Академический Документы
Профессиональный Документы
Культура Документы
USP 35
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.
Official from August 1, 2012 Copyright (c) 2012 The United States Pharmacopeial Convention. All rights reserved.
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.
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.