A headspace GC/MS analysis method for the simultaneous determination of residual vinyl chloride (VC) and vinylidene chloride (VDC) in polyvinyl chloride (PVC) and polyvinylidene chloride (PVDC) products was developed. A test sample was swelled overnight with N,Ndimethylacetamide in a sealed vial. The vial was incubated for 1 hour at 90ΐ, then the headspace gas was analyzed by GC/MS using a PLOT capillary column. The recoveries from spiked PVC and PVDC samples were 90.0ῌ112.3 for VC and 85.2ῌ108.3 for VDC. The determination limits were 0.01 mg/g for VC and 0.06 mg/g for VDC, respectively. By this method, VC was detected in two PVC water supply pipes at the levels of 0.61 and 0.01 mg/g. On the other hand, VC and VDC were not detected in any of the food container-packages or toys tested.
Organotin compounds in polyvinyl chloride toys were determined by GC/MS after ethyl derivatization with sodium tetraethylborate. The samples were 12 balls, 12 soft toys, 10 food toys and 13 face masks for children.Monooctyltin, dioctyltin and trioctyltin compounds were found in all face masks at the levels of 74.8ῒ917 mg/g, 474ῒ3,960 mg/g and 1.0ῒ213 mg/g, respectively. They also were detected in 6 balls, 4 soft toys and 1 food toy. Monomethyltin and dimethyltin compounds were found in 8 face masks at the levels of 40.9ῒ227 mg/g and 222ῒ1,450 mg/g, respectively. Monobutyltin and dibutyltin (DBT) compounds were found in 1 ball, 3 food toys and 5 face masks. In particular, 1 ball and 4 face masks contained toxic DBT at the levels of 527ῒ999 mg/g.
A simultaneous determination method for 9 organotin compounds in polyvinyl chloride (PVC) and silicone products used as kitchen utensils and food packages was developed using ethyl derivatization with sodium tetraethylborate (NaBEt 4). Organotin compounds were extracted with acetoneῌhexane (3 : 7) from the samples after acidification and the extract was filtered and concentrated at under 40. After centrifugal separation, these compounds were derivatized with 2 NaBEt 4 solution and determined by GC/MS. This method was applicable for simple routine analysis. Recoveries of spiked compounds were 49.1ῑ118.1 for 3 PVC products and 88.8ῑ 102.2 for a siliconized paper. Monooctyltin, dioctyltin and trioctyltin compounds were found in all PVC food containers at the levels of 123ῑ1,380 mg/g, 1,770ῑ13,200 mg/g and 6.6ῑ139 mg/g, respectively. They also were found in 3 gloves, 5 spouts, 1 hose and 5 pipes. Some PVC products contained monomethyltin, dimethyltin, trimethyltin, monobutyltin and dibutyltin compounds at the levels of 97.3ῑ433 mg/g, 96.5ῑ5,120 mg/g, 8.5ῑ24.9 mg/g, 1.2ῑ852 mg/g and 1.2ῑ29.4 mg/g, respectively.
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