Strong Ammonia Solution
Strong Ammonia Solution is a solution of NH3, containing NLT 27.0% and NMT 31.0% (w/w) of NH3. On exposure to air, it loses ammonia rapidly.
[CautionUse care in handling Strong Ammonia Solution because of the caustic nature of the Solution and the irritating properties of its vapor. Cool the container well before opening, and cover the closure with a cloth or similar material while opening. Do not taste Strong Ammonia Solution, and avoid inhalation of its vapor. ]
Analysis: Hold a glass rod moistened with hydrochloric acid near the surface of the Solution.
Acceptance criteria: Dense, white fumes are produced.
Sample: Transfer quickly a portion of Strong Ammonia Solution to a stoppered, thick-walled container (a pressure bottle is suitable) to obtain a column height of about 20 cm, insert the stopper, and cool the container and contents to 10 or lower. Accurately weigh a glass-stoppered, 125-mL conical flask containing 35.0 mL of 1 N sulfuric acid VS. Insert a graduated 10-mL measuring pipet into the cooled solution, allow the liquid to rise in the pipet without vacuum, remove the pipet, wipe off adhering liquid, and discard the first mL of the solution permitted to run from the pipet. Hold the pipet just above the surface of the 1 N sulfuric acid VS in the conical flask, and transfer about 2 mL of the solution into the flask. Insert the stopper, and again weigh to obtain the weight of the portion taken of the Sample.
(See Titrimetry 541.)
Mode: Residual titration
Titrant: 1 N sulfuric acid VS
Back titrant: 1 N sodium hydroxide VS
Blank: Proceed as directed for the Sample, omitting the Strong Ammonia Solution
Endpoint detection: Colorimetric
Calculate the percentage of NH3 in the portion of the Sample taken:
Result = [(B V) × N × F × 100]/W
Acceptance criteria: 27.0%31.0%
• Heavy Metals, Method I 231
Test preparation: Evaporate 1.7 mL on a steam bath to dryness, add to the residue 1 mL of 3 N hydrochloric acid, and evaporate to dryness. Dissolve the residue in 2 mL of 1 N acetic acid, and dilute with water to 25 mL.
Analysis: Proceed as directed in the chapter.
Acceptance criteria: NMT 13 ppm
• Limit of Nonvolatile Residue
Sample: 10 mL
Analysis: Evaporate the Sample in a tared platinum or porcelain dish to dryness, and dry at 105 for 1 h.
Acceptance criteria: NMT 5 mg of residue remains (0.05%).
• Readily Oxidizable Substances
Sample solution: 4 mL of Strong Ammonia Solution
Analysis: Mix the Sample solution with 6 mL of water, and add a slight excess of 2 N sulfuric acid and 0.10 mL of 0.1 N potassium permanganate.
Acceptance criteria: The pink color does not completely disappear within 10 min.
• Packaging and Storage: Preserve in tight containers, at a temperature not above 25.