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J. Soc. Cosmet. Chem., 35, 207-220 (July 1984) Quantitation of anionic surfactants in aqueous systems via Fourier transform infrared spectroscopy MARIE SABO, JOHN GROSS, and IRA E. ROSENBERG, Clairol Incorporated, 2 Blachley Road, StamJ•rd, CT 06922. Received January 23, 1984. Synopsis An innovative sample cell, called a CIRCLE (Cylindrical Internal Reflectance Cell), for use in a Fourier transform infrared spectrometer (FTIR) has been tested for its applicability to quantitative anionic surfactant analyses in aqueous systems. Preliminary studies show excellent results for the quantitation of sodium lauryl sulfate, ammonium lauryl sulfate, sodium laureth sulfates, and alpha olefin sulfonate raw materials. In addition, a limited number of shampoo finished products containing these raw materials have been analyzed directly and, again, show excellent results. The distinct advantages of the FTIR procedure over the commonly employed mixed indicator titration method include no sample or reagent preparations, no subjective evaluations of end-points, and rapid analysis time. The use of computer-assisted spectral subtraction and the possibility of spectral storage on floppy disks are discussed. INTRODUCTION Presently, the quantitation of anionic surfactants is most commonly accomplished via a two-phase titration method. The Epton titration (1,2) employs methylene blue as the indicator while the Comit6 International des D6riv6s Tensio-actifs (CID) method (3,4) makes use of a mixed indicator, dimidium bromide/disulphine blue. This latter method is the ASTM standard test method. As with most visual titrations, the pro- cedures are tedious, the end-point determinations are somewhat subjective, and the precision of results may be poor. The use of infrared spectroscopy for qualitative identification of anionic surfactants has been reported (5,6), as has a method of quantitative analysis (7). The latter, however, required derivatization reactions prior to instrumental analysis in the infrared region. An innovative sample cell for use in a Fourier transform infrared spectrometer (FTIR) has prompted this investigation into its possible applicability to surfactant quantitation in aqueous systems. The cell, called a CIRCLE (Cylindrical Internal Reflectance Cell), is a multiple internal reflectance accessory which allows for the analysis of aqueous samples in the IR region. Five raw materials, sodium lauryl sulfate (SLS), ammonium lauryl sulfate (ALS), sodium lauryl ether sulfate (SLES- lEO), sodium lauryl di-ether sulfate (SLES-2EO), and sodium 2O7