Method for determining and analyzing primary and secondary elements in dolomite and magnesite based on ICP-AES
Through the ICP-AES method, the matrix effect problem during the determination and analysis of primary and secondary elements in dolomite and magnesite was solved. Through pretreatment and calibration curve drawing, interference factors are calculated and deviations are evaluated, and more accurate and stable measurement results are achieved.
Patent Information
- Application Number
- CN202510847270.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-24
- Publication Date
- 2025-08-15
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
In the prior art, when the primary and secondary elements of dolomite and magnesite are measured and analyzed, the matrix effect between different elements leads to deviations in the measurement results, how to weaken the interference of matrix effect and improve the accuracy of the measurement analysis.
Through the ICP-AES method, pre-treatment data of dolomite and magnesite samples were obtained, calibration curves were drawn, spectral line interference was analyzed, element intensity and concentration interference factors were calculated, deviation degree was evaluated, and correction measures were taken, such as adjusting the measurement conditions and optimizing sample pre-treatment to reduce matrix interference.
The accuracy and stability of the determination of primary and secondary elements in dolomite and magnesite are improved, ensuring that the measurement results reflect the true content of elements in the sample, and achieving stricter quality control and consistency of analytical batches.
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Figure CN120490064A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of determination and analysis of major and minor elements, and in particular to a determination and analysis method of major and minor elements in dolomite and magnesite based on ICP-AES. Background Art
[0002] Dolomite and magnesite are calcium and magnesium salt minerals widely distributed in nature. Their chemical composition primarily contains calcium, magnesium, and silicon, as well as manganese, aluminum, phosphorus, and iron. In steel and metallurgical enterprises, dolomite and magnesite are primarily used for slag formation and refractory materials during iron and steelmaking. Their quality directly impacts the quality of finished products and equipment safety during steelmaking. Therefore, accurate and rapid determination of the elements in dolomite and magnesite is crucial. ICP-AES (Inductively Coupled Plasma Atomic Emission Spectroscopy) is a highly efficient elemental analysis method that can quickly and accurately determine the major and minor element contents in dolomite and magnesite, providing strong data support for mineral quality assessment, industrial applications, and scientific research.
[0003] In the existing technology, when determining and analyzing major and minor elements in dolomite and magnesite, the interaction between different elements can easily lead to matrix effects, which in turn causes deviations in the measurement results. Therefore, how to weaken the interference of matrix effects between different elements, evaluate the degree of deviation in the measurement and analysis, and improve the accuracy of the determination and analysis of major and minor elements are the problems we need to solve. To this end, a method for the determination and analysis of major and minor elements in dolomite and magnesite based on ICP-AES is proposed. Summary of the Invention
[0004] The present invention aims to provide an analytical method for determining major and minor elements in dolomite and magnesite based on ICP-AES, so as to solve the problems raised in the above-mentioned background technology.
[0005] In order to solve the above technical problems, the technical solution adopted by the present invention is: The ICP-AES analysis method for the determination of major and minor elements in dolomite and magnesite includes the following steps: Step 1: obtaining dolomite and magnesite test samples, and pre-treating the test samples to reduce interfering substances in the matrix; Step 2: Obtain the spectral interference of each element based on the measured sample, and draw the calibration curve of each element to obtain the interference of the calibration curve of each element, ensuring that the calibration curve has a good linear relationship within the linear range and the correlation coefficient is not less than 0.999; Step 3: ICP-AES is performed on the pre-processed measurement data to obtain characteristic spectral lines, and the content of each element is calculated based on the characteristic spectral lines. At the same time, the measurement data of the measurement sample is obtained, including the emission intensity and concentration of each element; Step 4: sorting the measurement data and extracting the measurement interference factors, specifically the element intensity interference factor and the element concentration interference factor; Step 5: Analyze the measurement data and combine the measurement interference factors to obtain the element intensity interference index and element concentration interference index, evaluate the deviation degree of the measurement data, and obtain the measurement report at the same time; Step 6: Obtain the deviation assessment coefficient based on the element intensity interference index and the element concentration interference index, and determine the different deviation levels of the element determination deviation in combination with the measurement data. Set deviation assessment thresholds for different deviation levels and generate an assessment report at the same time, including the content of each element, the degree of deviation, and possible interference factors. Corrective measures are formulated, such as adjusting the measurement conditions, optimizing the sample pretreatment steps, etc., to improve the measurement accuracy.
[0006] A further improvement of the technical solution of the present invention is that in step 1, the process of obtaining the measurement sample is as follows: Step 101: Collect samples from dolomite and magnesite ores, crush and grind the collected samples to achieve an appropriate particle size, thereby reducing the particle size and increasing the contact area between the sample and the digestion acid, thereby facilitating subsequent digestion and measurement; Step 102: weighing dolomite and magnesite samples, and adding a digestion acid, such as hydrochloric acid or nitric acid, to the weighed samples. The type and amount of the digestion acid should be determined based on the properties of the sample, the matrix composition, and the requirements for the element to be determined. Generally, the selection and amount of the digestion acid should be able to completely digest the sample and minimize interfering substances in the matrix. The sample with the added digestion acid is placed on a heating device, such as a hot plate or a digestion tank, for heating and digestion, and the heating temperature and time are controlled to ensure complete digestion of the sample and reduce the generation of impurities. Step 103: adding a diluent, such as water, dilute hydrochloric acid or dilute nitric acid, to the digested sample to dissolve the residue and adjust the acidity and volume of the solution; Step 104 , filtering the adjusted test sample to remove impurities to obtain a test solution.
[0007] A further improvement of the technical solution of the present invention is that in step 2, the process of drawing the calibration curve of each element is: Step 201: Using pretreated dolomite and magnesite samples for measurement, the ICP-AES radio frequency power, carrier gas flow rate, and observation height are set. The radio frequency power should be selected to ensure that the plasma is stable and can effectively excite the elements in the sample. A carrier gas flow rate that is too fast or too slow may affect the accuracy of the measurement results. The observation height should be selected to capture the strongest characteristic spectral line signal. Step 202: Use the configured ICP-AES instrument to perform a spectral line scan on the sample to obtain the characteristic spectral line of each element and record the position of the characteristic spectral line of each element. At the same time, check for spectral line overlap and mark interfering spectral lines. For elements with interference, it is necessary to select an appropriate analysis line to avoid the influence of interfering substances. Step 203: Prepare a standard solution containing the major and minor elements in dolomite and magnesite, and draw a calibration curve for each element based on the characteristic spectral lines, with the concentration of the standard solution as the abscissa and the intensity of the characteristic spectral lines as the ordinate. The calibration curve should have a good linear relationship, and the correlation coefficient should be close to 1. Step 204 , observe the shape and trend of the calibration curve and check whether there are nonlinearities, bends or abnormal points in combination with the interference spectrum, obtain the interference elements, and evaluate the influence of the interference elements on the calibration curve.
[0008] A further improvement of the technical solution of the present invention is that in step 3, the process of obtaining the measurement data of the measurement sample is: Step 301: Process the detected characteristic spectral line data using an ICP-AES instrument, including subtracting background noise and correcting for instrument drift, and calculating the content of each element based on the intensity of the characteristic spectral line and the corresponding calibration curve; Step 302: record the element content of each measured sample, obtain measurement data and measurement sequence table, including sample number, element name, content, wavelength, intensity, element content and other information of characteristic spectrum line.
[0009] A further improvement of the technical solution of the present invention is that in step 4, the process of extracting and measuring interference factors is: Step 401: Obtain the raw data of all measured samples, including the intensity and wavelength of the characteristic spectral lines of each element, and integrate them into a unified data set. Step 402: Clean the integrated data set, analyze the characteristic spectral lines of each element, obtain interference spectral lines, calculate the ratio of the actual intensity of the characteristic spectral line of the test solution to the characteristic spectral line of the standard solution, and obtain the intensity interference factor; Step 403 compares the concentrations of target elements in different measurement samples, analyzes the relationship between concentration changes and interference factors, and performs feature extraction for chemical interference, physical interference, and ionization interference, respectively, to obtain concentration interference factors. Chemical interference may involve the generation of compounds that are difficult to volatilize or dissociate, and features are extracted by analyzing the generation conditions of these compounds; physical interference may involve sample dilution, viscosity changes, etc., and features are extracted by measuring changes in these physical quantities; ionization interference may involve changes in the degree of ionization, and features are extracted by analyzing changes in ionization energy.
[0010] The further improvement of the technical solution of the present invention is that: step 501, according to the intensity and wavelength information of the characteristic spectrum line, the correction intensity value of each element is calculated to eliminate the influence of the interference spectrum line; Step 502, using the corrected characteristic line intensity value, calculate the ratio of the actual intensity of the characteristic line of the test solution to the intensity of the characteristic line of the standard solution to obtain the element intensity interference index; Step 503, calculating the element concentration interference index based on the measurement sequence table in the measurement data and in combination with the element concentration interference factor; Step 504 , combining the element intensity interference index and the element concentration interference index, calculating the degree of dispersion of the measurement data, evaluating the degree of deviation of the measurement data, and arranging the measurement data, the element intensity interference index and the element concentration interference index, and the degree of deviation to generate a measurement report.
[0011] A further improvement of the technical solution of the present invention is that the calculation formula of the element intensity interference index is: ; Where I is the element intensity interference index, is the actual intensity of the characteristic spectrum line of the solution to be tested, is the baseline intensity of the characteristic spectrum of the standard solution, k is a proportional constant used to adjust the influence of the exponential function, C is the concentration of the element in the solution to be tested, is the reference concentration of the element in the standard solution, a is the base of the logarithm, and is usually greater than 0 and not equal to 1; The calculation formula of the element concentration interference index is: ; Where N is the element concentration interference index, To measure the concentration of an element in a solution, is the baseline concentration of the element in the standard solution, i is a proportional constant used to adjust the influence of the exponential function, and b is the base of the logarithm, which is usually greater than 0 and not equal to 1.
[0012] A further improvement of the technical solution of the present invention is that in step 6, the process of obtaining the deviation assessment coefficient and the assessment report is as follows: Step 601: combining the element intensity interference index and the element concentration interference index to analyze the correlation between the interference degree during element determination and the element intensity interference index and the element concentration interference index; Step 602: assign different weights to the element intensity interference index and the element concentration interference index, perform weighted calculation on the two indices, and obtain a deviation evaluation coefficient; Step 603: setting different deviation levels according to the degree of deviation of the measured data, namely slight deviation level, moderate deviation level, and severe deviation level; Step 604 , matching different deviation levels with deviation assessment coefficients, and setting deviation assessment thresholds for different deviation levels; Step 605, organize the collected measurement data, calculated deviation assessment coefficients and divided deviation levels, and write an assessment report, including information such as data source, data processing method, calculation process of deviation assessment coefficients, basis for deviation level division and deviation level of each sample, and perform interference source analysis on the measurement of bias deviation, obtain analysis results, and take corresponding corrective measures. For example, if the interference comes from contamination in the sample preparation process, the sample preparation process can be optimized; if the interference comes from errors in instruments and equipment, the instruments and equipment can be calibrated and maintained.
[0013] A further improvement of the technical solution of the present invention is that the calculation formula of the deviation evaluation coefficient is: ; Where D is the deviation evaluation coefficient, I is the element intensity interference index, N is the element concentration interference index, and is a constant used to adjust the influence of the exponential and logarithmic functions.
[0014] A further improvement of the technical solution of the present invention is that: the multiple deviation levels correspond to multiple deviation assessment thresholds, wherein the deviation assessment thresholds include an upper threshold and a lower threshold; The plurality of deviation levels and the plurality of deviation assessment thresholds satisfy the following relationship: Slight deviation from the level ; Moderate deviation level ; Severe deviation level ; Among them, D is the deviation assessment coefficient, T1 is the upper threshold corresponding to the slight deviation level and the lower threshold corresponding to the moderate deviation level, and T2 is the upper threshold corresponding to the moderate deviation level and the lower threshold corresponding to the severe deviation level.
[0015] Due to the adoption of the above technical solution, the present invention has the following technical advancements compared to the prior art: The present invention provides an analytical method for the determination of major and minor elements in dolomite and magnesite based on ICP-AES. By analyzing the interference of spectral lines in detail, the source and influence of the interfering spectral lines are determined, and targeted measures are taken to correct them. At the same time, the element concentration interference factors are evaluated to find concentration measurement deviations caused by factors such as chemical interference, physical interference and ionization interference. These deviations are corrected by optimizing sample pretreatment methods, adjusting instrument operating conditions, and other means. This ensures that the measurement results more accurately reflect the true content of the elements in the sample, thereby improving the reliability and stability of the analytical method.
[0016] The present invention provides an analytical method for the determination of major and minor elements in dolomite and magnesite based on ICP-AES. By using the element intensity interference index and the element concentration interference index, combined with the setting of the deviation assessment coefficient and the deviation level, the interference can be accurately assessed and corrected, and stricter quality control can be achieved. This not only improves the analytical quality of a single sample, but also helps to improve the consistency and accuracy of the entire analytical batch, by analyzing the determination of bias deviation and taking corresponding corrective measures.
[0017] The present invention provides an ICP-AES-based determination and analysis method for major and minor elements in dolomite and magnesite. By optimizing instrument parameters and adopting a suitable calibration method, the ICP-AES-based determination and analysis accurately determines the contents of major and minor elements in dolomite and magnesite. When drawing a calibration curve, a series of standard solutions matching the sample matrix are used to effectively reduce the influence of matrix effects and improve the accuracy of the determination. Through multiple parallel determinations and strict data quality control, the repeatability and reproducibility of the determination results are ensured to be good, and the error range is controlled within an extremely small range. This provides a reliable basis for applications in various fields and makes decisions based on these data more scientific and reasonable. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] In order to more clearly illustrate the embodiments of the present application 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 described in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.
[0019] Figure 1 is a flow chart of the method of the present invention; Figure 2 This is a flow chart for obtaining the element intensity interference index and the element concentration interference index of the present invention; Figure 3 This is a flow chart for obtaining the deviation evaluation coefficient of the present invention. DETAILED DESCRIPTION
[0020] To make the objectives, technical solutions, and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.
[0021] Example 1, as Figures 1 to 3 As shown, the present invention provides an analysis method for determining major and minor elements in dolomite and magnesite based on ICP-AES, comprising the following steps: Step 1, obtain the determination samples of dolomite and magnesite, and pretreat the determination samples to reduce the interfering substances in the matrix; the process of obtaining the determination samples is: collect samples from the ores of dolomite and magnesite respectively, crush and grind the collected samples to achieve an appropriate particle size, so as to reduce the particle size and increase the contact area between the sample and the digestion acid, so as to facilitate subsequent digestion and determination, weigh the dolomite and magnesite samples, and add digestion acid, such as hydrochloric acid, nitric acid, etc., to the weighed samples. The type and amount of the digestion acid should be determined according to the nature of the sample and the matrix composition. The amount of digestion acid should be determined based on the sample size and the requirements of the elements to be determined. Generally, the selection and dosage of the digestion acid should be able to completely digest the sample and minimize interfering substances in the matrix. The sample with the digestion acid added is placed on a heating device for heating digestion, such as a hot plate or a digestion tank, and the heating temperature and time are controlled to ensure complete digestion of the sample and reduce the generation of impurities. Based on the digested sample, a diluent, such as water, dilute hydrochloric acid or dilute nitric acid, is added to dissolve the residue and adjust the acidity and volume of the solution. The adjusted sample is filtered to eliminate impurities to obtain a test solution; Step 2: Obtain the spectral line interference of each element based on the measured sample, draw the calibration curve of each element, obtain the calibration curve interference of each element, ensure that the calibration curve has a good linear relationship within the linear range, and the correlation coefficient is not less than 0.999; the process of drawing the calibration curve of each element is as follows: use pretreated dolomite and magnesite to measure the sample, set the radio frequency power, carrier gas flow rate, and observation height of ICP-AES, among which the selection of radio frequency power should ensure that the plasma is stable and can effectively excite the elements in the sample, and the carrier gas flow rate that is too fast or too slow may affect the accuracy of the measurement result. The selection of observation height should be able to capture the strongest characteristic spectral line signal, and use the set ICP-AES instrument to measure Scan the sample for spectral lines to obtain the characteristic spectral lines of each element, and record the position of the characteristic spectral lines of each element. At the same time, check for spectral line overlap and mark interfering spectral lines. For elements with interference, it is necessary to select appropriate analytical lines to avoid the influence of interfering substances. Prepare standard solutions containing the major and minor elements in dolomite and magnesite, and draw calibration curves for each element in combination with the characteristic spectral lines, with the concentration of the standard solution as the horizontal axis and the intensity of the characteristic spectral lines as the vertical axis. The calibration curve should have a good linear relationship, and the correlation coefficient should be close to 1. Observe the shape and trend of the calibration curve and combine it with the interference spectral lines to check for nonlinearity, bending or abnormal points, obtain the interfering elements, and evaluate the degree of influence of the interfering elements on the calibration curve; Step 3, performing ICP-AES measurement on the pre-processed measurement data to obtain characteristic spectral lines, and calculating the content of each element based on the characteristic spectral lines, and simultaneously obtaining measurement data of the measurement sample, including the emission intensity and concentration of each element; the process of obtaining the measurement data of the measurement sample is: using the ICP-AES instrument to process the detected characteristic spectral line data, including deducting background noise and correcting instrument drift, calculating the content of each element based on the intensity of the characteristic spectral line and the corresponding calibration curve, recording the element content of each measurement sample, obtaining measurement data and a measurement sequence table, including sample number, element name, content, wavelength of the characteristic spectral line, intensity, element content, and other information; Step 4, organize the measurement data and extract the measurement interference factors, specifically the element intensity interference factor and the element concentration interference factor; the process of extracting the measurement interference factors is: obtaining the original data of all the measurement samples, including the characteristic spectral line intensity and wavelength of each element, and integrating them into a unified data set, performing data cleaning on the integrated data set, and analyzing the characteristic spectral lines of each element to obtain the interference spectral lines, calculating the ratio of the actual intensity of the characteristic spectral line of the test solution to the characteristic spectral line of the standard solution, obtaining the intensity interference factor, comparing the concentration of the target element in different measurement samples, analyzing the relationship between the concentration change and the interference factor, performing feature extraction for chemical interference, physical interference and ionization interference respectively, and obtaining the concentration interference factor, wherein chemical interference may involve the generation of compounds that are difficult to volatilize or dissociate, and the features are extracted by analyzing the generation conditions of these compounds; physical interference may involve sample dilution, viscosity change, etc., and the features are extracted by measuring the changes in these physical quantities; ionization interference may involve changes in the degree of ionization, and the features are extracted by analyzing the changes in ionization energy; Step 5, analyzing the measurement data and combining the measurement interference factor to obtain the element intensity interference index and the element concentration interference index, evaluating the deviation degree of the measurement data, and obtaining the measurement report at the same time; the process of obtaining the element intensity interference index and the element concentration interference index is as follows: according to the intensity and wavelength information of the characteristic spectral line, calculating the corrected intensity value of each element to eliminate the influence of the interference spectral line, using the corrected characteristic spectral line intensity value, calculating the ratio of the actual intensity of the characteristic spectral line of the test solution to the intensity of the characteristic spectral line of the standard solution, obtaining the element intensity interference index, according to the measurement sequence table in the measurement data and combined with the element concentration interference factor, calculating the element concentration interference index, combining the element intensity interference index and the element concentration interference index, calculating the discrete degree of the measurement data, evaluating the deviation degree of the measurement data, and arranging the measurement data, the element intensity interference index and the element concentration interference index, and the deviation degree to generate a measurement report; Step 6: obtain the deviation assessment coefficient based on the element intensity interference index and the element concentration interference index, and determine different deviation levels of the element determination deviation in combination with the measurement data, set deviation assessment thresholds for different deviation levels, and generate an assessment report at the same time, including the content of each element, the degree of deviation, and possible interference factors, and formulate corrective measures, such as adjusting the measurement conditions, optimizing the sample pretreatment steps, etc., to improve the measurement accuracy; the process of obtaining the deviation assessment coefficient and the assessment report is as follows: combining the element intensity interference index and the element concentration interference index, analyzing the correlation between the degree of interference during the element determination and the element intensity interference index and the element concentration interference index, assigning different weights to the element intensity interference index and the element concentration interference index, and performing weighted calculation on the two indices to obtain the deviation assessment coefficient. According to the degree of deviation of the measurement data, different deviation levels are set, namely slight deviation level, moderate deviation level, and severe deviation level. Different deviation levels are matched with deviation assessment coefficients, and deviation assessment thresholds are set for different deviation levels. The collected measurement data, calculated deviation assessment coefficients, and divided deviation levels are sorted out, and an assessment report is written, including information such as data source, data processing method, calculation process of deviation assessment coefficient, basis for deviation level division, and deviation level of each sample. Interference source analysis is performed on the measurement of severe deviation, and analysis results are obtained. At the same time, corresponding corrective measures are taken. For example, if the interference comes from contamination in the sample preparation process, the sample preparation process can be optimized; if the interference comes from errors in instruments and equipment, the instruments and equipment can be calibrated and maintained.
[0022] Example 2, as Figures 1 to 3 As shown, based on Example 1, the present invention provides a technical solution: Preferably, the calculation formula of the element intensity interference index is: ; Where I is the element intensity interference index, is the actual intensity of the characteristic spectrum line of the solution to be tested, is the baseline intensity of the characteristic spectrum of the standard solution, k is a proportional constant used to adjust the influence of the exponential function, C is the concentration of the element in the solution to be tested, is the reference concentration of the element in the standard solution, a is the base of the logarithm, and is usually greater than 0 and not equal to 1; The calculation formula of element concentration interference index is: ; Where N is the element concentration interference index, To measure the concentration of an element in a solution, is the baseline concentration of the element in the standard solution, i is a proportional constant used to adjust the influence of the exponential function, and b is the base of the logarithm, which is usually greater than 0 and not equal to 1; The calculation formula of the deviation assessment coefficient is: ; Where D is the deviation evaluation coefficient, I is the element intensity interference index, N is the element concentration interference index, and is a constant used to adjust the influence of exponential and logarithmic functions; The multiple deviation levels correspond to multiple deviation assessment thresholds, wherein the deviation assessment thresholds include an upper threshold and a lower threshold; The multiple deviation levels and the multiple deviation assessment thresholds satisfy the following relationship: Slight deviation from the level ; Moderate deviation level ; Severe deviation level ; Among them, D is the deviation assessment coefficient, T1 is the upper threshold corresponding to the slight deviation level and the lower threshold corresponding to the moderate deviation level, and T2 is the upper threshold corresponding to the moderate deviation level and the lower threshold corresponding to the severe deviation level.
[0023] The above are only specific embodiments of the present application, but the scope of protection of this application is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in this application should be included in the scope of protection of this application. Therefore, the scope of protection of this application should be based on the scope of protection of the claims.
Claims
1. The ICP-AES method for the determination of major and minor elements in dolomite and magnesite is characterized by: The following steps are involved: Step 1: obtaining measurement samples of dolomite and magnesite, and pre-treating the measurement samples; Step 2: Obtain the spectral line interference of each element based on the measured sample, and draw the calibration curve of each element to obtain the calibration curve interference of each element; Step 3: Perform ICP-AES measurement on the pre-processed measurement data to obtain characteristic spectral lines, calculate the content of each element based on the characteristic spectral lines, and simultaneously obtain measurement data of the measurement sample; Step 4: sorting the measurement data and extracting the measurement interference factors, specifically the element intensity interference factor and the element concentration interference factor; Step 5: Analyze the measurement data and combine the measurement interference factors to obtain the element intensity interference index and element concentration interference index, evaluate the deviation degree of the measurement data, and obtain the measurement report at the same time; Step 6: Obtain the deviation assessment coefficient based on the element intensity interference index and the element concentration interference index, and determine different deviation levels of the element measurement deviation in combination with the measurement data. Set deviation assessment thresholds for different deviation levels, generate an assessment report, and formulate corrective measures.
2. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 1, wherein: In step 1, the process of obtaining the measurement sample is as follows: Step 101, collecting samples from dolomite and magnesite ores respectively, and crushing and grinding the collected samples; Step 102, weighing dolomite and magnesite samples, adding digestion acid to the weighed samples, placing the samples with added digestion acid on a heating device for heating and digestion, and controlling the heating temperature and time; Step 103, adding a diluent to the digested sample to dissolve the residue and adjust the acidity and volume of the solution; Step 104 , filtering the adjusted test sample to remove impurities to obtain a test solution.
3. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 2, wherein: In step 2, the process of drawing the calibration curve of each element is as follows: Step 201, using pre-treated dolomite and magnesite samples for measurement, setting the radio frequency power, carrier gas flow rate, and observation height of the ICP-AES; Step 202: Use the configured ICP-AES instrument to perform a spectral line scan on the sample to obtain the characteristic spectral line of each element, record the position of the characteristic spectral line of each element, and simultaneously perform a spectral line overlap check to mark interfering spectral lines. Step 203, preparing a standard solution containing the major and minor elements in dolomite and magnesite, and drawing a calibration curve for each element based on the characteristic spectral lines, with the concentration of the standard solution as the abscissa and the intensity of the characteristic spectral lines as the ordinate; Step 204 , observe the shape and trend of the calibration curve and combine it with the interference spectrum to obtain the interfering elements and evaluate the influence of the interfering elements on the calibration curve.
4. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 3, wherein: In step 3, the process of obtaining the measurement data of the measurement sample is as follows: Step 301: Process the detected characteristic spectral line data using an ICP-AES instrument, and calculate the content of each element based on the intensity of the characteristic spectral line and the corresponding calibration curve; Step 302: Record the element content of each measured sample, and obtain measurement data and a measurement sequence table.
5. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 4, characterized in that: In step 4, the process of extracting and measuring interference factors is as follows: Step 401: Obtain the raw data of all measured samples and integrate them into a unified data set: Step 402: Clean the integrated data set, analyze the characteristic spectral lines of each element, obtain interference spectral lines, calculate the ratio of the actual intensity of the characteristic spectral line of the test solution to the characteristic spectral line of the standard solution, and obtain the intensity interference factor; Step 403 : comparing the concentrations of target elements in different measurement samples, performing feature extraction on chemical interference, physical interference and ionization interference respectively, and obtaining concentration interference factors.
6. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 5, characterized in that: In step 5, the process of obtaining the element intensity interference index and the element concentration interference index is as follows: Step 501, calculating the corrected intensity value of each element based on the intensity and wavelength information of the characteristic spectral line; Step 502, using the corrected characteristic line intensity value, calculate the ratio of the actual intensity of the characteristic line of the test solution to the intensity of the characteristic line of the standard solution to obtain the element intensity interference index; Step 503, calculating the element concentration interference index based on the measurement sequence table in the measurement data and in combination with the element concentration interference factor; Step 504 , combining the element intensity interference index and the element concentration interference index, calculating the degree of dispersion of the measurement data, evaluating the degree of deviation of the measurement data, and arranging the measurement data, the element intensity interference index and the element concentration interference index, and the degree of deviation to generate a measurement report.
7. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 6, characterized in that: The calculation formula of the element intensity interference index is: ; Where I is the element intensity interference index, is the actual intensity of the characteristic spectrum line of the solution to be tested, is the baseline intensity of the characteristic spectrum of the standard solution, k is a proportional constant, C is the concentration of the element in the solution to be tested, is the reference concentration of the element in the standard solution, and a is the base of the logarithm; The calculation formula of the element concentration interference index is: ; Where N is the element concentration interference index, To measure the concentration of an element in a solution, is the reference concentration of the element in the standard solution, i is a proportional constant, and b is the base of the logarithm.
8. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 7, characterized in that: In step 6, the process of obtaining the deviation assessment coefficient and the assessment report is as follows: Step 601: combining the element intensity interference index and the element concentration interference index to analyze the correlation between the interference degree during element determination and the element intensity interference index and the element concentration interference index; Step 602: assign different weights to the element intensity interference index and the element concentration interference index, perform weighted calculation on the two indices, and obtain a deviation evaluation coefficient; Step 603: setting different deviation levels according to the degree of deviation of the measured data, namely slight deviation level, moderate deviation level, and severe deviation level; Step 604 , matching different deviation levels with deviation assessment coefficients, and setting deviation assessment thresholds for different deviation levels; Step 605: The collected measurement data, calculated deviation evaluation coefficients, and classified deviation levels are sorted out, an evaluation report is compiled, interference sources are analyzed for the measurement of severe deviations, and corresponding correction measures are taken.
9. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 8, characterized in that: The calculation formula of the deviation evaluation coefficient is: ; Where D is the deviation evaluation coefficient, I is the element intensity interference index, N is the element concentration interference index, and are all constants.
10. The method for determining major and minor elements in dolomite and magnesite based on ICP-AES according to claim 9, characterized in that: The plurality of deviation levels correspond to a plurality of deviation assessment thresholds, wherein the deviation assessment thresholds include an upper threshold and a lower threshold; The plurality of deviation levels and the plurality of deviation assessment thresholds satisfy the following relationship: Slight deviation from the level ; Moderate deviation level ; Severe deviation level ; Among them, D is the deviation assessment coefficient, T1 is the upper threshold corresponding to the slight deviation level and the lower threshold corresponding to the moderate deviation level, and T2 is the upper threshold corresponding to the moderate deviation level and the lower threshold corresponding to the severe deviation level.
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