Hexachlorophene in Deodorants Spectrophotometric Method
First Action 1974
Final Action 1978
A. Apparatus
(a) Chromatographic equipment.—Insert 2 cm plug of glass wool in bottom of tube 55 cm long ´ 2.5 cm od with constricted tip 2.5 cm long and 8 mm od. Provide with brass tamper of diameter slightly smaller than id of tube, and fittings, including pressure gage,for applying pressure to top of column.
(b) Spectrophotometer.—Capable of isolating band £5 nm in region 220–360 nm.
B. Reagents
(a) Silanized Celite.—Weigh ca 700 g Celite 545 into 4 L beaker,add 3 L HCl (1 + 4), and stir thoroughly. Heat on steam bath several hours, stirring occasionally. Filter slurry through Büchner under vacuum and wash withH2Ountil washings are Fe- and Cl-free. Suck dry, transfer to beaker, and dry ca 15 h at 135°C. Transfer ca 150 g dried Celite to crystallizing dish, and let stand in air 30 min. In well-ventilated hood, pour 25 mL GE SC-77 Dri-Film (General Electric Co., 1 River Rd, Schenectady,NY12305, USA) into bottom of large glass desiccator. Place dish containing Celite on porcelain support in desiccator, and let stand in closed desiccator 4 h. Remove dish, and let stand in hood until residual HCl dissipates.
