A new LC/MS method has been developed for the simultaneous measurement, in water and wastewater samples, of all species contained in commercial samples of linear type of alcohol ethoxylate (AE) surfactants including fatty alcohols. The method requires derivatization of the terminal hydroxyl of each surfactant species with 2-fluoro-N-methylpyridinium p-toluenesulfonate, which imparts a permanent cationic charge, allowing all species including the fatty alcohols and those with only one ethoxylate to be effectively detected by electrospray MS. Detection limits of typically <10 ppt for each individual species were attained in treated wastewater, in which total AE concentrations (combination of up to 114 individual species) are not expected to exceed 10 ppb. The method was validated for clean water as well as sewage influent and effluent samples.
A new thermospray liquid chromatography/mass spectrometry (LC/MS) method for quantitative determination of trace levels of alcohol ethoxylates (AE) in dilute aqueous environmental samples has been developed. This method has been validated for use in aquatic safety assessments to determine concentrations of total AE and individual AE species. This validation was accomplished by determination of recoveries of spiked AE samples from waste treatment plant effluents and receiving waters. The method distinguishes highly branched propylenebased AE from isomeric linear ethylene-based AE. Surfactants are used in large volumes in a broad variety of household and commercial detergents and cleaning products. After use, the surfactants are usually disposed into a wastewater treatment system and the effluents ultimately are released into surface waters. Biodegradation and other removal mechanisms greatly reduce the mass and concen-' Shell Development Co.
This report describes a method for obtaining the concentrations of the total and individual alcohol ethoxylate (AE) species in sewage treatment plant (STP) effluents by using electrospray liquid chromatography/mass spectrometry (LC/MS). This is a more advantageous method for quantitative analysis of AE in environmental matrices as compared with a previous thermospray LC/MS method. This new method is more sensitive, uses less solvents, utilizes a deuterated internal standard blend [C 13 D 27 O(CH 2 CH 2 O) n H, where n varies from 0 to 21 with an average of n = 9], which corresponds more closely to the AE, and it is a more robust instrumental technique. In this report, we document the results for validation of the electrospray LC/MS method by spike recovery of AE from STP effluent and influent samples. JAOCS 74, 765-773 (1997).
Reaction of [Pt 2 (-S) 2 (PPh 3) 4 ] with a number of transition metal iodo complexes leads to the formation of the cationic iodo analogue [Pt 2 (-S)(-I)(PPh 3) 4 ] + , identified using electrospray ionisation mass spectrometry (ESI MS). Synthetic routes to this complex were developed, using the reaction of [Pt 2 (-S) 2 (PPh 3) 4 ] with either [PtI 2 (PPh 3) 2 ] or elemental iodine. The complex was characterised by NMR spectroscopy, ESI MS and an X-ray structure determination, which reveals the presence of a planar, disordered {Pt 2 SI} + core. Monitoring the iodine reaction by ESI MS allows the identification of various iodine species, including the short-lived intermediate [Pt 2 (-S) 2 (PPh 3) 4 I] + , which allows a mechanism for the reaction to be proposed.
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