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Journal Article 
Determination of organotin compounds in polyvinyl chloride products by GC 
Takami, K; Okumura, T; Yamasaki, H; Nakamoto, M 
Bunseki Kagaku / Analysis Chemistry
ISSN: 0525-1931 
Organotin compounds (OTC) in polyvinyl chloride (PVC) products were converted to their propyl derivatives and determined simultaneously with a GC apparatus equipped with a flame photometric detecor (FPD). A 0.1~1.0 g amount of a PVC sample was dissolved in 15 ml of tetrahydrofuran (THF) under refluxing condition for 1 h. The THF extract was made up 20 ml with THF. A 0.1~5 ml volume of the extract (containing below 5 jig of OTC) was mixed with a 2~5 ml volume of 2 M propylmagnesium bromide (PMB) THF solution and allowed to stand for 30 min. The excess PMB in the mixture was deactivated by adding 10 ml of 0.5 M sulfuric acid. The mixture was filtered, and the residue was washed twice with 5 ml of ethanol. The propyl derivatives (Rn-Pr4-nSn) in the combined filtrates, mixed with water, was extracted with hexane. The hexane extract was dehydrated with anhydrous sodium sulfate, filtered and concentrated to 5ml. An aliquot of the concentrated sample was analyzed by GC with FPD which was equipped with a 600-nm cut-on interference filter to monitor the tetraalkyltin compounds. GC conditions were as follows: column, Ultra-2 (crosslinked 5% phenyl methyl silicone gum, 0.32 mm i.d.×25m, df=0.52μm), column temp. = 70 °C(4 min)-4°C/min-240 °C, helium (2ml/min), injection and detection temp. = 260 °C, split ratio = 1/4. OTC in the PVC products were identified on the basis of retention times and determined by peak height method. Recoveries of OTC from a PVC resin product were 88.3~99.6% and relative standard deviations were 2.7~6.8%. The detection limits of OTC were 0.1 ng as their chloride. The limit of determination was 2μg/g, when 1 g of the resin was analyzed. © 1988, The Japan Society for Analytical Chemistry. All rights reserved. 
alkylation of organotin compounds with Grignard reagent; determination of organotin compounds by capillary GC; GC-flame photometric detection; polyvinyl chloride resin