DoD ELAP and QSM 5.1 A Laboratory Perspective. Larry Penfold Quality Compliance Director

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1 DoD ELAP and QSM 5.1 A Laboratory Perspective Larry Penfold Quality Compliance Director

2 Discussion Topics Quality Systems Manual (QSM) V.5.1 released Jan What it means for laboratory accreditations Changes to methods already existing in Version 5.0 Examples of QC details for new methods in Version 5.1 Coordination with the laboratory during project set up and consideration of technical alternatives Note: Material presented here taken from TestAmerica s own review, presentations by the EDQW at the April 2017 meeting in Phoenix, and FAQs posted on DoD DENIX website

3 DoD ELAP Program DoD Environmental Laboratory Accreditation Program (ELAP) continues as it has before with 3 third-party accrediting bodies (ABs) Labs are in process of being audited to QSM 5.1 By end of 2018, all labs will have to have been audited to 5.1 During this 2-year audit cycle, labs can perform under the new version: QSM 5.1 Preface: Current accreditation to DoD QSM Version 5.0 is considered equivalent to accreditation to this manual

4 Lab Submittals To Become Accredited for a Method 1. SOP 2. Method validation results 3. Technical justification of method modifications 4. Calibration results 5. LOD/LOQ demonstration data 6. 2 successful PT results 7. Standards traceability 8. Laboratory control limits 9. Example data package 10.Training records

5 Special Accreditation Requirements for PFAS To become accredited for polyfluoroalkyl substances (PFAS): Results for 2 PFAS PTs first available January this year On-site assessment to QSM 5.1; this is the only method that requires a preliminary on-site assessment EDQW review and approval of on-site assessment documentation Method that will appear on scope: PFAS by LCMSMS Compliant with QSM 5.1 Table B-15

6 Process Leading To Release of QSM Version 5.1 Written by EDQW members representing Armed Services within the DoD and members of the DOE Draft released for comments late summer comments received 70 comments accepted and incorporated into not accepted 29 comments held for inclusion in QSM Version 6.0 Signed January 4, 2017 Effective immediately

7 What Is New and Significant Advertised as minimal change Many clarifications and editorial changes A number of technical alternatives that TestAmerica requested in the past are included in QSM now New QC tables: PFAS by LC/MS/MS, TO14 / TO15 by GC/MS SVOCs by GC/MS in SIM Mode Incremental Sampling Methodology (ISM) Some methods (i.e., 8330B and ISM) may require more communication with the lab to set up details in advance of delivering samples (to be discussed later in presentation)

8 Requirements for Notification of Data Quality Problems If data quality problems found in the course of data reviews or audits, lab must notify customers within 15 business days and submit a corrective action plan to customers within 30 business days If inappropriate practices found at the laboratory, lab must notify their accreditation body (AB) within 15 business days and submit a corrective action plan to the AB within 30 business days Failure to notify in a timely manner is grounds for immediate suspension of accreditation

9 QSM 5.1 Also Has Some Significant Analytical Changes TestAmerica completed a review and found more than 100 individual changes affecting how analyses are conducted and documented Some are significant from an analyst s perspective We prepared a comparison document outlining all of the changes (copies available on request, instructions at end of presentation) Discussion of some of the changes follows

10 Changes to Methods In Earlier Versions of QSM Chemical Testing, Module 4: LOQ verifications must be performed on the worst case combination when multiple preparation and cleanup techniques used Radiochemical Testing, Module 6 & Tables B-16 to B-21 Many changes, see TestAmerica comparison document One apparent error: When radiological instrument performance check results are outside limits, this is treated as a CCV failure to be corrected and rerun within 1 hour or complete a new energy calibration (multi-day procedure) instrument performance checks CCV, DOE has agreed to change this

11 Changes to Existing Methods (continued) QC Tables for Organic Methods: If surrogate spike recoveries are outside limits, reanalysis is not necessary when chromatographic interference is obvious, but the lab s customer must be notified prior to reporting, and the condition described in the report case narrative

12 Changes to Existing Methods (continued) GC and HPLC, Tables B-1 and B-2: Usual requirements for establishing RT window width for target compounds no longer applies to methods using internal standardization Instead, there are new QC limits for internal standards: RT RRT units from RT of midpoint standard in ICAL, and Internal standard signal (area or height) within -50% to +100% of signal for midpoint ICAL standard

13 Changes to Existing Methods (continued) Explosives by HPLC, LC/MS or LC/MS/MS, Table B-3: Notes that drying soils to constant weight may introduce bias [one alternative to discuss with project team is to limit drying to extent to avoid caking on sieve] Appropriateness of sieving soils is to be determined by each project Mentions that grinding may introduce bias and is not recommended for certain compounds, not specified All soils must be subsampled in ISM style, including those not initially dried, ground, or sieved

14 Changes to Existing Methods (continued) Metals by AA, ICP or ICPMS, Tables B-7 to B-9: Low-level calibration check required for all methods, including CVAA and GFAA, with recovery within 20% of expected value Calibration blank acceptance limit changed from <LOD to ½ LOQ or 1/10 samples or 1/10 reg. limit ND sample results can be reported if blank exceeds limits

15 QC for New Methods in QSM 5.1 PFAS by LC/MS/MS, Table B-15: For solids, entire sample homogenized before subsampling [potential contamination risk] Pretreatment with SPE cleanup cartridges required Must use standards containing both branched and linear isomers, when commercially available Specific ion transitions must be used, with >10:1 SNR for quantitation ions and > 3:1 SNR for qualifier ions Mass spectral acquisition with minimum of 10 scans/peak

16 QC for New Methods in QSM 5.1 (continued) SVOC Analysis by GC/MS SIM, Table B-22: Apparently written for analysis of PAHs DFTPP tune included, but degradation and tailing checks are not required Fluoranthene-d10 and 2-methylnaphthalene-d10 are required surrogates Minimum of 3 ions used for analysis Agreement within 30% with intensities in ref. spectrum SNR >10:1 for quantitation ions SNR > 3:1 for qualifier ions

17 QC for New Methods in QSM 5.1 (continued) Incremental Sampling Methodology, Table B-23: Written for non-volatile parameters, i.e., explosives, metals, and PAHs [would require discussion with lab to establish alternate approach for ISM applied to volatile parameters] States that grinding LCS is always required [massive-size LCS materials not commercially available for parameters other than explosives, and would require discussion with lab] Lab triplicates required for all ISM work

18 Calculating Holding Times, EDQW response to FAQ Holding time (HT) calculations are consistent with units in which they are expressed If HT expressed in hours, then HT is tracked to the hour, exceedance when final hour has elapsed If HT expressed in days, then HT is tracked to the day, exceedance when final calendar day has elapsed, with the day of collection counted as day zero The exception is when HT is expressed in months, in which case HT is tracked to the day

19 Waivers to QSM Requirements Labs are only accredited after they have documented the ability to meet all QSM requirements without exceptions Module 2, Section Waivers from QSM requirements are allowed if: Requested in writing with technical justification Justification must relate to specific project Only approved on a project-specific basis Approved by appropriate DoD chemist This is the process that TestAmerica has understood to be in effect for many years

20 TestAmerica s Approach to Presenting Technical Alternatives We have not done a good job in presenting reasonable technical alternatives With often little time to respond to client RFPs, we have been submitting proposals with a list of requested exceptions, without sufficient explanation of their purpose and potential value to the project In some cases, the list of requested exceptions included methods that didn t pertain to the project at hand This has generated understandable criticism of our approach and skepticism as to the purpose

21 Establishing a Project-Specific Technical Approach We believe that there is great benefit in engaging with our clients during the project setup period Some details to be discussed are clarifications of options that are fully compliant with the QSM, for example: QSM Module 4, Section a) ii) includes an exception to blank acceptance limits for common lab contaminants, QSM does not define a list of common lab contaminants If the list were communicated in advance, wouldn t it potentially save everyone time and avoid misunderstandings?

22 Project-Specific Technical Approach (continued) Some aspects of the technical approach that we would want to discuss clearly are exceptions to QSM requirements and would require written approval We will only propose exceptions that might improve project efficiency, and that are consistent with project-specific data quality objectives (DQOs) We can explain what the benefit to the project might be, but we need the discussion to understand how well any particular technical alternative fits project DQOs

23 Example of a Technical Alternative for Project Consideration Reporting ND sample results when the CCV %D for a known poor performer is marginally above acceptance limits For example, if CCV result for benzoic acid (a known poor performer) is 22% D, exceeding the 20% D limit and associated samples have ND results Are those results invalid? it depends on DQOs The lab can perform reanalysis of the samples, but that would add time and add complexity to reviews and validation

24 Example of a Technical Alternative (continued) If benzoic acid is not a critical compound of concern, and The validation criterion that is being used would qualify the ND results with an UJ flag, rather than reject with an R flag Wouldn t it save everyone involved in the project time and effort if we anticipate the outcome for a known poor performer and establish project-specific guidelines in writing for reporting ND results in advance? Wouldn t that make the project more efficient without sacrificing project objectives?

25 TestAmerica s New Approach to Technical Alternatives In every bid or proposal we are including a request to discuss technical details in advance of receiving samples, preferably during QAPP development TestAmerica has extensive experience with these methods and the program, we have the data to demonstrate what analytical approaches will work well and which are likely to have a high failure rate We can bring this information to the discussions

26 TestAmerica s Approach (continued) The list of technical concerns to be discussed is shorter given the many constructive changes in QSM 5.1 But some technical concerns still remain, and it is important to discuss them in advance We want to be successful, and We want your projects to be successful Including the lab in project setup meetings is an important part of ensuring project success

27 TestAmerica Labs in DoD and DOE Programs DoD ELAP DOECAP Anchorage - Mobile Labs* yes Burlington, VT yes Denver, CO yes yes Knoxville, TN yes yes Richland, WA yes yes Savannah, GA yes Seattle, WA yes St. Louis, MO yes yes Sacramento, CA yes yes * extension of Seattle lab s accreditation 27

28 Ask The Expert Webinar Series Thank you for attending DoD ELAP and QSM 5.1 A Laboratory Perspective To submit a question, type it into the Questions panel in the GoToWebinar toolbar and click Send. If you have any additional questions for today s presenter you may submit them directly to: Please be sure to visit the Ask the Expert Webinar Series web page for other scheduled webinars at: To view a recording of this webinar session, please contact: testamericawebinars@beedeebee.com

Project Planning Considerations For Emerging Contaminants. Ed Corl NAVSEA LQAO

Project Planning Considerations For Emerging Contaminants Ed Corl NAVSEA LQAO Report Documentation Page Form Approved OMB No. 0704-0188 Public reporting burden for the collection of information is estimated