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USP 35

Chemical Tests / 281 Residue on Ignition 151

CONTROL OF THE INSTRUMENTS PERFORMANCE

As the mercury porosimetry technique is considered as a comparative test, no details are given in this chapter. However, it is recommended that a stable comparison material should be tested on a regular basis to monitor instrument calibration and performance.vUSP35

Figure 2. Volumepressure curve as semilogarithmic plot.

REPORTING OF RESULTS
The pressure readings are converted to pore diameter by means of the Washburn equation or by another model. The surface tension of mercury, , depends not only on the temperature and the material, but alsoin the case of markedly curved surface areason the radius of curvature. In general, values between 0.41 N m1 and 0.52 N m1 are measured at room temperature. If the value is not known, = 0.48 N m1 can be used. The contact angle of mercury in most cases is more than 90. It may be determined using a contact angle instrument. If the value is not known, 130 can be used. Report the values of contact angle, surface tension, and the model used in the calculation. Visualization of the data can be done with several types of graphs. Frequently, in a graphical representation, the pore diameter is plotted on the abscissa and the dependent intruded specific volume on the ordinate to give the pore size distribution. It is appropriate here to choose a logarithmic scale for the abscissa (see Figure 3). The spaces between the particles of the solid sample are included as pores in the calculation. If the pores differ in size from the voids, the latter can be separated by choosing the relevant pore size range. Extrusion curves may not be used for calculating the pore size distribution (for hysteresis, see Figure 2), because an intruded part of the mercury always remains in the pore system. The retention ratio may be useful for the qualitative characterization of pores that are only accessible via narrow openings (ink-bottle pores). The most common characteristic values, such as the total intruded specific volume, the mean, and the median pore diameter are calculated from the pore size distribution. Moreover, sufficient information should be documented about the sample, the sample preparation, the evacuation conditions, and the instrument used.

271 READILY CARBONIZABLE SUBSTANCES TEST

In tests for readily carbonizable substances, unless otherwise directed, add the specified quantity of the substance, finely powdered if in solid form, in small portions to the comparison container, which is made of colorless glass resistant to the action of sulfuric acid and contains the specified volume of sulfuric acid (see under Reagent Specifications in the section Reagents, Indicators, and Solutions). Stir the mixture with a glass rod until solution is complete, allow the solution to stand for 15 minutes, unless otherwise directed, and compare the color of the solution with that of the specified Matching Fluid (see Color and Achromicity 631) in a comparison container, which also is of colorless glass and has the same internal and cross-section dimensions, viewing the fluids transversely against a background of white porcelain or white glass. When heat is directed in order to effect solution of the substance in the sulfuric acid, mix the sample and the acid in a test tube, heat as directed, and transfer the solution to the comparison container for matching with the designated Matching Fluid (see Color and Achromicity 631).

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 (33). 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. ProcedureIgnite 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 31 to 2 g of the substance, or3 the amount specified in the individual monograph, in the crucible.

Figure 3. Pore volume distribution as semilogarithmic plot.

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152 281 Residue on Ignition / Chemical Tests

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,3unless otherwise directed in the individual monograph,3 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, 3unless another temperature is specified in the individual monograph,3 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. 3Conduct 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.3

USP 35
mL of water. Transfer the solution with the aid of about 20 mL of water to a 150-mL beaker, and heat gently to the boiling temperature. Boil for 10 minutes, and allow the solution to cool to room temperature. ProcedureTreat the Standard Solution, the Test Solution, and the reagent blank consisting of 25 mL of dilute nitric acid (1 in 30) and 25 mL of water, concomitantly and in parallel, as follows. Add ammonium hydroxide solution (1 in 2) to adjust to a pH of 2.0 0.2. Dilute with water to 60 mL, and transfer to a low-actinic separator with the aid of 10 mL of water, adding the 10 mL of rinsings to the separator. Add 200 mg of hydroxylamine hydrochloride, swirl to dissolve, immediately add 5.0 mL of Diaminonaphthalene Solution, insert the stopper, and swirl to mix. Allow the solution to stand at room temperature for 100 minutes. Add 5.0 mL of cyclohexane, shake vigorously for 2 minutes, and allow the layers to separate. Discard the aqueous layer, and centrifuge the cyclohexane extract to remove any dispersed water. Determine the absorbances of the cyclohexane extracts of the Test Solution and the Standard Solution in a 1-cm cell at the wavelength of maximum absorbance at about 380 nm, with a suitable spectrophotometer, using the cyclohexane extract of the reagent blank as the blank, and compare the absorbances: the absorbance of the Test Solution is not greater than that of the Standard Solution where a 200-mg test specimen has been taken, or is not greater than one-half that of the Standard Solution where a 100-mg test specimen has been taken.

OTHER TESTS AND ASSAYS

301 ACID-NEUTRALIZING CAPACITY

291 SELENIUM
Stock SolutionDissolve 40.0 mg of metallic selenium in 100 mL of dilute nitric acid (1 in 2) in a 1000-mL volumetric flask, warming gently on a steam bath if necessary to effect solution, add water to volume, and mix. Pipet 5 mL of this solution into a 200-mL volumetric flask, add water to volume, and mix. Each mL of the resulting solution contains the equivalent of 1 g of selenium (Se). Diaminonaphthalene SolutionDissolve 100 mg of 2,3diaminonaphthalene and 500 mg of hydroxylamine hydrochloride in 0.1 N hydrochloric acid to make 100 mL. Prepare this solution fresh on the day of use. Standard SolutionPipet 6 mL of Stock Solution into a 150-mL beaker, and add 25 mL of dilute nitric acid (1 in 30) and 25 mL of water. Test SolutionClean combustion of the test material is an important factor in conducting the test. For compounds that burn poorly and produce soot, the addition of magnesium oxide usually results in more thorough combustion and reduces soot formation. Where the need to add magnesium oxide has been identified, it is specified in the individual monograph. Using a 1000-mL combustion flask and using 25 mL of dilute nitric acid (1 in 30) as the absorbing liquid, proceed as directed under Oxygen Flask Combustion 471, using a test specimen weighing 100 to 200 mg, unless directed otherwise in the individual monograph. Upon completion of the combustion, place a few mL of water in the cup, loosen the stopper, and rinse the stopper, the specimen holder, and the sides of the flask with about 10

NOTEAll tests shall be conducted at a temperature of 37 3. Standardization of pH MeterStandardize a pH meter using the 0.05 m potassium biphthalate and 0.05 m potassium tetraoxalate standardizing buffers as described under pH 791. Magnetic StirrerTransfer 100 mL of water to a 250-mL beaker containing a 40- 10-mm (or other suitable size) magnetic stirring bar that is coated with solid perfluorocarbon and has a spin ring at its center. Adjust the power setting of the magnetic stirrer to produce a stirring rate of 300 30 rpm when the stirring bar is centered in the beaker, as determined by a suitable optical tachometer. Test Preparation PowdersTransfer the accurately weighed portion of the substance specified in the individual monograph to a 250mL beaker, add 70 mL of water, and mix on the Magnetic Stirrer for 1 minute. Effervescent SolidsTransfer an accurately weighed quantity, equivalent to the minimum labeled dosage, to a 250mL beaker, add 10 mL of water, and swirl the beaker gently while allowing the reaction to subside. Add another 10 mL of water, and swirl gently. Wash the walls of the beaker with 50 mL of water, and mix on the Magnetic Stirrer for 1 minute. Suspensions and Other LiquidsShake the container until the contents are uniform, and determine the density. Transfer an accurately weighed quantity of the uniform mixture, equivalent to the minimum labeled dosage, to a 250-mL

Official from August 1, 2012 Copyright (c) 2012 The United States Pharmacopeial Convention. All rights reserved.