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Tributyltin (TBT) has been used in marine antifouling paints for several years. Tributyltin has recently been demonstrated to be highly toxic to many types of shellfish at extremely low levels. This combination has led to a need for determining tributyltin [and its degradation products, dibutyltin (DBT) and monobutyltin (MBT)] in seawater.  

Bu3Sn+ X-

Tributyltin

 

Levels of tributyltin below one part per billion must be accurately identified and quantitated. WCAS has implemented a method for determining these compounds in seawater and marine sediments. The method consists of extracting the pollutants into tropolone/hexane, concentrating the extract, then reacting the organotins using a Grignard reagent to form tetraalkyltin derivatives. The derivatives are then easily separated and detected using gas chromatography with a flame  photometric detector (FPD).  

Tributyltin method development data indicate that we can achieve detection limits in water of 0.04 ppb for TBT, 0.05 for DBT and 0.2 for MBT. Detection limits in sediment are somewhat higher, ranging from 1 ppb for MBT down to 0.3 ppb for TBT. For a quotation...

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tributyltin analysis


TBT by GCMS,  1/8/2002

For additional specificity or confirmation of the GC results, one should consider analysis of the extracts by GCMS.  The mass spectrum, on the right, of hexyltributyltin was obtained in the full scan mode from a 6 ug/mL standard.  These ions represent the M-29 (-Et) and M-57 (-Bu), and show the isotopic pattern of Sn.

To improve sensitivity to that comparable to the GC-FPD analysis described above, selected ion monitoring (SIM) was used.  The chromatogram below shows the 263 ion for a 28.5 ug/L standard, equivalent to 57 ppt in a seawater sample.

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