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Reagents
suitable grade. The intent is that a suitable reagent grade agents in such solvents and of such definite concentrations
available commercially shall be used. as to be suitable for the specified purposes.
Occasionally, additional test(s) augment the designation 4.6 Volumetric Solutions (VS): Volumetric solutions are
suitable grade, as indicated in the text. Listed also are solutions of reagents of known concentration intended pri-
some, but not all, reagents that are required only in deter- marily for use in quantitative determinations.
mining the quality of other reagents. For those reagents
that are not listed, satisfactory specifications are available in 4.7 Water: As elsewhere in the U.S. Pharmacopeia, where
standard reference publications. water, without qualification, is mentioned in the tests for
reagents or in directions for preparing any solutions, Purified
1.3 USP or NF or FCC Grade Water (USP monograph) is always to be used.
In the instances in which a reagent required in a U.S.
Pharmacopeia or National Formulary test or assay meets the 4.7.1 CARBON DIOXIDE-FREE WATER: It is Purified Water that
requirements in the monograph for that article appearing in has been boiled vigorously for 5 min or more and allowed
this U.S. Pharmacopeia or the National Formulary or the cur- to cool while protected from absorption of carbon dioxide
rent edition of the Food Chemicals Codex (FCC), it suffices to from the atmosphere, or Purified Water that has a resistivity
refer to the corresponding monograph in one of the these of NLT 18 Mohm-cm.
three compendia. In such cases it is to be understood that 4.7.2 DEAERATED WATER: For purposes other than dissolu-
the specifications are minimum requirements and that any tion and drug release testing, it is Purified Water that has
substance meeting more rigid specifications for chemical pu- been treated to reduce the content of dissolved air by suita-
rity is suitable. ble means, such as by boiling vigorously for 5 min and cool-
ing or by application of ultrasonic vibration.
4.7.3 PARTICLE-FREE WATER: It is water that has been passed
2. PACKAGING AND STORAGE through a suitable filter of 0.22-m pore size.
Reagents and solutions should be preserved in tight con- 4.7.4 ORGANIC-FREE WATER: It is Purified Water that pro-
tainers made of resistant glass or other suitable material. duces no significantly interfering peaks when chromato-
Directions for storage in light-resistant containers should be graphed as indicated in Residual Solvents 467, Identification,
carefully observed. Control, and Quantification of Residual Solvents.
Stoppers and stopcocks brought into contact with sub-
stances capable of attacking or penetrating their surfaces 5. CHROMATOGRAPHIC SOLVENTS AND
may be given a protective coating of a thin film of a suita-
ble lubricant unless specifically interdicted. CARRIER GASES
The chromatographic procedures set forth in the U.S.
Pharmacopeia may require use of solvents and gases that
have been especially purified for such use. The purpose may
be (a) to exclude certain impurities that interfere with the
proper conduct of the test procedure, or (b) to extend the pressure or other chromatographic uses are available as spe-
life of a column by reducing the buildup of impurities on cialty products from various reagent supply houses, al-
the column. Where solvents and gases are called for in though there is no assurance that similar products from dif-
chromatographic procedures, it is the responsibility of the ferent suppliers are of equivalent suitability in any given
analyst to ensure the suitability of the solvent or gas for the procedure.
specific use. Solvents and gases suitable for specific high-
Reagents
1. DEFINITIONS PROCEDURE: Place the distilling flask in an upright posi-
tion in the perforation in the asbestos board, and connect it
1.1 Blank to the condenser.
A blank consists of the same quantities of the same re- Measure 100 mL of the liquid to be tested in a graduated
agents treated in the same manner as the specimen under cylinder, and transfer to the boiling flask together with
test. some device to prevent bumping. Use the cylinder as the
receiver for the distillate. Insert the thermometer, and heat
1.2 Control so as to distill at the rate of 35 mL/min. Make a preliminary
A control is a blank to which has been added the limiting trial, if necessary, to determine the adjustment for the
quantity of the substance being tested for, or is a specified proper rate of heating. Read the thermometer when about
comparison solution prepared as directed in the particular 20 drops have distilled and thereafter at volumes of distillate
test. of 5, 10, 40, 50, 60, 90, and 95 mL. Continue the distilla-
tion until the dry point is reached.
2. DESCRIPTION OF THE REAGENT ENTRY The Boiling or Distilling Range is the interval between the
temperatures when 1 mL and 95 mL, respectively, have dis-
See Figure 1. tilled.
6.2 Amino Nitrogen Test in Reagents
Determine the percentage of loss on drying of the sample
3. VISUAL COMPARISONS in appropriate conditions. Transfer about 500 mg of the
sample to a 100-mL beaker. Add 20 mL of water. Adjust the
For color and turbidity comparisons, proceed as directed pH potentiometrically with 0.1 N hydrochloric acid or 0.2 N
in Spectrophotometry and Light-Scattering 851, Visual Com- sodium hydroxide to 6.0. Add 10 mL of formaldehyde solu-
parison. The tubes used in this procedure are frequently tion. Titrate the solution potentiometrically with 0.2 N so-
called Nessler tubes. dium hydroxide to a pH of 9.0. Calculate the percentage of
In making visual comparisons of the densities of turbid amino nitrogen:
fluids, compensate for difference in color, if necessary, by
viewing the turbidity through a column of water, the depth
of which is determined by the volume specified in the indi-
Reagents