CN115753963A - Analysis and detection method for tin content in high-purity gallium - Google Patents
Analysis and detection method for tin content in high-purity gallium Download PDFInfo
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 90
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 45
- 238000004458 analytical method Methods 0.000 title abstract description 10
- 238000001514 detection method Methods 0.000 title description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012085 test solution Substances 0.000 claims abstract description 26
- 239000012086 standard solution Substances 0.000 claims abstract description 24
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 22
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000243 solution Substances 0.000 claims abstract description 21
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 17
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 claims abstract description 11
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 claims abstract description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 8
- 239000012498 ultrapure water Substances 0.000 claims abstract description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 239000000523 sample Substances 0.000 claims description 18
- 239000012488 sample solution Substances 0.000 claims description 18
- 238000005259 measurement Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- KSWRZJNADSIDKV-UHFFFAOYSA-N 8-amino-3-hydroxynaphthalene-1,6-disulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=C2C(N)=CC(S(O)(=O)=O)=CC2=C1 KSWRZJNADSIDKV-UHFFFAOYSA-N 0.000 claims description 3
- 238000010813 internal standard method Methods 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 description 62
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000009614 chemical analysis method Methods 0.000 description 4
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 3
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004886 process control Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A method for analyzing and detecting tin content in high-purity gallium comprises the steps of weighing a high-purity gallium sample, completely decomposing the high-purity gallium sample by hydrochloric acid and nitric acid, adding a hydrochloric acid solution, extracting gallium trichloride by using butyl acetate which is washed and purified by hydrochloric acid and ultrapure water in advance, transferring the aqueous solution to a volumetric flask, adding an yttrium internal standard element, controlling the concentration of yttrium in the solution to be 2-20 ng/mL, and fixing the volume by water to obtain a test solution. Adding yttrium internal standard elements consistent with the test solution, preparing a series of tin standard solutions, simultaneously measuring the mass intensity of tin by adopting an inductively coupled plasma mass spectrometry, subtracting the mass intensity of tin in a zero-concentration solution, drawing a working curve of tin by taking the mass concentration as a horizontal coordinate and the mass intensity as a vertical coordinate after the mass intensity is corrected by the yttrium internal standard elements, and then calculating the tin content in the high-purity gallium. The invention can treat high purity gallium content of 5-2000X 10 ‑7 % tin content is measured, the accuracy is high, the method reproducibility is good, the operation is simple and convenient, and the analysis efficiency is high.
Description
Technical Field
The invention relates to the technical field of high-purity substance analysis and detection methods. In particular to an analysis and detection method for tin content in high-purity gallium and gallium chemical products.
Background
High-purity gallium (with purity of over 99.999%) is used as the second-generation semiconductor material, mainly for producing gallium arsenide. Height ofThe content of the impurity elements in the pure gallium raw material has important influence on the performance of the gallium arsenide semiconductor, and the content of the impurity elements in the pure gallium raw material needs to be accurately measured. The high purity gallium product contains a small amount of tin, the tin content is about 5-2000 x 10 -7 % influences the photoelectric effect of gallium arsenide.
The reported analysis and detection method has the industrial standard YS/T38.2-2009 part 2 of high-purity gallium chemical analysis method: the method is characterized in that the method comprises an inductively coupled plasma mass spectrometry for measuring the amounts of magnesium, titanium, chromium, manganese, nickel, cobalt, copper, zinc, cadmium, tin, lead and bismuth, and an industry standard YS/T474-2021 inductively coupled plasma mass spectrometry for measuring trace elements by a high-purity gallium chemical analysis method. The standards adopt gallium trichloride to volatilize and remove the gallium matrix, the volatilization efficiency is low, the speed is slow, and sometimes, the volatilization of one sample needs more than 8 hours, which is not beneficial to the process control in scientific research and production. Chinese patent CN202110525400.4 discloses a glow discharge mass spectrometry high-purity gallium test method, which adopts glow discharge mass spectrometry to measure with larger error. In order to better satisfy scientific research production and process control of high-purity gallium, an analysis method needs to be improved, and the detection efficiency of a high-purity gallium sample is improved.
Disclosure of Invention
The invention aims to fill the blank of the prior art and provide a method for preparing high-purity gallium with the purity of 5-2000 multiplied by 10 -7 % tin content, high detection efficiency and analysis accuracy, and good reproducibility.
The technical scheme adopted by the invention is as follows:
a method for analyzing and detecting the tin content in high-purity gallium comprises the following steps:
(1) Weighing 0.5000-10.0000 g of high-purity gallium sample with the purity not less than 99.999% in a 50-200 mL polytetrafluoroethylene beaker, adding 5-15 mL of water, 3-20 mL of hydrochloric acid solution and 3-20 mL of nitric acid solution, covering a watch glass, heating and completely decomposing at 80-250 ℃, taking down and cooling to room temperature to prepare a sample solution;
(2) Alternatively using ultrapure water with the resistivity more than or equal to 18M omega and hydrochloric acid (1 +1) to shake and purify butyl acetate;
(3) Adding hydrochloric acid (1 + 1) which is 1-5 times of the volume of the sample solution, uniformly mixing, allowing the sample solution to pass through purified butyl acetate, oscillating and extracting gallium trichloride in a separating funnel, transferring the aqueous solution to a 50-500 mL volumetric flask, adding yttrium internal standard element, controlling the concentration of yttrium in the solution to be 2-20 ng/mL, diluting with water to a scale, and uniformly mixing, wherein the volume is the volume V of the test solution;
(4) Transferring a tin standard solution containing 50-10000 ng/mL of tin, and adding an internal standard element yttrium into a group of 50-500 mL volumetric flasks to obtain a tin series standard solution, wherein the concentration of the tin series standard solution is consistent with that of yttrium in the test solution; under the same measurement condition with the test solution, simultaneously measuring the mass intensity of tin in the series of standard solutions, subtracting the mass intensity of tin in the zero-concentration solution, and drawing a working curve of the tin by taking the mass concentration as an abscissa and the mass intensity as an ordinate;
(5) Calculating the content of tin in the high-purity gallium:
the tin content is calculated by mass fraction w Sn Counted in number of 10 -7 % expressed, calculated as:
in the formula:
rho is the mass concentration of tin in the test solution which is obtained by checking the working curve, and the unit is ng/mL;
ρ 0 checking the mass concentration of tin in the reagent blank test solution from the working curve, wherein the unit is ng/mL;
v is the volume of the test solution, and the unit is mL;
m is the mass of the high-purity gallium sample and the unit is g.
Further, the mass intensity of tin in the series of standard solutions measured in the step (4) is measured by using an inductively coupled plasma mass spectrometry, and interference is eliminated by an internal standard method.
The invention has at least the following beneficial effects:
1) The invention can be used for 5-2000 multiplied by 10 in high-purity gallium -7 The determination of the tin content makes up the defects of the prior art;
2) According to the method, the gallium matrix is extracted and separated by butyl acetate, the interference is eliminated by adopting an internal standard method, and then the tin is measured by adopting an inductively coupled plasma mass spectrometry, so that the sample analysis error is greatly reduced, the accuracy is high, and the method reproducibility is good;
3) The speed of extracting and separating the gallium substrate by butyl acetate is very high, and the requirements of scientific research production and process control of high-purity gallium can be better met.
4) The method is simple and convenient to operate, less in used reagent amount and environment-friendly, and butyl acetate can be washed by hydrochloric acid (1 + 1) and ultrapure water for repeated use.
Detailed Description
The present invention will be further illustrated with reference to the following examples.
A method for analyzing and detecting the tin content in high-purity gallium comprises the following steps:
(1) Weighing 0.5000-10.0000 g of high-purity gallium sample with the purity not less than 99.999% in a 50-200 mL polytetrafluoroethylene beaker, adding 5-15 mL of water, 3-20 mL of hydrochloric acid solution and 3-20 mL of nitric acid solution, covering a watch glass, heating and decomposing at 80-250 ℃, taking down and cooling to room temperature to prepare a sample solution;
(2) Oscillating and purifying butyl acetate by alternately adopting ultrapure water with the resistivity of more than or equal to 18M omega and hydrochloric acid (1+1);
(3) Adding hydrochloric acid (1 + 1) which is 1-5 times of the volume of the sample solution, uniformly mixing, allowing the sample solution to pass through purified butyl acetate, oscillating and extracting gallium trichloride in a separating funnel, transferring the aqueous solution to a 50-500 mL volumetric flask, adding an yttrium internal standard element, controlling the concentration of yttrium in the solution to be 2-20 ng/mL, diluting with water to a scale, and uniformly mixing, wherein the volume is a test solution volume V;
(4) Transferring a tin standard solution containing 50-10000 ng/mL of tin, and adding an internal standard element yttrium into a group of 50-500 mL volumetric flasks to obtain a tin series standard solution, wherein the concentration of the tin series standard solution is consistent with that of yttrium in the test solution; simultaneously measuring the mass intensity of tin in the series of standard solutions under the same measurement condition as the test solution, subtracting the mass intensity of tin in the zero-concentration solution, and drawing a working curve of the tin by taking the mass concentration as a horizontal coordinate and the mass intensity as a vertical coordinate;
(5) Calculating the content of tin in the high-purity gallium:
the tin content is calculated as mass fraction w Sn Counting the number as 10 -7 % expressed, calculated as:
in the formula:
rho is the mass concentration of tin in the test solution which is obtained by checking the working curve, and the unit is ng/mL;
ρ 0 checking the mass concentration of tin in the reagent blank test solution from the working curve, wherein the unit is ng/mL;
v is the volume of the test solution, and the unit is mL;
m is the mass of the high-purity gallium sample and the unit is g.
Example 1
The method for analyzing and detecting the tin content in the high-purity gallium comprises the following steps:
(1) Weighing 0.5000g of high-purity gallium sample with purity not less than 99.999% in a 50mL polytetrafluoroethylene beaker, adding 5mL of water, 3mL of hydrochloric acid and 3mL of nitric acid solution, covering a watch glass, heating and decomposing at 80 ℃ completely, taking down and cooling to room temperature to prepare a sample solution;
(2) And oscillating and purifying butyl acetate in a separating funnel by alternately adopting hydrochloric acid (1 + 1) and ultrapure water with the resistivity more than or equal to 18M omega. The butyl acetate can be reused;
(3) Adding 15mL of hydrochloric acid (1 + 1) into the sample solution, uniformly mixing, oscillating and extracting gallium trichloride from the sample solution through purified butyl acetate in a separating funnel, transferring the aqueous solution into a 50mL volumetric flask, adding 500ng of yttrium internal standard element, diluting with water to a scale, and uniformly mixing to obtain a test solution volume V;
(4) Transferring a tin standard solution containing 50-1000 ng, and adding 500ng of internal standard element yttrium into a set of 50mL volumetric flasks to obtain a tin series standard solution; under the same measurement condition with the test solution, the mass intensity of tin in the series of standard solutions is measured at the same time, the mass intensity of tin in the zero-concentration solution is subtracted, and a working curve of tin is drawn, wherein the working curve is shown in table 1.
Table 1 example 1 operating curve
(5) Calculating the tin content:
according to the formula
And calculating the tin content.
Content of tin
The content of tin in the sample is 675 multiplied by 10 -7 ％。
The content of tin in the sample is 681 multiplied by 10 measured by inductively coupled plasma mass spectrometry of the standard YS/T38.2-2009 -7 ％。
Example 2
The method for analyzing and detecting the tin content in the high-purity gallium comprises the following steps:
(1) Weighing 4.0000g of a high-purity gallium sample with the purity not less than 99.999 percent in a 100mL polytetrafluoroethylene beaker, adding 10mL of water, 10mL of hydrochloric acid and 6mL of nitric acid solution, covering a watch glass, heating and completely decomposing at 120 ℃, taking down and cooling to room temperature to prepare a sample solution;
(2) Alternatively using hydrochloric acid (1 + 1) and ultrapure water with the resistivity more than or equal to 18M omega for butyl acetate, and oscillating and purifying in a separating funnel;
(3) Adding 50mL of hydrochloric acid (1 + 1) into the sample solution, uniformly mixing, oscillating and extracting gallium trichloride from the sample solution through purified butyl acetate in a separating funnel, transferring the aqueous solution into a 100mL volumetric flask, adding 1000ng of yttrium internal standard element, diluting with water to a scale, and uniformly mixing, wherein the volume is the volume V of the test solution;
(4) Transferring a tin standard solution containing 500-2500 ng, and adding 1000ng of internal standard element yttrium into a group of 100mL volumetric flasks to obtain a tin series standard solution; under the same measurement condition with the test solution, the mass intensity of tin in the series of standard solutions is measured simultaneously, the mass intensity of tin in the zero-concentration solution is subtracted, a working curve of tin is drawn by taking the mass concentration as an abscissa and the mass intensity as an ordinate, and the working curve is shown in table 2.
Table 2 example 2 operating curves
(5) Calculating the tin content:
according to the formula
And calculating the tin content.
Content of tin
The content of tin in the sample is determined to be 519X 10 -7 ％。
The content of tin in the sample was 533X 10 as determined by inductively coupled plasma mass spectrometry using the standard YS/T474-2021 -7 ％。
Example 3
The method for analyzing and detecting the tin content in the high-purity gallium comprises the following steps:
(1) Weighing 10.0000g of a high-purity gallium sample with the purity not less than 99.999 percent in a 200mL polytetrafluoroethylene beaker, adding 15mL of water, 20mL of hydrochloric acid and 20mL of nitric acid solution, covering a watch glass, heating and decomposing at 250 ℃ completely, taking down and cooling to room temperature to prepare a sample solution;
(2) Alternatively using hydrochloric acid (1 + 1) and ultrapure water with the resistivity more than or equal to 18M omega for butyl acetate, and oscillating and purifying in a separating funnel;
(3) Adding 200mL of hydrochloric acid (1 + 1) into the sample solution, uniformly mixing, oscillating and extracting gallium trichloride from the sample solution through purified butyl acetate in a separating funnel, transferring the aqueous solution into a 500mL volumetric flask, adding 5000ng of yttrium internal standard element, diluting with water to a scale, and uniformly mixing, wherein the volume is the volume V of the test solution;
(4) Transferring a tin standard solution containing 50-250 ng, adding 5000ng of an internal standard element yttrium into a set of 500mL volumetric flasks to obtain a tin series standard solution, simultaneously measuring the mass intensity of tin in the series standard solution under the same measurement condition as the test solution, subtracting the mass intensity of tin in the zero-concentration solution, and drawing a working curve of tin by taking the mass concentration as a horizontal coordinate and the mass intensity as a vertical coordinate, wherein the working curve is shown in Table 3.
Table 3 example 3 working curve
(5) Calculating the tin content:
according to the formula
And calculating the tin content.
Content of tin
The content of tin in the sample is 14 multiplied by 10 -7 ％。
The content of tin in the sample was 12X 10 as measured by inductively coupled plasma mass spectrometry using the standard YS/T38.2-2009 -7 ％。
The invention has high detection efficiency, the detection time is not more than 4 hours each time, compared with the prior art, the method improves the analysis and detection efficiency, and the detection range of tin is 5-2000 multiplied by 10 -7 Percent, can meet the detection of tin in the existing high-purity gallium, and the accuracy is similar to YS/T38.2-2009 part 2 of the chemical analysis method of high-purity gallium: compared with the YS/T474-2021 (inductively coupled plasma mass spectrometry for measuring trace elements by high-purity gallium chemical analysis method), the inductively coupled plasma mass spectrometry for measuring the amounts of magnesium, titanium, chromium, manganese, nickel, cobalt, copper, zinc, cadmium, tin, lead and bismuth has no significant difference.
All percentages stated in the present invention are percentages by mass, unless otherwise stated.
Claims (2)
1. The method for analyzing and detecting the tin content in the high-purity gallium is characterized by comprising the following steps of:
(1) Weighing 0.5000-10.0000 g of high-purity gallium sample with the purity not less than 99.999% in a 50-200 mL polytetrafluoroethylene beaker, adding 5-15 mL of water, 3-20 mL of hydrochloric acid solution and 3-20 mL of nitric acid solution, covering a watch glass, heating and completely decomposing at 80-250 ℃, taking down and cooling to room temperature to prepare a sample solution;
(2) Alternatively using ultrapure water with the resistivity more than or equal to 18M omega and hydrochloric acid (1 +1) to shake and purify butyl acetate;
(3) Adding hydrochloric acid (1 + 1) which is 1-5 times of the volume of the sample solution, uniformly mixing, allowing the sample solution to pass through purified butyl acetate, oscillating and extracting gallium trichloride in a separating funnel, transferring the aqueous solution to a 50-500 mL volumetric flask, adding an yttrium internal standard element, controlling the concentration of yttrium in the solution to be 2-20 ng/mL, diluting with water to a scale, and uniformly mixing, wherein the volume is a test solution volume V;
(4) Transferring a tin standard solution containing 50-10000 ng/mL of tin, and adding an internal standard element yttrium into a group of 50-500 mL volumetric flasks to obtain a tin series standard solution, wherein the concentration of the tin series standard solution is consistent with that of yttrium in the test solution; under the same measurement condition with the test solution, simultaneously measuring the mass intensity of tin in the series of standard solutions, subtracting the mass intensity of tin in the zero-concentration solution, and drawing a working curve of the tin by taking the mass concentration as an abscissa and the mass intensity as an ordinate;
(5) Calculating the content of tin in the high-purity gallium:
the tin content is calculated as mass fraction w Sn Counted in number of 10 -7 % is calculated as:
in the formula:
rho is the mass concentration of tin in the test solution which is obtained by checking the working curve, and the unit is ng/mL;
ρ 0 checking the mass concentration of tin in the reagent blank test solution from the working curve, wherein the unit is ng/mL;
v is the volume of the test solution, and the unit is mL;
m is the mass of the high-purity gallium sample and the unit is g.
2. The method according to claim 1, wherein the mass intensity of tin in the measurement series of standard solutions in step (4) is measured by inductively coupled plasma mass spectrometry, and interference is eliminated by an internal standard method.
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