Heavy metals,Method Iá231ñ
Prepare the
Test Preparationas follows.Dissolve 1g in 10mLof water,add 3.0mLof glacial acetic acid,dilute with water to 25mL,and adjust with glacial acetic acid to a pHbetween 3.8and 4.0,measured with a pHmeter.Prepare the
Monitor Preparationas directed for
Test Preparation,2.0mLof
Standard Lead Solutionbeing added:the limit is 0.002%.
Limit of sodium
Potassium chloride solution
Dissolve 100g of potassium chloride in water to make 1000mL.
Standard solutions
Transfer 127.1mg of sodium chloride,previously dried at 105

for 2hours and accurately weighed,to a 500-mLvolumetric flask,add water to volume,and mix.Transfer 10.0mLof this solution to a 100-mLvolumetric flask,dilute with water to volume,and mix.Transfer 2.0,5.0,and 10.0mLof this solution to separate 100-mLvolumetric flasks,add 10.0mLof
Potassium chloride solutionto each flask,dilute with water to volume,and mix.These
Standard solutionscontain 0.2,0.5,and 1.0µg 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 0.2g of Potassium Acetate,accurately weighed,to a 100-mLvolumetric flask containing about 50mLof water,and swirl to dissolve.Add 10.0mLof 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 10.0mLof Potassium chloride solutionto a 100-mLvolumetric flask,dilute with water to volume,and mix.
Procedure
Concomitantly determine the absorbances of the
Standard solutionsand the
Test solutionat the sodium emission line of 589nm,with a suitable atomic absorption spectrophotometer (see
Spectrophotometry and Light-Scattering á851ñ)equipped with a sodium hollow-cathode lamp and an oxidizing airacetylene flame,using the
Blank solutionto zero the instrument.Plot the absorbances of the
Standard solutionsversus 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
Wis the quantity,in g,of Potassium Acetate taken to prepare the
Test solution;and
Dis the extent of dilution of the
Test solution:not more than 0.03%of sodium is found.