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  • Evaluation of the mixed aggregate method as an alternative to the bismuth active substances and cobalt thiocyanate active substances procedures for the determination of nonionic surfactants in raw and treated sewage.

Evaluation of the mixed aggregate method as an alternative to the bismuth active substances and cobalt thiocyanate active substances procedures for the determination of nonionic surfactants in raw and treated sewage.

Journal of AOAC International (2002-03-07)
Encarnación Borrego, Dolores Sicilia, Soledad Rubio, Dolores Pérez-Bendito
ABSTRACT

The mixed aggregate (MA) method was evaluated for the routine determination of total ethoxylated nonionic surfactants in municipal raw and treated sewage. Nonionics in wastewater samples were enriched with a C8 solid-phase extraction cartridge, eluted with ethyl acetate-methanol, and separated from interferences with stacked strong anionic (quaternary ammonium form) and cationic (benzenesulfonic acid form) exchange columns. Sample extracts were evaporated to dryness and redissolved in distilled water. The total amount of ethoxylates, on a weight basis, was determined by measuring the critical micelle concentration of a mixed micelle made up of ethoxylates and the anionic surfactant sodium dodecyl sulfate, used as the reagent. The dye Coomassie Brilliant Blue G was used as a photometric probe. The minimum amount of ethoxylate required for a single determination was 1 microg. For raw sewage samples, mean recoveries and standard deviations were 98 +/- 6 and 98 +/- 4% at fortification levels of 0.3 and 0.6 microg/mL, respectively. For treated sewage samples, mean recoveries and standard deviations were 95 +/- 2 and 100 +/- 2% at fortification levels of 0.03 and 0.06 microg/mL, respectively. The MA method and the classical bismuth active substances and cobalt thiocyanate active substances procedures were compared. The former offers some significant advantages over the classical procedures in terms of sensitivity, selectivity, precision, simplicity, and rapidity; the type of response is independent of both the molecular weight and the chain length of the surfactant.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Cobalt(II) thiocyanate, 96%
Sigma-Aldrich
Cobalt(II) thiocyanate, 99.9% trace metals basis