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CCl3F 137.37

Methane, trichlorofluoro-.
Trichlorofluoromethane [75-69-4].
» Trichloromonofluoromethane contains not less than 99.6 percent and not more than 100.0 percent of CCl3F, calculated on the anhydrous basis.
Packaging and storage— Preserve in tight cylinders, and avoid exposure to excessive heat.
Identification— The IR absorption spectrum of it, determined in a 10-cm cell with sodium chloride windows, at atmospheric pressure, exhibits maxima, among others, at the following wavelengths, in µm: 4.67 (m), 5.95 (m), 7.28 (s), 8.06 (m), 9.2 (vs), 10.7 (vs), 11.8 (vs), and 13.4 (m). The stronger maxima are best obtained at pressures less than 10 mm of mercury.
Boiling temperature: approximately 24, determined as directed under Approximate Boiling Temperature (see Aerosols, Nasal Sprays, Metered-Dose Inhalers, and Dry Powder Inhalers 601).
Water: not more than 0.001%, determined as directed under Water Content (see Aerosols, Nasal Sprays, Metered-Dose Inhalers, and Dry Powder Inhalers 601and Method Ic under Water Determination 921).
High-boiling residues: not more than 0.01%, determined as directed for High-Boiling Residues, Method I, under Aerosols, Nasal Sprays, Metered-Dose Inhalers, and Dry Powder Inhalers 601.
Chromatographic purity— In the chromatogram recorded for the Assay, identify the peaks due to dichlorodifluoromethane and dichlorotetrafluoroethane from relative retention times observed on chromatographing the Resolution preparation: the sum of these two peak areas is not greater than 0.2% of the total of all peak areas; and the sum of the areas of all peaks other than that for trichloromonofluoromethane is not greater than 0.4% of the total of all peak areas.
Inorganic chlorides— Place 5 mL of anhydrous methanol in a test tube, add 3 drops of a saturated solution of silver nitrate in anhydrous methanol, shake, and add 7 g of Trichloromonofluoromethane: no opalescence or turbidity is produced.
Residual solvents 467: meets the requirements.
(Official January 1, 2007)
Resolution preparation and Chromatographic system—Proceed as directed in the Assay under Dichlorodifluoromethane.
Assay preparation— Introduce the liquid phase of Trichloromonofluoromethane into an evacuated headspace vial.
Procedure— Inject the gas phase headspace Assay preparation into the chromatograph, record the chromatogram, and measure the peak areas. Calculate the percentage (a/a) of CCl3F in the portion of Trichloromonofluoromethane taken.
Auxiliary Information— Staff Liaison : Daniel K. Bempong, Ph.D., Scientist
Expert Committee : (MDPS05) Monograph Development-Pulmonary and Steroids
USP29–NF24 Page 3451
Pharmacopeial Forum : Volume No. 27(1) Page 1825
Phone Number : 1-301-816-8143