Determination of organotin compounds by headspace solid-phase microextraction–gas chromatography–pulsed flame-photometric detection (HS-SPME–GC–PFPD)

Abstract

A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 mum PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L(-1) in water and close to ng (Sn) kg(-1) in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices.

Experimental design for TBT quantification by isotope dilution SPE–GC–ICP–MS under the European water framework directive

“…Such approach was especially interesting to not lose the information concerning the two phases, NH 2 /C18 and SCX, whose data were mostly unusable for model development. Therefore, to include in data treatment the information associated with the experiments previously excluded (n. 3,6,8,14,15,20,23,24,25,27,32,33), we have defined another way to express the results, the "blank to signal" …”

“…The DOE allowed to evaluate many experimental conditions, with less experimental work and with a structured approach. Experimental design methodology was successfully used for analysis of OTC to optimize the conditions affecting the headspace solid-phase microextraction in ultra-pure water [22], sediments [23], fish and natural waters [24] [25].…”

“…The phase NH 2 /C18 with both elution solvents (CH 2 Cl 2 and THF) was always associated with the presence of blanks significantly higher than the blank average. The SCX phase was involved in 7 experiments(10,12,16,23,25,27,35): the mixture 0.3 M NH 4 Cl in MeOH/HAc/H 2 O…”

Study of Ruggedness Hs-Spme Procedure for Organotin Analysis by Gc-PFPD

“…However, in order to obtain reliable results for simultaneous determination of volatile and semi-volatile organotins the application of at least two internal standards for SPME in headspace mode appears as mandatory 12 . In this study, Tripropyltin (TPrT) and Diheptyltin (DHepT) were used as internal standards for volatile (Monobutyltin-MBT, Dibutyltin-DBT, TBT and Monophenyltin-MPhT) and semi-volatiles compounds (Diphenytin-DPhT and TPhT), respectively.…”

Evaluation of Microwave-Assisted Extraction for Organotin Determination in Vegetal and Soil Matrices

“…In general, the performance of several analytical methods has been evaluated for the determination of the OTC in environmental samples. Methods based on a derivatization step with sodium tetraethylborate (NaBEt 4 ), a preconcentration using a liquid-liquid extraction (LLE) with isooctane, followed by gas chromatography (GC) and pulsed flame photometric detection (PFPD) have been widely studied, proving them suitable for the determination of OTC in environmental matrices [16][17][18][19][20]. Nevertheless, prior to the analysis, the OTCs must be extracted from the solid matrix.…”