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4 Test method
When the reagents and water used in this standard are not marked with other special requirements, the analytical reagents and the tertiary water specified in GB/T6682 shall be used
The standard titration solutions, standard solutions for impurity determination, preparations and products used in this standard shall be prepared in accordance with GB/T601, GB/T602, and GB/T603 unless other requirements are indicated
4.
The sample is titrated with potassium bromate standard titration solution in an acid medium
4.
4.
4.
4.
4.
Weigh 0.
Do a blank test at the same time
4.
Antimony content (X 1 ) expressed in mass percentage (calculated according to formula (1):
Where: V 1 -the volume of the potassium bromate standard titration solution consumed by the sample, ml;
V 0 —Blank consumption volume of potassium bromate standard titration solution, mL;
c— The actual concentration of potassium bromate standard titration solution, mol/L;
0.
m—the mass of the sample, g
4.
Take the arithmetic average of the two measurement results as the measurement result
.
The difference between the two parallel determination results shall not be more than 0.
2%
.
4.
2 Determination of chloride
4.
2.
1 Reagents and solutions
4.
2.
1.
1 Nitric acid solution: 1+7
.
4.
2.
1.
2 Tartaric acid solution: 100g/L
.
4.
2.
1.
3 Silver nitrate solution: c(AgNO 3 )=0.
1mol/L
.
4.
2.
1.
4 Chloride standard solution: 1ml solution contains 0.
1mg C-
.
4.
2.
2 Analysis steps
Weigh 0.
2g sample (accurate to 0.
01g), place it in a 50mL colorimetric tube, add 15mL tartaric acid solution to dissolve, add 1mL nitric acid solution, 3 drops of silver nitrate solution, add water to the mark, shake well, and place for 5min
.
Compared with the standard turbidity solution, the turbidity should not be greater than the turbidity of the standard turbidity solution
.
Standard turbidity solution: Take the chloride standard solution (0.
04mL for superior product, 0.
06mL for first-class product, and 0.
2mL for qualified product), and process the same as the sample at the same time
.
4.
3 Determination of iron
4.
3.
1 Reagents and solutions
4.
3.
1.
1 Hydrochloric acid solution: 1+5
.
4.
3.
1.
2 Hydrogen peroxide solution: 1+9
.
4.
3.
1.
3 Ammonium thiocyanate solution: 100g/L
.
4.
3.
1.
4 Tartaric acid solution: 100g/L
.
4.
3.
1.
5 Iron standard solution: 1mL solution contains 0.
1mg Fe
.
4.
3.
2 Analysis steps
Weigh 0.
2g sample (accurate to 0.
01g), place it in a test tube, add 10mL tartaric acid solution to dissolve, add 1mL hydrochloric acid solution and 1ml hydrogen peroxide solution, heat to boiling, cool to room temperature and transfer it into a 50mL colorimetric tube.
Add 1 mL of ammonium thiocyanate solution, add water to the mark, and mix well
.
The color should not be darker than the standard colorimetric solution
.
Standard colorimetric solution: Take the iron standard solution (0.
04mL for superior product, 0.
06mL for first-class product, and 0.
1mL for qualified product), and process the same as the sample at the same time
.
4.
4 Dissolution test
4.
4.
1 Reagents
Ethylene glycol
.
4.
4.
2 Analysis steps
Weigh 0.
3g of the sample (accurate to 0.
01g), place it in a 25mL colorimetric tube, add 10mL of ethylene glycol , and shake it well until the sample is dissolved
.
Horizontal visual inspection, it should be a colorless and transparent solution
.
Related Links: Industrial Antimony Acetate (1)