1. Department of Defense (DoD) Updates for 2016
Alyssa Wingard
NAVSEA 04X6
Fred McLean
BMT Group

2. Agenda: Areas of Concern for DoD in 2016
DoD Environmental Laboratory Accreditation Program (ELAP) Update
Emerging Contaminants - PFAS
Quality Systems Manual (QSM) 5.1/Quality Systems for Analytical Services (QSAS) 3.1 Update
Questions

3. Areas of Concern for DoD
Waivers
Inappropriate Practices
Combined Assessments
Environmental Monitoring and Data Quality Workshop

4. Waivers 4.4.4.1 Tenders and Contracts (DoD only)
Waivers from QSM requirements must be requested in writing from the appropriate DoD Chemist on a project-specific basis and shall include technical justification. Documentation for approval must be maintained.
*** A laboratory must have the documented ability to meet all QSM requirements in order to be accredited. Laboratories cannot submit variances to ABs to allow deviation from QSM requirements as part of their accreditation. Variances must be project specific. ***

5. Inappropriate Practices
4.9.4 All DoD ELAP laboratories must report any instances of inappropriate and prohibited laboratory practices, as detailed in Section of the DoD QSM, to their AB within fifteen (15) business days of discovery. All DoD ELAP laboratories must submit records of associated corrections taken or proposed corrective actions to their AB within thirty (30) business days of discovery. The respective AB will then have the responsibility of informing the EDQW of the laboratory’s deviation from the requirements of the QSM. If the AB is not notified within fifteen (15) business days the AB will immediately suspend the laboratory’s DoD ELAP accreditation. The respective ABs and the EDQW deem these infractions as quite serious and appreciate the cooperation from all involved parties.

6. Inappropriate Practices
DoD/DOE (Guidance) Willful avoidance of approved corrective action implementation may result in loss of DoD ELAP accreditation or in DOECAP Priority I findings. As a result, work may be discontinued until implementation is verified by the DoD ELAP AB or DOECAP Operations Team, as appropriate.

7. Instances 6 Instances Communicated
4 Actual Instances of Inappropriate Practice
Laboratories were required to notify all affected clients
Thorough investigation of data sets

8. Combined Assessments State and DoD ELAP Trained Assessors
Assessor Pool
Terms and Conditions

9. Environmental Monitoring and Data Quality Workshop
U.S. Bureau of Land Management National Training Center
Phoenix, AZ | April , 2017
Save the Date !

10. DoD ELAP Update Number of labs Changes from previous years
Common DOD/DOE LABS
Changes in accreditation bodies

11. DoD ELAP Status AB
2016
2015
2014
2013
2012
2011
2010
A2LA 25 22 27 29 30 24 15
PJLA 28 31 23 12
ANAB dba LAB* 41
ANAB 11 14 21
LAB* 32 19
Total Labs 93 98 99
102 67
*ANAB acquired LAB December 2015.

12. DoD and DOE Common Laboratories
ALS – Salt Lake, Fort Collins
American Radiation Services (ARS)
BC Laboratories
Brooks Applied Labs
Eberline Analytical – Oak Ridge
Eurofins Frontier Global Sciences *
GEL Laboratories
Microbac *
Shealy Environmental
TestAmerica – Knoxville, St. Louis, Denver, Richland, West Sacramento
15 Laboratories Total; *2 additions

13. Per- and Polyfluoroalkyl Substance
Group of fluorinated organic chemicals commonly called PFCs and PFASs
Uses include coatings on fabrics, carpet, paper packaging, cookware, chrome plating processes, manufacturing processes, and aqueous film forming foam (AFFF) used as a fire suppressant

14. Per- and Polyfluoroalkyl Substance
The EPA has issued health advisories in drinking water for two of these chemicals, Perfluorooctanoic acid (PFOA) and Perfluorooctane sulfonate (PFOS). [May 2016]
PFOA: < 70 ppt
PFOS: < 70 ppt
If both present, PFOA and PFOS
combined: < 70 ppt

15. Per- and Polyfluoroalkyl Substance
The EPA has issued a Provisional Peer-Reviewed Toxicology Value (PPRTV) for Perfluorobutane sulfonate (PFBS). [July 2014]
Subchronic p-RfD (mg/kg-day): 0.2
Chronic p-RfD (mg/kg-day): 0.02

16. Per- and Polyfluoroalkyl Substance
DoD MERIT classifies PFOA and PFOS as emerging chemicals (ECs) of probable high impact due to the extensive use AFFF at military sites.
DoD is in the process of evaluating all sites that have had known or suspect release of PFASs within 1 mile up-gradient of a drinking water source.

17. Per- and Polyfluoroalkyl Substance
EDQW Initiative Relating to PFASs:
Working with AFFF Tech Warrant Holder to evaluate all previously used and current MIL SPEC approved AFFF formulations for a short list of PFASs, including PFOA and PFOS

18. Per- and Polyfluoroalkyl Substance
EDQW Initiative Relating to PFASs:
Working with the EPA to develop and validate groundwater/surface water and soil/sediment sampling and preparation and analysis methods for 24 PFASs
Working with Standards providers to ensure all needed standards are available for the EPA method development

19. Per- and Polyfluoroalkyl Substance
EDQW Initiative Relating to PFASs:
Working with Proficiency Test Sample Providers to develop PT samples for GS/SW and Soil/Sediment matrices for the 24 analyte list
Develop QC tables for routine and AFFF analysis for DoD QSM Version 5.1

20. Per- and Polyfluoroalkyl Substance
EDQW Initiative Relating to PFASs:
Assist in ESTCP Project “Rapid Transfer Information Transfer Among Key Stakekholders on PFASs at Contaminated Military Sites” through information workshops

21. QSM 5.1/QSAS 3.1 UPDATE

22. QSM 5.1/QSAS 3.1 Changes Preface:
Current accreditation to QSM 5.0 is considered
equivalent. (DoD only)
Volume 1, Module 1: Proficiency Testing (PT)
3.2.2 addition (DOE only)
Laboratories that receive unacceptable results for consecutive rounds of MAPEP testing shall notify the DOECAP Operations Team/DOE contract holders within 15 business days.
For non-MAPEP PTs, labs must maintain proficiency for two out of every three rounds and shall notify the DOECAP Operations Team/DOE contract holders within 15 business days from receipt of the third unacceptable result.

23. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
3.0 Additional Definitions
Analytical Method
Deuterated Monitoring Compounds (DMCs)
Incremental Sampling Method (ISM)
Linear Dynamic Range (LDR)
Selected Ion Monitoring (SIM)

24. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
Data Review
Quality Manager or designee shall review a minimum of 10% of all data on a quarterly basis. If data quality issues are discovered, the client shall be notified within 15 business days.
Tenders and Contracts (DoD only)
Waivers from QSM requirements must be requested in writing from the appropriate DoD Chemist on a project-specific basis and shall include technical justification. Documentation
for approval must be maintained.

25. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
Subcontracting
All subcontracted or outsourced management systems elements (such as data review, data processing, project management, and IT support) or outsourced personnel must comply with the laboratory’s overall management system, comply with this Standard, and are subject to review/approval by the DoD/DOE customer.

26. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
4.9.3 Nonconforming work
Notify all affected customers of potential data quality issues within 15 business days of discovery.
4.9.4 Inappropriate work (DoD only)
All instances of inappropriate and prohibited practices must be reported to their Accreditation Body (AB) within 15 business days of discovery.
Guidance
Willful avoidance of approved corrective actions may result in loss of DoD ELAP accreditation or in DOE Priority I findings. As a result, work may be discontinued.

27. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
Internal Audits
Laboratories shall notify DoD/DOE clients within 15 business days of discovery of any investigation that casts doubt upon the validity of test results.
Internal Audits
Review shall also include raw electronic data files derived from test reports.
4.9.4 Data Integrity (DoD only)
All instances of inappropriate and prohibited practices must be reported to their Accreditation Body (AB) within 15 business days of discovery.

28. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
iii LIMS
Software change control methods must be implemented and documented.
Table 5-1. Performance Checks
If an out of control temperature notification has been sent out, the lab is expected to respond within 24 hrs.
Storage (DOE only)
e. Laboratories shall develop and maintain procedures for sample receiving and login that minimizes changes in thermal preservation.
f. Laboratory shall document if thermal preservation is not maintained in accordance with sample receiving and login procedures. The client shall be notified in writing if thermal preservation is not maintained.

29. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 2 Quality Systems (QS) General Requirements:
Radioactive Materials Management and Control (DOE Only)
6.1.3
Radiological survey equipment must be calibrated annually and calibrated backup survey equipment must be available during the time that the survey equipment is out for recalibration.
6.4.10
A certificate of disposal or destruction shall be obtained for all samples sent to a treatment, Storage, and Disposal Facility (TSDF).

30. QSM 5.1/QSAS 3.1 Changes Volume 1, Module 3 Asbestos Testing:
Microscopy
A gold standard grid shall be used to obtain the characteristic diffraction rings.
Microscopy
Both stereoscope and polarized light microscope
shall be aligned and checked.
b. All alignments and function checks shall be documented.

31. QSM 5.1/QSAS 3.1 Changes
Volume 1, Module 4
Chemical Testing

32. 1.5.e Method Validation
Methods must be validated when substantive modifications are made to reference methods (i.e., stoichiometry, technology, mass tuning acceptance criteria, quant ions, compressing digestion/extraction timeframes, reducing reagent/solvent volumes, changing solvents, or compressing instrument run times).
g Calibration
For metals analysis, the laboratory may report a sample result with a response above the calibration range if the laboratory analyzes and passes (within 10% of true value) a high level check standard that exceeds the sample concentration but is within the Linear Dynamic Range.

33. 1.7.2.e Continuing Calibration Verification (CCV)
For failed consecutive CCVs, correct problem and rerun CCV or alternatively, recalibrate instrument.
Confirmation
Confirmation is necessary for all results greater than the Detection Limit (DL).
Blanks
If the blank exceeds ½ the LOQ or is greater than 1/10th the regulatory limit then blank is considered contaminated.

35. 1.3 Terms and Definitions
Equations from MARLAP Chapter 18 (Z-scores) added.
1.5.4 Combined Standard Uncertainty
For counting methodologies where very low counts are possible, MARLAP equation may be used with acceptance by the client.
1.7.1 Detector Efficiency
When sources used for efficiency are not from NIST/International traceable standards they are considered “working reference materials” [defined through ASTM C1128].
1.7.1 Performance Checks
Use of consecutive performance checks defined as similar to CCVs in the chemistry Module.
FWHM resolution of alpha/gamma detectors shall be evaluated
prior to use and following repair; measured FWHM resolution
shall be trended.

36. 1.7.1.xiii Background Measurement
Gas Proportional Counters: long background measurements shall be performed monthly (but some clients may specify TNI language – weekly).
LCS
m. LCS shall contain at least one analyte reported for samples; should be at least five times but not greater than 20 times RL.
i) Except – some programs may require at least 10 times MDA.
v) Standard containing reported analyte not available, an LCS analyte having similar separation chemistry/energy/decay shall be used.
Matrix Spike Evaluation
If activity is less than 5 times the spiking level, MS recoveries shall be within %.
If activity is greater than 5 times the spiking level, |ZMS|≤3 is used.

37. Background
Background contamination monitoring samples shall be analyzed at a sufficiently low level of detection to confirm that no impacts to client samples have occurred due to cross-contamination.
1.8.1 Alpha Spectrometry
d). FWHM peak energy within ±50 KeV.
1.8.2 Lucas Cell – Radon
a). SOP for sample analysis by Lucas Cell shall incorporate and adhere to EPA Method (current). Radium-226 in DW (Radon Emanation Technique) shall adhere to this standard unless otherwise defined and accepted by client.
d). Same cell/detector combination used to establish calibration factors shall be used for background measurements.
e). Bubbler used for Radium-226 standardization shall not be used for samples.

38. 7.0 Data Validation reports for third party review
Appendix A
7.0 Data Validation reports for third party review
Standards Traceability shall be included in Stages 3 and 4.
Appendix B Tables- Global
Organics by GC/HPLC/MS:
1. RT window width 0.03 minutes added
2. IS section added (if used)
3. When ICAL not performed, daily initial CCV can be used for RT update
4. Sample/MSD RPD applicable only if sample concentration is ≥LOQ
5. Surrogate spike: if obvious chromatographic interference is present, reanalysis may not be necessary
6. Confirmation required for all results >DL

39. Appendix B Tables- Global Organics by GC/HPLC/MS:
Table B-3 (8830B)
1. Incorporates Grinding Blanks/Method Blanks, Drying/Sieving and Spiking of Surrogates/LCS
Inorganics by AA/ICP-AES/MS:
Low Level CCV (Daily) within 20% at the LOQ; a separate standard or recalculate against the calibration curve
ICB/CCB after every ICV/CCV. CCBs may not be reanalyzed without reanalysis of the associated samples
ICS-A criteria: all non-spiked project analytes <1/2 LOQ

40. New Tables Added:
B-15 PFAS Using LC/MS/MS and ID with IS Quantification
B-20 Radon Scintillation (Ra-226 by Lucas Cell)
B-21 GC/MS of Air Samples
B-22 Organic Semi-VOA by GC/MS in SIM Mode
B-23 Incremental Sampling Methodology (ISM) Soil Preparation for Large Volume Samples (1 Kg or greater)
B-24 PFOA/PFOS in AFFF Formulations by LC/MS/MS and ID

41. No Changes!
Volume 1, Module 5 Microbiological Testing Volume 1, Module 7 Toxicity Testing Appendix C: LCS Limits Appendix D: Non-Destructive Assay

42. QSM 5.1/QSAS 3.1 Timeline
PRESENTATION AT ASP WORKSHOP: ROLL-OUT! COMMENT PERIOD ONGOING 01 JANUARY 2017: FINAL CHANGES INCORPORATED BEGIN ASSESSOR TRAINING CHANGES ARE CONSIDERED MINOR (FOR DoD ELAP) EXPECT TO BEGIN ACCREDITATION DURING THE NEXT CYCLE STARTING MID-2017

43. Questions? More Information?
Alyssa Wingard Fred McLean