Challenges Seen in the Development and Delivery of EPA 537 R1 Challenges Seen in the Development and Delivery of EPA 537 R1.1 (and DOD-modification) August 9, 2018 William Perry QA Manager GCAL Laboratories – Baton Rouge, LA

Intro Two years ago – just sitting on a bench, not running. Summer of 2016 this was sitting on a bench not yet running – waiting for the market to develop. Two years ago – just sitting on a bench, not running.

Development/Certification Publish 537.1 SOP Start dev. 537.1 Complete 537.1 Valid Pack Publish B-15 SOP 2016 Rcv draft QSM 5.1 Start dev B-15 SEP OCT NOV DEC Talking w/ Wellington @ ID Talking w/ PTPs AB Packages 537.1 submitted Rcv copy of final QSM 5.1 First PT WS 1st PT WP-HW 2017 Publish B-15 SOP First samples JAN FEB MAR APR MAY DOD EA Sched/Called off DOD EA auditor training DOD EA DOD Scope Awarded Three months later – validation work almost completed for 537.1. By December, validation package and scope expansion package in with AB. EA schedule for January, but cancelled because new DOD method finalized. January – February 2018, revising method to isotopic dilution, March 2018 rest of initial PTs. Certification in 8 months after starting (after creating two SOPs on two differing methods where only one method has a formal method). First samples began arriving 9 months after starting method development. LELAP EA 2017 Run Time reduced Vi reduced NOV DEC JAN FEB MAR 2018 2nd PTs 3rd PTs 2018 also: AF 3x blind study (March) Client EA (July – focused on PFAS) DOD EA (July – 2x reviewing PFAS)

Issues Internal EIS mapping Standards sourcing MeOH contamination HPLC water batching Sample container specification Run duration change - Delay column impact - PFOS/PFHxS underestimation Decreasing required sample volume Cartridge contamination 3 PT targets fail (out of 360 targets tested – we do all targets) Validator training on how to read the trace report. Ion Ratio reset External 1st DOD EA findings DOD validation package requests Level IV package needs Client EA Finding: variance with other labs (PFOS/HFHxS underestimation due to baseline not extending to branch-chained isomers) 2nd DOD EA findings. Blank contamination (or is it time to replace the delay column?) NEW This does not count the numerous questions on items such as how is result calculated?

Summary Issue Lesson Learned Client Impact HPLC Water Can use our own water but must have a batching/tracking system. None Teflon liners Order MeOH that does not come with this, also sample containers, water containers. Interferences Delay column Don’t assume: delays contaminants, not analytes. Run natives whenever changing method to assure all isomers are located. These apparently have short life spans. Bias low, Blank contamination. Total PFOS/PFHxS Assumption lead to baseline not being extended. Bias low Validator training Total PFOS/PFHxS issue could easily been caught. Bad cartridge lot Assumption that cartridges remain of equal quality from batch to batch. Bias high Ion Ratio reset QC controls are only good if they are understood, managed properly and used False negatives

Double Blind PT Fail – Outlier Double blind PT from client. We failed (bias high). After careful checking of calculations and addressing concerns from client that we were consistently biased high, demonstrated that the study results were an outlier (per Grubb’s Test) form data on overall single blind PTs. PT fail has now been bracketed by two successful PTs.

Branch-Chain Enrichment/ Baseline Redraw Significance (PFOS): ~10% (with minimal branch-chained enrichment) ~50% (with significant branch-chained enrichment) Note: %D can vary wildly at low concentrations (“J”) Issue: Migration in groundwater causes “enrichment” Service sold as total PFOS/PFHxS (on our instrument issue does not affect other compounds) Assumed move to shorter run cause isomers to merge – this was wrong Once we identified nonconformance, defined the issue to be ### sample, # sites, # States, all waters. Every location sampled that is a water (and not AFFF) appears to be branch-chained enriched. Degree of bias depends on how much the samples were enriched, also how significant the matrix interferences are (can cause false negatives, or significant positive bias if resolution or cleanup cannot address) In standards, impactable branch chain isomers represent ~18% of total weight.

Branch-Chain Enrichment/ Baseline Redraw Significance (PFHxS): 0% (with minimal branch-chained enrichment) ~50% (with significant branch-chained enrichment) Note: %D can vary wildly at low concentrations (“J”). Also redrawing of baselines can cause redraw results to be less than original results. Issue: Migration in groundwater causes “enrichment” Service sold as total PFOS/PFHxS (on our instrument issue does not affect other compounds) Assumed move to shorter run cause isomers to merge – this was wrong Once we identified nonconformance, defined the issue to be ### sample, # sites, # States, all waters. Every location sampled that is a water (and not AFFF) appears to be branch-chained enriched. Degree of bias depends on how much the samples were enriched, also how significant the matrix interferences are (can cause false negatives, or significant positive bias if resolution or cleanup cannot address) In standards, impactable branch chain isomers represent ~18% of total weight.

Conclusion A rough few years, a lot of questions, many jumps to assumptions by lab and clients, a complicated learning curve. We are only where we are because of the challenges thrown our way by competitors and customers. LOE by QAM: About 4 hours every 2 weeks since beginning responding to questions and issues.

Questions William Perry GCAL-QA 225-214-7077 william.perry@gcal.com For more information: William Perry GCAL-QA william.perry@gcal.com 225-214-7077