JB/T 9220.10-1999 Chemical analysis of acidic slag from foundry cupola - Determination of sulfur content by barium sulfate gravimetric method

JB/T 9220.10-1999 JB/T 9220.10-1999 Chemical analysis of acidic slag from foundry cupola - Determination of sulfur content by barium sulfate gravimetric method JB/T9220.10-1999 Standard download decompression password: www.bzxz.net

JB/T 9220.10
This standard is a revision of JB/Z284.1087 "Chemical Analysis Method of Acidic Slag of Casting Iron Furnace: Determination of Sulfur Content by Barium Sulfate Refraction Method". Editorial changes have been made to the original standard, and the main technical content has not changed.
This standard replaces JB/Z284.1087 from the date of implementation. This standard is proposed by the National Technical Committee for Foundry Standardization and is under the jurisdiction of the drafting units of this standard: Shanghai Diesel Engine, Nanchang Diesel Engine Factory, Guiyang Foundry, Shenyang Foundry, Haituo Steam Company, Huashi Iron and Steel Plant, Wuxi Diesel Engine Factory, Changzhou Diesel Engine Factory, etc. Main drafters of this standard: Gong Zhihan, etc.www.bzxz.net
Standard of the Machinery Industry of the People's Republic of China
Chemical analysis methods for acid slay of cupola-Determination of sulphur by gravimetric methodusing barium sulfate
JB/T 9220.10
—1999
Replaces JB/Z.284.10-87
This standard specifies the determination of sulfur content in chemical analysis methods. Determination range: 0.10%~2.00%. This standard is applicable to the analysis of the composition of acid slag of cupola. 2 Test conditions
The sample is alkali-melted to convert the sulfide in the sample into soluble sulfate, and then leached and filtered to remove precipitation such as hydroxide and carbonate. In dilute hydrochloric acid solution, sulfate is quantitatively precipitated with barium chloride, and filtered, washed, burned, weighed, and converted to the percentage of sulfur. 3 Reagent preparation
3.1 Mixed flux: 1 part of anhydrous sodium carbonate and 2 parts of zinc oxide. 3.2 Anhydrous ethanol.
3.3 Sodium carbonate solution (1%).
Glacial acetic acid (density 1.05g/mL).
3.5 Hydrogen peroxide (density 1.10g/ml). 3.6 Methyl red solution (0.1%): prepared with anhydrous ethanol (3.2). 3.7
Hydrochloric acid (density 1.19g/mL).
Hydrochloric acid (1-+-1).
Hydrochloric acid (1+200).
: Barium chloride solution (10%).
Silver nitrate solution (1%).
4 Analysis steps
4.1 Sample quantity
Take 1.0000g of sample.
4.2 Blank test
Carry out a blank test together with the sample.
4.3 Determination
4.3.1 Mix the sample (4.1) with 8g of mixed flux (3.1), place it in a 30mL platinum crucible with a small amount of mixed flux (3.1), spread 2g of mixed flux on it, cover it, and sinter it in a high-temperature furnace at 900~950C for 60~70min. Note: A good sample should be separated from the crucible wall and form a sintered block in the crucible, which is very easy to take out. Otherwise, if the time is short, the sulfur conversion will be incomplete; if the time is long and the temperature is too high, it will easily become a molten block, which is difficult to remove with water.
Approved by the State Machinery Industry Bureau on 1999-06-24, implemented on 2000-01-01
JB/T9220.10—1999
4.3.2 Take out and cool, transfer the sintered block to a 250mL beaker, moisten it with a small amount of water, and crush it with a rubbing rod. Wash the platinum snail and the pot lid with hot water. Add hot water to make the solution volume about 50-80 ml. Add 1-3 mL of anhydrous ethanol (3.2). Heat and boil for 1-2 min. 4.3.3 While hot, use slow quantitative filter paper and a small amount of quantitative filter paper pulp to filter into a 500 mL beaker (keep the precipitate in the original beaker as much as possible). Add 50 mL of freshly boiled sodium carbonate solution (3.3) to the original beaker, stir well, continue filtering, and then wash the precipitate and filter paper with hot sodium carbonate solution (3.3) 5-6 times.
4.3.4 Add 1 ml of glacial acetic acid (3.4), 5 drops of hydrogen peroxide (3.5), 1-2 drops of methyl red solution (3.6) to the warm filtrate, add hydrochloric acid (3.7) to neutralize until it turns red, add 3 mL of hydrochloric acid (3.8), add water to make the solution volume about 300 ml. Stir, cover with Table III, and heat until large bubbles appear.
4.3.5 Remove, rinse Table III and the beaker wall with hot water, heat and add 10ml barium chloride solution (3.10) dropwise while stirring continuously, continue stirring for 3-5min, keep warm at 60-70℃ for 2h, and leave at room temperature overnight. 4.3.6 Filter with slow quantitative filter paper and a small amount of quantitative filter paper pulp, carefully wipe off the precipitate adhering to the wall with a wiper, wash the beaker and precipitate with hydrochloric acid (3.9) 2-3 times. Discard the filtrate. 4.3.7 Wash the precipitate with hot water until there is no chloride ion [check with silver nitrate solution (3.11)]. Filter the washing liquid into the original beaker. 4.3.8+ Add 2ml barium chloride solution (3.10) to the washing filtrate, heat and evaporate until almost. Add 1ml hydrochloric acid (3.8) and 25ml water, heat to boil, remove, and leave at room temperature overnight. Filter with slow quantitative filter paper and a small amount of quantitative filter paper pulp, and wash the precipitate with hot water until there is no chloride ion [check with nitric acid solution (3.11)]. 4.3.9 Place the precipitate obtained twice together with the filter paper and pulp in a constant amount of platinum, dry and ash, cover the crucible with a crucible cover, and burn in a high-temperature furnace at 800℃ for 30 minutes. Take out and cool slightly and place in a desiccator, weigh after cooling to room temperature, and repeat the burning until the weight is clear. Calculation of analysis results
Calculate the percentage of sulfur according to formula (1):
_[(m=m2)-ml×0.137 4×100%
where: m1-mass of platinum crucible and precipitate, gm
mass of platinum crucible, g;
blank amount·g;
-sample weight, g,
C.137 4-conversion factor of sulfuric acid converted to sulfur. 6 Tolerance
The difference in analysis results between laboratories should not be greater than the tolerance listed in Table 1. When calibrating with standard samples, the result deviation shall not exceed 1/2 of the tolerance listed in Table 1.
Sulfur content
0. 100~0. 500
>0.500~-2.00
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