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Method development for the determination of residual fluorotelomer raw materials and perflurooctanoate in fluorotelomer-based products by gas chromatography and liquid chromatography mass spectrometry
Authors:Larsen Barbara S  Stchur Peter  Szostek Bogdan  Bachmura Stanley F  Rowand Raymond C  Prickett Keith B  Korzeniowski Stephen H  Buck Robert C
Affiliation:DuPont Corporate Center for Analytical Sciences, Central Research and Development, Experimental Station, Wilmington, DE 19880, USA. barbara.s.larsen@usa.dupont.com
Abstract:The methodology for the determination of perfluorooctanoate (C(7)F(15)COO-, PFO), fluorotelomer alcohols (FTOHs: 6-2, 8-2, and 10-2), perfluorooctyl iodide (PFOI), and 8-2-8 fluorotelomer alcohol ester in complex fluorotelomer-based commercial products has been demonstrated and validated. Sample preparation procedures allowing determination of residual levels of these compounds were developed. The analytes were detected either by LC/MS/MS (PFO), LC/MS (FTOHs), or GC/MS (PFOI, 8-2-8 ester). The methods were validated by investigating the recoveries of analytes spiked at multiple levels to authentic sample matrices. The recoveries generally were between 70 and 130%. The limits of detection were in sub-microg/g range and the limits of quantitation were in the mug/g range. The methods were applied to fluorotelomer-based raw materials and fluorotelomer-based surfactants and polymeric products and represent methods useful for the determination of higher carbon chain length homologs as well.
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