Method for testing purity of metal rubidium

Abstract

According to the method for testing the purity of the metal rubidium, an organic alcohol-nitric acid solution system is adopted to dissolve a metal rubidium sample, organic alcohol can accelerate the dissolution rate of the metal rubidium sample, on one hand, the contact time of the metal rubidium sample and air can be greatly shortened, and the spontaneous combustion risk of the metal rubidium sample in the air is reduced; therefore, the safety of the whole test process is improved; on the other hand, the dissolution efficiency is improved, so that the possibility that the metal rubidium sample is exposed in the air for a long time is reduced, impurities in the air are prevented from being mixed into a sample system to interfere a test result, and the accuracy of the test result is improved; meanwhile, the nine impurity elements are accurately tested by combining two high-sensitivity and high-precision analysis means of inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry, and the accuracy of the test result is further guaranteed by calculating the total mass of the impurities and converting the purity of the metal rubidium.

Description

A method for testing the purity of metallic rubidium Technical Field

[0001] This invention belongs to the field of analytical chemistry technology, and specifically relates to a method for testing the purity of metallic rubidium. Background Technology

[0002] Rubidium, a rare and strategically important emerging metal, has been widely used in specialty materials, information technology, biomedicine, and quantum computing due to its excellent optoelectronic properties and favorable physicochemical characteristics. As an alkali metal, rubidium is soft, has a low melting point, and is easily ionized. It is spontaneously combustible in air and burns violently or even explodes upon contact with water, requiring storage in dry mineral oil or sealed in an inert gas environment. The production of metallic rubidium is significantly limited by extraction technology, and its purity is a core indicator for research into extraction processes and for the production and sale of rubidium products.

[0003] Currently, according to the industry standard YS / T1246—2018 "Russium", the purity of high-purity (content above 99%) metallic rubidium is determined by the impurity reduction method. That is, after determining the content of nine impurities in metallic rubidium, namely lithium, sodium, potassium, cesium, calcium, magnesium, iron, aluminum and lead, the impurity content is subtracted from 100% to obtain the purity of metallic rubidium.

[0004] The method for testing the purity of rubidium in metallic rubidium disclosed in the relevant technology is as follows: expose the metallic rubidium sample to air for natural oxidation for more than 15 hours, and use the moisture in the air to dissolve the metallic rubidium sample; test the mass concentration of impurity elements in metallic rubidium by inductively coupled plasma mass spectrometry and atomic emission spectrometry, and then obtain the purity of metallic rubidium sample. The relevant technical solution has the following problems: (1) After sampling, the sample is removed from the environment and exposed to air, and may still spontaneously combust, which poses a high safety risk; (2) Rubidium is easily oxidized in air to form rubidium superoxide, and when using the moisture in the air to dissolve the sample, the moisture content cannot be quantitatively controlled, making it difficult to determine whether rubidium and its oxides have reacted completely, which directly affects the accuracy of the analysis results; (3) The sample amount of this method is extremely small, and the analysis of impurity element content in rubidium belongs to trace element analysis. The sample is exposed to air for more than 15 hours, which not only results in low dissolution efficiency, but may also introduce impurity elements such as sodium, calcium, and magnesium in the air, which will further interfere with the accuracy of the analysis results. Summary of the Invention

[0005] This application addresses the aforementioned issues and aims to provide a method for testing the purity of metallic rubidium. This method balances high safety, high testing efficiency, and high accuracy.

[0006] To achieve the above objectives, this application provides a method for testing the purity of metallic rubidium, comprising: S1: dissolving a metallic rubidium sample in an organic alcohol solvent to obtain an intermediate; adding nitric acid solution to the intermediate to leach impurity elements, the impurity elements including lithium, sodium, potassium, calcium, magnesium, iron, aluminum, lead, and cesium (9 elements in total); adjusting the volume to obtain a test solution; performing a blank test to obtain a blank solution, the blank solution comprising a mixture of organic alcohol solvent and nitric acid solution; S2: determining the impurity element content in the metallic rubidium sample; S2 includes S2-1 to S2-3: S2-1: performing inductively coupled plasma atomic emission spectrometry (ICP-AES) on the test solution and the blank solution to obtain the purity of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after subtracting the blank. S2-2: Take the test solution and blank solution for inductively coupled plasma mass spectrometry (ICP-MS) to obtain the mass concentration of cesium in the test solution after subtracting the blank; S2-3: Based on the mass concentration of impurity elements in the test solution after subtracting the blank and the volume of the test solution, calculate the mass of impurity elements in the rubidium metal sample. The mass concentration of impurity elements in the test solution after subtracting the blank is the sum of the total mass concentration of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after subtracting the blank and the mass concentration of cesium in the test solution after subtracting the blank; S3: Subtract the mass of impurity elements in the rubidium metal sample from the mass of the rubidium metal sample to obtain the mass of rubidium in the rubidium metal sample. The purity of rubidium in the rubidium metal sample is obtained by the ratio of the mass of rubidium to the mass of the rubidium metal sample.

[0007] In some embodiments, the organic alcohol solvent includes methanol and ethanol.

[0008] In some embodiments, the mass of the rubidium metal sample is 0.1 g to 0.5 g.

[0009] In some embodiments, the volume of the organic alcohol solvent is 1 mL to 6 mL.

[0010] In some embodiments, the nitric acid solution has a volume fraction of 2% to 5%.

[0011] In some embodiments, the volume ratio of the organic alcohol solvent to the nitric acid solution is 1:9 or 2:8.

[0012] In some embodiments, in S1, the mass of the rubidium metal sample is 0.1 g to 0.3 g, and the volume of the organic alcohol solvent is 1 mL to 4 mL.

[0013] In some embodiments, in S1, the mass of the rubidium metal sample is 0.3 g to 0.5 g, and the volume of the organic alcohol solvent is 4 mL to 6 mL.

[0014] In some implementations, S1 is performed in an argon atmosphere equipped with a precision balance.

[0015] In some implementations, the water content in the argon atmosphere is less than 1 μg / mL.

[0016] In some implementations, the oxygen content in the argon atmosphere is less than 1 μg / mL.

[0017] In some implementations, the leakage rate of the argon atmosphere is less than 0.001 vol% / h.

[0018] In some embodiments, S2-1 includes: S2-1-1: Performing inductively coupled plasma atomic emission spectrometry (ICP-AES) on the test solution and blank solution, recording the spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution and blank solution, and substituting each spectral signal intensity value into the corresponding impurity element standard curve and blank standard curve to obtain the concentrations of lithium, sodium, potassium, calcium, magnesium, iron, and aluminum in the test solution and blank solution, respectively. The mass concentration of lead; S2-1-2: Subtract the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the blank solution from the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after blank subtraction; The impurity element standard curve and the blank standard curve are plotted using the following steps: S101: Preparation N bottles of blank standard solutions containing all eight impurity elements, with progressively increasing mass concentrations, were prepared. No rubidium matrix was added to any of the blank standard solutions, where N is a positive integer from 3 to 5. N bottles of impurity element standard solutions containing all eight impurity elements, with progressively increasing mass concentrations, were also prepared. The same mass concentration of rubidium matrix was added to each impurity element standard solution, where N is a positive integer from 3 to 5. S102: Inductively coupled plasma atomic emission spectrometry (ICP-AES) was performed on each impurity element standard solution and the blank standard solution in ascending order of mass concentration. Record the spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solution and blank standard solution. Plot the impurity element standard curves and blank standard curves for lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solution and blank standard solution, respectively, with the mass concentration of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solution and blank standard solution as the x-axis and the corresponding spectral signal intensity values ​​as the y-axis.

[0019] In some embodiments, in S101, the mass concentration of the rubidium matrix in the impurity element standard solution is the ratio of the mass of the metallic rubidium sample to the molar mass of the rubidium matrix and the volume of the solution to be tested.

[0020] In some embodiments, S2-2 includes: S2-2-1: During the determination of the mass concentration of cesium in the test solution and blank solution using inductively coupled plasma mass spectrometry (ICP-MS), an indium internal standard is added online, with an indium internal standard mass concentration of 1 ng / mL; S2-2-2: The mass concentration of cesium in the test solution and blank solution is diluted to 0.1 ng / mL-10 ng / mL; ICP-MS is performed on the diluted test solution and blank solution, and the mass spectral intensity values ​​of cesium in the test solution and blank solution and the indium internal standard are recorded; The ratio of the mass spectral intensity value of cesium in the test solution and blank solution to the indium internal standard mass spectral intensity value is substituted into the cesium standard curve to obtain the original measured value, which is then multiplied by the dilution factor to obtain the mass concentration of cesium in the test solution and the mass concentration of cesium in the blank solution; S2-2-3: The mass concentration of cesium in the test solution is... The mass concentration of cesium in the test solution is obtained by subtracting the mass concentration of cesium in the blank solution from the mass concentration of cesium in the blank solution. The cesium standard curve is plotted using the following steps: S201: Prepare Q bottles of cesium standard solutions with sequentially increasing mass concentrations, where Q is a positive integer from 3 to 5; S202: Perform inductively coupled plasma mass spectrometry (ICP-MS) on each bottle of cesium standard solution in ascending order of mass concentration, adding an indium internal standard at a concentration of 1 ng / mL online, and recording the mass spectrometric intensity values ​​of cesium in each bottle of cesium standard solution and the indium internal standard; S203: Plot the cesium standard curve with the mass concentration of cesium in each cesium standard solution as the x-axis and the ratio of the mass spectrometric intensity value of cesium in the cesium standard solution to the indium internal standard as the y-axis.

[0021] This application achieves the following effects: The rubidium purity testing method provided in this application uses an organic alcohol-nitric acid solution system to dissolve the rubidium sample. The organic alcohol can accelerate the dissolution rate of the rubidium sample, which on the one hand can significantly shorten the contact time between the rubidium sample and air, reducing the risk of spontaneous combustion in air, thereby improving the safety of the entire testing process; on the other hand, the improved dissolution efficiency reduces the possibility of the rubidium sample being exposed to air for a long time, avoiding the interference of impurities in the air with the test results, and improving the accuracy of the test results. At the same time, it combines two highly sensitive and precise analytical methods, inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry, to accurately test nine impurity elements. By calculating the total mass of impurities and converting it to the purity of rubidium, the accuracy of the test results is further guaranteed. Attached Figure Description

[0022] Figure 1 is a flowchart of the test method for the purity of metallic rubidium provided in this application. Detailed Implementation

[0023] The following detailed description, with appropriate reference to the accompanying drawings, provides a flowchart illustrating an embodiment of a method for testing the purity of metallic rubidium according to this application. However, unnecessary details may be omitted. For example, detailed descriptions of well-known matters and repetitive descriptions of essentially identical structures may be omitted. This is to avoid unnecessarily lengthy explanations and to facilitate understanding by those skilled in the art. Furthermore, the accompanying drawings and the following description are provided to enable those skilled in the art to fully understand this application and are not intended to limit the subject matter of the claims.

[0024] The "range" disclosed in this application is defined by a lower limit and an upper limit. A given range is defined by selecting a lower limit and an upper limit, which define the boundaries of a particular range. Ranges defined in this way can include or exclude endpoints and can be arbitrarily combined; that is, any lower limit can be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a specific parameter, it is expected that ranges of 60-110 and 80-120 are also included. Furthermore, if minimum range values ​​of 1 and 2 are listed, and if maximum range values ​​of 3, 4, and 5 are listed, then the following ranges are all expected: 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5. In this application, unless otherwise stated, the numerical range "ab" represents a shortened representation of any combination of real numbers between a and b, where a and b are real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed in this article; "0-5" is simply a shortened representation of these numerical combinations. Furthermore, when a parameter is stated as an integer ≥2, it is equivalent to disclosing that the parameter is, for example, an integer such as 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0025] Unless otherwise specified, all embodiments and optional embodiments of this application can be combined to form new technical solutions.

[0026] Unless otherwise specified, all technical features and optional technical features of this application may be combined to form new technical solutions.

[0027] Unless otherwise specified, all steps of this application may be performed sequentially or randomly, preferably sequentially. For example, if the method includes steps (a) and (b), it means that the method may include steps (a) and (b) performed sequentially, or it may include steps (b) and (a) performed sequentially. For example, if the method may also include step (c), it means that step (c) may be added to the method in any order. For example, the method may include steps (a), (b), and (c), or it may include steps (a), (c), and (b), or it may include steps (c), (a), and (b), etc.

[0028] Unless otherwise specified, the terms used in this application have the common meanings as commonly understood by those skilled in the art.

[0029] Unless otherwise specified, the values ​​of the parameters mentioned in this application can be tested using various testing methods commonly used in the art, such as the testing methods provided in this application.

[0030] The method for testing the purity of rubidium in metallic rubidium disclosed in the relevant technology is as follows: the rubidium sample is exposed to air for natural oxidation for more than 15 hours, and the rubidium sample is dissolved by the moisture in the air; the mass concentration of impurity elements in metallic rubidium is tested by inductively coupled plasma mass spectrometry and atomic emission spectrometry, and then the purity of the rubidium sample is obtained. The relevant technical solution has the following problems: (1) After sampling, the sample is removed from the glove box and exposed to air, and spontaneous combustion may still occur, which poses a high safety risk; (2) Rubidium is easily oxidized in air to form rubidium superoxide, and when the sample is dissolved by the moisture in the air, the moisture content cannot be quantitatively controlled, making it difficult to determine whether rubidium and its oxides have reacted completely, which directly affects the accuracy of the analysis results; (3) The sample amount of this method is extremely small, and the analysis of the impurity element content in rubidium belongs to trace element analysis. The sample is exposed to air for more than 15 hours, which not only results in low dissolution efficiency, but may also introduce impurity elements such as sodium, calcium, and magnesium in the air, which will further interfere with the accuracy of the analysis results.

[0031] To address the aforementioned technical problems, this application discloses a method for testing the purity of metallic rubidium. This method balances high safety, high testing efficiency, and high accuracy.

[0032] The following is a detailed description of the scheme disclosed in this application.

[0033] Referring to Figure 1, this application discloses a method for testing the purity of metallic rubidium, the method comprising S1 to S3.

[0034] S1: Dissolve the rubidium metal sample in an organic alcohol solvent to obtain an intermediate. Add nitric acid solution to the intermediate to leach out impurity elements, including nine elements: lithium, sodium, potassium, calcium, magnesium, iron, aluminum, lead, and cesium. After adjusting the volume, obtain the test solution and perform a blank test to obtain a blank solution, which is a mixture of organic alcohol solvent and nitric acid solution. S2: Determine the impurity element content in the rubidium metal sample. S2 includes S2-1 to S2-3: S2-1: Take the test solution and blank solution for inductively coupled plasma atomic emission spectrometry (ICP-AES) to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after subtracting the blank. S2-2: Take the test solution... Inductively coupled plasma mass spectrometry (ICP-MS) was performed on the blank solution to obtain the mass concentration of cesium in the test solution after blank subtraction; S2-3: Based on the mass concentration of impurity elements in the test solution after blank subtraction and the volume of the test solution, the mass of impurity elements in the metallic rubidium sample was calculated. The mass concentration of impurity elements in the test solution after blank subtraction was the sum of the total mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after blank subtraction and the mass concentration of cesium in the test solution after blank subtraction; S3: The mass of rubidium in the metallic rubidium sample was obtained by subtracting the mass of impurity elements from the mass of the metallic rubidium sample. The purity of rubidium in the metallic rubidium sample was obtained by the ratio of the mass of rubidium to the mass of the metallic rubidium sample.

[0035] The rubidium purity testing method provided in this application uses an organic alcohol-nitric acid solution system to dissolve the rubidium sample. The organic alcohol can accelerate the dissolution rate of the rubidium sample, which on the one hand significantly shortens the contact time between the rubidium sample and air, reducing the risk of spontaneous combustion in air and thus improving the safety of the entire testing process; on the other hand, the improved dissolution efficiency reduces the possibility of the rubidium sample being exposed to air for a long time, avoiding the interference of impurities in the air with the test results and improving the accuracy of the test results. At the same time, it combines two highly sensitive and precise analytical methods, inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry, to accurately test nine impurity elements. By calculating the total mass of impurities and converting it into the purity of rubidium, the accuracy of the test results is further guaranteed.

[0036] This application does not specify a particular mass of the rubidium metal sample for symmetrical measurement; the appropriate mass of the rubidium metal sample can be selected according to the requirements.

[0037] In some embodiments, when preparing 10 mL of the test solution, the mass of the rubidium metal sample can be between 0.1 g and 0.5 g. A mass within this range facilitates sufficient reaction between the rubidium metal sample and the organic alcohol solvent and nitric acid solution during subsequent dissolution, while avoiding increased testing difficulty or matrix effect interference due to excessive rubidium metal sample. For example, the mass of the rubidium metal sample can be 0.1 g, 0.2 g, 0.3 g, 0.4 g, 0.5 g, or any value between two of these values.

[0038] In this application, "organic alcohol solvent" refers to alcohol compounds that can react with alkali metals. This application does not specifically limit the organic alcohol solvent; by example, organic alcohol solvents may include, but are not limited to, methanol, ethanol, isopropanol, etc.

[0039] In some embodiments, the organic alcohol solvent includes methanol. The reaction between methanol and alkali metal rubidium is mild and rapid, taking only a few minutes to complete and slowly releasing hydrogen gas, which is unlikely to cause an explosion; therefore, using methanol as the organic alcohol solvent is beneficial to further improve the safety and analytical efficiency of the testing process.

[0040] This application does not specify the amount (volume) of organic alcohol solvent to be added; the amount of organic alcohol solvent to be added can be selected according to the mass of the rubidium metal sample.

[0041] In some embodiments, the mass of the rubidium metal sample is 0.1 g to 0.5 g, and an organic alcohol solvent of 1 mL to 6 mL can be used. The volume of the organic alcohol solvent is within the above range, sufficient to allow the rubidium metal sample to react completely and dissolve, while avoiding the introduction of unnecessary background interference from excessive organic alcohol solvent. Exemplarily, the organic alcohol solvent can be 1 mL, 2 mL, 3 mL, 4 mL, 5 mL, 6 mL, or any value between two of these values.

[0042] In some embodiments, the mass of the rubidium metal sample is 0.1 g to 0.3 g, and 1 mL to 4 mL of organic alcohol solvent can be used. By selecting the above-mentioned volume of organic alcohol solvent, the rapid reaction and complete dissolution of the rubidium metal sample can be promoted, without introducing too much organic alcohol solvent and interfering with subsequent spectroscopic or mass spectroscopic analysis.

[0043] In some embodiments, the mass of the rubidium metal sample is 0.3 g to 0.5 g, and 4 mL to 6 mL of organic alcohol solvent can be used. By selecting the above-mentioned volume of organic alcohol solvent, the rapid reaction and complete dissolution of the rubidium metal sample can be promoted, without introducing too much organic alcohol solvent and interfering with subsequent spectroscopic or mass spectroscopic analysis.

[0044] In this application, "nitric acid solution" is used as an auxiliary reagent to adjust the acidity of the test solution and promote the complete dissolution of the rubidium metal sample.

[0045] This application does not specify the volume fraction (concentration) of the nitric acid solution; the volume fraction of the nitric acid solution can be selected according to requirements.

[0046] In some embodiments, the volume fraction of the nitric acid solution is 2% to 5%. Choosing a nitric acid solution with a volume fraction range helps to ensure the dissolution efficiency of the rubidium metal sample while avoiding corrosion of the sample or equipment by the strong acid. Exemplarily, the volume fraction of the nitric acid solution is 2%, 2.5%, 3%, 3.5%, 4%, 4%, 4.5%, 5%, or any value between two of these two values.

[0047] In some embodiments, the volume ratio of the organic alcohol solvent to the nitric acid solution is 1:9 or 2:8. This helps to ensure the dissolution efficiency of the rubidium metal sample without interfering with subsequent spectroscopic or mass spectrometric analyses due to the introduction of excessive organic alcohol solvent. Exemplarily, the volume ratio of the organic alcohol solvent to the nitric acid solution is 1:9, 1.2:8.8, 1.4:8.6, 1.6:8.4, 1.8:8.2, 2:8, or any value between two of these values.

[0048] In some embodiments, S1, the mass of the rubidium metal sample is 0.1 g, the volume of methanol is 1 mL, and the test solution is prepared using 9 mL of 2% nitric acid solution. This embodiment, by setting reasonable parameters for the rubidium metal sample mass, the volume of the organic alcohol solvent, the concentration of the nitric acid solution, and both the concentration and volume of the nitric acid solution, facilitates safe and efficient processing of the rubidium metal sample, providing stable sample conditions for subsequent impurity element analysis.

[0049] In practice, rubidium metal samples are highly reactive metals that are extremely prone to spontaneous combustion in air or violent reaction and even explosion upon contact with water. To enhance testing safety, in some implementations, S1 is performed in an argon atmosphere to prevent the rubidium metal sample from coming into contact with air.

[0050] The argon atmosphere environment may include, but is not limited to, glove boxes and glove bags.

[0051] In some embodiments, S1 is performed in an argon atmosphere equipped with a precision balance. Processing the rubidium metal sample in an argon atmosphere effectively prevents spontaneous combustion or water-induced explosion when the sample is exposed to air, thus improving experimental safety. Furthermore, an argon atmosphere reduces the risk of introducing external impurities, ensuring the accuracy of subsequent analytical results.

[0052] In some embodiments, the oxygen content in the argon atmosphere is less than 1 μg / mL. Oxidation reactions are highly likely to occur during the processing of rubidium metal samples. This application controls the oxygen content in the argon atmosphere to below 1 μg / mL, effectively preventing the rubidium metal samples from being oxidized and forming oxides, thereby reducing the risk of impurity introduction and ensuring the accuracy of subsequent analytical results. Exemplarily, the oxygen content in the argon atmosphere is 0.1 μg / mL, 0.2 μg / mL, 0.3 μg / mL, 0.4 μg / mL, 0.5 μg / mL, 0.6 μg / mL, 0.7 μg / mL, 0.8 μg / mL, 0.9 μg / mL, 1 μg / mL, or any value between two of these two values.

[0053] In some embodiments, the leakage rate of the argon atmosphere is less than 0.001 vol% / h. By controlling the leakage rate of the argon atmosphere to below 0.001 vol% / h, this application can ensure the stability and sealing of the argon atmosphere throughout the entire rubidium purity testing process, preventing outside air from entering the operating area, thereby reducing the risk of impurity introduction and ensuring the accuracy of subsequent analytical results. Exemplarily, the argon atmosphere leakage rate is 0.0001 vol% / h, 0.0002 vol% / h, 0.0003 vol% / h, 0.0004 vol% / h, 0.0005 vol% / h, 0.0006 vol% / h, 0.0007 vol% / h, 0.0008 vol% / h, 0.0009 vol% / h, 0.001 vol% / h, or a value between any two of these two values.

[0054] In this application, the impurities in the rubidium metal sample can be divided into two categories. One category contains eight impurity elements: lithium, sodium, potassium, magnesium, iron, aluminum, and lead. The other category contains cesium.

[0055] In step S2-1 of this application, inductively coupled plasma atomic emission spectrometry (ICP-AES) is used to test for lithium, sodium, potassium, magnesium, iron, aluminum, and lead. ICP-AES can simultaneously test multiple elements, thereby improving testing efficiency.

[0056] In some implementations, the matrix matching standard curve method can be used to test the mass of lithium, sodium, potassium, magnesium, iron, aluminum and lead elements. Specifically, S2-1 includes S2-1-1 to S2-1-3.

[0057] S2-1-1: Inductively coupled plasma atomic emission spectrometry (ICP-AES) is performed on the test solution and blank solution to record the spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test and blank solutions. These spectral signal intensity values ​​are then substituted into the corresponding impurity element standard curves and blank standard curves to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test and blank solutions, respectively. In S2-1-1, ICP-AES is performed on the test solution to obtain the spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead. These signal intensity values ​​are then substituted into the previously plotted impurity element standard curves, and the corresponding mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead are calculated using linear regression equations.

[0058] S2-1-2: Subtract the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the blank solution from the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after subtracting the blank.

[0059] The impurity element standard curve and blank standard curve are plotted using the following steps: S101: Prepare N bottles of blank standard solutions with progressively increasing mass concentrations containing all 8 impurity elements. No rubidium matrix is ​​added to any of the blank standard solutions, where N is a positive integer from 3 to 5. Prepare N bottles of impurity element standard solutions with progressively increasing mass concentrations containing all 8 impurity elements. The same mass concentration of rubidium matrix is ​​added to each of the impurity element standard solutions, where N is a positive integer from 3 to 5. The preparation process of the standard solutions for lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead is explained using N=5 as an example. In some specific embodiments, five bottles of mixed standard solutions of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead can be prepared, with mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead of 0.01 μg / mL, 0.05 μg / mL, 0.1 μg / mL, 0.5 μg / mL, and 2 μg / mL, respectively. Each bottle of standard solution also contains rubidium of the same mass concentration as a matrix component.

[0060] S102: Inductively coupled plasma atomic emission spectrometry (ICP-AES) was performed on each bottle of impurity element standard solution and blank standard solution in order of increasing mass concentration. The spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solution and blank standard solution were recorded. The purpose of performing the tests in order of increasing mass concentration is to ensure that the spectral intensity value shows a good linear relationship with the change of mass concentration, thereby further ensuring the accuracy of subsequent test results.

[0061] S103: Plot impurity element standard curves and blank standard curves for lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in impurity element standard solutions and blank standard solutions, respectively, with the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solutions and blank standard solutions as the x-axis and the corresponding spectral signal intensity values ​​as the y-axis. The linear correlation coefficient should be ≥0.999.

[0062] In this embodiment, the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead are calculated by plotting standard curves for the impurity elements and combining this with inductively coupled plasma atomic emission spectrometry (ICP-AES). The same matrix components as the test solution are added to the impurity element standard solution to eliminate the influence of the matrix effect, making the impurity standard solution and the test solution more chemically similar, thereby reducing errors and improving the accuracy of the test results.

[0063] In some embodiments, the mass concentration of the rubidium matrix in the impurity element standard solution is the ratio of the mass of the metallic rubidium sample to the molar mass of the rubidium matrix and the volume of the test solution. In this embodiment, by using the ratio of the mass of the metallic rubidium sample to the volume of the test solution formed after its dissolution as the mass concentration of rubidium in the impurity element standard solution, consistency of the rubidium mass concentration in the impurity element standard solution and the test solution is achieved. This ensures matrix matching between the impurity element standard solution and the test solution, significantly eliminating interference caused by matrix effects and thus improving the accuracy of the test results.

[0064] The preparation process of the impurity element standard solution is as follows: First, determine the target mass concentration of rubidium in the standard solution to be prepared (this concentration is consistent with the rubidium concentration in the test solution) by using the ratio of the mass of the rubidium sample to the molar mass of rubidium in the sample and the volume of the test solution formed after dissolution; second, based on the above target mass concentration and the mass fraction of rubidium in rubidium chloride, calculate the specific mass of rubidium chloride required to prepare the impurity element standard solution with the target concentration; finally, add the calculated mass of rubidium chloride to the impurity element standard solution to complete the preparation of the standard solution.

[0065] Rubidium metal samples typically contain cesium. Since cesium is difficult to analyze stably and accurately using inductively coupled plasma mass spectrometry (ICP-MS), this application employs ICP-MS to test for cesium, ensuring the accuracy of the test results.

[0066] In some implementations, S2-2 includes S2-2-1 to S2-2-3.

[0067] S2-2-1: During the determination of the mass concentration of cesium in the test solution and blank solution by inductively coupled plasma mass spectrometry, an indium internal standard was added online with a mass concentration of 1 ng / mL.

[0068] Adding indium as an internal standard online during the testing of the test solution can correct the influence of factors such as instrument drift and matrix interference on the measurement results, monitor and ensure the consistency of test conditions, thereby reducing sources of error and improving the accuracy of test results. Indium was chosen as the internal standard because it has stable response characteristics in mass spectrometry and does not react chemically with the analyte.

[0069] S2-2-2: Dilute the cesium concentration in the test solution and blank solution to 0.1 ng / mL-10 ng / mL; perform inductively coupled plasma mass spectrometry (ICP-MS) on the diluted test solution and blank solution, and record the mass spectral intensity values ​​of cesium and indium (internal standard); perform ICP-MS on the diluted test solution and blank solution, and record the mass spectral intensity values ​​of cesium and indium (internal standard). Intensity value; Substitute the ratio of the mass spectrometry intensity value of cesium in the solution to that of the internal standard indium into the standard curve to obtain the original measurement value, and then multiply it by the dilution factor to obtain the mass concentration of cesium in the solution; Substitute the ratio of the mass spectrometry intensity value of cesium in the test solution and the blank solution to that of the internal standard indium into the cesium standard curve to obtain the original measurement value, and then multiply it by the dilution factor to obtain the mass concentration of cesium in the test solution and the mass concentration of cesium in the blank solution; S 2-2-3: The mass concentration of cesium in the test solution is subtracted from the mass concentration of cesium in the blank solution to obtain the mass concentration of cesium in the test solution after subtracting the blank. The cesium standard curve is plotted using the following steps: S201: Prepare Q bottles of cesium standard solutions with progressively increasing cesium mass concentrations, where Q is a positive integer from 3 to 5; S202: Inductively couple each bottle of cesium standard solution in ascending order of cesium mass concentration. Combined plasma mass spectrometry (PMS) was used for the test. Indium internal standard was added online at a concentration of 1 ng / mL. The mass spectrometry intensity values ​​of cesium in each cesium standard solution and the internal standard indium were recorded. S203: A cesium standard curve was plotted with the mass concentration of cesium in each cesium standard solution as the x-axis and the ratio of the mass spectrometry intensity value of cesium in the cesium standard solution to the mass spectrometry intensity value of the internal standard indium as the y-axis. The linear correlation coefficient should be ≥0.999.

[0070] In some embodiments, step S2-2-3 further includes diluting the test solution to a mass concentration of 0.1 ng / mL to 10 ng / mL. Diluting the test solution before inductively coupled plasma mass spectrometry (ICP-MS) testing ensures that the cesium concentration in the test solution falls within the optimal linear response range of ICP-MS. Furthermore, the dilution operation simultaneously reduces the concentration of matrix components in the test solution, further weakening the interference of matrix effects on cesium detection, thereby improving the accuracy of the test results.

[0071] The following are embodiments of this application. The embodiments described below are exemplary and are only used to explain this application, and should not be construed as limiting this application. Unless otherwise stated, all reagents used are commercially available, and all equipment used is conventional equipment. The patent uses analytical grade reagents conforming to national standards and water with a resistivity of not less than 18.2 MΩ•cm. Other reagents used include nitric acid solution (ρ≈1.42 g / mL), methanol (ω≥99.9%), rubidium chloride (ω≥99.5%), argon gas with a purity ≥99.999%, and oxygen.

[0072] 1. Construction of standard curves for impurity elements: S101: Prepare N bottles of blank standard solutions containing all eight impurity elements, with progressively increasing mass concentrations. No rubidium matrix is ​​added to any of the blank standard solutions, where N is a positive integer from 3 to 5. Prepare standard solutions for lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead using rubidium chloride and nitric acid solutions, respectively. The mass concentrations of each element's standard solution are shown in Tables 1 and 2. All standard solutions contain 11765 µg / mL of rubidium.

[0073] Table 1: Standard solutions of calcium, magnesium, aluminum, iron, and lithium:

[0074] Table 2: Standard solutions of sodium, potassium, and lead:

[0075] S102: In order of increasing mass concentration, inductively coupled plasma atomic emission spectrometry (ICP-AES) was performed on each bottle of impurity element standard solution and blank standard solution. The spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solution and blank standard solution were recorded. The mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead were measured using an ICP-AES spectrometer. According to the instrument's analytical principle, analytical lines with high intensity, high sensitivity, and no mutual interference between coexisting elements should be selected. In addition, based on the spectra of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead, analytical lines with good peak shape, low interference, and simple background should be selected. The final analytical spectra of each element are detailed in Table 3.

[0076] Table 3: Spectral lines for lithium, sodium, potassium, calcium, magnesium, aluminum, iron, and lead:

[0077] The operating conditions and parameters of inductively coupled plasma spectroscopy are shown in Table 4. Using an organic sample introduction system, the spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the standard solutions of each impurity element were measured sequentially from low to high concentration at specific spectral lines (see Table 3).

[0078] Based on the direct proportionality between spectral intensity and mass concentration, standard curves (impurity element standard curves) for each element (lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead) are obtained, and the linear correlation coefficient should be ≥0.999.

[0079] Table 4: Operating conditions and parameter values ​​for inductively coupled plasma spectroscopy:

[0080] Table 5: Detection limits of inductively coupled plasma spectroscopy:

[0081] S103: Plot the impurity element standard curves and blank standard curves for lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solutions and blank standard solutions, respectively, with the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solutions and blank standard solutions as the x-axis and the corresponding spectral signal intensity values ​​as the y-axis.

[0082] 2. Plotting the cesium standard curve: S201: Prepare cesium standard solutions in bottles Q with progressively increasing cesium concentrations, where Q is a positive integer from 3 to 5; see Table 6 for the mass concentrations of the cesium standard solutions.

[0083] Table 6: Standard solutions of cesium:

[0084] S202: Following the order of cesium concentration from low to high, inductively coupled plasma mass spectrometry (ICP-MS) was performed on each cesium standard solution. Indium internal standard was added online at a concentration of 1 ng / mL. The mass spectrometric intensity values ​​of cesium in each standard solution and the indium internal standard were recorded. An ICP-MS instrument was used, and a high intensity was selected based on the instrument's analytical principles. The operating conditions and parameters of ICP-MS are shown in Table 7. The mass spectrometric intensity values ​​of cesium in the standard solution and the indium internal standard were measured sequentially from low to high concentration.

[0085] Table 7: Operating conditions and parameters of inductively coupled plasma mass spectrometry:

[0086] S203: The cesium standard curve is plotted with the mass concentration of cesium in each cesium standard solution as the abscissa and the ratio of the mass spectrometry intensity of cesium in the cesium standard solution to the mass spectrometry intensity of the internal standard indium as the ordinate.

[0087] Example 1S1: Weigh approximately 0.1 g of rubidium metal sample into a centrifuge tube under an inert (argon) atmosphere. The mass of the rubidium metal sample is recorded as m, accurate to 0.001 g. Add 1 mL of methanol. After the rubidium metal sample has reacted completely, transfer the solution to a 10 mL volumetric flask and dilute to the mark with nitric acid solution (2% by volume). Mix well. The volume of the solution to be tested is recorded as V.

[0088] To complete the blank test along with the sample, a mixture of methanol and 20% (v / v) nitric acid solution at a volume ratio of 1:9 was used as the blank sample to obtain the blank solution.

[0089] S2-1: Under the working conditions and parameters listed in Table 4, inductively coupled plasma atomic emission spectrometry (ICP-AES) was performed on the test solution and the blank solution. The mass concentration of impurity elements in the blank sample is expressed as follows: , The mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the blank sample.

[0090] After subtracting the blank, the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after blank subtraction are obtained; S2-1-1: Inductively coupled plasma atomic emission spectrometry (ICP-AES) is performed on the test solution and the blank solution. The spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution and the blank solution are recorded. The spectral signal intensity values ​​are substituted into the corresponding impurity element standard curve and blank standard curve, respectively, to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution and the blank solution. S2-1-2: Subtract the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the blank solution from the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after subtracting the blank concentrations.

[0091] S2-2-1: Under the working conditions and parameters recorded in Table 7, during the determination of the mass concentration of cesium in the test solution and blank solution using inductively coupled plasma mass spectrometry (ICP-MS), an indium internal standard was added online at a concentration of 1 ng / mL. S2-2-2: The mass concentration of cesium in the test solution and blank solution was diluted to 0.1 ng / mL–10 ng / mL. ICP-MS was then performed on the diluted test solution and blank solution, and the mass spectral intensity values ​​of cesium and indium were recorded. The ratio of the mass spectral intensity value of cesium to that of indium was substituted into the cesium standard curve to obtain the original measured value. This original value was then multiplied by the dilution factor to obtain the mass concentration of cesium in the test solution and the blank solution.

[0092] S2-2-3: The mass concentration of cesium in the test solution is obtained by subtracting the mass concentration of cesium in the blank solution from the mass concentration of cesium in the test solution after deducting the blank.

[0093] S2-3: Calculate the mass of impurity elements in the rubidium sample based on the product of the mass concentration of impurity elements in the test solution after blank subtraction and the volume of the test solution. The mass concentration of impurity elements in the test solution after blank subtraction is the sum of the total mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after blank subtraction and the mass concentration of cesium in the test solution after blank subtraction; where the mass concentration of impurity elements in the test solution after blank subtraction is expressed as... .

[0094] The mass of impurity elements in a metallic rubidium sample is expressed as: . The mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, lead, and cesium in the solution to be tested are given. This represents the mass concentration of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, lead, and cesium in the blank solution.

[0095] S3: Based on the difference method, the mass of rubidium in the rubidium sample is obtained by subtracting the mass of impurity elements from the mass of the rubidium sample. The purity of rubidium in the rubidium sample is then obtained by the ratio of the mass of rubidium to the mass of the rubidium sample.

[0096] The purity of rubidium metal (Rb) is calculated using the following formula: (Rb is expressed as a mass fraction of...) ):

[0097] In the formula: m is the mass of the rubidium metal sample, in grams (g).

[0098] Comparative Example 1 used the same method as Example 1 to test the purity of rubidium in the rubidium sample, except that in S1, methanol was not used to dissolve the rubidium sample; instead, the rubidium sample was left in the air, and the moisture in the air dissolved the rubidium sample. Also, in S2, inductively coupled plasma atomic emission spectrometry with an organic sample introduction system was not used for sample testing.

[0099] Spiked recovery test Before dissolving the rubidium metal sample in methanol-nitric acid solution, standard solutions of lithium, calcium, magnesium, aluminum, iron, and lead with a concentration of 0.1 μg / mL, and standard solutions of sodium, potassium, and cesium with a concentration of 1 μg / mL, were added to methanol to obtain the test solutions. The test solutions were tested using the same method as in Example 1. The mass concentrations of lithium, calcium, magnesium, aluminum, iron, lead, sodium, potassium, and cesium in the rubidium metal sample were measured, and the spiked recoveries were calculated after subtracting the blank (see Table 8).

[0100] Spike recovery rate is the core indicator characterizing the accuracy of the test method in this application. The closer the spike recovery rate is to 100%, the higher the accuracy of the test method; the further the spike recovery rate deviates from 100%, the lower the accuracy of the test method.

[0101] Table 8: Spike Recovery Rate

[0102] Statistics on sample dissolution time The time interval between the completion of the weighing operation of the rubidium metal sample and the completion of the preparation operation of the test solution is defined as the sample dissolution time. The sample dissolution time is the core indicator characterizing the test efficiency of the test method of this application. The shorter the sample dissolution time, the higher the test efficiency of the corresponding test method, and the longer the sample dissolution time, the lower the test efficiency of the corresponding test method.

[0103] Table 9

[0104] It should be noted that this application is not limited to the above-described embodiments. The above embodiments are merely examples, and any embodiments with the same structure and effect as the technical concept within the scope of this application are included in the technical scope of this application. Furthermore, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways of constructing by combining some of the constituent elements of the embodiments, without departing from the spirit of this application, are also included in the scope of this application.

Claims

1. A method for testing the purity of metallic rubidium, characterized in that, include: S1: Dissolve the rubidium metal sample in an organic alcohol solvent to obtain an intermediate. Add nitric acid solution to the intermediate to leach impurity elements, which include nine elements: lithium, sodium, potassium, calcium, magnesium, iron, aluminum, lead, and cesium. After adjusting the volume, obtain the test solution and perform a blank test to obtain a blank solution. The blank solution consists of a mixture of the organic alcohol solvent and the nitric acid solution. S2: Determine the impurity element content in the rubidium metal sample. S2 includes S2-1 to S2-3: S2-1: Take the test solution and the blank solution for inductively coupled plasma atomic emission spectrometry (ICP-AES) to obtain the mass concentration of the eight impurity elements (lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead) in the test solution after subtracting the blank. S2-2: Take the test solution and the blank solution for IES... S2-3: The mass concentration of cesium in the test solution after blank subtraction is obtained by inductively coupled plasma mass spectrometry (ICP-MS) of the white solution; S2-3: The mass of impurity elements in the rubidium metal sample is calculated based on the product of the mass concentration of impurity elements in the test solution after blank subtraction and the volume of the test solution. The mass concentration of impurity elements in the test solution after blank subtraction is the sum of the total mass concentration of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after blank subtraction and the mass concentration of cesium in the test solution after blank subtraction; S3: The mass of rubidium in the rubidium metal sample is obtained by subtracting the mass of impurity elements from the mass of the rubidium metal sample. The purity of rubidium in the rubidium metal sample is obtained by the ratio of the mass of rubidium to the mass of the rubidium metal sample.

2. The test method according to claim 1, characterized in that, The organic alcohol solvents include methanol and ethanol.

3. The test method according to claim 1, characterized in that, The S1 satisfies the following: (1) the mass of the rubidium metal sample is 0.1 g to 0.5 g; (2) the volume of the organic alcohol solvent is 1 mL to 6 mL; (3) the volume fraction of the nitric acid solution is 2% to 5%; and (4) the volume ratio of the organic alcohol solvent to the nitric acid solution is 1:9 or 2:

8.

4. The test method according to claim 3, characterized in that, In S1, the mass of the rubidium metal sample is 0.1 g to 0.3 g, and the volume of the organic alcohol solvent is 1 mL to 4 mL.

5. The test method according to claim 3, characterized in that, In S1, the mass of the rubidium metal sample is 0.3g to 0.5g, and the volume of the organic alcohol solvent is 4mL to 6mL.

6. The method for testing the purity of metallic rubidium according to claim 1, characterized in that, The test environment of S1 meets the following requirements: (1) it is carried out in an argon atmosphere with a precision balance; (2) the water content of the argon atmosphere is less than 1 μg / mL; (3) the oxygen content of the argon atmosphere is less than 1 μg / mL; (4) the leakage rate of the argon atmosphere is less than 0.001 vol% / h.

7. The test method according to any one of claims 1 to 6, characterized in that, S2-1 includes: S2-1-1: Performing inductively coupled plasma atomic emission spectrometry (ICP-AES) on the test solution and the blank solution, recording the spectral signal intensity values ​​of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution and the blank solution, and substituting each spectral signal intensity value into the corresponding impurity element standard curve and blank standard curve to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution and the blank solution, respectively; S2 -1-2: Subtract the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the blank solution from the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution to obtain the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the test solution after deducting the blank. The impurity element standard curve and the blank standard curve are plotted using the following steps: S101: Prepare a solution containing all eight impurities. N bottles of blank standard solutions with progressively increasing mass concentrations of the elements are prepared, each without rubidium matrix, where N is a positive integer from 3 to 5; N bottles of impurity element standard solutions with progressively increasing mass concentrations are prepared, each containing the same mass concentration of rubidium matrix, where N is a positive integer from 3 to 5; S102: Inductively coupled plasma atomic emission spectrometry (ICP-AES) is performed on each of the impurity element standard solutions and the blank standard solutions in ascending order of mass concentration, and the results of the impurity element tests are recorded. S103: Plot the impurity element standard curves and the blank standard curves for lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the standard solution and the blank standard solution, respectively, with the mass concentrations of lithium, sodium, potassium, calcium, magnesium, iron, aluminum, and lead in the impurity element standard solution and the blank standard solution as the abscissa and the corresponding spectral signal intensity values ​​as the ordinate.

8. The test method according to claim 7, characterized in that, In step S101, the mass concentration of the rubidium matrix in the impurity element standard solution is the ratio of the mass of the metallic rubidium sample to the molar mass of the rubidium matrix and the volume of the solution to be tested.

9. The test method according to any one of claims 1 to 8, characterized in that, S2-2 includes: S2-2-1: During the determination of the mass concentration of cesium in the test solution and the blank solution using the inductively coupled plasma mass spectrometry (ICP-MS), an indium internal standard is added online, with a concentration of 1 ng / mL; S2-2-2: The mass concentration of cesium in the test solution and the blank solution is diluted to 0.1 ng / mL-10 ng / mL; ICP-MS is performed on the diluted test solution and the blank solution, and the mass spectral intensity values ​​of cesium and indium are recorded; The ratio of the mass spectral intensity value of cesium to indium is substituted into the cesium standard curve to obtain the original measured value, which is then multiplied by the dilution factor to obtain the mass concentration of cesium in the test solution and the blank solution; S2-2-3: The mass concentration of cesium in the test solution and the blank solution is diluted to 0.1 ng / mL-10 ng / mL; Inductively coupled plasma mass spectrometry is performed on the diluted test solution and the blank solution, and the mass spectral intensity value of indium is recorded; The mass concentration of cesium in the test solution and the blank solution is then multiplied by the dilution factor to obtain the mass concentration of cesium in the test solution and the mass concentration of cesium in the blank solution; The mass concentration of cesium in the test solution is obtained by subtracting the mass concentration of cesium in the blank solution from the mass concentration of cesium in the test solution after deducting the blank. The cesium standard curve is plotted using the following steps: S201: Prepare Q bottles of cesium standard solutions with progressively increasing cesium mass concentrations, where Q is a positive integer from 3 to 5; S202: Sequentially irradiate each bottle of cesium standard solution according to its increasing cesium mass concentration. Inductively coupled plasma mass spectrometry (ICP-MS) was used for testing. Indium internal standard was added online at a concentration of 1 ng / mL. The mass spectrometric intensity values ​​of cesium in each cesium standard solution and the internal standard indium were recorded. S203: The cesium standard curve was plotted with the mass concentration of cesium in each cesium standard solution as the x-axis and the ratio of the mass spectrometric intensity value of cesium in the cesium standard solution to the mass spectrometric intensity value of the internal standard indium as the y-axis.

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