Citation:

Robbins, Z., X. Liu, B. Schumacher, M. Smeltz, AND H. Liberatore. Method Development for Thermal Desorption-Gas Chromatography-Tandem Mass Spectrometry (TD-GC-MS/MS) Analysis of Trace Level Fluorotelomer Alcohols Emitted from Consumer Products. JOURNAL OF CHROMATOGRAPHY A. Elsevier Science Ltd, New York, NY, 1705:NA, (2923). https://doi.org/10.1016/j.chroma.2023.464204

Impact/Purpose:

The indoor environment is one of the primary pathways for exposure to per- and polyfluoroalkyl substances (PFAS) due to direct (i.e., skin contact or ingestion) or indirect exposures (i.e., inhalation of suspended particles and gases) to consumer products and building materials. While the United States Environmental Protection Agency (EPA) is rapidly expanding the scientific foundation for PFAS research and risk management in water, soils, sediments, biosolids, biota, and outdoor air, there are limited efforts devoted to understanding source, fate, and transport of vapor-phase PFAS in indoor air.  A TD-GC-MS/MS analytical method for trace level analysis of FTOHs in indoor air is needed to understand an important uncertainty in current exposure estimates attributed to emissions of PFAS from consumer products and building materials.  This work reports method development for TD-GC-MS/MS analysis of trace levels of fluorotelomer alcohols (FTOHs) emissions from consumer products as well as GC-MS/MS analysis of FTOHs in solid and liquid consumer products. The following FTOHs were selected for this study: 1H, 1H, 2H, 2H-perfluorohexan-1-ol (4:2 FTOH; CAS No. 2043-47-2), 1H, 1H, 2H, 2H-perfluorooctan-1-ol (6:2 FTOH; CAS No. 647-42-7), 1H, 1H, 2H, 2H-perfluorodecan-1-ol (8:2 FTOH; CAS No. 678-39-7), and 1H, 1H, 2H, 2H-perfluorododecan-1-ol (10:2 FTOH; CAS No. 865-86-1). Developed methods were evaluated by instrument detection limits (IDLs), quality assurance checks of target standards purchased from different vendors, TD sorbent tube stability and breakthrough, and standard solution storage stability. The TD-GC-MS/MS method was utilized to measure FTOH emissions from consumer products in micro chambers to determine their emission parameters. 

Description:

The scientific foundation for per- and polyfluoroalkyl substances (PFAS) measurements in water, soils, sediments, biosolids, biota, and outdoor air has rapidly expanded, however, there are limited efforts devoted to developing analytical methods to measure vapor-phase PFAS in indoor air. A gas chromatography-tandem mass spectrometry (GC-MS/MS) method coupled with thermal desorption (TD) sorbent tube analysis was developed to quantify trace levels of fluorotelomer alcohols (FTOHs) emitted from consumer products in the indoor environment. Method evaluation included determination of instrument detection limits (IDLs), quality assurance checks of target standards purchased from different vendors, sample loss during storage, and TD sorbent breakthrough with tubes coupled in-series. The IDLs for TD-GC-MS/MS analyses ranged from 0.07 – 0.09 ng/tube. No significant loss of FTOHs was observed during stability tests over 28 days with relative standard deviations (RSDs) of spiked TD tubes ranged from 3.1 – 7.7% and the RSDs of polypropylene copolymer vial storage of standard solutions ranging from 4.3 – 8.4%. TD tube breakthrough was minimal with recovered FTOHs in the second tubes <1% of the spiked concentrations in the first tubes with carrier gas volume up to 20 L. The method has been applied to determine FTOH emissions from three consumer products in micro chambers. A liquid stone cleaner/sealer product contained the highest levels of 6:2, 8:2, and 10:2 FTOHs, while the mattress pad products contained lower levels of 8:2 and 10:2 FTOHs. The emission parameters, including the initial emission factors and first order decay rate constants, were obtained based on the experimental data. The developed methods are sensitive and specific for analysis of all four target FTOHs with chamber testing. The methods can be extended to indoor air sampling and could be applicable to ambient air sampling.

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