A method for the determination of nonionics ill low eoncn (0-20 ppm) has been developed. This method is based on the formation of a blue complex between ammonium cobaltothiocyanate reagent and a polyethoxylated compound. This complex is extracted into benzene ~rom a saturated salt solution and measured with a spectrophotometer at 320 m~. The absorbance reading is compared to a standard.The method requires only a single extraction and no prelbninary cohen step is necessary. It is sensitive to polyethoxylated compounds containing three or more moles of ethylene oxide. We have used this method to detect as little as 0.01 mg of nonionic in 100 ml of sample (0.1 ppm). Reaction conditions, sensitivity differences between compounds, interferences and suitability for use in biodegradation studies have been investigated. The accuracy and repeatability of this method is ±3% relative at 20 ppm eoncn.
The structural analysis of micro quantities of alkyl aryl sulfonates by presently known chemical and spectroscopic techniques has been an exceedingly difficult task. The formidable nature of such analyses is due largely to the essential nonvolatility of the sulfonates, a fact which precludes the application of gas‐liquid chromatography and mass spectrometric techniques.
The present paper describes an approach wherein gas chromatography is made applicable to analysis of micro quantities of sulfonates. The key to the approach is a microchemical desulfonation procedure. This process yields the parent hydrocarbon, which is volatile and hence amenable to analysis by gas‐liquid chromatography and mass spectrometry.
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