Heavy metals, Method I 231
Prepare the
Test Preparation as follows. Dissolve 1 g in 10 mL of water, add 3.0 mL of glacial acetic acid, dilute with water to 25 mL, and adjust with glacial acetic acid to a pH between 3.8 and 4.0, measured with a pH meter. Prepare the
Monitor Preparation as directed for
Test Preparation, 2.0 mL of
Standard Lead Solution being added: the limit is 0.002%.
Limit of sodium
Potassium chloride solution
Dissolve 100 g of potassium chloride in water to make 1000 mL.
Standard solutions
Transfer 127.1 mg of sodium chloride, previously dried at 105
for 2 hours and accurately weighed, to a 500-mL volumetric flask, add water to volume, and mix. Transfer 10.0 mL of this solution to a 100-mL volumetric flask, dilute with water to volume, and mix. Transfer 2.0, 5.0, and 10.0 mL of this solution to separate 100-mL volumetric flasks, add 10.0 mL of
Potassium chloride solution to each flask, dilute with water to volume, and mix. These
Standard solutions contain 0.2, 0.5, and 1.0 µg of sodium per mL, respectively.
[NOTEConcentrations of sodium in the
Standard solutions may be modified to fit the linear or working range of the atomic absorption spectrophotometer.
]
Test solution
Transfer about 0.2 g of Potassium Acetate, accurately weighed, to a 100-mL volumetric flask containing about 50 mL of water, and swirl to dissolve. Add 10.0 mL of Potassium chloride solution, dilute with water to volume, and mix. [NOTEThe concentration of Potassium Acetate in the Test solution may be modified by using a different quantity or by further dilution to bring the absorption response within the range of responses obtained from the Standard solutions.]
Blank solution
Transfer 10.0 mL of Potassium chloride solution to a 100-mL volumetric flask, dilute with water to volume, and mix.
Procedure
Concomitantly determine the absorbances of the
Standard solutions and the
Test solution at the sodium emission line of 589 nm, with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-Scattering 851) equipped with a sodium hollow-cathode lamp and an oxidizing airacetylene flame, using the
Blank solution to zero the instrument. Plot the absorbances of the
Standard solutions versus concentration, in µg per mL, of sodium, and draw the straight line best fitting the plotted points. From the graph so obtained, determine the concentration
C, in µg per mL, of sodium in the
Test solution. Calculate the percentage of sodium in the portion of Potassium Acetate taken by the formula:
CD / 10,000W,
in which
W is the quantity, in g, of Potassium Acetate taken to prepare the
Test solution; and
D is the extent of dilution of the
Test solution: not more than 0.03% of sodium is found.
Assay
Dissolve about 200 mg of Potassium Acetate, previously dried and accurately weighed, in 25 mL of glacial acetic acid, add 2 drops of
crystal violet TS, and titrate with 0.1 N perchloric acid VS to a green endpoint. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N perchloric acid is equivalent to 9.814 mg of C
2H
3KO
2.