- •1.1 Introduction
- •1.2 Sample preparation and clean-up procedures
- •1.2.1 Liquid-liquid extraction
- •1.2.2 Solid phase extraction
- •1.2.3 Purge and trap
- •1.2.5 Derivatization
- •1.2.6 Clean-up procedures
- •1.3 Instrumentation
- •1.3.1 Gas chromatography
- •1.3.1.1 Capillary columns
- •1.3.1.2 Sample introduction systems
- •1.3.2 High performance liquid chromatography
- •1.3.2.1 Hplc columns
- •1.3.2.2 Hplc detectors
- •Volatile organic compounds
- •2.1 Introduction
- •2.2 Compounds
- •2.3 General Procedure
- •2.4 Sensitivity
- •3.1 Introduction
- •3.2 Compounds
- •3.3 General Procedure
- •3.4 Sensitivity
- •3.5.1 Procedure 1: Solid phase extraction/cgc/ms
- •4.1 Introduction
- •4.2 Compounds
- •4.3 General Procedure
- •4.4 Sensitivity
- •4.5 Detailed Procedures
- •4.5.1 Procedure 1: pah analysis using hplc (epa 550.0)
- •5.1 Introduction
- •5.2 Compounds
- •5.3 General Procedure
- •5.4 Sensitivity
- •6.1 Introduction
- •7.1 Introduction
- •7.2 Compounds
- •7.3 General Procedure
- •9.1 Introduction
- •9.3 General Procedure
- •9.4 Sensitivity
- •9.5 Detailed Procedures
- •9.5.1 Procedure 1: Tropolone extraction/cgc/aed or cgc/ms
- •10.1 Introduction
- •10.2 Compounds
- •10.3 General Procedure
- •10.4 Sensitivity
- •10.5 Detailed Procedures
- •11.1 Introduction
- •12.1 Introduction
- •12.2 Compounds
- •13.1 Introduction
- •100-90-80-70-60 50 40 30 20-10-0-
- •20 30 40
- •Iceland
- •Ireland
9.1 Introduction
The analysis of mono-, di-, tri- and tetra-alkylated organotin compounds in environmental samples is becoming increasingly important.
The EC priority pollutants list contains eight organotin compounds which can be analysed after derivatization by capillary gas chromatography/atomic emission detection (CGC/AED) or capillary gas chromatography/mass spectroscopy (CGC/MS). The methods described are applicable for the analysis of organo-metallic micropollutants in general e.g. organolead, organomercury and organo-arsenic compounds.
9.2 Compounds |
|
|
Methyltin trichloride |
Tributyltin oxide |
(EC) |
Dimethyltin dichloride |
Tributyltin salts |
|
Trimethyltin chloride |
Tetrapropyltin |
|
Tripropyltin chloride |
Tetrabutyltin |
(EC) |
Dipropyltin dichloride |
Tetrapentyltin |
|
Butyltin trichloride |
Triphenyltin acetate |
(EC) |
Dibutyltin dichloride (EC) |
Triphenyltin chloride |
(EC) |
Dibutyltin oxide (EC) |
Triphenyltin hydroxide |
(EC) |
Dibutyltin salts (EC) |
|
|
(EC): Included on the European Community Priority Pollutants |
list. |
9.3 General Procedure
Water is acidified and extracted with a complexing agent, such as a tropolone or a sodium diethyl dithiocarbamate (NaDDTC) solution. The organotin compounds are derivatized to the tetra-alkyl compounds with a Grignard reagent and are analysed by CGC/AED at the 303.4 nm tin emission line or by CGC/MS operated in the ion monitoring mode.
Organotin Compounds 9 187
The following abbreviations are used for the organotin derivatives*:
Derivatization
with PeMgBr (b)
Derivative Abbreviation
Methyltin trichloride Dimethyltin dichloride Trimethyltin chloride Dipropyltin dichloride Tripropyltin chloride Butyltin trichloride Dibutyltin dichloride Dibutyltin oxide Dibutyltin salts Tributyltin oxide Tributyltin salts Tetrapropyltin Tetrabutyltin Tetrapentyltin Triphenyltin acetate Triphenyltin chloride Triphenyltin hydroxide
Derivatization with MeMgBr (a) Derivative Abbrevation
Tetramethyltin |
TeMT |
Methyltripentyltin |
MMT |
Tetramethyltin |
TeMT |
Dimethyldipentyltin |
DMT |
Tetramethyltin |
TeMT |
Trimethylpentyltin |
TMT |
Dipropyldimethyltin |
DPrT |
Dipropyldipentyltin |
DPrT |
Tripropylmethyltin |
TPrT |
Tripropylpentyltin |
TPrT |
Butyltrimethyltin |
МВТ |
Butyltripentyltin |
МВТ |
Dibutyldimethyltin |
DBT |
Dibutyldipentyltin |
DBT |
Dibutyldimethyltin |
DBT |
Dibutyldipentyltin |
DBT |
Dibutyldimethyltin |
DBT |
Dibutyldipentyltin |
DBT |
Tributylmethyltin |
TBT |
Tributylpentyltin |
TBT |
Tributylmethyltin |
TBT |
Tributylpentyltin |
TBT |
Tetrapropyltin |
TePrT |
Tetrapropyltin |
TePrT |
Tetrabutyltin |
TeBT |
Tetrabutyltin |
TeBT |
Tetrapentyltin |
TePT |
Tetrapentyltin |
TePT |
Triphenylmethyltin |
TPhT |
Triphenylp entyltin |
TPhT |
Triphenylmethyltin |
TPhT |
Triphenylpentyltin |
TPhT |
Triphenylmethyltin |
TPhT |
Triphenylpentyltin |
TPhT |
(a): methylmagnesium bromide (b): pentylmagnesium bromide
* abbreviations used in literature, mostly no information on R of the Grignard reagent.
Figure 9.1: Organotin compounds.
188
9 Organotin compounds