The flame photometer characteristically
is equipped with a photomultiplier phototube detector for determination
of calcium or sodium, a red sensitive phototube detector for the determination
of potassium, a monochromator, an adjustable exit slit, sensitiviy controls
and an oxyacetylene burner. An oxyhydrogen burner is necessary for the
determination of potassium in the presence of large amounts of calcium.
Standard Calcium Ion Solution- Transfer 249.7 mg of calcium carbonate, previously dried at 300ºC for 3 hours and cooled in a desiccator for 2 hours, to a 100-mL volumetric flask, dissolve in a mixture of 20 mL of water and 5 mL of 3 N hydrochloric acid, dilute with water to volume, and mix. Each mL contains 1.00 mg of calcium ion (Ca). Standard Potassium Ion Solution- Transfer 190.7 mg of Potassium chloride previously dried at 105ºC for 2 hours, to a 100-mL volumetric flask, dissolve in water, dilute with water to volume, and mix. Each mL contains 1.00 mg of potassium ion (K). Standard Sodium Ion Solution- Transfer 254.2 mg of sodium chloride, previously dried at 105ºC for 2 hours, to a 100-mL volumetrie flask, dissolve in water, dilute with water to volume, and mix. Each mL contains 1.00 mg of sodium ion (Na). Standard Preparation- Transfer a 50-mL aliquot of the Test Preparation to a 100-mL volumetric flask, add the volume(s) of Standard Ion Solution(s) specified in the individual monograph, dilute with water to volume, and mix. Quantitatively dilute aliquots of this solution with water as necessary to bring the concentration of the ion to be determined into the proper range for the flame photometer used. Test Preparation- Unless otherwise
directed in the individual monograph, transfer 2.000 g of test specimen
to a 100-mL volumetric flask, chill in an ice bath, add-5 mL of nitríc
acid, swirl to dissolve and allow to warm to room temperature. Heat gently,
if necessary, to obtain a clear or just slightly turbid mixture. Cool to
room temperature, if necessary, dilute with water to volume and mix. Filter
or centrifuge if necessary, to obtain a clear solution.
The requirements of the test are
met if the value of T minus B is less than or equal to the value
of S minus T.
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