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Fast and Economical PFAS Extraction Using Strata PFAS - SCIENCE UNFILTERED

Strata PFAS

PFAS are a class of highly stable synthetic organic compounds used in a wide variety of industrial and commercial applications. They are also highly stable in the environment and strongly bioaccumulate. As a result, they have become ubiquitous throughout the globe and are often referred to in today's media as "Forever Chemicals". Consequently, PFAS levels need to be tested in drinking water and more recently methods have been developed to measure PFAS in other environmental matrices that require more complex clean-up solutions, such as wastewater, soils, and sediments.

Accurate, Precise, and Economical PFAS Extraction Solution

The United States Department of Defense (DOD) is dealing with extensive PFAS contamination owing to the widespread use of PFAS-based Aqueous Film Forming Foam (AFFF) used as fire suppression foams at many military installations. As a result, DOD developed its own PFAS analytical guideline to help solve their installations' unique environmental monitoring and clean-up challenges. The US EPA and DOD have been working jointly to validate EPA 1633 Analysis of Per- and Polyfluoroalkyl Substances (PFAS) in Aqueous, Solid, Biosolids, and Tissue Samples by LC-MS/MS. A single-lab validated draft method is the result of this collaboration method and calls for the use of a polymeric weak anion exchange (WAX) SPE sorbent in combination with graphitized carbon black (GCB) powder. For water samples, the process involves an initial SPE using a WAX cartridge followed by dGCB or the use of a second cartridge. For solid samples, dGCB is added to an initial ammonium hydroxide wash, followed by the WAX SPE cartridge.

Both methods add time, cost, and chances for increased errors to the clean-up procedure and present the opportunity for loss of analytes and introduction of imprecision.

Strata PFAS SPE, wherein the two sorbents are contained within a single tube, offers the opportunity for decreased sample processing time and increased accuracy and precision. Strata PFAS is a stacked single cartridge solution with polymeric WAX and GCB sorbents that functions as a traditional Solid Phase Extraction (SPE) cartridge with a built-in polishing step. When comparing different recoveries for a small subset of analytes for a WAX SPE and dSPE GCB method versus Strata PFAS, the recovery is greatly improved using Strata PFAS. The results are shown in Table 1.

A routine Laboratory Control Sample (LCS) was conducted by a commercial testing laboratory highly experienced with PFAS analysis. The LCS had been spiked with all 32 target analytes at 25 μg/L and was analyzed with a batch of field samples to demonstrate method performance and data acceptability.

As shown in Table 2, all 32 analytes were well within method recovery limits with an average recovery of 98.8% and a mean recovery of 99.0%, thereby demonstrating acceptability of the use of Strata PFAS in the performance DOD QSM5.1/5.3 as well as draft EPA 1633.

SPE Conditions for Analyte Extraction Using Strata PFAS SPE

Cartridge: Strata PFAS 200 mg WAX/50 mg GCB/ 6 mL)
Part No.: CS0-9207
Condition 1: 4 mL 0.3 % Ammonium hydroxide
Condition 2: 4 mL Methanol
Equilibrate: 5 mL Water
Load: Add sample at 4 mL/min
Wash: 2x 4 mL Water
Elute: 2x 4 mL 0.3 % Ammonium hydroxide in
Evaporate: Methanol to dryness and reconstitute to 1 mL with Methanol/Water (96:4)

Table 1: Recovery Comparisons of WAX SPE and dSPE using GCB vs Strata® PFAS Single Cartridge Method

Analyte
WAX SPE + dSPE GCB
% Recovery
Strata PFAS Stacked Cartridge
% Recovery
13C2-PFDoDA
77
84.5
13C2-PFTeDA
62
84.0
PFODA
38
78.3
PFHxDA
63
89.3


Table 2: Recovery of QSM 5.3 Target Analytes from a Laboratory Control Sample Using Strata PFAS SPE (WAX/GCB)

Analyte
Actual Concentration
Sample Result
% Recovery

Method Recommendation

Limits

Pass/Fail
PFBA
25.600
22.640
88
84-135
Pass
PFPeA
25.600
22.157
87
75-138
Pass
PFBS
22.640
22.300
99
81-133
Pass
4:2-FTS
23.920
22.078
92
64-134
Pass
PFHxA
25.600
24.644
96
80-137
Pass
PFPeS
24.000
21.699
90
82-132
Pass
HFPODA
25.600
26.336
103
70-130
Pass
PFHpA
25.600
27.018
106
80-140
Pass
PFHxS
24.200
24.713
102
71-131
Pass
DONA
24.120
26.083
108
70-130
Pass
6:2-FTS
24.280
24.217
100
51-155
Pass
PFHpS
24.360
23.015
94
80-129
Pass
PFOA
25.600
25.043
98
83-138
Pass
PFOS
24.480
22.492
92
54-139
Pass
PFNA
25.600
25.872
101
73-140
Pass
9Cl-PF3ONS
23.840
21.863
92
70-130
Pass
PFNS
24.560
21.993
90
71-121
Pass
PFDA
25.600
25.047
98
78-137
Pass
8:2-FTS
24.520
22.231
91
62-133
Pass
PFOSA
25.600
25.714
100
73-121
Pass
NMEFOSAA
25.600
30.906
121
53-136
Pass
PFDS
24.640
22.873
93
69-124
Pass
PFUnDA
25.600
26.353
103
70-134
Pass
NEtFOSAA
25.600
28.765
112
59-145
Pass
11Cl-PF3OUdS
24.120
22.625
94
70-130
Pass
PFDoDA
25.600
27.710
108
75-139
Pass
10:2-FTS
24.680
26.626
108
50-124
Pass
PFDoS
24.800
21.509
87
39-121
Pass
PFTrDA
25.600
25.814
101
67-144
Pass
PFTeDA
25.600
25.446
99
79-134
Pass
PFHxDA
25.600
29.662
116
36-136
Pass
PFODA
25.600
27.373
107
10-124
Pass

Andrew Patterson1 , Charles Neslund2 , Robert Brown2 , Sam Lodge3 , David Kennedy3 , and Brian Marshall3

1
Eurofins Environment Testing America, 800 Riverside Pkwy, Sacramento, CA, 95605, USA 2 Eurofins Environment Testing America, 2425 New Holland Pike, Lancaster, PA 17601, USA 3 Phenomenex, Inc., 411 Madrid Ave., Torrance, CA 90501, USA