2 Background correction:

[0050] The background is subtracted using the one-point method. The intensity of the analytical line after subtracting the background is calculated according to formula (1):

[0051] I N =IP -I B (1)

[0052] Where: I N is the intensity of the analytical line after background subtraction; I P is the peak intensity; I B is the background intensity.

[0053] 2.3 Drift correction: Correct instrument drift by measuring standardized samples.

[0054] 2.4 Preparation of calibration series

[0055] Graphite standard materials GBW03119 and GBW03120 were selected; at the same time, in order to ensure that each component has a sufficiently wide content range and an appropriate content gradient to meet the needs of graphite ore sample testing, stream sediments (GBW07301a, GBW07302a, GBW07304a, GBW07305a, GBW07310, GBW07358, GBW07359, GBW07360), soils (GBW07401, GBW07402a, GBW07403-GBW07408), rocks Calibration curves were prepared using 36 national primary reference materials, including GBW07103-GBW07107, GBW07109-GBW07113, GBW07120, GBW07121, and GBW07122, as well as GBW03112a, GBW0113a, GBW03116, GBW03122a, GBW03134, GBW07101, and GBW07102. The content ranges of the calibration curves for each component are shown in Table 2. GBW07423 was selected as the standardization sample for drift correction. The content ranges of each component in the reference materials / samples are shown in Table 2.

[0056] 2.5 Calibration and correction

[0057] Calibration, matrix effect correction and spectral line overlap interference correction are performed by mathematical regression. The calculation formula is:

[0058] W i =(aI 2 i +bI i +c)(1+∑α ij W j )+∑B ik W k (2)

[0059] Among them, W i represents the certified value of the analytical element i in the standard substance (or the content of the analytical element i in the unknown sample after matrix correction); b and c represent the calibration curve constants of the analytical element i; Ii represents the X-ray intensity (or internal standard intensity ratio) of the analyzed element i in the standard substance (or unknown sample); α ij W represents the influence coefficient of coexisting element j on the analyzed element i (theoretical α coefficient); j Indicates the content of coexisting element j; B ik W represents the interference correction coefficient of the spectral line overlap of the interfering element k on the analyzed element i; k Indicates the content of interfering element K (or the intensity of X-rays).

[0060] The recommended value of element i of the reference material is corrected for matrix effects by the theoretical α coefficient to obtain the apparent content. The measured intensity and apparent content of the analyzed element are then used to calculate the calibration curve constant using regression calculation using formula (2).

[0061] As a specific measurement embodiment, the following process and results are provided.

[0062] Enter the measurement conditions of the analytical elements, the theoretical α coefficient and the content of each substance in the standard substance (recommended value). Also enter the name of the standardized sample and measure the elemental analysis line intensity of the standardized sample. Then enter the name of the standard substance and measure the elemental analysis line intensity of the standard substance. After measuring the intensity of each analytical element in a series of standard samples, use the mathematical correction mode for regression analysis to obtain the calibration curve constants a, b, c and the spectral line overlap interference correction coefficient B. ik Store in computer software.

[0063] Measuring unknown samples: Enter the name of the unknown sample. First measure the standard sample, then measure the intensity of the element analysis line of the unknown sample.

[0064] Result calculation: The intensity of the analytical element of the unknown sample is measured, and the computer software calculates the content according to formula (2) and automatically prints out the analysis results.

[0065] Precision: Two graphite ore reference materials, GBW03119 and GBW03120, were selected and the contents of Al2O3, SiO2, TFe2O3, MgO, CaO, K2O, Na2O, TiO2, MnO, and P2O5 were determined according to the experimental method. Twelve parallel determinations were performed to examine the precision of the method. The results are shown in Table 3. Table 3 shows that the relative standard deviations (RSDs, n=12) of the determination results for the ten components were all less than 1%.

[0066] The above Tables 1 to 3 are as follows:

[0067] Table 1 XRF measurement conditions

[0068] Table1 Analytical parameters of XRF

[0069]

[0070] Table 2 Content range of each component in standard substances / samples

[0071] Table 2 Content range of each component in CRMs ω / %

[0072]

[0073] Table 3 Determination results of 10 components in graphite ore standard material (n=12)

[0074] Table 3 Determination results of 10components in graphite orecertified reference materials ω / %

[0075]

[0076] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0077] This document uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only intended to help understand the core concept of the present invention. At the same time, those skilled in the art will find that the specific implementation methods and application scopes may vary based on the concept of the present invention. In summary, the contents of this specification should not be construed as limiting the present invention.

Claims

1. A method for determining impurity components in graphite ore, characterized in that: include: Preparation of standardized samples; Using an X-ray fluorescence spectrometer to measure the sample to be tested and the standardized sample respectively, and determining the elemental analysis line intensity of the sample to be tested and the elemental analysis line intensity of the standardized sample; Performing regression analysis on the elemental analysis line intensity of the standardized sample using a mathematical correction model to determine relevant parameters; the relevant parameters include a calibration curve constant and a spectral line overlap interference correction coefficient; The content is calculated based on the element analysis line intensity of the sample to be tested and the relevant parameters to obtain the impurity components in the target graphite ore.

2. The method for determining impurity components in graphite ore according to claim 1, wherein The preparation process of the standardized sample is as follows: The sample was first ashed and then melted at 1150°C on an automatic flame melting machine using a melting method to prepare a standardized sample; wherein, in the melting method, anhydrous lithium tetraborate was used as a flux, ammonium nitrate was used as an oxidant, lithium bromide was used as a release agent, and the mass ratio of the sample to the flux was 1:

7.

3. The method for determining impurity components in graphite ore according to claim 2, wherein The process of first ashing the sample and then melting it at 1150°C on an automatic flame melting machine to prepare the standardized sample is as follows: Weigh 0.7 g of sample into a magnetic crucible, place it in the center of a muffle furnace, gradually heat it from low temperature to 800°C, and burn it for 30 minutes. Take it out, cool it slightly, and move it into a desiccator to room temperature. Add 7.0 g of anhydrous lithium tetraborate-lithium metaborate mixed flux, stir it evenly, and move it into a platinum-gold alloy crucible. Add 8 drops of saturated ammonium nitrate solution as an oxidant and 2 drops of lithium bromide solution as a release agent. Place it on an automatic flame melting machine and melt and mold it at 1150°C. After the molding is completed, remove the sample, label it, and store it in a desiccator.

4. The method for determining impurity components in graphite ore according to claim 3, wherein The mass ratio of the anhydrous lithium tetraborate-lithium metaborate mixed flux is 67:

33.

5. The method for determining impurity components in graphite ore according to claim 3, wherein The setting parameters of the automatic flame melting machine are: sample melting time 240s, mixing time 840s, pouring time 30s, and cooling time 120s.

6. The method for determining impurity components in graphite ore according to claim 1, wherein The mathematical correction mode includes background correction, drift correction and calibration correction.

7. The method for determining impurity components in graphite ore according to claim 1, wherein The formula for calculating the content is: W i =(aI 2 i +bI i +c)(1+∑α ij W j )+∑B ik W k Among them, W i represents the content of the analytical element i in the unknown sample after matrix correction; a, b, c represent the calibration curve constants of the analytical element i; I i represents the X-ray intensity of the analyzed element i in the unknown sample; α ij W represents the influence coefficient of coexisting element j on analysis element i; j Indicates the content of coexisting element j; B ik W represents the interference correction coefficient of the spectral line overlap of the interfering element k on the analyzed element i; k Indicates the content of interfering element K.

8. A system for measuring impurity components in graphite ore, characterized in that: include: Sample preparation unit, used for preparing standardized samples; A sample measuring unit, configured to measure the sample to be tested and the standardized sample respectively using an X-ray fluorescence spectrometer, and determine the elemental analysis line intensity of the sample to be tested and the elemental analysis line intensity of the standardized sample; A regression analysis unit, configured to perform regression analysis on the elemental analysis line intensity of the standardized sample using a mathematical correction model to determine relevant parameters; the relevant parameters include a calibration curve constant and a spectral line overlap interference correction coefficient; The component determination unit is used to calculate the content based on the element analysis line intensity of the sample to be tested and the related parameters to obtain the impurity components in the target graphite ore.

9. An electronic device, characterized in that: The electronic device comprises a memory and a processor, wherein the memory is used to store a computer program, and the processor runs the computer program to enable the electronic device to perform the method for determining impurity components in graphite ore according to any one of claims 1 to 7.

10. A computer-readable storage medium, characterized in that The computer program is stored therein, and when the computer program is executed by a processor, the method for determining the impurity components in the graphite ore according to any one of claims 1 to 7 is implemented.

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