Determination of thiodyglycol in groundwater using solid-phase extraction followed by gas chromatography with mass spectrometric detection in the selected-ion mode.
A highly sensitive analytical procedure is described for determining thiodiglycol in groundwater. Samples are initially fortified with 3,3'-thiodipropanol (surrogate), then both species are extracted using sequential solid-phase extraction with both C18 and Ambersorb 572 columns. The C18 column, which removes extraneous groundwater components, is discarded; the Ambersorb 572 column is dried thoroughly before eluting polar components with a small volume of dichloromethane. The extract is taken to dryness using dry flowing nitrogen, and the resulting residue is derivatized using N-(tert.-butyldimethylsilyl)-N-methyltrifluoroacetamide and pyridine. The derivatized products are diluted to a final volume with toluene, chromatographed using a fused-silica capillary column, and detected with a quadrupole mass spectrometric detector in its selected-ion mode. Two independent, statistically unbiased, procedures were used to evaluate the detection limits for thiodiglycol; the values ranged between 4 and 16 microg(-1) groundwater.
Chemical and Analytical Sciences Division, Oak Ridge National Laboratory, TN 37831-6120, USA.  tomkinsba@ornl.gov
B A
BA
Tomkins
G A
GA
Sega
D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity; D013438:Sulfhydryl Compounds / Q000032:analysis*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D013438:Sulfhydryl Compounds; D014874:Water Pollutants, Chemical; C047519:2,2'-thiodiethanol