This standard specifies the determination method of sulfur content in antimony concentrate. This standard is applicable to the determination of sulfur content in antimony concentrate. Determination range: 1% to 30%. GB/T 15080.8-1994 Chemical analysis method for antimony concentrate Determination of sulfur content GB/T15080.8-1994 Standard download decompression password: www.bzxz.net

UDC 669.754 : 543. 06
National Standard of the People's Republic of China
GB/T15080.1~15080.9--94
Methods for chemical analysis of antimony concentrates
Published on May 11, 1994
Implemented on December 1, 1994
State Administration of Technical Supervision
National Standard of the People's Republic of China
Methods for chemical analysis of antimony concentrates
Determination of sulfur content
Antimony concentrates---Determination of sulfur content
Subject content and scope of application
This standard specifies the method for determining the sulfur content in antimony concentrate. This standard is applicable to the determination of sulfur content in antimony concentrate. Determination range: 1% to 30%. 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 15080.8---94
The sample is burned in a high-temperature air flow to convert sulfur into sulfur dioxide, which is absorbed and oxidized into sulfuric acid with hydrogen peroxide. Methyl red-methylene blue solution is used as a mixed indicator and titrated with sodium hydroxide standard titration solution until the solution changes from purple-red to bright green. 4 Reagents
4.1 Potassium hydroxide.
4.2 Anhydrous calcium chloride.
4.3 Hydrogen peroxide absorption solution (1+19). 4.4 Standard sodium hydroxide titration solution (c(NaOH) = 0.15 mol/L]. 4.4.1 Preparation: Weigh 6 g of sodium hydroxide, place in a 250 mL beaker, dissolve in water without carbon dioxide, transfer to a 1000 mL volumetric flask, and dilute to scale with water without carbon dioxide, mix well. Store in a plastic bottle. 4.4.2 Calibration: Weigh three portions of 1.0000 g of potassium hydrogen phthalate (reference reagent) that has been dried at 100-105 °C for 2 h, place in a 300 mL conical flask, add 60 mL of water to dissolve, add 2 drops of phenolic acid indicator (10 g/L ethanol solution), and titrate with sodium hydroxide standard titration solution until a slightly reddish color is the end point.
Perform a blank test along with the calibration.
Calculate the actual concentration of sodium hydroxide standard titration solution (4.4) according to formula (1). m
(V, V.) X 0. 204 2
Wherein: c-actual concentration of sodium hydroxide standard titration solution (4.4), mol/Lm~mass of potassium hydrogen phthalate.g;
-volume of sodium hydroxide standard titration solution (4.4) consumed in titrating potassium hydrogen phthalate solution, mL; State Technical Supervision Bureau approved 1994-05-11 26
implemented on 1994-12-01
GB/T 15080.8-94
V. —-volume of sodium hydroxide standard titration solution (4.4) consumed by blank solution in calibration, mL; 0. 204 2-
-mass of potassium hydrogen phthalate equivalent to 1.00mL sodium hydroxide standard titration solution Cc(NaOH)=1.000mol/L), expressed in grams.
The average of the three calibration results is the actual concentration of the sodium hydroxide standard titration solution (4.4). The range of the volume of the sodium hydroxide standard titration solution (4.4) consumed in the parallel calibration should not exceed 0.10mL. 4.5 Methyl red-methylene blue mixed indicator: 20 parts of methyl red ethanol solution (0.3g/L) and 3 parts of methylene blue solution (1g/L) are mixed. 5 Apparatus
The apparatus used is shown in the figure below.
Schematic diagram of the sulfur-based device for combustion neutralization titration 12
1-Air inlet; 2-Gas washing bottle: Containing potassium permanganate (40g/L) solution prepared with potassium hydroxide (400g/L) solution; 3-Drying tower: 4-Flowmeter; 5-Temperature automatic controller, with platinum thermocouple; 6-Tube electric furnace 7-Unglazed porcelain tube; 8-Unglazed porcelain boat; 9-Dust collector; 10-50mL basic burette, 11, 12-Glass absorber; 13-Buffer bottle (500mL); 14-Two-way piston; 15-Vacuum pump 6 Sample
6.1 The particle size of the sample should be less than 0.100mm.
6.2 The sample should be dried at 100-105℃ for 1h and placed in a desiccator to cool to room temperature. 7 Analysis steps
7.1 Test material
Weigh the sample according to Table 1, accurate to 0.0001g. Table 1
Sulfur content, %
1.00~~10.00
>10:00
Carry out two independent determinations and take the average value. 7.2 Determination
7.2.1 Place the test material (7.1) evenly in the combustion porcelain boat and put it in the desiccator. 7.2.2 Turn on the power supply, raise the furnace temperature to 900℃, and put it in the automatic control state. Test material amount, g
7.2.3 Add 50~60mL of hydrogen peroxide absorption solution (4.3) and 1mL of methyl red-methylene blue mixed indicator (4.5) into the glass absorber. www.bzxz.net
7.2.4 Connect the device according to the diagram, start the vacuum pump, adjust the air flow rate to 2L/min, and check the sealing of the sulfur determination device. Then adjust the air flow rate to 0.5L/min, and titrate with sodium hydroxide standard titration solution (4.4) until the solution just turns bright green. Ignore the reading. 7.2.5 Push the porcelain boat (7.2.1) containing the sample into the highest temperature of the burning porcelain tube, quickly plug the porcelain tube, pass air at a flow rate of 0.5L/min, burn the sample, and titrate with sodium hydroxide standard titration solution (4.4). Keep the solution just bright green. After burning for 10 minutes, increase the air flow rate to 2L/min, continue burning for 2 minutes, then wash the air guide tube of the glass absorber with water, and continue titrating with sodium hydroxide standard titration solution (4.4) until the solution changes from purple-red to bright green. This is the end point. 8 Expression of analysis results
Calculate the percentage of sulfur according to formula (2):
S(%) C: V× 0. 016 03
Wherein: c-
actual concentration of sodium hydroxide standard titration solution (4.4), mol/L; volume of sodium hydroxide standard titration solution (4.4) consumed by titrating the test solution, mL; -mass of the sample, g3
0.01603--mass of sulfur in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(NaOH)=1.000 mol/L].
The result should be expressed to two decimal places.
9 Tolerance
The difference in analysis results between laboratories should not be greater than the tolerance listed in Table 2. Table 2
Sulfur content
1.00~10.00
>10.00~20.00
>20.00～30.00
Additional remarks:
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is under the technical jurisdiction of 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 Luo Xicheng and Zeng Fusheng. 28
Allowable deviation
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