Comparison of Derivatization Methods for the Determination of Butyl- and Phenyl-tin Compounds in Mussels by Gas Chromatography

Abstract

Two different derivatization methods, alkylation with Grignard reagents, and ethylation with sodium tetraethylborate, were compared for the determination of organotin compounds, viz. tributyltin, dibutyltin, monobutyltin, triphenyltin, diphenyltin and monophenyltin, in mussel samples. Temperature, reaction time and concentration of Grignard reagents were optimized in the former method; in the latter the effect of pH, concentration of sodium tetraethylborate and reaction time were studied. In the derivatization with Grignard reagents hexyl, pentyl, propyl, ethyl and methyl were used as alkyl Grignard groups. A critical evaluation of the different derivatization methods is presented. © 1997 John Wiley & Sons, Ltd.

Trace Metal Speciation with ICP‐MS Detection

“…Extraction and derivatisation can be accomplished simultaneously or sequentially, as described in the following sections. The derivatisation techniques most often applied are hydride generation with NaBH 4 , ethylation with NaBEt 4 or Grignard alkylation, 271 and were recently reviewed by Morabito et al 272 An old, yet still very popular method is hydride generation 213 using NaBH 4 solution and simultaneous purging and cryotrapping of the volatilised compounds. This method can be applied to a wide range of elements (As, Ge, Se, Cd, Sn, Sb, Te, Hg, Pb, Bi), and has often been employed for the determination of methylated species of arsenic, germanium, tin and antimony.…”

“…198 After leaching or extraction from the solid, organotin species can be readily derivatised with NaBEt 4 and extracted into an organic solvent for GC-ICP-MS injection. 60,197,198,270,271 Detection limits in the lower fg level (absolute) are obtained.…”

Contaminação ambiental por compostos organoestânicos

“…A adição de grupos hexila e pentila têm a vantagem de proporcionar compostos derivados com volatilidade relativamente baixa, o que facilita a etapa de pré-concentração (que geralmente é feita por evaporação com fluxo de N 2 ), além de serem compostos que ainda não foram introduzidos no ambiente. O tempo de reação, a temperatura e a agitação da amostra durante a reação não afetam os produtos da derivação 68 .…”

A Simple Method for the Speciation of Organotin Compounds in Water Samples Using Ethylation and GC-QFAAS

“…However, the yield and reproducibility of the hydridization of phenyltins is low and losses of the analytes could occur [20]. Grignard derivatization yields are generally higher for all organotins [13,21], although this was also questioned in the literature [5]. However, this derivatization procedure is complex and time consuming and analyte losses could occur during these steps [20].…”

“…It appears to be more robust and accurate for extraction from environmental samples and the ethylated products can be analyzed directly by GC equipment (as opposed to hydridization using NaBH 4 ). However, lower derivatization ef®ciencies were generally obtained in real samples [21], thus a careful optimization step is often required.…”