This specification specifies the plasma spectrometry method for the determination of 12 impurities such as copper, manganese, magnesium, vanadium and titanium in high-purity gallium. This specification is applicable to the simultaneous determination of 12 impurities in high-purity gallium. The determination range is shown in Table 1. SJ 20713-1998 Plasma spectrometry method for the determination of 12 impurities such as copper, manganese, magnesium, vanadium and titanium in high-passivation gallium for gallium arsenide SJ20713-1998 Standard download decompression password: www.bzxz.net

Military Standard of the Electronic Industry of the People's Republic of China FL5971
SJ 20713—1998
Method for the determination of 12 species ofinpurities including copper, maganese, magpesium,vanadium, titanhm in high - purity gallium usedfor gallfum arsenide by ICP spectrometryPublished on 18 March 1998
Implemented on 15 May 1998
Approved by the Ministry of Electronics Industry of the People's Republic of China Military Standard of the Electronic Industry of the People's Republic of ChinaMethod for the determination of 12 spedes ofinpurities inchuding copper, maganese, magnesiumvanadium, titanhuan in high - purity galtfhum usedfor gallfun arsenkde by ICP spectroaetry1Scope
1.1Subject content
SI207131998
This standard specifies the plasma spectrometric determination method for 12 kinds of metal impurities such as copper, manganese, magnesium, vanadium and titanium in high-purity gallium. 1.2Scope of application
This standard is applicable to the simultaneous determination of 12 kinds of metal impurities in high-purity gallium. The determination range is shown in Table 1. Table 1
Mn, Li
2References
No provisions in this chapter.
3Definition
No provisions in this chapter.
4 General requirements
Ti Ba,
4.1 Atmospheric conditions for measurement
Published by the Ministry of Electronics Industry of the People's Republic of China on March 18, 1998 Measurement range
2 × 10-6 ~ 5× 10-s
5 × 10-6 ~ 5× 10-5
Implementation on May 1, 1998
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a. Ambient temperature: 18~28℃;
b. Relative humidity: <80%.
C. Atmospheric pressure: 86~106kPewwW.bzxz.Net
4.1 Laboratory requirements
The laboratory shall ensure a certain degree of cleanliness.
5 Detailed requirements
5.1 Method summary
SJ 20713 - 1998
The sample is dissolved in hydrochloric acid and nitric acid. In the hydrochloric acid medium, the main body is extracted and separated with isopropyl ether, and the impurities such as copper, manganese, magnesium, vanadium, titanium, etc. enriched in the water phase are determined by plasma spectrometry. 5.2 Reagents and materials
The water used in this standard is high-purity water: the secondary deionized water is distilled once with a sub-boiling distiller. 5.2.1 Hydrochloric acid: hydrochloric acid (super pure) is purified by isothermal diffusion method or sub-boiling distillation method, and its concentration is calibrated. 5.2.2 Hydrochloric acid (7.5mo/L): Prepare with hydrochloric acid (5.2.1). 5.2.3 Hydrochloric acid (6.0 mol/L): Prepare with hydrochloric acid (5.2.1). 5.2.4 Nitric acid: Purify nitric acid (superior grade) by secondary distillation in a quartz distiller, discard 10% of the head and tail fractions, and collect the middle fraction for later use.
5.2.5 Hydrochloric acid-nitric acid (5+1) mixed solution: Prepare with hydrochloric acid (5.2.1) and nitric acid (5.2.4). Prepare it when needed. 5.2.6 Isopropyl ether: First use hydroxylamine hydrochloride solution (100 g/L) and ammonium ferrous sulfate solution (200 g/L) in a separatory funnel to wash and vibrate to remove peroxides, then transfer to a distillation bottle, distill and purify on an 80% water bath, collect the distillate at 67~69℃, and saturate it with an equal volume of hydrochloric acid (5.2.2) before use. 5.2.7 Sulfuric acid: MOS pure.
5.2.8 Sulfuric acid (1+1): Prepare with sulfuric acid (5.2.7). 5.2.9 Sulfuric acid (1+19): Prepare with sulfuric acid (5.2.7). 5.2.10 Preparation of standard solution
5.2.10.1 Vanadium standard storage bath
Weigh 1.7852 g of vanadium pentoxide (spectrally pure) that has been pre-baked at 105°C for 1 hour and cooled, place in a 300 mL beaker, add 30 mL of hydrochloric acid (5.2.3), add 5 mL of nitric acid (5.2.4), and after complete dissolution, make up to 1000 mL and mix well. 1 mL of this solution contains 1 mg of vanadium
5.2.10.2 Magnesium standard stock solution
Weigh 1.6583 g of magnesium oxide (spectrally pure) that has been pre-calcined at 800°C to constant weight, place it in a 200 mL beaker, slowly add 20 mL of hydrochloric acid (5.2.3), dissolve it, cool it, transfer it to a 1000 mL volumetric flask, make up to volume with high-purity water, and mix it. 1 mL of this solution contains 1 mg of magnesium.
5.2.10.3 Chromium standard stock solution
Weigh 3.7347 g of potassium chromate (spectrally pure) that has been pre-calculated at 105°C for 1 hour and cooled, dissolve it in high-purity sodium hydroxide, transfer it to a 1000 mL volumetric flask, make up to volume with high-purity water, and mix it. 1 mL of this solution contains 1 mg of chromium. 5.2.10.4 Manganese standard stock solution
Weigh 1.5825g of manganese dioxide (spectrally pure) that has been pre-baked at 105℃ for 1h and cooled, add 30mL of hydrochloric acid 2
SJ 20713 - 1998
(5.2.3), and heat to dissolve. After dissolution, transfer to a 1000mL volumetric flask, dilute to volume with high-purity water, and mix. This solution contains 1ng manganese in 1mL.
5.2.10.5 Standard stock solution
Weigh 1.2726g of nickel oxide (spectrally pure) that has been pre-baked at 105℃ for 1h and cooled, place in a 300mL beaker, add a little high-purity water to moisten it, then add 30mL of hydrochloric acid (5.2.3), heat at low temperature to dissolve, transfer to a 1000mL volumetric flask after dissolution, dilute to volume with high-purity water, and mix. This solution contains 1mL of nickel. 5.2.10.6 Standard storage solution for steel
Weigh 1.2518g of copper oxide (spectrally pure) powder that has been baked at 105℃ for 1h and cooled, place it in a 300mL beaker, add a small amount of commercially pure water to moisten it, add 30mL of hydrochloric acid (5.2.3), and dissolve it at low temperature. After it is completely dissolved, transfer it to a 1000mL volumetric flask, make up to volume with high-purity water, and mix it. This solution contains 1mZn in 1mL. 5.2.10.7 Standard storage solution for zinc
Weigh 1.2446g of zinc oxide (spectrally pure) that has been baked at 105℃ for 1h and cooled, place it in a 300mL beaker, add a small amount of high-purity water to moisten it, add 30mL of hydrochloric acid (5.2.3), and dissolve it at low temperature. After it is dissolved, cool it to room temperature, transfer it to a 1000mL volumetric flask, make up to volume with commercially pure water, and mix it. This solution contains 1mg zinc in 1mL. 5.2.10.B Cobalt Standard Stock Solution
Weigh 1.4072g of cobalt trioxide (spectrally pure) that has been pre-baked at 105℃ for 1h and cooled, place in a 100mL beaker, add 20mL of hydrochloric acid (5.2.3), transfer to a 1000mL volumetric flask, dilute to volume with high-purity water, and mix well. This solution contains 1rg of cobalt per ml.
5.2.10.9 Lithium Standard Stock Solution
Weigh 5.3228g of lithium carbonate (spectrally pure), place in a 300mL beaker, add 150mL of high-purity water, slowly add hydrochloric acid (5.2.3) until completely dissolved, boil to remove carbon dioxide, cool, transfer to a 1000mL volumetric flask, dilute to volume with high-purity water, and mix well. This solution contains [rmg of lithium per ml. 5.2.10.10 Cadmium standard stock solution
Weigh 1.1424 g of cadmium oxide (spectrally pure) that has been pre-baked at 105°C for 1 hour and cooled, place it in a 300 mL beaker, add 25 mL of hydrochloric acid (5.2.3), dissolve completely, cool, transfer to a 1000 mL volumetric flask, dilute to volume with high-purity water, and mix. This solution contains 1 mg of cadmium in 1 mL.
5.2.10.11 Barium standard stock solution
Weigh 1.7785 g of barium nitride (spectrally pure), dissolve it in a small amount of boiled high-purity water, cool, transfer to a 1000 mL volumetric flask, dilute to volume with high-purity water, and mix. This solution contains 1 mg of barium in 1 mL. 5.2.10.12 Titanium standard stock solution
Weigh 5.0.139g of potassium fluorotitanate (spectrally pure) previously baked at 105℃ for 1h and cooled is placed in a 100ml platinum crucible, 30ml of mercaptic acid (5.2.8) is added, heated and evaporated until white smoke is emitted, removed and cooled, about 10ml of high-purity water is blown along the blood wall, smoke is emitted again, and water is added again. This operation is repeated three times, and finally it is leached with sulfuric acid (5.2.9), transferred to a 1000ml container, fixed to volume with sulfuric acid (5.2.9), and shaken well. This solution contains 1ml of titanium in 1ml. 5.2.10.13 Mixed standard storage solution
Accurately pipette a certain amount of standard storage solution (5.2.10.1~5.2.10.11) to prepare the first set of five concentrations of standard solutions (11 elements): the concentrations of various elements per ml are: 0.5, 0.1, 0.05, 0.02, 0gg, respectively, and the solution is hydrochloric acid medium (hydrogen chloride content is 3.6%). 5.2.10.14 Single standard solution
—3—
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SJ 20713 - 1998
Accurately pipette a certain amount of standard storage solution (5.2.10.12) to prepare the second set of five concentration solutions, with titanium content of 0.5, 01, 0.05, 0.02, and 0 per milliliter, respectively, and the solution is hydrochloric acid medium (hydrogen chloride content is 3.6%). 5.3 Instrument
The instrument used is ICP multi-channel spectrometer or other equivalent emission spectrometer. 5.4 Analysis steps
5.4.1 Test sample
Take 1.00g of test sample.
5.4.2 Blank test
Carry out a blank test with the test sample.
5.4.3 Matrix separation and impurity enrichment
Put the sample (5.4.1) in a 50mL quartz beaker, add about 6mL of mixed acid (5.2.5), cover the surface with blood, heat at low temperature to dissolve the sample, and use a small amount of hydrochloric acid (5.2.1) to drive out the excess nitric acid. Remove and cool to room temperature, transfer to a 50mL quartz separatory funnel, rinse the beaker with hydrochloric acid (5.2.2), and add the washing liquid to the separatory funnel to make the final volume 10mL. Add 10mL of isopropyl ether (5.2.6), shake for 5min, let it stand for stratification, transfer the aqueous phase to another separatory funnel, and repeat the extraction with 10mL of isopropyl ether (5.2.6) once more, transfer the aqueous phase to 10mL, polytetrafluoroethylene, and place the crucible in a dustproof evaporation. Evaporate and concentrate to about 0.5mL on a low-temperature graphite electric furnace, add 0.4mL hydrochloric acid (5.2.2) to wash the crucible, transfer to a 2mL colorimetric tube, dilute with high-purity water, and shake well. 5.4.4 Determination
5.4.4.1 Analysis line wavelength see Table 2
Table 2 Analysis line wavelength
Analysis line wavelength
Broken line wavelength
5.4.4.2 Ignite the plasma, and input the sample after the instrument stabilizes. Yuan An
Analysis line wavelength
5.4.4.3 Input the first set of standard solutions and the second set of standard solutions in order from low concentration to high concentration, and the computer automatically draws the working curve.
6.4.4.4 After the working curve is completed, input the sample blank solution and sample solution into the plasma for determination. 5.5 Calculation of analysis results
The percentage content (%) of the measured element is calculated as follows: V× (Ci- Ca) ×10-6
×100%
Wherein: X—
Percentage content of the measured element, %;
Co~—impurity concentration in the blank solution of the sample, pe/mL; Ci impurity concentration in the sample solution, /mL;
SJ 20713 1998
V-—sample volume, mL;
—sample mass, number.
5.6 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 3. Table 3
Content range
> 2× 10-6 ~ 5× 10-6
>5× 10- ~ 1× 10-5
>1× 10- ~- 5× 10~5
Additional remarks:
This standard is under the jurisdiction of China Electronics Technology Standardization Institute. This standard was drafted by the 46th Institute of the Ministry of Electronics Industry. Drafters of this standard: Zhang Shuzhen, Wang Chunmei, Wu Qiong, Duan Shuguang. Project code: B65003
Tolerance
2×10-6
4×10-6
5 ×10-6
-KAoNrKAca-6 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 3. Table 3
Content range
> 2× 10-6 ~ 5× 10-6
>5× 10- ~ 1× 10-5
>1× 10- ~- 5× 10~5
Additional remarks:
This standard is under the jurisdiction of the China Electronics Technology Standardization Institute. This standard was drafted by the 46th Institute of the Ministry of Electronics Industry. Drafters of this standard: Zhang Shuzhen, Wang Chunmei, Wu Qiong, Duan Shuguang. Project code: B65003
Allowable difference
2×10-6
4×10-6
5 ×10-6
-KAoNrKAca-6 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 3. Table 3
Content range
> 2× 10-6 ~ 5× 10-6
>5× 10- ~ 1× 10-5
>1× 10- ~- 5× 10~5
Additional remarks:
This standard is under the jurisdiction of the China Electronics Technology Standardization Institute. This standard was drafted by the 46th Institute of the Ministry of Electronics Industry. Drafters of this standard: Zhang Shuzhen, Wang Chunmei, Wu Qiong, Duan Shuguang. Project code: B65003
Allowable difference
2×10-6
4×10-6
5 ×10-6
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