A gas chromatography/mass spectrometry (GC/MS) method by a solid-phase adsorption/liquid extraction has been used for the determination of phthalates in indoor air. Round robin tests using this method for eleven phthalates such as dimethyl phthalate (DMP), diethyl phthalate-d
4 (DEP-d
4), di-
n-propyl phthalate (DPrP), di-
n-butyl phthalate (DnBP), di-
n-butyl phthalate-d
4 (DnBP-d
4), di-
n-pentyl phthalate (DPnP), dihexyl phthalate (DHxP), benzyl-
n-butyl phthalate-d
4 (BnBP-d
4), dicyclohexyl phthalate (DcHP), di- (2-ethylhexyl) phthalate (DEHP), and di- (2-ethylhexyl) phthalate-d
4 (DEHP-d
4), and the related compound such as di- (2-ethylhexyl) adipate-d
8 (DEHA-d
8) were conducted by 16 laboratories.
Three kinds of test samples were analyzed by each laboratory: a) hexane solution (sample A) of the phthalates, b) an adsorbent (sample B) to which hexane solution of the phthalates was directly added, c) an adsorbent (sample C) through which a 300l volume of air was passed after addition of hexane solution of the phthalates. The phthalates were extracted from the adsorbents by 2 ml of dichloromethane after addition of fluoranthene-d
10 as an internal standard and then determined by the gas chromatography/mass spectrometry (GC/MS) .
Three phthalates, DMP, DnBP and DEHP, were detected in the solvent and blank samples and thus the one third of their data was not considered. The intra-laboratory relative standard deviations (RSDs) of the values for sample A were less than 10% except for DnBP and DEPH. Their inter-laboratory RSDs were in the range of 7.0-40% except for DEPH and increased with the increase of molecular weight of the phthalates. The intra- and interlaboratory RSDs of the values for sample B were in the range of 5.0-17% and 15-45%, respectively. The intra- and inter-laboratory RSDs of the values for sample C were in the range of 5.0-12% and 15-50%, respectively.
These results indicated that the nine phthalates including their deuterated derivatives except for DMP, DnBP and DEPH could be determined precisely by using this method. It should be noted to pay precious attention for analysis and pretreatment of DMP, DnBP and DEPH because of their serious contamination and the possibility of matrix effect extracted from the adsorbent on column separation.
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