281 RESIDUE ON IGNITION
Portions of this general chapter have been harmonized with the corresponding texts of the European Pharmacopoeia and the Japanese Pharmacopoeia. The portions that are not harmonized are marked with symbols (). The harmonized texts of these pharmacopeias are therefore interchangeable, and the methods of the European Pharmacopoeia and/or the Japanese Pharmacopoeia may be used for demonstration of compliance instead of the present United States Pharmacopeia general chapter. These pharmacopeias have undertaken not to make any unilateral change to this harmonized chapter.
The Residue on Ignition / Sulfated Ash test uses a procedure to measure the amount of residual substance not volatilized from a sample when the sample is ignited in the presence of sulfuric acid according to the procedure described below. This test is usually used for determining the content of inorganic impurities in an organic substance.
Procedure Ignite a suitable crucible (for example, silica, platinum, quartz, or porcelain) at 600 ± 50 for 30 minutes, cool the crucible in a desiccator (silica gel or other suitable desiccant), and weigh it accurately. Weigh accurately 1 to 2 g of the substance, or the amount specified in the individual monograph, in the crucible.
Moisten the sample with a small amount (usually 1 mL) of sulfuric acid, then heat gently at a temperature as low as practicable until the sample is thoroughly charred. Cool; then,unless otherwise directed in the individual monograph, moisten the residue with a small amount (usually 1 mL) of sulfuric acid; heat gently until white fumes are no longer evolved; and ignite at 600 ± 50, unless another temperature is specified in the individual monograph, until the residue is completely incinerated. Ensure that flames are not produced at any time during the procedure. Cool the crucible in a desiccator (silica gel or other suitable desiccant), weigh accurately, and calculate the percentage of residue.
Unless otherwise specified, if the amount of the residue so obtained exceeds the limit specified in the individual monograph, repeat the moistening with sulfuric acid, heating and igniting as before, using a 30-minute ignition period, until two consecutive weighings of the residue do not differ by more than 0.5 mg or until the percentage of residue complies with the limit in the individual monograph.
Conduct the ignition in a well-ventilated hood, but protected from air currents, and at as low a temperature as is possible to effect the complete combustion of the carbon. A muffle furnace may be used, if desired, and its use is recommended for the final ignition at 600 ± 50.
Calibration of the muffle furnace may be carried out using an appropriate digital temperature meter and a working thermocouple probe calibrated against a standard thermocouple traceable to the National Institute of Standards and Technology.
Verify the accuracy of the measuring and controlling circuitry of the muffle furnace by checking the positions in the furnace at the control set point temperature of intended use. Select positions that reflect the eventual method of use with respect to location of the specimen under test. The tolerance is ±25 at each position measured.
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USP32NF27 Page 138Pharmacopeial Forum: Volume No. 31(5) Page 1526