Am. Caricchia et al., ANALYTICAL METHODS FOR THE DETERMINATION OF ORGANOTINS IN THE MARINE-ENVIRONMENT, International journal of environmental analytical chemistry, 53(1), 1993, pp. 37-52
Analytical procedures for the determination of organotin compounds in
sea water, sediments and mussels have been adopted in our laboratory,
intercomparison/certification exercises with other European laboratori
es giving satisfactory results. The characteristics of the different m
ethodologies are discussed, the balance between practical and analytic
al aspects leading to the selection of the following procedures. For w
ater samples two alternative extraction techniques are used: liquid/li
quid extraction (0.3% tropolone in methylene chloride) or liquid/solid
extraction (C18- or Carbopack B-loaded extraction tubes). Solid-phase
extraction ensures good results and is more suitable in the field, av
oiding high volumes of organic solvents and transport of fragile glass
ware. Extraction tubes can be easily stored, and problems with the tra
nsfer of whole samples to the laboratory, and storage and conservation
problems are prevented. For sediments and mussels, sonication (0.05%
tropolone in methanol) can be used as the extraction procedure. Final
detection is performed by GC (FPD or MS detection) after pentylation.
GC-MS is generally necessary to confirm doubtful results in highly pol
luted sediments, particularly if high sulphur levels are present. AAS
can be used as an alternative detection technique after selective elut
ion from the solid-phase tubes without any derivatization. The detecti
on limits are in the low-ppt range for water samples and in the low-pp
b range for sediments and mussel samples, with a precision generally b
etter than 10% for water samples and better than 15% for sediments and
mussels.