Ammonium Sulfate
(NH4)2SO4 132.14
Ammonium sulfate
[7783-20-2].
(a moe' nee um sul' fate).
(NH4)2SO4 132.14
Ammonium sulfate
[7783-20-2].DEFINITION
Ammonium Sulfate contains NLT 99.0% and NMT 100.5% of (NH4)2SO4.
IDENTIFICATION
• A. Identification Tests—General, Ammonium 
191
:
A solution (1 in 20) meets the requirements.
191:
A solution (1 in 20) meets the requirements.
• B. Identification Tests—General, Sulfate 191:
A solution (1 in 20) meets the requirements.
191:
A solution (1 in 20) meets the requirements.
ASSAY
• Procedure
Sample:
2.5 g of Ammonium Sulfate
Titrimetric system
(See Titrimetry 541.)
541.)
Mode:
Residual titration
Titrant:
1 N sodium hydroxide VS
Back titrant:
1 N sulfuric acid VS
Endpoint detection:
Colorimetric
Blank:
50.0 mL of 1 N sodium hydroxide VS, accurately measured
Analysis:
Add the Sample to a 500-mL conical flask and dissolve in 50 mL of water. Add 50.0 mL of 1 N sodium hydroxide VS, place a filter funnel loosely in the neck of the flask, and boil until ammonia is expelled (about 10–15 min), as determined with litmus paper. Cool, add 0.15 mL of thymol blue TS, and titrate the excess sodium hydroxide with 1 N sulfuric acid VS. Perform a blank determination.
Calculate the percentage of ammonium sulfate [(NH4)2SO4] in the Sample taken:
Result = [(B 
V) × N × F ×100]/W
V) × N × F ×100]/W
| B | = | = 1 N sulfuric acid VS consumed by the Blank (mL) |
| V | = | = 1 N sulfuric acid VS consumed by the Sample (mL) |
| N | = | = actual normality of the Back titrant (mEq/mL) |
| F | = | = equivalency factor, 66.07 mg/mEq |
| W | = | = weight of the Sample (mg) |
Acceptance criteria:
99.0%–100.5%
IMPURITIES
• Limit of Insoluble Matter
Sample:
20 g
Analysis:
Transfer the Sample to a covered beaker, and dissolve in 200 mL of water. Heat to boiling, and warm on a steam bath for 1 h. Filter the hot solution through a tared sintered-glass crucible of medium porosity (10–15 µm). Wash the beaker and the filter with hot water, dry the crucible at 105
, cool in a desiccator, and weigh.
, cool in a desiccator, and weigh.
Acceptance criteria:
NMT 1 mg of insoluble matter is found (0.005%).
• Limit of Phosphate
Standard phosphate solution, Phosphate reagent A, and Phosphate reagent B:
Prepare as directed for Phosphate in Reagents under Reagents, Indicators, and Solutions—General Tests for Reagents.
Sample:
4.0 g
Control:
0.2 mL of Standard phosphate solution
Analysis
[Note—The tests for the Sample and the Control are made preferably in matched color-comparison tubes. ]
Dissolve the Sample in 25 mL of 0.5 N sulfuric acid, add 1 mL each of Phosphate reagent A and Phosphate reagent B, and allow to stand at room temperature for 2 h. Proceed with the Control using the same quantities of the same reagents as in the test for the Sample.
Acceptance criteria:
Any blue color obtained from the Sample should not exceed that produced from the Control (NMT 5 ppm).
• Chloride and Sulfate, Chloride 221
221
Standard chloride solution:
Transfer 165 mg of sodium chloride to a 100-mL volumetric flask. Dissolve in and dilute with water to volume. Transfer 10.0 mL to a 1000-mL volumetric flask, and dilute with water to volume to obtain a solution having a concentration of 10 µg/mL of chloride.
Acceptance criteria:
A 2-g portion shows no more chloride than corresponds to 1.0 mL of Standard chloride solution (NMT 5 ppm).
• Limit of Nitrate
Standard nitrate solution and Brucine sulfate solution:
Prepare as directed for Nitrate in Reagents under Reagents, Indicators, and Solutions—General Tests for Reagents.
Sample solution:
Dissolve 1.0 g in 3 mL of water by heating in a boiling water bath, and add Brucine sulfate solution to make 50 mL.
Control solution:
To 1.0 mL of Standard nitrate solution add 1.0 g of ammonium nitrate, then add Brucine sulfate solution to make 50 mL.
Blank:
50 mL of Brucine sulfate solution
Analysis:
Heat the Sample solution, Control solution, and Blank in a boiling water bath for 15 min with periodic gentle swirling, then cool rapidly in an ice bath to room temperature. Adjust a suitable spectrophotometer with the Blank to zero absorbance at 410 nm. Determine the absorbance of the Sample solution, note the result, and adjust the instrument with the Sample solution to zero absorbance. Determine the absorbance of the Control solution.
Acceptance criteria:
The absorbance reading for the Sample solution does not exceed that for the Control solution (NMT 10 ppm).
• Iron 241
241
Sample solution:
Dissolve 2.0 g in 40 mL of water, and add 2 mL of hydrochloric acid.
Acceptance criteria:
NMT 5 ppm
SPECIFIC TESTS
• Microbial Enumeration Tests 61 and Tests for Specified Microorganisms 62:
The total aerobic microbial count does not exceed 1000 cfu/g, and the total combined molds and yeasts count does not exceed 10 cfu/g.
61 and Tests for Specified Microorganisms 62:
The total aerobic microbial count does not exceed 1000 cfu/g, and the total combined molds and yeasts count does not exceed 10 cfu/g.
• pH 791:
5.0–6.0 in a solution (1 in 20)
791:
5.0–6.0 in a solution (1 in 20)
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in well-closed containers. No storage requirements are specified.
Auxiliary Information—
Please check for your question in the FAQs before contacting USP.
| Topic/Question | Contact | Expert Committee |
|---|---|---|
| Monograph | Robert H. Lafaver, M.S.
Scientific Liaison 1-301-816-8335 |
(EXC2010) Monographs - Excipients |
| 61 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
| 62 |
Radhakrishna S Tirumalai, Ph.D.
Principal Scientific Liaison 1-301-816-8339 |
(GCM2010) General Chapters - Microbiology |
USP35–NF30 Page 1699
Pharmacopeial Forum: Volume No. 30(3) Page 966