GB/T 4373.3-1984 Chemical analysis of arsenic - Barium sulfate gravimetric method for the determination of sulfur content

GB/T 4373.3-1984 Chemical analysis of arsenic - Determination of sulfur content by barium sulfate gravimetric method GB/T4373.3-1984 standard download decompression password: www.bzxz.net

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Chemical analysis method for arsenic
Determination of sulfur content by barium sulphate gravimetric method
Methods for chenic anaiysis uf arsenicThe barium sulphate gravimetric methodfor the determination of sulphur contentThis standard is applicable to the determination of sulfur content. Determination range: 0.10～0.50%. JDC669.778:543
GB 4373.3 -- 84
This standard complies with GB1467-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
The sample is dissolved in nitric acid and potassium chlorate, and hydrochloric acid is added to evaporate it. At a hydrochloric acid acidity of about 0.2N, a solution of sodium oxide is added to form a barium sulphate precipitate. The barium sulphate is filtered, burned and the mass of the barium sulphate is weighed. 2 Reagents
2.1 Potassium chlorate.
2.2 Hydrochloric acid (specific gravity 1.19)
2.3 Nitric acid Potassium monochlorate saturated solution: Add the acid to nitric acid (specific gravity 1.42), stir until it is completely dissolved and the added potassium chloride no longer dissolves.
2.4 Nitride solution (10). Use after filtering. 2.5 Silver nitrate solution (1.0%)
3 Sample
3.1 The sample must be sieved through an 80-day sieve, and the diameter of the sieve should not exceed 2mm. 3.2 After adding the sample, store it in a desiccator and weigh it for analysis on the same day. Weigh the sample according to the ratio of 3:1. 4 Analysis steps
4.1 Determination of the number of samples
Weigh two samples for determination and take the average value. 4.2 Samples
Weigh 1.600g of sample.
4.3 Vacuum test
Carry out vacuum test with the sample.
4.4 Determination
4.4.1 Place the sample (4.2) in a 400l beaker, moisten it with a small amount of water, and slowly add 25ml of nitric acid-potassium chlorate and solution (2.3) under continuous shaking (do not do this Do not heat it to prevent explosion). If necessary, add 2-3g potassium fluoride (2.1). When the violent reaction stops, move the crumbs to an electric furnace, heat and dissolve, and evaporate. Remove and cool slightly, add 10ml hydrochloric acid (2.2), wash the ring and the button with water, and evaporate at low temperature. Remove, add 10ml hydrochloric acid (2.2), and evaporate at low temperature again. Remove, add 3ml hydrochloric acid (2.2), 50ml water, heat to dissolve the salt, filter with medium-speed filter paper, wash the beaker and precipitate with hot water for 12 times, and dilute the filtrate with 200ml water. National Bureau of Standards 1984-0430 Issued
1985·0401 Implementation
GB 4373.3-84
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4.4.2 Boil the solution, remove it, add 25ml of chlorinated sodium solution (2.4) under constant stirring, and boil it for 510)min. Let it stand at 50-60℃ for more than 2h.
4.4.3 Filter it with slow-fixed filter paper, wash the beaker and precipitate with hot water, transfer all the precipitate in the beaker to the filter paper, and wash the precipitate with natural water until the washing liquid is free of fluoride ions [check with silver nitrate (2.5)]. 4.4.4 Transfer the filter paper and the precipitate to a constant-weight porcelain crucible, ash it on an electric furnace, transfer it to a high-temperature furnace with rising temperature, and burn it at 800-850℃ for 30min. Take it out and put it in a desiccator, cool it to room temperature, and weigh it. Repeat burning, cooling, and weighing until the final result is reached.
5 Calculation of analysis results
Calculate the percentage of sulfur according to the following formula:
(m2-ml)_ (ms-m3) ×0.1374
S(%) = -
-×100
Wherein: m is the mass of glass and sodium sulfate, g
m4 is the mass of the blank made with the sample, g; m3 is the mass of the sample, g;
is the conversion factor of sodium sulfate to sulfur. The analysis results are expressed to two decimal places. 6 Tolerance
The difference between the analysis results of laboratories should not be greater than the tolerance listed in the following table. Sulfur
0.10～0.20
0.20 ~ 0,35
0.35 ～0.50
Additional remarks:
This standard was proposed by China Nonferrous Metals Industry Corporation. This standard was drafted by the Hunan Shuimenshan Mining Bureau. This standard was drafted by the Hunan Shuikoushan Mining Research Institute. The main drafters of this standard were Sun Xiaohui and Liu Binbin.
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