Page 4 - Application Notebook - PFAS Analysis

SHIMADZU | WHITE PAPER Ultra-fast LC-MS/MS Analysis of PFAS in Environmental Waters

 Validated Methods for Analyzing PFAS PFAS in environmental waters using LC-MS/MS. In the
interim, laboratories are using in-house developed
Liquid chromatography coupled to triple-quadrupole methods (e.g. modified EPA Method 537) or methods
mass spectrometry (LC-MS/MS) is widely used for the that have been developed by non-governmental
determination of PFAS in water matrices because of its standardization bodies, such as ASTM International
high sensitivity and specificity. Given the social and ISO.
importance of PFAS monitoring, standardized analytical
methods for LC-MS/MS need to be developed and ASTM International has developed ASTM D7979-17
validated to ensure that all results are consistent and [16] and ASTM D7968-17a [17] for PFAS analysis in
reliable, particularly if the data were to be used for environmental waters and soil, respectively. The main
enforcing regulation. difference between these ASTM methods lies in the
sample preparation steps. After the extraction of
In September 2009, US EPA published EPA Method samples, the procedures and LC-MS/MS methods are
537 Version 1.1 [14] for the determination of fourteen essentially the same. Shimadzu is one of the members
PFAS compounds in drinking water. This method was of the ASTM D19.06 Task Group’s independent,
later employed for the monitoring of the selected PFAS second laboratory validation of ASTM D7979. This
during the Unregulated Contaminant Monitoring Rule 3 white paper describes the work related to the
(UCMR3). However, for environmental waters (e.g. validation. Table 1 summarizes the various LC-MS/MS
non-potable water, surface water, wastewater and methods for PFAS testing in various environmental
groundwater) and soil matrices, there are no standard water and soil matrices.
EPA methods available. US EPA is currently
developing EPA Method 8327 [15] for the analysis of

Table 1. Comparison between the various EPA and ASTM Methods for PFAS testing in water matrices.

Method EPA 537 [14] ASTM D7979 [16] ASTM D7968 [17] EPA 8327 [15]

14 Targets 21 Targets 21 Targets 24 PFAS compounds
PFAS Compounds 3 Surrogates 9 Surrogates 9 Surrogates (details to be
3 ISTDs announced)

Groundwater, Surface
water and
Sludge, Influent, Wastewater.
Sample Matrices Drinking Water Effluent and Soil
Wastewater
(<0.2% solids) Sample collection
procedure to be
prescribed.

Dilute 5 mL with 5 mL Extract 2 g with
250 mL  SPE  10 mL 50% Methanol Direct Injection
Sample Preparation Methanol  Filter 
1 mL  Filter  Direct Method
Direct Injection
Injection

Injection Volume 10 µL 30 µL 30 µL To be announced

External Calibration External Calibration
(Isotope Dilution or (Isotope Dilution or
Quantitation Internal Standard Internal Standard Internal Standard To be announced
allowed) allowed)