Method for detecting content of metal and metalloid impurities in high-purity tin precursor

Abstract

The invention discloses a method for detecting the content of metal and metalloid impurities in a high-purity tin precursor, and relates to the technical field of detection.The detection method comprises the steps that an ICP-MS / MS instrument is used for establishing a standard curve and a regression equation reflecting the relation between the concentration of the metal or metalloid impurities and a response signal value; according to the method, the to-be-detected solution is detected, the content of the metal impurities is calculated according to the regression equation, and the interference of a matrix on element detection can be effectively reduced by optimizing the pretreatment method of the to-be-detected solution, selecting detection parameters of the ICP-MS / MS instrument on various metal impurities and other test conditions, so that the detection result tends to be true, and the accuracy of the detection result is improved.

Description

Technical Field

[0001] The present invention relates to the field of detection technology, and in particular to a method for detecting the content of metal and metalloid impurities in a high-purity tin precursor. Background Art

[0002] The measurement of trace metal impurities in high-purity electronic chemicals generally adopts the I CP-MS analysis method. The test mode of traditional I CP-MS analysis instruments such as Thermo Fisher i CAP RQ can complete the test of most elements in the collision mode, but it cannot eliminate the polyatomic ion interference, oxide interference, double charge interference, hydride interference and isobaric interference in mass spectrometry interference, as well as the matrix effect and physical effect in non-mass spectrometry interference; for example, when testing tetra(dimethylamino)tin (TDMASn) samples, the isotopes of Sn are: 112Sn 2+ 、114Sn 2+ 、115Sn 2+ 、116Sn 2+ 、117Sn 2+ 、118Sn 2+ 、119Sn 2+ 、120Sn 2+ 、122Sn 2+ 、124Sn 2+ 10 elements interfered by Sn matrix are: (112Sn 2+ ++)56Fe,(114Sn 2+ ++)57Fe,(116Sn 2 + ++)58Fe,(116Sn 2+ ++)58N i,(118Sn 2+ ++)59Co,(112Sn 2+ +1H+interference)113I n,(120Sn 2+ +1H interference)121Sb, (122Sn 2+ +1H+interference)123Sb,(Sn 2+ +16O 2+ ) isotope of Ba (130Ba 2+ ,132Ba 2+ ,134Ba 2 + ,135Ba 2+ ,136Ba 2+ ,138Ba 2+ ) will cause interference.

[0003] The existing testing methods still have many problems when testing certain electronic chemicals. The interference of the matrix will lead to incomplete analysis of impurity types. The instrument detection limit of some elements is very high, and the true value of the interfered elements in the product cannot be determined. At the same time, the background signal of some light elements is also difficult to reduce, and the instrument detection limit will be high. For low-concentration products, it is difficult to judge whether some light elements are detected or it is difficult to determine the true value. In addition, the isotopes of the matrix will interfere with the isotopes of some target impurity elements, which makes it impossible to select other isotopes of the target impurity elements for testing, and it is impossible to eliminate the matrix effect as much as possible in the test method, resulting in the inability to analyze the true value of the impurity element content, which significantly affects the production and application of electronic chemicals with strict requirements. Summary of the invention

[0004] The purpose of the present invention is to provide a method for detecting the content of metal and metalloid impurities in a high-purity tin precursor to solve the following technical problems:

[0005] How to reduce the interference of the matrix on the detection of metal and metalloid impurity elements and improve the accuracy and reliability of the detection method.

[0006] The purpose of the present invention can be achieved by the following technical solutions:

[0007] The present invention discloses a method for detecting the content of metal and metalloid impurities in a high-purity tin precursor, the method comprising the following steps: using an I CP-MS / MS testing instrument to establish a standard curve and a regression equation reflecting the relationship between the concentration of metal or metalloid impurities and the response signal value;

[0008] When the I CP-MS / MS testing instrument tests Li, Na, Mg, Al, K, Ca, Cr, Fe, Mn, Ni, Co, Cu, Ga, In, Sb, and Ba impurities, it adopts Cool NH3 mode or NH3 mode, the nebulizer gas flow rate is 0.7-0.9 L / min, the plasma gas flow rate is 12-16 L / min, the auxiliary gas flow rate is 0.8-1.0 L / min, the octapole deflection voltage is -10 to -5 V, and the energy discrimination is -8 to -5 V.

[0009] Furthermore, the detection method also includes the steps of treating a high-purity tin precursor sample by a digestion method to obtain a test solution, and passing the test solution into an I CP-MS / MS testing instrument to detect and obtain the concentration of metal or metalloid impurities.

[0010] Furthermore, the digestion treatment method is: take the tin precursor sample to be tested into a polytetrafluoroethylene bottle, add ultrapure concentrated hydrofluoric acid and ultrapure concentrated nitric acid to digest the sample into a clear acidic solution, and then dilute the acidic solution in the previous step with ultrapure water, and evenly disperse it to obtain the solution to be tested.

[0011] Furthermore, the digestion treatment method is specifically as follows: take 10-40 mg of the tin precursor sample to be tested into a polytetrafluoroethylene bottle, add 1-5 mL of ultrapure concentrated hydrofluoric acid and 0.5-3 mL of ultrapure concentrated nitric acid to digest the sample into a clear acidic solution, and then dilute the acidic solution in the previous step to 35-70 mL with ultrapure water, and evenly disperse to obtain the solution to be tested.

[0012] Furthermore, the detection method also includes the steps of configuring and detecting at least 3 working curve solutions to establish the standard curve and regression equation; in the working curve solutions, the concentrations of the metal and metalloid impurities are both 50-3000 ng / L; for the same impurity, its concentration in each working curve solution is different from each other.

[0013] In one embodiment, the detection method includes preparing a working curve solution 1 in which the concentration of each metal and metalloid impurity is 150-240 ng / L, a working curve solution 2 in which the concentration of each metal and metalloid impurity is 400-600 ng / L, and a working curve solution 3 in which the concentration of each metal and metalloid impurity is 900-1100 ng / L.

[0014] Furthermore, the method for detecting the content of metal and metalloid impurities in the high-purity tin precursor comprises the following steps:

[0015] (1) treating a high-purity tin precursor sample by a digestion method to obtain a test solution; (2) adding a standard reagent to at least three parallel test solutions to prepare at least three working curve solutions with different concentrations; in the working curve solution, the concentration of the metal and metalloid impurities is 50-3000 ng / L; (3) using an ICP-MS / MS instrument to test the above working curve solutions, and establishing a standard curve and regression equation reflecting the relationship between the concentration of the metal or metalloid impurities and the response signal value; (4) using an ICP-MS / MS instrument to test the test solution in (1), and calculating the impurity content therein according to the regression equation.

[0016] In one embodiment, when the impurities of Li, Na, Mg, Al, K, Ca, Cr, Fe, Mn, Ni, Co, Cu, and Ga are tested using an I CP-MS / MS test instrument, a Cool NH3 mode is used, with a nebulizer gas flow rate of 0.7-0.9 L / min, a plasma gas flow rate of 12-16 L / min, an auxiliary gas flow rate of 0.8-1.0 L / min, an octapole deflection voltage of -10 V, and an energy discrimination of -5 V.

[0017] In one embodiment, when the I CP-MS / MS testing instrument is used to test the impurities of In, Sb, and Ba, the NH3 mode is used, the nebulizer gas flow rate is 0.7-0.9 L / min, the plasma gas flow rate is 12-16 L / min, the auxiliary gas flow rate is 0.8-1.0 L / min, the octapole deflection voltage is -5 V, and the energy discrimination is -8 V.

[0018] Furthermore, when the I CP-MS / MS testing instrument tests Zn, Ge, Rb, Sr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Sn, Ce, Hf, Ta, W, Os, Re, Ir, Pt, Au, Hg, Tl, Pb, Bi, Th, and U, the He mode is adopted, the nebulizer gas flow rate is 0.5-0.8L / min, the plasma gas flow rate is 15-17L / min, the auxiliary gas flow rate is 0.7-0.9L / min, the octapole deflection voltage is -18 to -15V, and the energy discrimination is 3-5V.

[0019] Furthermore, when the I CP-MS / MS testing instrument tests Be and B impurities, the No Gas mode is adopted, the nebulizer gas flow rate is 0.4-0.7 L / min, the plasma gas flow rate is 14-17 L / min, the auxiliary gas is 0.8-1.0 L / min, the octapole deflection voltage is -10 to -8 V, and the energy discrimination is 4-7 V.

[0020] Furthermore, when using the I CP-MS / MS testing instrument to test Ti, V, As, Y, and Zr impurities, the 02 mode was adopted, the nebulizer gas flow rate was 0.7-0.9 L / min, the plasma gas flow rate was 12-15 L / min, the auxiliary gas was 0.7-0.9 L / min, the octapole deflection voltage was -3 to -1 V, and the energy discrimination was -7 to -5 V.

[0021] Further, the tin precursor includes but is not limited to tin tetrachloride, tin diiodide, tetramethyltin, tetraethyltin, tetra(dimethylamino)tin, tetra(methylethylamino)tin, tetra(diethylamino)tin, bis(1-dimethylamino-2-methyl-2-propoxy)tin, tin acetylacetonate, bis(trimethylsilyl)amine tin, Sn( i PrAMD)2、Sn( i PrFMD)2, any one of tin acetate.

[0022] Beneficial effects of the present invention:

[0023] 1. The present invention selects the Cold NH3 mode when analyzing light elements. This mode uses low-temperature plasma and ammonia as reaction gases. Adding NH3 gas collision in the low ionization energy plant area can effectively remove impurity interference and reduce the background value of the measured element, thereby reducing the element instrument detection limit to the lowest possible level. For example, the problem of high instrument detection limit of 40Ca due to the interference of 40Ar has always been difficult to solve. However, under the Cold-NH3 mode and specific detection parameters, low-temperature plasma can reduce argon interference such as Ar. + ,ArH + and ArO + The formation of Ar + Ca + background interference.

[0024] 2. In order to further reduce the impact of interferences, the present invention sets specific parameters for use in conjunction with each other so that conditions such as carrier gas flow rate, auxiliary gas flow rate, RF forward power, etc. are all within the optimal range, thereby avoiding the generation of interferences and reducing the impact of interferences.

[0025] 3. The present invention solves this problem by selecting different collision modes and mass number transfers through energy discrimination, charge transfer, proton transfer, etc. For a specific reaction mode, the octapole deflection voltage is precisely controlled, and suitable reaction gas, axial acceleration and energy discrimination conditions are selected to selectively eliminate specific interfering ions and substrates without affecting the analyte ions, thereby improving the accuracy and sensitivity of the analysis and ensuring accurate detection of low-concentration samples. DETAILED DESCRIPTION

[0026] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] Example 1

[0028] This embodiment discloses a method for detecting the content of metal and metalloid impurities in a high-purity tin precursor. Taking TDMASn as an example, the detection method is carried out in the following steps.

[0029] Step 1: Prepare 4 test solutions

[0030] Four TDMASn samples to be tested were taken in parallel into polytetrafluoroethylene screw-mouth bottles, each with a mass of 20 mg. They were placed on a clean room workbench, and 3 mL of ultrapure concentrated hydrofluoric acid and 1 mL of ultrapure concentrated nitric acid were added to digest them into a clear acidic solution. The acidic solution was then diluted to 50 mL with 18.2 MΩ·cm ultrapure water and evenly dispersed to obtain four solutions to be tested. The blank solution was also diluted under the same conditions for testing.

[0031] Step 2: Prepare 3 working curve solutions

[0032] (1) Preparation of element standard solution

[0033] Element standard solution 1: containing the elements Al, As, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ho, In, K, La, Li, Lu, Mg, Mn, Na, Nd, Ni, P, Pb, Pr, Rb, Re, Sc, Se, Sm, Sr, Tb, Th, Tl, Tm, U, V, Y, Yb, Zn, the concentration of each element is 10 mg / L;

[0034] Element standard solution 2: contains the elements Ag, Ge, Hf, Mo, Nb, Sb, Si, Sn, Ta, Te, Ti, W, and Zr, and the concentration of each element is 10 mg / L;

[0035] Element standard solution 3: contains the elements Au, Ir, Os, Pd, Pt, Rh, and Ru, and the concentration of each element is 10 mg / L.

[0036] (2) Preparation of standard stock solution

[0037] Standard stock solution 1: Dilute element standard solution 1 with 18.2 MΩ·cm ultrapure water to obtain a standard stock solution 1 with a concentration of 100 μg / L for each element;

[0038] Standard stock solution 2: Dilute element standard solution 2 with 18.2MΩ·cm ultrapure water to obtain a standard stock solution 2 with a concentration of 100μg / L for each element;

[0039] Standard stock solution 3: Dilute the element standard solution 3 with 18.2 MΩ·cm ultrapure water to obtain a standard stock solution 3 with a concentration of 100 μg / L for each element.

[0040] (3) Preparation of working curve solution

[0041] The standard stock solution 1, the standard stock solution 2, and the standard stock solution 3 are simultaneously added to the three parallel test solutions prepared in step 1 to obtain a working curve solution 1 containing all the above elements and the element concentration is 200 ng / L, a working curve solution 2 containing all the above elements and the element concentration is 500 ng / L, and a working curve solution 3 containing all the above elements and the element concentration is 1000 ng / L.

[0042] Step 3: Obtain standard curve and regression equation

[0043] The above working curve solution 1, working curve solution 2 and working curve solution 3 were detected using an I CP-MS / MS testing instrument to obtain a standard curve and a regression equation reflecting the relationship between element concentration and response signal value.

[0044] Among them, the I CP-MS / MS test instrument uses Agilent 8900, the peak acquisition mode is 1 point mode, the number of repetitions is 3, the number of scans / repetitions is 10, and the detection parameters for each element are as follows:

[0045] When testing the impurities of Li, Na, Mg, Al, K, Ca, Cr, Fe, Mn, Ni, Co, Cu, and Ga in the sample, the Cool NH3 mode was used, the scanning type was cascade, the RF power was 1000W, the nebulizer gas flow rate was 0.9L / min, the nebulizer chamber temperature was 2°C, the plasma gas flow rate was 15L / min, the compensation gas flow rate was 0.9L / min, the auxiliary gas was 0.9L / min, the sampling depth was 18mm, the octapole deflection voltage was -10V, the axial acceleration was 1.5V, and the energy discrimination was -5V;

[0046] When testing Be and B impurities in the sample, the No Gas mode was used, the scanning type was single-rod, the RF power was 1500W, the nebulizer gas flow rate was 0.7L / min, the plasma gas flow rate was 15L / min, the compensation gas flow rate was 0.48L / min, the auxiliary gas flow rate was 0.9L / min, the sampling depth was 9mm, the octapole deflection voltage was -8V, the axial acceleration was 0V, and the energy discrimination was 5V;

[0047] When testing Zn, Ge, Rb, Sr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Sn, Ce, Hf, Ta, W, Os, Re, Ir, Pt, Au, Hg, Tl, Pb, Bi, Th, and U in the sample, the He mode is adopted, the scanning type is single-rod, the RF power is 1500W, the nebulizer gas flow rate is 0.7L / min, the plasma gas flow rate is 15L / min, the compensation gas flow rate is 0.48L / min, the auxiliary gas flow rate is 0.9L / min, the sampling depth is 9mm, the octapole deflection voltage is -18V, the axial acceleration is 1V, and the energy discrimination is 3V;

[0048] When testing Ti, V, As, Y, and Zr impurities in the sample, the 02 mode was used, the scanning type was cascade, the RF power was 1500W, the nebulizer gas flow rate was 0.7L / min, the plasma gas flow rate was 15L / min, the compensation gas flow rate was 0.48L / min, the auxiliary gas flow rate was 0.9L / min, the sampling depth was 9mm, the octapole deflection voltage was -3V, the axial acceleration was 1.5V, and the energy discrimination was -7V;

[0049] When testing the impurities of In, Sb, and Ba in the sample, the NH3 mode was used, the scanning type was cascade, the RF power was 1500W, the nebulizer gas flow rate was 0.7L / min, the plasma gas flow rate was 15L / min, the compensation gas flow rate was 0.36L / min, the auxiliary gas was 0.9L / min, the sampling depth was 10mm, the octapole deflection voltage was -5V, the axial acceleration was 1.5V, and the energy discrimination was -8V.

[0050] A standard curve was drawn according to the test results, and a regression equation was established based on the element concentration value (i.e., x value) and the instrument response signal value CPS (i.e., y value). The obtained regression equations of each element are listed in Table 1. Table 1 is as follows:

[0051] Table 1

[0052]

[0053]

[0054]

[0055] Step 5: Detect the content of metal or metalloid impurities

[0056] The solution to be tested in step 1 was tested using I CP-MS / MS (Agilent 8900), and the metal impurity content was calculated based on the regression equation.

[0057] The instrument detection limits and background equivalent concentrations of the metal impurity content in this method are listed in Table 2. Table 2 is as follows:

[0058] Table 2

[0059]

[0060]

[0061] Comparative Example 1

[0062] Compared with Example 1, the only difference is that the test instrument is replaced by Thermo Fisher i CAP RQ from Agilent 8900, the acquisition channel is mode 1, the retention time is 0.05s, the number of repetitions is 3, and the number of scans / repetitions is 10;

[0063] When testing the impurities of Li, Na, Mg, Al, K, Ca, Cr, Fe, Mn and Ba in the sample, the CoolIns mode was adopted, the scanning type was single-rod, the RF power was 520W, the atomizing gas flow rate was 1.2061L / min, the plasma gas flow rate was 14L / min, the auxiliary gas was 0.8L / min, the sampling depth was 10mm, the horizontal position of the matrix tube was 1.24mm, the vertical position of the matrix tube was -0.75mm, the extraction lens voltage was -200V, the focusing lens voltage was 14V, the extraction lens cathode voltage was -35V, the CCT focusing lens voltage was -20V, the CCT entrance voltage was -120V, and the CCT deflection voltage was -18V.

[0064] When testing B, Be, Ti, V, Cu, Ni, Zn, Ga, Ge, As, Sr, Nb, Zr, Mo, Ru, Rh, Pd, Ag, Cd, In, Sb, Hf, Ta, W, Os, Ir, Pt, Au, Tl, Pb, Bi, Th, and U in the sample, the He mode was adopted, the scanning type was single-rod, the RF power was 1550W, the atomizing gas flow rate was 1.030L / min, the plasma gas flow rate was 14L / min, the auxiliary gas was 0.8L / min, the sampling depth was 5mm, the horizontal position of the rectangular tube was 0.44mm, the vertical position of the rectangular tube was -0.42mm, the extraction lens voltage was -188V, the focusing lens voltage was -7.5V, the extraction lens cathode voltage was 0V, the CCT focusing lens voltage was 2.5V, the CCT entrance voltage was -110V, and the CCT deflection voltage was -21V;

[0065] The other conditions are exactly the same, and the instrument detection limit and background equivalent concentration of the metal impurity content in this method are listed in Table 3. Table 3 is as follows:

[0066] Table 3

[0067]

[0068]

[0069] By analyzing the data in Tables 2-3, it can be found that the instrument detection limits of light elements tested using the Thermo Fisher iCAP RQ instrument in Comparative Example 1 are mostly above 15 ppt, and the instrument detection limits of Na, K, Ca, Fe, In, Sb, and Ba are several times higher than the detection results in Example 1, while the instrument detection limits of light elements tested in Example 1 are mostly only a few ppt or even less than 1 ppt, which shows that the method of Example 1 can significantly improve the instrument detection limits of Na, K, Ca, Fe, In, Sb, and Ba compared with Comparative Example 1.

[0070] Comparative Example 2

[0071] Compared with Example 1, the only difference is that when testing the impurities of Li, Be, B, Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Co, Cu, Zn, In, Sb, and Ba in the TDMASn sample, the He mode is adopted, the scanning type is single-rod, the RF power is 1500W, the atomizing gas flow rate is 0.7L / min, the plasma gas flow rate is 15L / min, the auxiliary gas is 0.9L / min, the sampling depth is 9mm, the octapole deflection voltage is -18V, the axial acceleration is 1V, and the energy discrimination is 3V; the other conditions are exactly the same, and the instrument detection limit and the background equivalent concentration of the metal impurity content in the method are listed in Table 4, which is as follows:

[0072] Table 4

[0073] Test items Instrument detection limit Background equivalent concentration unit Li 6.49 8.67 ppt Be 0.46 2.00 ppt B 41.42 298.74 ppt Na 262.11 458.81 ppt Mg 33.41 86.07 ppt Al 108.65 133.58 ppt K 271.61 2960.83 ppt Ca 453.37 1079.87 ppt Ti 14.89 14.24 ppt V 5.10 8.10 ppt Cr 8.51 14.08 ppt Mn 4.69 8.98 ppt Fe 34.58 458.84 ppt Ni 74.73 2689.81 ppt Co 27.73 3053.87 ppt Cu 92.76 112.73 ppt In 324.42 851.47 ppt Sb 266.54 603.92 ppt Ba 541.33 766.00 ppt

[0074] By analyzing the data in Table 4, it can be seen that the instrument detection limits of light elements in He mode are mostly above 30 ppt, and the LOD values ​​of Na, K, Ca, Fe, In, Sb, and Ba are even as high as several hundred ppt, while the instrument detection limits of light elements tested in Example 1 are mostly only a few ppt or even below 1 ppt, which means that compared with Comparative Example 2, the instrument detection limits of Na, K, Ca, Fe, In, Sb, and Ba in Example 1 can be significantly improved.

[0075] Test Case

[0076] After the TDMASn samples were treated according to Example 1, the metal impurity content in the samples was tested by the corresponding method to verify the repeatability, reproducibility, linearity and recovery rate of the method. The standard curve can reflect the linear quantitative relationship curve between the different concentrations of the analyzed substance and the instrument response signal value. The correlation coefficient R value of the calibration curve of each ion to be measured should meet R≥0.990; repeatability and reproducibility are measured under controlled conditions, reflecting the size of the error in the measurement system, and are expressed by relative standard deviation (RSD), requiring repeatability RSD≤10% and reproducibility RSD≤

[0077] 10%; the recovery rate is usually used to evaluate the accuracy and reliability of the method, and the standard requires a recovery rate between 80% and 120%; the linear correlation coefficient, repeatability, reproducibility and recovery rate obtained by verifying TDMASn are listed in Table 5, which is as follows: Table 5

[0078]

[0079] By analyzing the data in Table 5, it can be seen that the linear correlation coefficient, repeatability, reproducibility and recovery rate obtained by detecting the TDMASn sample using the method of Example 1 all meet the standard requirements and have high method reliability.

[0080] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A method for detecting the content of metal and metalloid impurities in a high-purity tin precursor, characterized in that: The detection method comprises the following steps: using an I CP-MS / MS testing instrument to establish a standard curve and a regression equation reflecting the relationship between the concentration of metal or metalloid impurities and the response signal value; When the I CP-MS / MS testing instrument tests Li, Na, Mg, Al, K, Ca, Cr, Fe, Mn, Ni, Co, Cu, Ga, In, Sb, and Ba impurities, it adopts Cool NH3 mode or NH3 mode, the nebulizer gas flow rate is 0.7-0.9 L / min, the plasma gas flow rate is 12-16 L / min, the auxiliary gas flow rate is 0.8-1.0 L / min, the octapole deflection voltage is -10 to -5 V, and the energy discrimination is -8 to -5 V.

2. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1, characterized in that: The detection method also includes the steps of treating a high-purity tin precursor sample with a digestion method to obtain a solution to be tested, and passing the solution to be tested into an I CP-MS / MS testing instrument to detect and obtain the concentration of metal or metalloid impurities.

3. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 2, characterized in that: The digestion method is as follows: take the tin precursor sample to be tested into a polytetrafluoroethylene bottle, add ultrapure concentrated hydrofluoric acid and ultrapure concentrated nitric acid to digest the sample into a clear acidic solution, and then dilute the acidic solution in the previous step with ultrapure water, and disperse it evenly to obtain the solution to be tested.

4. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1 or 2, characterized in that: When the I CP-MS / MS testing instrument tests Zn, Ge, Rb, Sr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, Sn, Ce, Hf, Ta, W, Os, Re, Ir, Pt, Au, Hg, Tl, Pb, Bi, Th, and U, the He mode is adopted, the nebulizer gas flow rate is 0.5-0.8 L / min, the plasma gas flow rate is 15-17 L / min, the auxiliary gas flow rate is 0.7-0.9 L / min, the octapole deflection voltage is -18 to -15 V, and the energy discrimination is 3-5 V.

5. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1 or 2, characterized in that: When the I CP-MS / MS testing instrument tests Be and B impurities, the No Gas mode is adopted, the nebulizer gas flow rate is 0.4-0.7 L / min, the plasma gas flow rate is 14-17 L / min, the auxiliary gas flow rate is 0.8-1.0 L / min, the octapole deflection voltage is -10 to -8 V, and the energy discrimination is 4-7 V.

6. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1 or 2, characterized in that: When using ICP-MS / MS testing instrument to test Ti, V, As, Y, and Zr impurities, use 02 mode, nebulizer gas flow rate 0.7-0.9L / min, plasma gas flow rate 12-15L / min, auxiliary gas 0.7-0.9L / min, octapole deflection voltage -3 to -1V, energy discrimination -7 to -5V.

7. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1, characterized in that: The detection method also includes the steps of configuring and detecting at least three working curve solutions to establish the standard curve and regression equation; in the working curve solutions, the concentrations of the metal and metalloid impurities are both 50-3000 ng / L; for the same impurity, its concentration in each working curve solution is different from each other.

8. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 2, characterized in that: The digestion method is as follows: take 10-40 mg of the tin precursor sample to be tested into a polytetrafluoroethylene bottle, add 1-5 mL of ultrapure concentrated hydrofluoric acid and 0.5-3 mL of ultrapure concentrated nitric acid to digest the sample into a clear acidic solution, and then dilute the acidic solution in the previous step to 35-70 mL with ultrapure water, and disperse evenly to obtain the solution to be tested.

9. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1, characterized in that: When testing Li, Na, Mg, Al, K, Ca, Cr, Fe, Mn, Ni, Co, Cu, and Ga impurities, the Cool NH3 mode was used, the atomizing gas flow rate was 0.7-0.9 L / min, the plasma gas flow rate was 12-16 L / min, the auxiliary gas flow rate was 0.8-1.0 L / min, the octapole deflection voltage was -10 V, and the energy discrimination was -5 V. And / or, when testing In, Sb, and Ba impurities, use NH3 mode, atomizing gas flow rate 0.7-0.9 L / min, plasma gas flow rate 12-16 L / min, auxiliary gas flow rate 0.8-1.0 L / min, octapole deflection voltage -5 V, energy discrimination -8 V.

10. The method for detecting the content of metal and metalloid impurities in a high-purity tin precursor according to claim 1, characterized in that: The tin precursor includes tin tetrachloride, tin diiodide, tetramethyltin, tetraethyltin, tetra(dimethylamino)tin, tetra(methylethylamino)tin, tetra(diethylamino)tin, bis(1-dimethylamino-2-methyl-2-propoxy)tin, tin acetylacetonate, bis(trimethylsilyl)amine tin, Sn( i PrAMD)2、Sn( i PrFMD)2, any one of tin acetate.

Images