GB/T 15080.2-1994 Chemical analysis method for antimony concentrates Determination of arsenic content GB/T15080.2-1994 standard download decompression password: www.bzxz.net

UDC669.754：543.06
National Standard of the People's Republic of China
GB/T 15080. 1~~15080. 9--94
Methods for chemical analysis of antimony concentrates
Published on 1994-05-11
Implemented on 1994-12-01
Published by the State Administration of Technical Supervision
National Standard of the People's Republic of China
Methods for chemical analysis of antimony concentrates
Antimony concentrates-Determination of arsenic content
Subject content and scope of application
This standard specifies the method for the determination of arsenic content in antimony concentrate. This standard is applicable to the determination of arsenic content in concentrate. Determination range: 0.1%~3%. 2 Reference standards
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB1467 General principles and general provisions for chemical analysis methods for metallurgical products 3 Method summary
GB/T 15080.2--94
The sample is decomposed with sulfuric acid-potassium sulfate, and the carbonized filter paper is used as a reducing agent and a co-solvent. In a hydrochloric acid solution of not less than 9 mol/L, benzene is added to extract arsenic trichloride, and water is used for back extraction. In a hydrochloric acid medium, methyl orange is used as an indicator, and trivalent arsenic is titrated with potassium bromate standard titration solution. 4 Reagents
4.1 Potassium sulfate.
Sulfuric acid (pl.84 g/mL).
4.3 Hydrochloric acid (p1.19 g/mL).
4.4 Benzene.
4.5 Hydrochloric acid (3+1).
4.6 Hydrochloric acid (1+1).
4.7 Arsenic standard solution: Weigh 1.3203g arsenic trioxide (standard reagent, pre-dried at 100-105C for 1h, placed in a desiccator, cooled to room temperature), place in a 250ml beaker, add 20mL sodium hydroxide solution (200g/L) to dissolve until clear, add 100mL water and 10mL sulfuric acid (1+1), cool to room temperature, transfer to a 1000mL volumetric flask, dilute to scale with water, mix, this solution contains 1mg arsenic per mL.
4.8 Potassium bromate standard titration solution.
4.8.1 Preparation: Weigh 0.28g potassium bromate and place in a 250mL beaker, add 100mL water to dissolve, transfer to a 1000mL volumetric flask, dilute to scale with water, mix.
4.8.2 Calibration: Take three portions of 10.00 mL of arsenic standard solution (4.7) and add them into a 125 mL separatory funnel containing 45 mL of hydrochloric acid (4.3) and mix well. The following operations are carried out according to 6.3.3~~~6.3.6. Perform a blank test along with the calibration.
Calculate the actual concentration of potassium bromate standard titration solution (4.8) according to formula (1): Approved by the State Bureau of Technical Supervision on May 11, 1994 and implemented on December 1, 1994
Wherein: c
GB/T15080.2-94
c = (V, V.)× 0. 037 46
-actual concentration of potassium bromate standard titration solution (4.8), mol/Lm—-mass of arsenic.g;
V, volume of potassium bromate standard titration solution (4.8) consumed in one titration of arsenic, mL; V. ——The volume of potassium bromate standard titration solution (4.8) consumed by the blank solution in the calibration, mL; (1)
0.03746—The mass equivalent to 1.00mL of potassium bromate standard titration solution Cc (1/6KBrO) = 1.000mol/LJ, expressed in grams.
The average of the three calibration results is the actual concentration of the potassium bromate standard titration solution (4.8). The range of the volume of potassium bromate standard titration solution (4.8) consumed in parallel calibration should not exceed 0.20mL. 4.9 Methyl orange indicator (1g/L).
5 Sample.
5.1 The particle size of the sample should be less than 0.100mm. www.bzxz.net
5.2 The sample should be dried at 100-105℃ for 1h and placed in a desiccator to cool to room temperature. 6 Analysis steps
6.1 Test material
Weigh the sample according to Table 1, accurate to 0.0001g. Table 1
Arsenic content.%
0. 10 ~1. 00
Carry out two independent determinations and take the average value. 6.2 Blank test
Carry out a blank test along with the test material.
6.3 Determination
Test material quantity,
6.3.1 Place the test material (6.1) in a 300mL conical flask, moisten it with a small amount of water, add 1g potassium sulfate (4.1), add 12mL sulfuric acid (4.2) and place it on an electric furnace to heat. After most of the sulfur is driven off, cover it with surface III, dissolve it for 1h at a temperature that keeps the solution slightly boiling, add about 3cm2 of qualitative filter paper, continue to heat until the dark red color of the solution disappears after the filter paper is carbonized, and remove it to cool. 6.3.2 Add 5 mL of water, mix well and cool to room temperature, add 45 mL of hydrochloric acid (4.3), mix well, and transfer the test solution to a 125 mL separatory funnel with a small amount of hydrochloric acid (4.5).
6.3.3 Add 60 mL of benzene (4.4), shake and extract for 1 min [pay attention to exhaust], let stand to separate, transfer the aqueous phase to another 125 mL separatory funnel pre-filled with 20 mL of benzene (4.4), shake and extract for 1 min, let stand to separate, discard the aqueous phase, and combine the organic phase in the first separatory funnel.
6.3.4 Use 5 mL of hydrochloric acid (4.5) to drip and wash the neck and stopper of the separatory funnel, shake for 30 seconds, let stand to separate, and discard the aqueous phase. Repeat the washing with hydrochloric acid (4.5) twice, using 5 mL each time. After the third washing, let stand for 2 minutes to completely separate the aqueous phase. 6.3.5 Add 30 mL of water to the separatory funnel for back extraction, shake for 30 seconds, let stand to separate, and transfer the aqueous phase to a 250 mL conical flask. Add another 15 mL of water to the separatory funnel for back extraction, shake for 30 seconds, let stand to separate, and combine the aqueous phases in the conical flask. 6.3.6 Add 20 mL of hydrochloric acid (4.6) and 1 drop of methyl orange indicator (4.9) to the conical flask containing the aqueous phase. While maintaining the solution at 80~5
GB/T 15080.2—94
90℃, titrate with potassium bromate standard titration solution (4.8) until the red color of the solution just disappears. 7 Expression of analytical results
Calculate the percentage of arsenic according to formula (2):
As(%) × (Vz-V) ×0. 037 46 × 100..mo
Wherein: c--actual concentration of potassium bromate standard titration solution (4.8), mol/L; Vz--volume of potassium bromate standard titration solution (4.8) consumed by titrating test solution, mLV3--volume of potassium bromate standard titration solution (4.8) consumed by titrating blank solution, mLmo--mass of sample, g;
(2)
0.03746--mass of arsenic expressed in grams equivalent to 1.00mL potassium bromate standard titration solution Cc (1/6KBrO.) = 1.000mol/LJ.
8 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Shen content
0.10~0.30
>0. 30~0.50
>0. 50～1. 00
71. 00~3. 00
Additional instructions:
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is technically managed by Beijing Research Institute of Mining and Metallurgy. This standard is drafted by Xikuangshan Mining Bureau and Hunan Nonferrous Metals Research Institute. This standard is drafted by Xikuangshan Mining Bureau.
The main drafters of this standard are Liu Huachang and Zeng Fusheng. 6
Allowable difference
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