Method for measuring elements in manganese ore by using samarium internal standard through X-ray fluorescence spectrometry

Abstract

The invention relates to a method for measuring elements in manganese ore by using an X-ray fluorescence spectrometry samarium internal standard, which comprises the following steps: establishing a Sm internal standard method for Mn element to replace an ignition loss correction analysis method so as to simplify the analysis process and shorten the analysis time, mixing a sample with a flux, samarium oxide, a release agent and the like according to a certain proportion, and measuring the content of elements in the manganese ore by using an X-ray fluorescence spectrometry samarium internal standard method. And melting at high temperature to prepare a glass sheet for fluorescence analysis, and measuring main elements such as Mn, Fe, SiO2, CaO, MgO and P in manganese ore. By adopting an internal standard method, not only is the influence of ignition loss on an analysis result eliminated, but also the influence of deformation of a glass sheet forming mold and coexisting elements on the analysis result can be eliminated, and it is confirmed that the method is feasible through comparison of calibration curve linearity and chemical analysis data. The method adopts the samarium internal standard method to measure the elements in the manganese ore, is time-saving and labor-saving, short in analysis period and high in working efficiency, and is expected to be widely applied to the element measurement process of the manganese ore.

Description

Technical Field

[0001] The present application belongs to the technical field of ore element detection, and relates to a method for determining elements in manganese ore using samarium internal standard by X-ray fluorescence spectrometry, and specifically to a method for determining elements in manganese ore using samarium internal standard by X-ray fluorescence spectrometry, which can eliminate the influence of loss on ignition and coexisting elements on the analysis results. Background Art

[0002] There are over 150 known manganese-containing minerals in nature, belonging to various groups, including oxides, carbonates, silicates, sulfides, borates, tungstates, and phosphates. Common minerals with high manganese content include pyrolusite, psilomelane, manganite, henrolusite, ferromanganese, rhodochrosite, and pyrolusite. Manganese occurs naturally in various valence states, including II, III, IV, and VII. The main industrial uses of manganese ore include steelmaking, chemical industry, and light industry, with different requirements for the quality of the ore. The main quality indicators of manganese ore's chemical composition include manganese content, manganese-to-iron ratio, phosphorus-to-manganese ratio, and the content of impurities such as Fe, CaO, and SiO2.

[0003] X-ray fluorescence spectrometry is a commonly used instrumental analysis method for manganese ore analysis. Due to the wide variety and complex structure of manganese ores, X-ray fluorescence spectrometry is typically performed using the glass frit method to obtain satisfactory analytical results. The national standard GB / T 24519-2009, "Manganese ores - Determination of magnesium, aluminum, silicon, phosphorus, sulfur, potassium, calcium, titanium, manganese, iron, nickel, copper, zinc, barium, and lead contents - Wavelength dispersive X-ray fluorescence spectrometry," and the industry standard SN / T 2638.1-2010, "Manganese ores for import and export - Determination of manganese, iron, silicon, aluminum, calcium, magnesium, titanium, potassium, and phosphorus - Wavelength dispersive X-ray fluorescence spectrometry," both recommend the use of glass frits and the use of loss on ignition (LOI) to correct the analysis results. However, determining LIO is time-consuming and labor-intensive, resulting in long sample analysis cycles and low efficiency. Summary of the Invention

[0004] For the current national standard and industry standard test of elements in manganese ore, it is necessary to measure the loss on ignition, which is time-consuming and laborious, and the sample analysis cycle is long and the work efficiency is low. The purpose of this application is to provide a method for measuring elements in manganese ore using samarium internal standard by X-ray fluorescence spectrometry. In order to shorten the analysis cycle and improve work efficiency, an internal standard method is established to replace the loss on ignition correction analysis method. The analysis line of manganese element is usually MnKa (0.2103nm), and Sm (0.2199nm) is close to the MnKa wavelength, and manganese ore generally does not contain Sm. Sm is a relatively good internal standard element (easy to obtain, cheap, and close in wavelength). Sm is used as an internal standard and tested, and the analysis results are verified. The results show that the present invention adopts the internal standard method not only to eliminate the influence of loss on ignition on the analysis results, but also to eliminate the influence of deformation of glass sheet forming mold and coexisting elements on the analysis results. The method is feasible by comparing the linearity of the calibration curve and chemical analysis data.

[0005] The present application provides a method for determining elements in manganese ore using samarium internal standard by X-ray fluorescence spectrometry, comprising the following steps:

[0006] (1) Prepare standard materials: the element content range of the standard materials covers the element content range of the manganese ore sample;

[0007] (2) Preparation of standard samples: The flux, standard substance and samarium oxide are mixed uniformly, transferred to a platinum crucible, a first release agent and a second release agent are added, and the crucible is placed in a melting furnace for melting. After the melting is completed and cooled to room temperature, the standard sample to be tested is obtained;

[0008] (3) Preparation of calibration curves: The standard samples were subjected to X-ray fluorescence spectrometry to obtain the fluorescence intensity of each element. Samarium was used as an internal standard to calibrate manganese and iron. Based on the corresponding relationship between the element fluorescence intensity and concentration, calibration curves for various elements were obtained;

[0009] (4) Preparation of the test sample: The flux, the test substance, and samarium oxide were mixed uniformly, transferred to a platinum crucible, a first release agent and a second release agent were added, and the crucible was placed in a melting furnace for melting. After the melting was completed and cooled to room temperature, the test sample was obtained;

[0010] (5) Elemental testing in manganese ore: The sample to be tested is subjected to X-ray fluorescence spectrometry, in which manganese and iron elements are calibrated with samarium as the internal standard. The content of each element in the manganese ore is obtained based on the calibration curve.

[0011] At present, there are generally two X-ray fluorescence analysis methods for detecting elements in manganese ore. One is the national standard GB / T24519-2009 "Determination of the content of magnesium, aluminum, silicon, phosphorus, sulfur, potassium, calcium, titanium, manganese, iron, nickel, copper, zinc, barium and lead in manganese ore by wavelength dispersion X-ray fluorescence spectrometry", and the other is the industry standard SN / T 2638.1-2010 "Determination of the content of manganese, iron, silicon, aluminum, calcium, magnesium, titanium, potassium and phosphorus in imported and exported manganese ore by wavelength dispersion X-ray fluorescence spectrometry". Both methods use loss on ignition to correct the analysis results, and measuring loss on ignition is time-consuming and labor-intensive, and the time cycle is long and the efficiency is low. In view of the above problems, the present invention adopts an internal standard method instead of a loss on ignition determination method to correct the analysis results. The internal standard method has the advantages of short analysis time and high analysis efficiency. When using the internal standard method in X-ray fluorescence spectrometry, the selection of the internal standard element is particularly important. Internal standard elements are usually elements with an atomic number of plus or minus 1 for the element being analyzed. Mn is element 25. In theory, element 24, Cr, and element 26, Fe, are the best internal standards for Mn. However, manganese ore often contains Fe and Cr, making these two elements unsuitable for use as internal standards for Mn analysis in manganese ore. Elements with an atomic number of plus or minus 2 for Mn are Co and V, which are generally not present in Mn manganese ore. Therefore, attempts were made to use Co and V as internal standards for Mn analysis in manganese ore. However, experiments revealed that the linearity of the curve obtained using Co and V as internal standards did not meet the analytical requirements. The present invention continues to explore the principle of internal standard analysis by searching for suitable spectral lines around the Mn Kα line and discovering that the Sm Lα line is more suitable. However, manganese ore generally does not contain Sm, and although Sm is a rare earth element, its oxide, Sm2O3, is readily available and relatively inexpensive. Therefore, experiments were conducted using Sm as the internal standard. The results of the determination method of manganese ore elements using samarium internal standard in the present invention are basically consistent with those of the determination method using the national standard, indicating that the samarium internal standard method of the present invention can be applied to the element determination process of manganese ore.

[0012] The present invention also considers the impact of coexisting elements in the test results. The main elements of manganese ore are Mn, Fe, SiO2, CaO, MgO, and P. Sm is used as the internal standard for both Mn and Fe to correct for the matrix effect on the analysis results. SiO2 and CaO have high content and are more significantly affected by matrix elements. Mn and Fe, which have large content gradients and are relatively heavy, were used in matrix absorption enhancement correction experiments, and the experiments showed that the correction was significantly effective. Mg is affected by the Ca cubic line. Ca was used to perform an overlap correction experiment on Mg, and the results showed that the correction was effective. In the present invention, manganese ore contains multiple elements, and the matrix effects of different elements may have different effects on the X-ray fluorescence signal. If samarium is used as the internal standard for all elements, the influence of the matrix effect may not be completely eliminated. Different elements have different response characteristics to X-rays, and using a single element as the internal standard may not fully account for these differences. For example, some elements may absorb X-rays more strongly, while others may absorb them less strongly. Different elements in manganese ore may produce overlapping fluorescence spectrum peaks. If samarium is used as an internal standard for all elements, it is difficult to distinguish these overlapping signals, which may increase the uncertainty of the test results. Therefore, the present invention adopts a specific test result analysis method to improve the accuracy of the test for each element.

[0013] In some embodiments of the present application, the mass ratio of lithium tetraborate to lithium metaborate is 67:33.

[0014] In some embodiments of the present application, the first release agent is an aqueous solution of ammonium iodide with a mass concentration of 30%, and the second release agent is an aqueous solution of ammonium bromide with a mass concentration of 30%.

[0015] In some embodiments of the present application, the platinum crucible comprises 95% platinum and 5% gold.

[0016] In some embodiments of the present application, the melting machine is a TNRY-01C type fully automatic melting machine dedicated to X-ray fluorescence spectrometry analysis, with a melting temperature of 1050°C to 1100°C, a furnace rotation time of 720s, a front standing time of 120s, and a rear standing time of 10s.

[0017] In some embodiments of the present application, the total mass of the flux, the standard substance, and samarium oxide is 7.000 g, of which the flux is 6.000 g, the substance to be tested is 0.5000 g, and the samarium oxide is 0.5000 g.

[0018] In some embodiments of the present application, samarium oxide is used as an internal standard to calibrate manganese and iron.

[0019] In some embodiments of the present application, the preparation process of the sample to be tested is the same as the preparation process of the standard sample, specifically, the flux, the substance to be tested and samarium oxide are evenly mixed, transferred to a platinum crucible, a first release agent and a second release agent are added, and placed in a melting furnace for melting. After the melting is completed and cooled to room temperature, the sample to be tested is obtained, wherein the total mass of the flux, the substance to be tested and samarium oxide is 7.000 g, the flux is 6.000 g, the substance to be tested is 0.5000 g, and the samarium oxide is 0.5000 g.

[0020] In some embodiments of the present application, the amount of the first release agent added is 5 drops, and the amount of the second release agent added is 5 drops.

[0021] In the present invention, a first mold release agent and a second mold release agent are used in the preparation process of the sample to be tested. If ammonium iodide is used alone as the mold release agent, the melt is relatively viscous when the manganese content is high, and the demolding effect is poor. If ammonium bromide is used alone as the mold release agent, bubbles sometimes appear. Therefore, a mixed mold release agent of ammonium iodide and ammonium bromide is used.

[0022] In some embodiments of the present application, both the standard sample and the sample to be tested are molded in a mold, and the diameter of the mold is 32 mm.

[0023] In some embodiments of the present application, the test conditions of the X-ray fluorescence spectroscopy are: the light tube voltage is 40 kV and the current is 70 mA.

[0024] Compared with the prior art, this application achieves at least the following technical effects:

[0025] The present application relates to a method for determining elements in manganese ore by X-ray fluorescence spectrometry using samarium as an internal standard. The internal standard method not only eliminates the influence of loss on ignition on the analysis results, but also eliminates the influence of deformation of the glass sheet forming mold and coexisting elements on the analysis results. The feasibility of the method is confirmed by comparing the linearity of the calibration curve and chemical analysis data, and at least the following technical effects are obtained: (1) The method of the present invention can effectively correct the measurement deviation caused by the sample matrix effect by using samarium as an internal standard, thereby improving the precision and accuracy of the measurement results; (2) The method of the present invention is suitable for the simultaneous determination of multiple elements, including manganese, iron, silicon, calcium, magnesium and phosphorus, so that one analysis can obtain (3) The method of the present invention uses X-ray fluorescence spectrometry, which is a non-destructive and rapid analysis method that can obtain test results in a short time and does not require a complicated sample preparation process; (4) The method of the present invention uses standardized melting conditions and a fixed amount of internal standard addition to ensure the consistency and reproducibility of each analysis, which is convenient for analysis and comparison with national standard test methods; (5) The X-ray fluorescence spectrometry used in the present invention has a wide detection range and can provide reliable measurement results even at low concentrations; (6) The method of the present invention uses less sample volume and has a low analysis cost, which is convenient for rapid detection of a large number of samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 is the calibration curve for iron;

[0027] Figure 2 is the calibration curve for silica;

[0028] Figure 3 is the calibration curve for magnesium oxide;

[0029] Figure 4 is the calibration curve for manganese;

[0030] Figure 5 is the calibration curve for calcium oxide;

[0031] Figure 6 is the calibration curve for phosphorus;

[0032] Figure 7 This is the calibration curve of manganese when vanadium is used as the internal standard;

[0033] Figure 8 This is the calibration curve of manganese when cobalt is used as the internal standard. DETAILED DESCRIPTION

[0034] To make the purpose, technical solutions and advantages of the present invention more clear, the present invention is further described in detail below. However, it should be understood that the description herein is only for explaining the present invention and is not intended to limit the scope of the present invention.

[0035] Unless otherwise defined, all technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which the present invention pertains. The terms used in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The reagents and instruments used herein are all commercially available. The characterization methods involved can be found in the relevant descriptions in the prior art and will not be described in detail herein.

[0036] Experimental instruments and reagents

[0037] X-ray fluorescence spectrometers: MXF-N3 Plus, MXF-2400, XRF-1800;

[0038] Sample melting furnace: TNRY-01C;

[0039] Platinum crucible: 95% platinum 5% gold, used in conjunction with the melting furnace;

[0040] Flux: lithium tetraborate + lithium metaborate (67+33);

[0041] Samarium oxide: analytical grade;

[0042] First release agent: 30% ammonium iodide aqueous solution;

[0043] Second release agent: 30% ammonium bromide aqueous solution.

[0044] Preparation Example 1

[0045] Preparation of standard samples:

[0046] Accurately weigh 0.5000g of the standard substance, 0.5000g of samarium oxide, and 6.000g of the mixed flux into a 50mL porcelain crucible. Mix thoroughly and transfer to a platinum crucible. Add 5 drops of each release agent and place in a high-temperature melting furnace. Melt according to the programmed procedure to prepare glass slides for fluorescence analysis. Keep the prepared sample clean and test as soon as possible. Do not wipe the surface with any reagents before testing. The mold used for glass slide preparation has a diameter of 32mm. The programmed melting parameters are according to Table 1. The standard substances are prepared and mixed according to the data in Table 2.

[0047] Table 1 Melting conditions

[0048]

[0049] The element content range of the standard sample used to prepare the calibration curve in X-ray fluorescence spectrometry should cover the element content range of the analyzed sample. When the standard sample cannot meet the requirements, a reference reagent can be used for preparation. In this experiment, a total of 9 calibration samples were prepared. The content of each component is shown in Table 2. The element content range meets the analysis requirements of common manganese ores. All substances in the table below are national or industry standard substances. Since the oxides of iron and manganese elements vary in form, they are expressed in elemental form. The manganese oxide, iron oxide, calcium oxide, silicon dioxide, magnesium oxide, phosphorus oxide and inevitable trace elements in the table below together constitute the standard substances.

[0050] Table 2 Content of standard substances (%)

[0051]

[0052] Preparation Example 2

[0053] Preparation of test samples:

[0054] Accurately weigh 0.5000g of the substance to be tested, 0.5000g of samarium oxide, and 6.000g of the mixed flux into a 50mL porcelain crucible. Mix thoroughly and transfer to a platinum crucible. Add 5 drops of each of the two release agents. Place in a high-temperature melting furnace and melt according to the programmed procedure to prepare glass slides for fluorescence analysis. Keep the prepared slides clean and test as soon as possible. Do not wipe the surface with any reagents before testing. The slide size, programmed melting parameters, and fluorescence analysis parameters are the same as those in Preparation Example 1.

[0055] Example 1

[0056] Preparation of calibration curve:

[0057] The standard sample prepared in Example 1 was subjected to element fluorescence intensity measurement according to the conditions set in Table 3. After the measurement, the element fluorescence intensity will be automatically recorded in the group conditions. Based on the corresponding relationship between element fluorescence intensity and concentration, appropriate coexisting element correction was used to calculate the element calibration curve. The main element calibration curve is shown in Figure 1-6 .

[0058] Table 3 Element determination conditions

[0059]

[0060] Influence of coexisting elements:

[0061] The main elements in manganese ore are Mn, Fe, SiO2, CaO, MgO, and P. Sm was used as the internal standard for both Mn and Fe to correct for matrix effects on the analysis results. SiO2 and CaO, with their high content, are significantly affected by matrix elements. Mn and Fe, with their large content gradients and relatively high concentrations, were used for matrix absorption enhancement correction, demonstrating significant effectiveness. Mg is theoretically affected by the Ca cubic line, so Ca was used for overlap correction, demonstrating significant effectiveness. Table 4 compares the curve coefficients before and after SiO2, CaO, and MgO correction.

[0062] Table 4 Comparison of curve coefficients before and after correction of coexisting elements (%)

[0063]

[0064] From Table 4, it can be seen that manganese and iron elements are calibrated with samarium as the internal standard, while silicon dioxide and calcium oxide are calibrated with manganese or iron, and magnesium oxide is calibrated with calcium oxide. Such a calibration process can make the test results more accurate.

[0065] Repeatability test:

[0066] Two representative samples were selected based on their manganese content. Five samples were prepared for each sample according to standard sample preparation methods. The five samples with high manganese content were designated 7266-1, 7266-2, 7266-3, 7266-4, and 7266-5, while the five samples with low manganese content were designated S-1-1, S-1-2, S-1-3, S-1-4, and S-1-5. These samples were randomly placed on different positions on the instrument's turntable and independently measured. The two sets of data were statistically analyzed. The analysis results were evaluated according to the national standards GB / T6379, "Accuracy of measurement methods and results," and GB / T24519-2009, "Manganese ores - Determination of magnesium, aluminum, silicon, phosphorus, sulfur, potassium, calcium, titanium, manganese, iron, nickel, copper, zinc, and lead contents - Wavelength dispersive X-ray fluorescence spectrometry." The ranges of the five analytical results were less than the standard repeatability limit of 1.39, indicating no significant differences between the results. The results are shown in Tables 5 and 6.

[0067] Table 5 Repeatability test statistical data 1 (%)

[0068]

[0069] Table 6 Repeatability test statistical data 2 (%)

[0070]

[0071] It can be seen from Tables 5 and 6 that, regardless of whether the manganese content is high or low, the range of the five analysis results is less than 1.39 times the repeatability limit specified in the standard, indicating that the test results of the samarium internal standard test method for elements in manganese ore of the present invention are almost consistent with the test results of the national standard test method, and the method of the present invention can be used in practice.

[0072] Example 2

[0073] Test of the sample to be tested:

[0074] Ten samples were randomly selected from the user's production samples and recorded as 2023061506-37, 2023071006-60, 2023080706-67, 2023080406-69C, 2023080506-69 composite sample, 2023111806-83, 2023112706-100A, 2023120406-104B, 2023120506-103 and 2023092806-79B. The manganese content was analyzed using this method and compared with the user's chemical analysis results. The fluorescence analysis results and the chemical analysis results were compared with the allowable difference given in the national standard GB / T 1506-2016 "Manganese ore - Determination of manganese content - Potentiometric titration method and ammonium ferrous sulfate titration method". The deviation was within the allowable range. The results are shown in Table 7.

[0075] Table 7 Comparison of fluorescence and chemical analysis results (%)

[0076]

[0077] As can be seen from Table 7, the test results obtained by the samarium internal standard method of the present invention for determining manganese in manganese ore are compared with the test results obtained by the national standard chemical analysis method. The deviation between the two is very small, indicating that the samarium internal standard method of the present invention for determining elements in manganese ore is feasible and can be widely used in actual production processes.

[0078] The method of the present invention is based on the national standard GB / T24519-2009, "Manganese ore - Determination of magnesium, aluminum, silicon, phosphorus, sulfur, potassium, calcium, titanium, manganese, iron, nickel, copper, zinc, and lead contents - Wavelength dispersive X-ray fluorescence spectrometry." The method specifically optimizes the Mn elemental analysis method, establishing an internal standard method using Sm to replace the traditional loss on ignition correction analysis method to simplify the analysis process and shorten analysis time. Experiments have shown that the calibration curve established using standard samples has good linearity and the method has good accuracy. The X-ray fluorescence analysis results for elemental Mn are consistent with the chemical analysis results, and the analysis accuracy of elements such as iron, silicon, and phosphorus also meets the national standard requirements.

[0079] Comparative Example 1

[0080] The difference from Preparation Example 1 is that samarium oxide is replaced by an equal mass of vanadium pentoxide, Kα line is used, and the calibration curve test in Example 1 is performed.

[0081] Comparative Example 2

[0082] The difference from Preparation Example 1 is that samarium oxide is replaced by an equal mass of cobalt oxide, Kα line is used, and the calibration curve test in Example 1 is performed.

[0083] The calibration curves of Example 1 and Comparative Examples 1-2 are shown in Table 8. Figure 4 and Figure 7-8 .

[0084] Table 8 Comparison of internal standard data for different elements

[0085]

[0086] Note: The national standard GB / T 1506-2016 "Manganese ore - Determination of manganese content - Potentiometric titration and ammonium ferrous sulfate titration" gives an allowable error of 0.25% for 15% to 40%; 0.3% for >40% to 50%; and 0.4% for >50%.

[0087] As can be seen from Table 8, the average and maximum deviations of the curves using V and Co as internal standards exceed the allowable tolerances for chemical analysis methods. The maximum and average deviations of the curves using Sm as the internal standard are significantly better than those using V and Co as internal standards, and are both within the allowable tolerances. This indicates that only by using samarium as the internal standard element in the present invention can the rapid and efficient determination of various elements in manganese ore be achieved.

[0088] The applicant declares that while the above-mentioned examples illustrate a method for determining elements in manganese ore using X-ray fluorescence spectrometry with a samarium internal standard, the present application is not limited to the above-mentioned examples. This does not imply that the present application must rely on the above-mentioned examples for implementation. Persons skilled in the art should understand that any improvements to the present application, equivalent replacements for the raw materials of the present product, addition of auxiliary ingredients, and selection of specific methods, etc., fall within the scope of protection and disclosure of the present application.

[0089] The preferred embodiments of the present application are described in detail above. However, the present application is not limited to the specific details of the above embodiments. Within the technical concept of the present application, various simple modifications can be made to the technical solution of the present application, and these simple modifications all fall within the scope of protection of the present application.

[0090] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any appropriate manner unless there is any contradiction. In order to avoid unnecessary repetition, this application will not further describe various possible combinations.

Claims

1. A method for determining elements in manganese ore using samarium internal standard by X-ray fluorescence spectrometry, characterized in that: The following steps are involved: (1) Prepare standard materials: the element content range of the standard materials covers the element content range of the manganese ore samples; (2) preparing a standard sample: uniformly mixing the flux, the standard substance and samarium oxide, transferring the mixture into a platinum crucible, adding a first release agent and a second release agent, placing the mixture into a melting furnace for melting, and obtaining a standard sample to be tested after the melting is completed and the mixture is cooled to room temperature; (3) Preparation of calibration curve: The standard sample is subjected to X-ray fluorescence spectrometry to obtain the fluorescence intensity of each element. Samarium is used as an internal standard to calibrate manganese and iron. Based on the corresponding relationship between the fluorescence intensity and concentration of the element, the calibration curves of various elements are obtained; (4) preparing the sample to be tested: uniformly mixing the flux, the substance to be tested and samarium oxide, transferring the mixture into a platinum crucible, adding a first release agent and a second release agent, placing the mixture into a melting furnace for melting, and obtaining the sample to be tested after the melting is completed and the mixture is cooled to room temperature; (5) Element test in manganese ore: The sample to be tested is subjected to X-ray fluorescence spectrometry, in which manganese and iron elements are calibrated with samarium as the internal standard. The content of each element in the manganese ore is obtained based on the calibration curve.

2. The method according to claim 1, characterized in that: The flux is a mixture of lithium tetraborate and lithium metaborate, and the mass ratio of lithium tetraborate to lithium metaborate is 67:

33.

3. The method according to claim 1, characterized in that The first release agent is an ammonium iodide aqueous solution with a mass concentration of 30%, and the second release agent is an ammonium bromide aqueous solution with a mass concentration of 30%.

4. The method according to claim 1, characterized in that: Platinum crucible consists of 95% platinum and 5% gold.

5. The method according to claim 1, characterized in that The sample melting machine is a TNRY-01C fully automatic sample melting machine specially used for X-ray fluorescence spectrum analysis. The melting temperature is 1050℃~1100℃, the furnace rotation time is 720s, the front standing time is 120s, and the rear standing time is 10s.

6. The method according to claim 1, characterized in that The total mass of the flux, standard substance and samarium oxide is 7.000g, of which the flux is 6.000g, the substance to be tested is 0.5000g and the samarium oxide is 0.5000g.

7. The method according to claim 1, characterized in that Samarium oxide was used as an internal standard for calibration of manganese and iron.

8. The method according to claim 1, characterized in that: The first mold release agent was added in an amount of 5 drops, and the second mold release agent was added in an amount of 5 drops.

9. The method according to claim 1, characterized in that: Both the standard sample and the sample to be tested are formed in a mold, and the diameter of the mold is 32 mm.

10. The method according to claim 1, characterized in that The test conditions of X-ray fluorescence spectroscopy are: light tube voltage is 40 kV and current is 70 mA.

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