Fluorinated compounds constitute a diverse class of chemicals which have been globally manufactured since the 1950s and continue to be in use today. These compounds are the most commonly studied per- and polyfluoroalkyl substances (PFASs)/perfluorinated chemicals (PFCs) due to their widespread occurrence in the environment, including in human blood and remote arctic wildlife. Perfluoroalkyl acids (PFAAs) are the most studied of the PFASs/PFCs thanks to their historic widespread use and recently discovered bioaccumulation properties. The occurrence of PFAAs can arise from direct commercial use, but also from the degradation of precursor substances (i.e. PFAA-precursors). During the past 12 years, new sources for PFAA and PFAS compounds have been identified in the form of: 1) existing fluorinated compounds that may transform to PFAA/PFAS, and; 2) manufacturers’ replacement of older products with the introduction of novel fluorinated compounds that may degrade to produce PFAA/PFAS. Staying abreast of these changes requires methods that can measure per- and highly fluorinated compounds in all matrices relevant to the environment and potential bioaccumulation.
For the past decade, AXYS has helped clients with best-in-class analyses to measure PFAA compounds such PFOS and PFOA. Over time, AXYS has developed the broadest capabilities in isotope dilution quantification of a wide range of PFCs and fluorotelomer alcohols in multiple matrices including water, whole blood, serum, tissues and solid phase media (e.g. XAD beads).
AXYS’ newly expanded per- and polyfluorinated methods now include solid and aqueous methods for fluorotelomer sulfonates (FTSs), polyfluoroalkyl phosphoric acids (PAPs) and esters; and precursors, including perfluorooctane sulfonamides (PFOSAs) and fluorotelomer acids (FTAs). These compounds may produce PFAA or other PFAS compounds, or in some cases may require study themselves.
Perfluorinated carboxylates (PFCA) and sulfonates (PFSA) belong to larger classification of man-made chemicals and their precursors that are resistant to environmental breakdown and are pervasively present in the air, water, biota, and humans, called perfluorinated compounds (PFCs). The most studied PFCs are perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS), which are subject to emerging regulations for allowable levels in drinking water and fish, as well as existing restrictions on their manufacture and use.
In 2002, AXYS began tissue analysis for PFCs using in-house developed methods and LC-MS/MS and now offers isotope-dilution quantification for a broad range of PFCs and fluorotelomer alcohols (FTAs) in multiple matrices including water, whole blood, serum, tissues and solid phase media (e.g. XAD beads). The first nationally accredited Canadian commercial lab for PFC analysis, AXYS heads the forefront of commercial North American environmental analysis of PFCs.
Fluorotelomer sulfonates (FTS) are often observed at elevated concentrations at sites of aqueous film-forming foam (AFFF) application. Fluorotelomer sulfonate-based surfactants have mostly replaced PFOS -based surfactants in AFFF applications making measurement of FTS relevant.
AXYS has recently developed new methods for the quantitative analysis of FTSs in solid and aqueous matrices, including specific handling protocols for high-level samples which are common around AFFF-discharge sites.
Perfluorooctane sulfonamides (PFOSAs) are fluorinated compounds used either as surfactants or precursor compounds in the manufacture of fluorinated polymers. PFOSA was used extensively in North America as a surfactant before phase-out in 2000, but it is still manufactured in other parts of the world. PFOSA is bioaccumulative, and can also convert to PFOS via degradation in the environment, as well as via in vivo & in vitro biotransformation.
AXYS provides LC-MS/MS analysis for PFOSA and other select perfluorinated sulfonamides in a variety of matrices including water/effluent, soil/sediment/biosolids, tissue, serum, and urine.
Per- and polyfluoroalkyl precursors comprise a set of sulfonamide acetic acid (FOSAA), fluorotelomer carboxylic acids (FTCA) and fluorotelomer unsaturated carboxylic acids (FTUCA). They can transform to perfluorinated acids in the environment.
AXYS offers methods to measure per- and polyfluoroalkyl precursors in aqueous, effluent, soil and biosolid matrices by LC-MS/MS.
AXYS was the first nationally accredited Canadian commercial lab for PFC analysis and is NELAC accredited for PFC analysis in Florida, Minnesota and New Jersey. AXYS specializes in measurement of PFCs to low nanogram concentrations from standard sample sizes. Our specialized sampling and analytical procedures may allow for much lower detection limits and reduced sample sizes in human and sediment matrices.
Method AXYS Method ID Description Perfluorinated acids MLA-102 (high level water samples) Analytes of interest include 13 PFCs. This direct-injection method is suitable for characterization of contaminant spread in sites affected by use of aqueous film-forming foams (AFFF). Perfluorinated acids MLA-103 (low level water samples) Suitable for analysis of 13 PFCs in whole aqueous samples with low particulate content. Perfluorohexanoic acid (PFHxA) and Perfluoro [2-(2- methoxy-propoxy) propanoate] (PMPA) MLA-096 (Aqueous) This method can be used in conjunction with AXYS methods MLA-060 and MLA-081 for determination of PFCs and fluorotelomer sulfonates (FTS) in aqueous samples. Perfluoroalkyl acids (PFAAs) MLA-060 (Aqueous, including AFFF impacted groundwater), MLA-041 (Solid), MLA-043 (Tissue), MLA-042 (Serum), MLA-071 (Urine), MLA-076 (Air) 13 PFAAs from C4 to C12, including PFOA and PFOS. Level of detection is low ppt to low ppb. Fluorotelomer sulfonates (FTSs) MLA-081 (Aqueous), MLA-089 (Solid) Analysis of 3 FTS compounds. The level of detection is in the low ppb range. Perfluoroalkyl acid (PFAA) precursors MLA-094 (Aqueous), MLA-095 (Solid) Analysis of 9 Perfluorooctane sulfonamides (FOSAMs) and Fluorotelomer acids (FTAs). The level of detection is in the sub-ppb to low ppb range. Polyfluoroalkyl phosphate esters (PAPs) MLA-085 (Effluent), MLA-093 (Solid) Analysis of 10 phosphonate, phosphinate, monoPAP and diPAP compounds. The level of detection is in the low to mid ppb range.
AXYS has been performing analysis of per- and polyfluorinated substances since 2001. Notable clients include the US EPA, USGS, Environment Canada, Minnesota Pollution Control Agency, San Francisco Estuary Institute and Delaware River Basin Commission, among others. AXYS performs thousands of PFAS analyses a year in solid, aqueous, tissue, serum and air matrices. Some project examples:
Supporting Great Lakes AOC Investigations
AXYS provided analysis for the Great Lakes Area of Concern Investigation, including ambient water, high-volume sampling, precipitation, fish and sediment samples. Axys tested for PAHs, Dioxins, PCBs, OC pesticides including chlorobenzenes, current use pesticides (OC, ON, OP, triazine, pyrethroids), perfluorinated compounds, PBDPE, and PPCPs.
Analysis of FFAA Compounds Content in AFFF at DND AFFF Storage Facilities
900 AFFF and AFFF aqueous rinse samples from storage tanks were analyzed in 2008 – 2010. Survey included all DND bases with AFFF storage. Sample analyses were performed to determine PFOS and other perfluorinated compound content in AFFF, to meet regulatory requirements of <20 ppm PFOS content in AFFF product.
AXYS Counted on for Great Lakes Investigations
Since 2010 AXYS has performed PFC analysis in tissue and serum samples for USGS projects around Great Lakes avian contaminant investigations.
PFC Analysis for Minnesota Pollution Control Agency Since 2004
AXYS has provided analysis for MPCA’s PFC Monitoring projects for water, fish, invetabrates, soil, sediment, effluent, influent, biosolids, landfill leachates, ambient air and landfill gas and condensate matrices.
Environment Canada Chemical Management (CMP) Program counts on AXYS since 2009
Environment Canada Chemical Management (CMP) Program analyzes emerging contaminants in WWTP processes to determine the occurrence and solids/water partitioning. AXYS has performed PFC analysis of influent, effluent and biosolid samples for this program since 2009.