Method for measuring boron content in fluorite powder
Patent Information
- Application Number
- CN202411726505.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-28
- Publication Date
- 2025-03-14
AI Technical Summary
The field of fluorine chemical industry lacks effective methods for determining boron content in fluorite powder, which affects the production of electronic grade hydrofluoric acid.
The boron content in the acid solution was detected by inductively coupled plasma emission spectrometer, and the fluorite powder was digested with the acid solution through the pretreatment step to ensure that the boron element was fully dissolved.
The accurate determination of boron content in fluorite powder is achieved, the detection limit can reach the ppb level, the sample pre-processing is simple, the analysis results are accurate, and the recovery rate is between 90% and 110%.
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Abstract
Description
Technical Field
[0001] The present application relates to the field of fluorine chemical industry, and in particular to a method for determining the boron content in fluorite powder. Background Art
[0002] In the field of fluorine chemical industry, the raw material of anhydrous hydrofluoric acid is fluorite powder, which contains boron. Since the downstream production of electronic-grade hydrofluoric acid is affected by the boron content in industrial anhydrous hydrogen fluoride, the industry's requirements for boron in fluorite powder are getting higher and higher.
[0003] At present, there is no determination method and relevant standards for the boron content in fluorite powder in the fluorine chemical industry. Therefore, it is urgent to establish a determination method for the boron content in fluorite powder and provide a monitoring basis. Summary of the invention
[0004] In view of the above problems, the present application provides a method for determining the boron content in fluorite powder, which is simple and convenient, has strong selectivity, high accuracy, high sensitivity and low detection limit, thereby making up for the defect of the lack of a method for determining the boron content in fluorite powder in the prior art.
[0005] To achieve the above object, the present application provides a method for determining the boron content in fluorite powder, comprising the following steps:
[0006] Pretreatment: Digest the fluorite powder to be tested with an acid solution to obtain a pretreated product; take the aqueous phase of the pretreated product as the test solution;
[0007] Measurement: Use inductively coupled plasma emission spectrometer to detect the test liquid, obtain the boron content in the test liquid through analysis and calculation, and then calculate the boron content in fluorite powder.
[0008] Different from the existing technology, after the fluorite powder is pre-treated and digested with an acid solution, the boron element can be fully dissolved, and the boron content in the digestion solution is determined using an inductively coupled plasma emission spectrometer, with a detection limit of up to ppb level. The sample pre-processing is also relatively simple, and the machine operation program is controlled. The linear correlation coefficient of the standard curve can reach above 0.999, the analysis results are accurate, and the recovery rate is between 90% and 110%.
[0009] Furthermore, the detection wavelength is 249.772 nm.
[0010] Furthermore, the digestion temperature is 98-102°C.
[0011] Furthermore, in the pretreatment step, the fluorite powder to be tested is weighed with an accuracy of 0.0001g.
[0012] Furthermore, in the measurement step, the boron content in the test solution is calculated using the linear regression equation y=33.038x+7.5162, R 2=0.9998, where x is the mass concentration of boron in the test solution ug.L -1 , y is the response signal intensity.
[0013] Furthermore, the boron content in the fluorite powder is calculated using the following formula: I=xV / m×100%; wherein I is the boron content in the fluorite powder, in %, and x is the mass concentration of the boron element in the test solution, in ug.L -1 , V is the volume of the acid solution, the unit is L, m is the mass of the fluorite to be tested, the unit is ug.
[0014] The above-mentioned records related to the invention content are only an overview of the technical solution of the present application. In order to enable ordinary technicians in the field to more clearly understand the technical solution of the present application, and then implement it according to the written contents of the specification, and to make the above-mentioned purpose and other purposes, features and advantages of the present application easier to understand, the specific implementation methods of the present application are explained below. DETAILED DESCRIPTION
[0015] In order to explain the technical content, structural features, achieved objectives and effects of the technical solution in detail, the following is a detailed description in conjunction with specific embodiments.
[0016] In order to explain in detail the possible application scenarios, technical principles, specific schemes that can be implemented, and the purposes and effects that can be achieved, the following is a detailed description in conjunction with the specific embodiments listed. The embodiments described herein are only used to more clearly illustrate the technical solutions of the present application, and are therefore only used as examples, and cannot be used to limit the scope of protection of the present application.
[0017] Reference to "embodiment" herein means that the specific features, structures or characteristics described in conjunction with the embodiment may be included in at least one embodiment of the present application. The term "embodiment" appearing in various places in the specification does not necessarily refer to the same embodiment, nor does it particularly limit its independence or association with other embodiments. In principle, in the present application, as long as there is no technical contradiction or conflict, the various technical features mentioned in the embodiments can be combined in any way to form a corresponding implementable technical solution.
[0018] Unless otherwise defined, the technical terms used in this document have the same meanings as those generally understood by those skilled in the art to which this application belongs; the use of relevant terms in this document is only for describing specific embodiments and is not intended to limit this application.
[0019] In the description of this application, the term "and / or" is an expression used to describe the logical relationship between objects, indicating that three relationships may exist, for example, A and / or B, which means: A exists, B exists, and A and B exist at the same time. In addition, the character " / " in this article generally indicates that the objects before and after are in an "or" logical relationship.
[0020] In the present application, terms such as “first” and “second” are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship of quantity, priority or sequence between these entities or operations.
[0021] Without further limitations, in this application, the words "include", "comprises", "has" or other similar expressions used in the sentences are intended to cover non-exclusive inclusion. These expressions do not exclude the presence of additional elements in the process, method or product including the elements, so that the process, method or product including a series of elements may include not only those limited elements, but also other elements not explicitly listed, or also include elements inherent to such process, method or product.
[0022] Similar to the understanding in the Examination Guidelines, in this application, expressions such as "greater than", "less than", "exceed" and the like are understood to exclude the number itself; expressions such as "above", "below", "within" and the like are understood to include the number itself. In addition, in the description of the embodiments of this application, "multiple" means more than two (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups", "multiple times", etc., unless otherwise clearly and specifically limited.
[0023] The present application provides a method for determining the boron content in fluorite powder, comprising the following steps:
[0024] Pretreatment: Digest the fluorite powder to be tested with an acid solution to obtain a pretreated product; take the aqueous phase of the pretreated product as the test solution;
[0025] Measurement: The test liquid is detected by inductively coupled plasma emission spectrometer with a detection wavelength of 249.772nm. The boron content in the test liquid is obtained by analysis and calculation, and then the boron content in the fluorite powder is calculated.
[0026] Different from the existing technology, the fluorite powder is pre-treated and digested with an acid solution in the early stage, and the boron element is fully dissolved. The boron content in the digestion solution is determined using an inductively coupled plasma emission spectrometer, and the detection limit can reach the ppb level. The preliminary sample processing is also relatively simple, and the machine operation program is controlled. The linear correlation coefficient of the standard curve can reach above 0.999, the analysis results are accurate, and the recovery rate is between 90% and 110%.
[0027] Furthermore, the wavelength of 249.772 nm is the detection wavelength of the boron element, and the signal intensity of the boron element is the largest at this wavelength.
[0028] Furthermore, the digestion temperature is 98-102°C.
[0029] This temperature can improve the efficiency of the digestion of the acid solution. The digestion can be carried out by heating in a water bath, and the water bath pot can be shaken during the water bath process to fully digest the impurities including the boron element.
[0030] Furthermore, in the pretreatment step, the fluorite powder to be tested is weighed with an accuracy of 0.0001g.
[0031] Furthermore, in the measurement step, the boron content in the test solution is calculated using the linear regression equation y=33.038x+7.5162, R 2 =0.9998, where x is the mass concentration of boron in the test solution ug.L -1 , y is the response signal intensity.
[0032] Furthermore, the boron content in the fluorite powder is calculated using the following formula: I=xV / m×100%; wherein I is the boron content in the fluorite powder, in %, and x is the mass concentration of the boron element in the test solution, in ug.L -1 , V is the volume of the acid solution, the unit is L, m is the mass of the fluorite to be tested, the unit is ug.
[0033] Furthermore, the pretreatment step in the embodiment of the present application is carried out in two steps. First, a high-concentration acid solution is used to digest the fluorite powder to be tested, and then deionized water is further added to the acid solution volume V to obtain a pretreated product.
[0034] This treatment can increase the efficiency of digestion, allowing the boron ions in the fluorite powder to be fully dissolved in the acid solution. At the same time, it can replenish the loss of acid solution during high-temperature digestion to avoid affecting the analysis results.
[0035] The high-concentration acid solution used in the embodiment of the present application is a water regia solution obtained by mixing 36-38wt% hydrochloric acid and 65-68wt% nitric acid in a volume ratio of 3:1. The water regia solution in the embodiment of the present application is also prepared with deionized water. The water regia solution can digest most organic or inorganic substances, but the main component of fluorite, calcium fluoride, may not be completely digested in the water regia. Therefore, this embodiment takes the water phase after the pre-treated material is left to stand for 30 minutes to remove the undigested calcium fluoride precipitate to avoid its influence on the test results.
[0036] The inductively coupled plasma optical emission spectrometer used in the present embodiment is Agilent 5110.
[0037] The deionized water used in the embodiments of the present application has a conductivity (25° C.) of no more than 0.0055 mS / m.
[0038] The material of the volumetric flask used in the embodiment of the present application is tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer.
[0039] The standard substances used in the examples of the present application include: boron ion standard solution (CAS No.: 7440-42-8).
[0040] The standard solution preparation method used in the present application example is: accurately weigh an appropriate amount of boron ion standard solution, and use deionized water to make a concentration of 10000 μg.L -1 The standard stock solution is then diluted step by step with deionized water to form a series of standard working solutions of the required concentration.
[0041] The recovery rate described in this application refers to the proportion of boron ions that can be used for analysis after sample treatment. The recovery rate mainly examines accuracy. Accuracy refers to the degree of closeness between the result measured by the method and the true value or recognized reference value, sometimes also called authenticity. The recovery rate is a necessary condition for quantitative determination with a certain accuracy. Therefore, all test items related to quantitative determination need to verify accuracy, such as content determination, impurity quantitative test, etc. For preparations, recovery test is generally used for verification.
[0042] The relative standard deviation (RSD) mentioned in this application is also called standard deviation coefficient, coefficient of variation, coefficient of change, etc. It is the value obtained by dividing the standard deviation by the corresponding average value and multiplying it by 100%, which can be used to analyze the precision of the results in inspection and testing work.
[0043] The relative error δ described in this application refers to the value obtained by multiplying the ratio of the absolute error caused by the measurement to the measured (agreed) true value by 100%. The smaller the value of the relative error, the closer the actual test value is to the theoretical value, and thus the more accurate the experimental result is. Only when the experimental results are accurate to an acceptable range can they reflect the actual situation and obtain more reliable conclusions. Therefore, the size of the relative error is a direct indicator for measuring the accuracy of the experimental results, and is an important reference indicator for further judging the credibility of the experimental results based on the experimental results.
[0044] The present application uses the external standard method (standard curve equation) for quantitative analysis, with the concentration of the boron ion standard solution as the horizontal coordinate and the corresponding response signal intensity of 249.772nm as the vertical coordinate to draw a standard curve. By comparing the response signal intensity of the boron ion standard solution in the sample to be tested with the standard curve, the concentration of the boron element in the test solution can be obtained by converting the standard curve equation.
[0045] Example 1, standard curve equation and confirmation of detection and quantitation limits:
[0046] 1. Establishment of linear regression equation:
[0047] The concentration is 5-25.0 μg·L -1 (5, 10, 15, 20, 25 μg·L -1 ) of 5 boron standard working solutions as sample detection solutions;
[0048] Inductively coupled plasma optical emission spectrometer (ICP-OES) was used to detect the test solution, with deionized water as the blank sample, the detection wavelength was 249.772nm, the working power was 1.2KW, the pump speed was 12rpm, the observation mode was axial, the atomizer flow rate was 0.7L / min, the plasma gas flow rate was 12L / min, and the integration time was 3s; the response signal intensity shown in Table 1 was obtained. -1 ) as the horizontal coordinate, the response signal intensity as the vertical coordinate, and the standard curve is drawn to obtain the linear regression equation of boron element y=33.038x+7.5162 and the correlation coefficient R 2 =0.9998.
[0049] Table 1 Response signal intensity of boron element standard working solution
[0050] Boron ion content (ug / L) 0 5 10 15 20 25 Response signal strength y 14.61 166.76 334.88 501.64 668.55 836.52
[0051] 2. Determination of detection limit and quantification limit
[0052] The detection limit (LOD) and quantification limit (LOQ) were determined with a signal-to-noise ratio of 3 and a signal-to-noise ratio of 10, and the detection limit (LOD) of the present application was 0.68 ug / L, i.e. 0.68 ppb, and the quantification limit (LOQ) was 2.28 ug / L, i.e. 2.28 ppb.
[0053] Example 2 Determination of spiked recovery and precision
[0054] Six groups of fluorite powders with particle sizes less than 0.15 mm were used as samples, and standard working solutions of 2.28 ppb, 5 ppb, 10 ppb and 20 ppb were added respectively to carry out spiked recovery and precision experiments.
[0055] The experimental method is:
[0056] Pretreatment: Weigh 0.2g (accuracy to 0.0001g) of fluorite powder of 6 groups of samples to be tested respectively, add them into 20ml aqua regia solution, heat them in a water bath at 98-102℃ for 3h, add deionized water to 50ml to obtain the pretreated product; after the pretreated product is allowed to stand for 30min, take the aqueous phase solution as the test solution;
[0057] Measurement: Inductively coupled plasma emission spectrometer was used to detect the test liquid, the detection wavelength was 249.772nm, and the linear regression equation y=33.038x+7.5162 was used, R 2 =0.9998 The boron content in the test solution was calculated and analyzed. Three groups of each fluorite powder were tested to obtain the average boron content of the six fluorite powders.
[0058] Adding spikes: Add 2.28ppb, 5ppb, 10ppb, and 20ppb boron standard working solutions to the above 6 groups of fluorite powder samples to be tested, respectively, mix well, and dry to obtain 6 groups of spiked samples to be tested;
[0059] Pretreatment: Weigh 0.2g (accuracy to 0.0001g) of the spiked sample to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 50ml to obtain the pretreated spiked material; let the pretreated spiked material stand for 30min, and take the aqueous phase solution as the spiked test solution;
[0060] Measurement: Inductively coupled plasma emission spectrometer was used to detect the test liquid, the detection wavelength was 249.772nm, and the linear regression equation y=33.038x+7.5162 was used, R 2 =0.9998 to analyze and calculate the boron content in the spiked test solution; then calculate the recovery rate and RSD of different samples with different spiked amounts.
[0061] The results are shown in Table 2: At the spiked levels of 2.28 ppb, 5 ppb, 10 ppb, and 20 ppb, the recoveries of boron ranged from 97.51% to 105.94%, and the relative standard deviations were 0.0035% to 0.0059%, respectively. This also proves that the accuracy and precision of this method can meet the requirements for the detection of boron in fluorite.
[0062] Table 2 Spiked recovery and relative standard deviation
[0063]
[0064]
[0065] Example 3 Detection of boron content in fluorite powder
[0066] Pretreatment: weigh 2.0002g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 100ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min, and take the aqueous phase solution as the test solution;
[0067] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 1405.68; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 42.32ug.L -1
[0068] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000211%.
[0069] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug).
[0070] Example 4 Detection of boron content in fluorite powder
[0071] Pretreatment: weigh 2.0065g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 100ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min, and take the aqueous phase solution as the test solution;
[0072] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 948.77; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 28.49ug.L -1
[0073] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000142%.
[0074] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0075] Example 5 Detection of boron content in fluorite powder
[0076] Pretreatment: weigh 1.9985g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 100ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min and take the aqueous phase solution as the test solution;
[0077] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 647.79; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 19.38ug.L -1
[0078] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000097%.
[0079] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0080] Example 6 Detection of boron content in fluorite powder
[0081] Pretreatment: weigh 2.0034g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 100ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min, and take the aqueous phase solution as the test solution;
[0082] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 1225.30; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 36.86ug.L -1
[0083] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000184%.
[0084] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0085] Example 7 Detection of boron content in fluorite powder
[0086] Pretreatment: weigh 0.5852g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 50ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min to separate the layers, and take the aqueous phase solution as the test solution;
[0087] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 614.75; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 18.38ug.L -1
[0088] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000157%.
[0089] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0090] Example 8 Detection of boron content in fluorite powder
[0091] Pretreatment: weigh 0.2236g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 50ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min, and take the aqueous phase solution as the test solution;
[0092] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 187.90; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 5.46ug.L -1
[0093] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000122%.
[0094] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0095] Example 9 Detection of boron content in fluorite powder
[0096] Pretreatment: weigh 0.9814g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 50ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min to separate the layers, and take the aqueous phase solution as the test solution;
[0097] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 1116.27; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 33.56ug.L -1
[0098] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000171%.
[0099] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0100] Example 10 Detection of boron content in fluorite powder
[0101] Pretreatment: weigh 0.3829g of the fluorite powder to be tested, add it to 20ml of aqua regia solution, heat it in a water bath at 98-102℃ for 3h, add deionized water to 50ml to obtain a pretreatment solution; let the pretreatment solution stand for 30min, and take the upper aqueous phase solution as the test solution;
[0102] Measurement: The liquid to be tested was detected by inductively coupled plasma emission spectrometer, the detection wavelength was 249.772nm, and the corresponding signal intensity y was 523.57; the linear regression equation y = 33.038x + 7.5162, R 2 =0.9998Analysis and calculation show that the boron content in the test solution is x = 15.62ug.L -1
[0103] According to I=xV / m×100%, the boron content in fluorite powder is calculated to be 0.000204%.
[0104] (x is the mass concentration of boron in the test solution, y is the corresponding signal intensity, I is the boron content in fluorite powder, the unit is %, the unit is ug.L -1 , V is the volume of the acid solution on the machine, the unit is L, m is the mass of the fluorite to be tested, the unit is ug)
[0105] This technical solution provides a method for determining the boron content in fluorite powder. The detection limit of the method can reach the ppb level, the sample pre-processing is simple, the machine operation program control is convenient, the standard curve linear correlation coefficient can reach above 0.999, the detection limit is 0.68ppb, the quantitative limit (LOQ) is 2.28ppb, and the recovery rate is 90% to 110%. The method has high sensitivity, simple operation, rapidity and accuracy.
[0106] Finally, it should be noted that although the above embodiments have been described in the text of the specification of this application, this does not limit the scope of patent protection of this application. All technical solutions generated by replacing or modifying equivalent structures or equivalent processes based on the essential concept of this application using the contents recorded in the text of the specification of this application, as well as directly or indirectly implementing the technical solutions of the above embodiments in other related technical fields, are included in the scope of patent protection of this application.
Claims
1. A method for determining the boron content in fluorite powder, characterized in that: The following steps are involved: Pretreatment: Digest the fluorite powder to be tested with an acid solution to obtain a pretreated product; Take the aqueous phase of the pre-treated material as the test solution; Measurement: Use inductively coupled plasma emission spectrometer to detect the test liquid, obtain the boron content in the test liquid through analysis and calculation, and then calculate the boron content in fluorite powder.
2. The measuring method according to claim 1, characterized in that The detection wavelength is 249.772 nm.
3. The measuring method according to claim 1, characterized in that The digestion temperature is 98-102°C.
4. The measuring method according to claim 1, characterized in that In the pretreatment step, the fluorite powder to be tested is weighed with an accuracy of 0.0001g.
5. The assay method according to any one of claims 1 to 4, characterized in that: In the measurement step, the boron content in the test solution is calculated using the linear regression equation y=33.038x+7.5162, R 2 =0.9998, where x is the mass concentration of boron in the test solution ug.L -1 , y is the response signal intensity.
6. The determination method according to any one of claims 1 to 4, characterized in that: The boron content in the fluorite powder is calculated using the following formula: I = xV / m × 100%; where I is the boron content in the fluorite powder, in %, and x is the mass concentration of the boron element in the test solution, in ug.L -1 , V is the volume of the acid solution, the unit is L, m is the mass of the fluorite to be tested, the unit is ug.