This standard specifies the determination method of selenium content in antimony. This standard is applicable to the determination of selenium content in antimony. Determination range: 0.0005% to 0.060%. GB/T 3253.5-2001 Chemical analysis method for antimony Determination of selenium content GB/T3253.5-2001 Standard download decompression password: www.bzxz.net

KS 77.123. 60
National Standard of the People's Republic of China
GB/T 3253. 7 ~-3253.62001
Methods for chenicaf analysis of antimony2001- 07 -10 Implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
2001- 12 -01 Issued
1Scope
National Standard of the People's Republic of China
Methods for chenicaf analysis of antimony
Determination of selenium
Methods fur cheinicul waulysis uf smtiuuryDetrrrnination of seleniun Camlent This standard specifies the determination method of camlent content: This standard applies to the determination of camlent content, the range of determination: 0.000%~60%. 2 Methods
CB/T3253.5
Generation #G6/T3233.71982
Test the solution with salt and hydrogen peroxide, to make or base, such as acid reduction, the solution is not deep selected precipitation and coexisting impurities are separated by potassium arsenate, after a large excess of oxidizing agent, the reagent is tested with selenium monoxide to form a color complex, the solution is taken: the spectrophotometer is used at a wavelength of 150rm to generate light. The test solution contains 2m arsenic.29x, 3rg soft.2mg elastic fast determination. 3 Reagents
3.1 Calcium arsenate.
3.2 (1.15x/m..)
3.3 Nitric acid rl.12 g/mL)
3.4 ​​Hydrogen peroxide (30%:
3.5 Salt breakdown (1+13
3.6 Heat monohydrate (12.
3. B Toluene.
3. 9 Red Yong.sc mL).
3. 10 Water 1 - 4).
3.11 Liquid (3.8/): Take 0.1% oxidizing agent-containing solution 190g/1, add 55ml water. Acid (3.5) press water to dilute to 1)mL 3.72 Chemical solution (202/1.) slowly take 2% fluorine molybdenum (CC.H,)) and add 13.5) of sodium chloride (3.) dilute to 50mL and mix
3.13 Potassium hydroxide solution (1U/)
3.4 ​​Z_ ethylamine-sodium N-EITA> solution (5/) 35%%-amino acid combined with gel (according to the reagent> concentration (5/1.), prepare 3.6 ethanol source solution (1g) when using,
3-7 Wine label is difficult to store liquid, take 0 .1692g pure 92.99% 1,000m without adding 51 acid (3.! The General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China approved 18
70C1-17-01 implementation
/T3253.5-201
in clothing, hydrolyze 1% of carbon dioxide, and empty the mud with water. This deep l heart
3.18 Standard dye reduction: transfer 0.00ml. Standard foreign busy storage in 3 (m. volume bottle, dilute with water to the scale, mix, and observe.
4 Only instrument
spectrometer,
5 analysis step
safety table 1 soft joint test details: spray to
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Independently conduct two-stream determination and take half-value, 5.2 Empty test
The same sample is used for empty test.
5.3 Determination
Collect the long and obtain the body. ml
5.3.1 Put the sample (5.1) into a 100L beaker, add 5 (3.2), add 0.8m~1.5mL of selected chemical solution, and gently push the pressure while keeping the rate constant
5.3.2 Put the sample 511 into the bottle. Add salt (5.5 to the scale, filter and 5.3.3 Take more test solution according to Table 1 F00 beaker and use 3. Filter to 20mL5.3.4 Add 0.2mL oil solution, 1mL of chemical solution, and 1.5k~3.\z acid. Heat to a stagnation point and remove the medicine for 3s. Remove the cold moving
5.3.5 Transfer the test wave and steam to a 2 yuan 1m1. separatory funnel, wash with 10ml. salt 13. and then add 15mL of unsalted butter to the funnel, place and distribute, discard the large water phase, add 20mL of plastic (3.5) and 10mL of permanent, lightly add medicine 15, and then add the tea leather layer, add 1UraL of hydrochloric acid (3.6) to the large water phase 5.3.6 and add 1UraL of hydrochloric acid (3.6) to the funnel. Add 1\.23ml of potassium chromium sulfate. Strongly endure the vibration 1r.in. The two precipitates are completely dissolved in the water phase, let it stand and separate, the seawater phase is not small, and the water phase is washed with 10ml of water. · Iron liquid and the original, discard the next layer, add 0.2ml NaFIA to form an excess of 2L NaFIA. 5.3.7 Add 2 drops of tea filter water 3.2 and reduce to red (H1.~3.. 3ml. 3ml. 5.3.8 Adjust the acidity of the liquid to 12% with tar water (3.10), wash with a small amount of water, and add 4ml of water to the washing machine. Swirl for 1min. The layers are separated and the products are not related. 5.3.9 Transfer part of the mixture (.3.) to 2ml of absorbent III, use the blank test solution prepared with the trial as the reference, and place it at the spectrophotometer source for 43mrt. , measure its absorbance, and find out the organic composition on the working curve. 5.4 Working curve: 5.4.1 Transfer 0.1.(0.2.93.3.00. Small.c.5.50,0.0ml. The required amount should be placed in the corrected beaker: I. Sieve ≤20 1. Add two clean glues (3.5, GB/T3253.52, and proceed as follows 5.27-5.3.8: 19
5.4.2 Take a portion of the standard solution of organic material (5.4.1) and filter it with cotton wool, transfer it to a container 2cm tall, and measure its absorbance: take the reagent air as the standard, and the absorbance as the standard. 6. The results of the analysis are shown in Table 1. The results of the test are shown in Table 1. The results of the test are shown in Table 1. The results of the test are shown in Table 1. The results of the test are shown in Table 1. The results of the test are shown in Table 1.
The comparison of the results between the test laboratories is not significant. The allowable reduction values ​​are listed in Table 2.
Mass fraction of www.bzxz.net
0. 00 5-0. 062 3
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3 X --U.906
10. s 0--1. 0.0
2. 319--6, 031
>3. 237--. 66
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