A02.11_PWS-Annex-1_QSM Version 5.3 FINAL.pdf

Department of Defense (DoD)

Department of Energy (DOE)

Consolidated

Quality Systems Manual (QSM) for

Environmental Laboratories

Based on ISO/IEC 17025:2005(E)

ISO/IEC 17025:2017(E)

and

The NELAC Institute (TNI) Standards, Volume 1, (September 2009)

DoD Quality Systems Manual Version 5.3

Department of Defense (DoD)

Department of Energy (DOE)

Consolidated Quality Systems Manual (QSM) for

Environmental Laboratories JQRDAN.BRIAN.D.1141739820 Digitally signed by JORDAN.BRIAN.D.1141739820

Date: 2019.05.07 16:24:50 -05'00'

Brian Jordan Army Principal

Date

GILLETIE.JOHN.S.1123328350 Digitally signed by GILLmEJOHN.S.1 1 23328350 Date: 2019.05.07 14:42:03 -05'00'

JohnS. Gillette, Ph.D.

Air Force Principal

ADELSON.JORDAN.M.1268693 137

Jordan Adelson, Ph.D.

Navy Principal , EDQW Chair

Digitally signed by ADELSON.JORDAN.M.I268693137 ON: ccUS, o=U5. Government ou=DoD. ou=PKI, ou=USN, cn=ADELSONJORDAN.M.126869313 7 Date: 2019.0S.08 09:06:09 .()4'00'

DEBRA ROSANO Dlgltally signed by DEBRA ROSANO Date: 201 9.05.08 15:17:31 -04'00'

Date

Date

Debra Rosano Date Director Office of Sustainable Environmental Stewardship (AU-21) Office _of Environment, Health, Safety and Security Department of Energy

Note: This version of the DoD/DOE QSM supersedes previous versions of the Department of Energy Quality Systems for Analytical Services.

DoD/DOE QSM 5.3

Page i

Preface

The Department of Defense (DoD) Environmental Data Quality Workgroup (EDQW) and the

Department of Energy (DOE) Consolidated Audit Program (DOECAP) Data Quality Workgroup

(DOE-DQW) participants developed this manual called the DoD/DOE Quality Systems Manual

(QSM) for Environmental Laboratories. The DoD/DOE QSM provides baseline requirements for the establishment and management of quality systems for laboratories performing analytical testing services for the DoD and the DOE.

This manual is based on Volume 1 of The NELAC Institute (TNI) Standards (September 2009), which incorporates International Organization for Standards (ISO)/International Electrotechnical

Commission (IEC) 17025:2005, General requirements for the competence of testing and calibration laboratories and ISO/IEC17025:2017. Conformance to the requirements contained in this manual is mandatory for any laboratory that is 1) seeking or maintaining accreditation in accordance with the DoD Environmental Laboratory Accreditation Program (ELAP) or 2) seeking or maintaining accreditation in accordance with the DOE Consolidated Audit Program

Accreditation Program (DOECAP-AP). Laboratories that comply with the requirements of this manual must also comply with the TNI Standards (September 2009), ISO/IEC 17025:2005, and

ISO/IEC 17025:2017 (where noted in grey boxes), unless specific provisions in those standards are superseded by this document. Laboratories that are accredited to ISO/IEC 17025:2017 will meet the ISO 17025:2017 grey box reference requirements of DoD/DOE QSM Version 5.3.

To alleviate issues of copyright and provide a manual that is freely available to all, this manual is presented in a format which must be used in conjunction with the TNI Standards (September

2009), ISO/IEC 17025:2005, and ISO/IEC 17025:2017 standards. DoD/DOE specific language is presented as text and appendices in the order in which topics are addressed in the TNI

Standards. DoD/DOE text contains additional requirements, clarifications, and guidance to supplement the TNI Standards (September 2009), ISO/IEC 17025:2005, and ISO/IEC

17025:2017 language. New or more stringent requirements from the ISO/IEC 17025:2017 standard are referenced by grey boxes. Information that may be beneficial to a laboratory, but is not required, is marked as guidance. To the extent possible, DoD and DOE requirements have been consolidated. Text or appendices that are unique to either DoD or DOE are marked as such.

The DoD/DOE QSM is international in scope and applies to all laboratories regardless of size or complexity. Nothing in this document relieves any laboratory from complying with more stringent contract specifications, host-nation final governing standards, or federal, state, tribal, and local regulations. DoD ELAP Accreditation Bodies (AB) and the DOECAP-AP ABs will accredit laboratories to this version of the standard during their normal accreditation cycles.

Laboratories will be permitted to continue work on existing contracts under the project required version of the DoD/DOE QSM. Laboratories must be assessed to this version of the DOD/DOE

QSM during their routine accreditation cycle.

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The DoD and DOE reserve the right to periodically, and as necessary, issue new requirements or clarification to current requirements. These addenda will be published as an official memo and posted on DoD Environment, Safety, and Occupational Health Network and Information

Exchange (DENIX) and the DOE Sharepoint site.

This manual was created in the spirit of cooperation between agencies for the purpose of consolidating and improving quality systems. The DoD and DOE expert committee members wish to thank the many volunteers that provided insight and guidance into the resolution of complex scientific issues that are now a part of this document. Moving forward, the goal of continued data quality improvement will always be at the forefront of both the DoD EDQW and

DOE-DQW team.

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Table of Contents

PREFACE ................................................................................................................................... I

ACRONYM LIST

VOLUME 1, MODULE 1: PROFICIENCY TESTING (PT)

1.0 INTRODUCTION

2.0 REQUIREMENTS FOR ACCREDITATION (SECTION 2: DOD ONLY)

2.1 Initial Accreditation

2.2 Continuing Accreditation

3.0 REQUIREMENTS FOR PARTICIPATION (SECTION 3: DOE ONLY)

3.1 Initial Accreditation

3.2 Continued Participation

VOLUME 1, MODULE 2: QUALITY SYSTEMS GENERAL REQUIREMENTS

1.0 INTRODUCTION, SCOPE, AND APPLICABILITY

1.1 Introduction

1.2 Scope DoD/DOE (Clarification)

2.0 NORMATIVE REFERENCES (ISO/IEC 17025:2005(E), CLAUSE 2)

3.0 TERMS AND DEFINITIONS

3.1 Additional Terms and Definitions

4.0 MANAGEMENT REQUIREMENTS

4.1 Organization (ISO/IEC 17025:2005(E), Clause 4.1)

4.2 Management (ISO/IEC 17025:2005(E), Clause 4.2)

4.3 Document Control (ISO/IEC 17025/2005(E), Clause 4.3)

4.4 Review of Requests, Tenders and Contracts (ISO/IEC 17025/2005(E), Clause 4.4)

4.5 Subcontracting of Environmental Tests (ISO/IEC 17025/2005(E), Clause 4.5)

4.6 Purchasing Services and Supplies (ISO/IEC 17025/2005(E), Clause 4.6)

4.7 Service to the Client (ISO/IEC 17025/2005(E), Clause 4.7)

4.8 Complaints (ISO/IEC 17025/2005(E), Clause 4.8)

4.9 Control of Nonconforming Environmental Testing Work (ISO/IEC 17025/2005(E), Clause 4.9)

4.10 Improvement (ISO/IEC 17025/2005(E), Clause 4.10)

4.11 Corrective Action (ISO/IEC 17025/2005(E), Clause 4.11)

4.12 Preventive Action (ISO/IEC 17025/2005(E), Clause 4.12)

4.13 Control of Records (ISO/IEC 17025/2005(E), Clause 4.13)

4.14 Internal Audits (ISO/IEC 17025/2005(E), Clause 4.14)

4.15 Management Reviews (ISO/IEC 17025/2005(E), Clause 4.15)

4.16 Data Integrity Investigations (TNI Section 4.16)

5.0 TECHNICAL REQUIREMENTS

5.1 General (ISO/IEC 17025/2005(E), Clause 5.1)

5.2 Personnel (ISO/IEC 17025/2005(E), Clause 5.2)

5.3 Accommodation and Environmental Conditions (ISO/IEC 17025/2005(E), Clause 5.3)39

5.4 Environmental Methods and Method Validation (ISO/IEC 17025/2005(E), Clause 5.4) 39

5.5 Calibration Requirements (ISO/IEC17025:2005(E) Clause 5.5)

5.6 Measurement Traceability (ISO/IEC 17025:2005(E), Clause 5.6)

5.7 Collection of Samples (ISO/IEC 17025:2005(E), Clause 5.7)

5.8 Handling Samples and Test Items (ISO/IEC 17025:2005(E), Clause 5.8)

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5.9 Quality Assurance (QA) of Environmental Testing (ISO/IEC 17025:2005(E) Clause 5.9)

5.10 Reporting the Results (ISO/IEC 17025:2005(E) Clause 5.10)

6.0 HAZARDOUS AND RADIOACTIVE MATERIALS MANAGEMENT AND HEALTH AND

SAFETY PRACTICES (SECTION 6: DOE ONLY)

6.1 Radioactive Materials Management Plan

6.2 Waste Management Plan

6.3 Chemical Hygiene Plan (CHP)

6.4 Sample Receiving

VOLUME 1, MODULE 3: QUALITY SYSTEMS FOR ASBESTOS TESTING

1.0 ASBESTOS TESTING

1.1 Introduction

1.2 Scope

1.3 Terms and Definitions

1.4 Method Selection

1.5 Method Validation

1.6 Demonstration of Capability

1.7 Technical Requirements

VOLUME 1, MODULE 4: QUALITY SYSTEMS FOR CHEMICAL TESTING

1.0 CHEMICAL TESTING

1.1 Introduction

1.2 Scope

1.3 Terms and Definitions

1.4 Method Selection

1.5 Method Validation

1.6 Demonstration of Capability (DOC)

1.7 Technical Requirements

VOLUME 1, MODULE 5: QUALITY SYSTEMS FOR MICROBIOLOGICAL TESTING

VOLUME 1, MODULE 6: QUALITY SYSTEMS FOR RADIOCHEMICAL TESTING

1.0 RADIOCHEMICAL TESTING

1.1 Introduction

1.2 Scope

1.3 Terms and Definitions (DoD/DOE Clarification)

1.4 Method Selection

1.5 Method Validation

1.6 Demonstration of Capability (DOC)

1.7 Technical Requirements

1.8 Method Specific Directions DoD/DOE Requirements

VOLUME 1, MODULE 7: QUALITY SYSTEMS FOR TOXICITY TESTING

APPENDIX A: REPORTING REQUIREMENTS

1.0 COVER SHEET

2.0 TABLE OF CONTENTS

3.0 CASE NARRATIVE

4.0 ANALYTICAL RESULTS

5.0 SAMPLE MANAGEMENT RECORDS

6.0 QC INFORMATION

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7.0 DATA REPORTS FOR THIRD PARTY REVIEW OR VALIDATION

APPENDIX B: QUALITY CONTROL REQUIREMENTS

Table B-1. Organic Analysis by Gas Chromatography (GC) Table B-2. Organic Analysis by High-Performance Liquid Chromatography (HPLC) (Including Method 8330A) Table B-3. Nitroaromatics, Nitramines, and Nitrate Esters Analysis by HPLC, LC/MS, or LC/MS/MS (Method 8330B) Table B-4. Organic Analysis by Gas Chromatography/Mass Spectrometry (GC/MS) Table B-5. Dioxin/Furan Analysis by High-Resolution Gas Chromatography/Low- Resolution Mass Spectrometry (Method 8280) Table B-6. Dioxin/Furan Analysis by High-Resolution Gas Chromatography/High-Resolution Mass Spectrometry (Method 8290) Table B-7. Inorganic Analysis by Atomic Absorption Spectrophotometry (AA) Table B-8. Inorganic Analysis by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP/AES) Table B-9. Trace Metals Analysis by Inductively Coupled Plasma/Mass Spectrometry

(ICP/MS)

Table B-10. Inorganic Analysis by Colorimetric Hexavalent Chromium Table B-11. Cyanide Analysis Table B-12. Common Anions Analysis by Ion Chromatography (IC) Table B-13. Perchlorate by Mass Spectrometry Methods Table B-14. Chemical Warfare Agents by GC/MS Table B-15. Per- and Polyfluoroalkyl Substances (PFAS) Using Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS) With Isotope Dilution or Internal Standard Quantification in Matrices Other Than Drinking Water Table B-16. Alpha Spectrometry Table B-17. Gamma Spectrometry Table B-18. Gas Flow Proportional Counting Table B-19. Liquid Scintillation Counter Analysis Table B-20. Radon Scintillation (Ra-226 by Lucas Cell) Table B-21. GC/MS Analysis of Air Samples Table B-22. Organic Semi-Volatile Analysis by GC/MS in SIM Mode Table B-23. Incremental Sampling Methodology (ISM) Soil Preparation for Large Volume (1 kg or greater) Samples Other than Explosives

APPENDIX C: LABORATORY CONTROL SAMPLE (LCS) CONTROL LIMITS AND

REQUIREMENTS

1.0 INTRODUCTION

2.0 LCS LIMIT TABLES

Table C-1. Method 1668 Solid Matrix Table C-2. Method 1668 Aqueous Matrix Table C-3. Method 6010 Solid Matrix Table C-4. Method 6010 Aqueous Matrix Table C-5. Method 6020 Solid Matrix Table C-6. Method 6020 Aqueous Matrix Table C-7. Method 6850 Solid Matrix Table C-8. Method 6850 Aqueous Matrix Table C-9. Method 7196 Solid Matrix Table C-10. Method 7196 Aqueous Matrix Table C-11. Method 7470 - 7471 Series Solid Matrix

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Table C-12. Method 7470 - 7471 Series Aqueous Matrix Table C-13. Method 8015 (MOD) Solid Matrix Table C-14. Method 8015 (MOD) Aqueous Matrix Table C-15. Method 8081 Solid Matrix Table C-16. Method 8081 Aqueous Matrix Table C-17. Method 8082 Solid Matrix Table C-18. Method 8082 Aqueous Matrix Table C-19. Method 8141 Solid Matrix Table C-20. Method 8141 Aqueous Matrix Table C-21. Method 8151 Solid Matrix Table C-22. Method 8151 Aqueous Matrix Table C-23. Method 8260 Solid Matrix Table C-24. Method 8260 Aqueous Matrix Table C-25. Method 8270 Solid Matrix Table C-26. Method 8270 Aqueous Matrix Table C-27. Method 8270 SIM Solid Matrix Table C-28. Method 8270 SIM Aqueous Matrix Table C-29. Method 8290 Solid Matrix Table C-30. Method 8290 Aqueous Matrix Table C-31. Method 8310 Solid Matrix Table C-32. Method 8310 Aqueous Matrix Table C-33. Method 8321 Solid Matrix Table C-34. Method 8321 Aqueous Matrix Table C-35. Method 8330 Solid Matrix Table C-36. Method 8330 - 8330B Series Aqueous Matrix Table C-37. Method 8330B Solid Matrix Table C-38. Method 9010 - 9020 Series Solid Matrix Table C-39. Method 9010 - 9020 Series Aqueous Matrix Table C-40. Method 9056 Solid Matrix Table C-41. Method 9056 Aqueous Matrix Table C-42. Method RSK-175 Aqueous Matrix Table C-43. Method TO-15 Gas Matrix Table C-44. Method PFAS by LCMSMS Compliant with QSM Table B-15 Aqueous Matrix Table C-45. Method PFAS by LCMSMS Compliant with QSM Table B-15 Solid Matrix ... 329

APPENDIX D: NON-DESTRUCTIVE ASSAY (NDA)

1.0 QUALITY ASSURANCE

1.1 NDA System Calibration

1.2 NDA Method Detection Limit

1.3 Infinite Thickness

1.4 NDA Measurement Uncertainty

1.5 NDA Measurement Traceability

1.6 NDA Measurement System Software

1.7 Acceptable Knowledge

1.8 NDA Data Reporting, Review, and Verification

1.9 NDA Measurement Performance Evaluation

2.0 NDA QUALITY CONTROL

2.1 QC Procedures

2.2 NDA QC Requirements

3.0 QC ACTION LEVELS AND RESPONSE

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APPENDIX E: THE HANFORD ANALYTICAL SERVICES QUALITY ASSURANCE

REQUIREMENTS DOCUMENTS (HASQARD) SPECIFIC REQUIREMENTS CHECKLIST .. 358

Module 1

Acronym List

AA Atomic Absorption

AB Accreditation Body(ies)

AFFF Aqueous Film Forming Foam

AIHA American Industrial Hygiene Association

AK Acceptable Knowledge

ANSI American National Standards Institute

ASPM Analytical Services Program Manager

ASTM American Society for Testing and Materials

BFB Bromofluorobenzene

BS Blank Spike

BSC Background Subtraction Count

CAP Corrective Action Plan

CAS Chemical Abstracts Service

CCB Continuing Calibration Blank

CCV Continuing Calibration Verification

CCVRF Continuing Calibration Verification Response Factor

CFR Code of Federal Regulations

CHP Chemical Hygiene Plan

COC Chain of Custody

CPM Counts per Minute

CRM Certified Reference Material

CS Calibration Source

CSU Combined Standard Uncertainty

CWA Clean Water Act

DENIX DoD Environment, Safety, and Occupational Health Network and Information Exchange

DER Duplicate Error Ratio

DFTPP Decafluorotriphenylphoshpine

DL Detection Limit

DMC Deuterated Monitoring Compound

DMR-QA Discharge Monitoring Report - Quality Assurance

DOC Demonstration of Capability

DoD Department of Defense

DOE Department of Energy

DOECAP Department of Energy Consolidated Audit Program

DOECAP-AP Department of Energy Consolidated Audit Program Accreditation Program

DOE-DQW Department of Energy Data Quality Workgroup

DOT Department of Transportation

ECHO EPA’s Public Domain Enforcement and History Online

EDQW Environmental Data Quality Workgroup

EICP Extracted Ion Current Profile

EIS Extracted Internal Standard

ELAP Environmental Laboratory Accreditation Program

EM Electron Multiplier

EMPC Estimated Maximum Possible Concentration

EPA Environmental Protection Agency

EQL Estimated Quantitation Limit

FAQ Frequently Asked Questions

FLAA Flame Atomic Absorption

FTS Fluorotelomersulfonate

FWHM Full Width at Half Maximum g gram

GC Gas Chromatography

GC/MS Gas Chromatography/ Mass Spectrometry

GFAA Graphite Furnace Atomic Absorption

HASQARD Hanford Analytical Services Quality Assurance Requirements Documents

HAZWOPER Hazardous Waste Operator and Emergency Response

HPLC High Performance Liquid Chromatography

HRCC High-Resolution Concentration Calibration

ICAL Initial Calibration

ICALCT Initial Calibration - Cross-Talk Factors

ICALE Initial Calibration - Efficiency

ICALSA Initial Calibration - Self-Absorption Curve

ICB Initial Calibration Blank

ICC Instrument Contamination Check

ICP Inductively Coupled Plasma

ICP-AES Inductively Coupled Plasma - Atomic Emission Spectroscopy

ICP-MS Inductively Coupled Plasma - Mass Spectrometry

ICS Interference Check Solution

ICV Initial Calibration Verification

ID Identification

IDOC Initial Demonstration of Capability

IEC International Electrotechnical Commission

IECV Efficiency Calibration Verification

IEEE Institute of Electrical and Electronics Engineers

ILAC International Laboratory Accreditation Cooperation

IS Internal Standard

ISC Instrument Sensitivity Check

ISM Incremental Sampling Method

ISO International Organization for Standardization

IT Information Technology keV Kilo electron-volts (one thousand (103) electron-volts)

LC Liquid Chromatography

LC/MS Liquid Chromatography/ Mass Spectrometry

LC/MS/MS Liquid Chromatography/ Mass Spectrometry/ Mass Spectrometry

LCS Laboratory Control Sample

LCSD Laboratory Control Sample Duplicate

LDR Linear Dynamic Range

LIMS Laboratory Information Management System

LLCCV Low-Level Calibration Check Standard

LLD Lower Limit of Detection

LLQ Lower Limit of Quantitation

LOD Limit of Detection

LOQ Limit of Quantitation

LRB Laboratory Reagent Blank

MARLAP Multi-Agency Radiological Laboratory Analytical Protocols

MB Method Blank

MBM Method Background Measurement

MCA Multi-Channel Analyzer

MD Matrix Duplicate

MDA Minimum Detectable Activity

MDC Minimum Detectable Concentration

MDL Method Detection Limit

MeV Mega electron-volts (one million (106) electron-volts)

MPC Measurement Performance Criteria

MS Matrix Spike

MSA Method of Standard Additions

MSD Matrix Spike Duplicate

NBL New Brunswick Laboratory

NCSL Refers to National Conference of Standards Laboratories (now called NCSL International or NCSLI)

NDA Non-Destructive Assay

NELAC National Environmental Laboratory Accreditation Conference (now referred to only as The NELAC Institute, or TNI)

NELAP National Environmental Laboratory Accreditation Program

NEtFOSAA N-ethyl Perfouorooctanesulfonamidoacetic Acid

NFPA National Fire Protection Association

NIOSH National Institute for Occupational Safety and Health

NIST National Institute of Standards and Technology

NMeFOSAA N-methyl Perfluorooctanesulfonamidoacetic Acid

NMI National Metrological Institute

NOV Notice of Violation

NR Not reported

NRC Nuclear Regulatory Commission

PAH Polyaromatic Hydrocarbon

PCB Polychlorinated byphenyl

PCDD Polychlorinated dibenzodioxins

PCDF Polychlorinated dibenzofurans

PDS Post Digestion Spike

PE Performance Evaluation

PFAS Per- and Poly-fluoroalklyl Substances

PFBA Perfluorobutyric Acid

PFBS Perfluorobutanesulfonic Acid

PFHxS Perfluorohexanesulfonic Acid

PFOA Perfluorooctanoic Acid

PFOS Perfluorooctanesulfonic Acid

PFPeA Perfluoropentanoic Acid

POTW Publicly Owned Treatment Works

PPE Personal Protective Equipment

PPM Parts Per Million

PT Proficiency Testing

PTOB/PTPA Proficiency Testing Oversight Body/ Proficiency Testing Provider Accreditor

QA Quality Assurance

QAPP Quality Assurance Project Plan

QC Quality Control

QCAL Method Calibration - Quench Curve

QSM Quality Systems Manual

RCRA Resource Conservation and Recovery Act

RF Response Factor

RL Reporting Limit

RML Radioactive Materials License

ROI Regions of Interest

RPD Relative Percent Difference

RRF Relative Response Factor

RRT Relative Retention Time

RSD Relative Standard Deviation

RSO Radiation Safety Officer

RT Retention Time

S/N Signal to Noise Ratio

SAP Sampling and Analysis Plan

SD Standard deviation

SDG Sample Delivery Group

SDWA Safe Drinking Water Act

SI Système International d’unitès (International System of Units)

SICP Selected Ion Current Profile

SIM Selected Ion Monitoring

SNM Special Nuclear Material

SOP Standard Operating Procedure

SPE Solid Phase Extraction

SQA Software Quality Assurance

STS Sample Test Source

TCE Trichloroethylene

TEQ Toxicity Equivalents

TIC Tentatively Identified Compound

TMU Total Measurement Uncertainty

TNI The NELAC Institute

TPU Total Propagated Uncertainty

TSCA Toxic Substances Control Act

TSDF Treatment, Storage, and Disposal Facility

USDOE United States Department of Energy

USEPA United States Environmental Protection Agency

UV Ultraviolet

V&V Verification and Validation

VOA Volatile Organic Analysis

VOC Volatile Organic Compounds

WET Whole Effluent Toxicity

WP Water Pollution

WRM Working Reference Material

WS Water Supply

Volume 1, Module 1: Proficiency Testing (PT)

1.0 INTRODUCTION

This module provides baseline requirements for proficiency testing for laboratories performing analytical testing services for the Department of Defense (DoD) and the Department of Energy

(DOE). This module supersedes the entirety of Volume 1, Module 1 of The NELAC

Institute (TNI) standards (September 2009), which incorporates ISO/IEC 17025:2005(E).

2.0 REQUIREMENTS FOR ACCREDITATION (Section 2: DoD

Only)

2.1 Initial Accreditation

2.1.1 Initial Accreditation for DoD ELAP

To obtain initial accreditation for the Department of Defense Environmental Laboratory

Accreditation Program (DoD ELAP), the laboratory shall analyze at least two Proficiency Testing

(PT) samples for each combination of analyte-matrix-method (e.g., Trichloroethylene (TCE)-water-Method 624, TCE-water-Method 8260, TCE-soil-Method 8260, lead-soil-Method 6010, or lead-soil-Method 6020) that corresponds to its scope of accreditation. Laboratories that combine multiple methods into one Standard Operating Procedure (SOP) (e.g., SOP that combines

Method 624 volatiles & Method 8260 volatiles) can report those methods with a single PT sample. All other analyte-matrix-method combinations require unique PT samples.

2.1.2 PT Samples for Initial Accreditation

The PT samples used for initial accreditation shall be obtained from PT providers that are accredited under International Organization for Standardization/International Electrotechnical

Commission (ISO/IEC) 17043:2010(E) (General Requirements for Proficiency Testing) from an

International Laboratory Accreditation Cooperation (ILAC) approved signatory Accreditation

Body (AB).

2.1.3 PT Samples not from ISO/IEC 17043:2010(E) Accredited PT Provider

When PT samples cannot be obtained from an ISO/IEC 17043:2010(E) accredited PT provider, the laboratory shall obtain permission to use non- ISO/IEC 17043:2010(E) PT providers from their AB prior to analyzing the PT sample. The requirements and criteria from the PT provider must be met by the laboratory for the PT sample to be considered successful.

2.1.4 PT Samples for Analyte-matrix-method not from PT Provider

When PT samples for an analyte-matrix-method combination cannot be obtained from any PT provider, and the analyte-matrix-method combination is required for a scope of accreditation, the laboratory shall submit this fact in writing to their DoD ELAP AB. Other measures (e.g., precision, bias, and selectivity) as outlined in the 2009 TNI Standard Test Modules 3-7 must be performed to satisfy the PT requirement until those PT samples are available.

2.1.5 Analysis Date of PT Samples

The PT samples analyzed by the laboratory for initial DoD ELAP accreditation shall be no more than 12 months old. The analysis date between PT samples shall be at least 15 calendar days apart if two or more successive PT samples are performed.

2.1.6 PT Study Determination

The success or failure of any analyte-matrix-method combination for a PT study shall be determined by the PT provider under the requirements of the governing regulatory or ISO/IEC

17043:2010(E) statistically derived program.

2.1.7 PT Samples Same as Regular Environmental Samples

PT samples must be analyzed and evaluated in the same manner as regular environmental samples. A laboratory shall employ the same quality control, sequence of preparation and analytical steps, and replicates as used when analyzing routine samples.

2.2 Continuing Accreditation

2.2.1 Maintaining Accreditation

To maintain DoD ELAP accreditation, the laboratory shall successfully analyze at least two PT samples per calendar year for each analyte-matrix-method combination on their scope of accreditation. These PT samples shall be analyzed not less than 4 months and not to exceed 8 months apart. A PT sample for Whole Effluent Toxicity (WET) testing is required at least once per year.

2.2.2 Laboratory PT History

The laboratory shall maintain a history of at least two (2) successful PT rounds out of the most recent three (3) attempts for each analyte-matrix-method combination on their scope of accreditation. If PT samples are required for corrective action to reestablish history of successful

PT rounds, the analysis dates of successive corrective action PT samples shall be at least 15 calendar days apart.

2.2.3 Failure to Meet Criteria

Analyte-matrix-method combinations that do not meet the above criteria must be removed from the DoD ELAP scope of accreditation.

2.2.4 PT Samples Same as Regular Environmental Samples

3.0 REQUIREMENTS FOR PARTICIPATION (Section 3: DOE

Only)

3.1 Initial Accreditation

3.1.1 Initial Accreditation for DOECAP-Accreditation Program

To obtain initial accreditation for the Department of Energy Consolidated Audit Program-

Accreditation Program (DOECAP-AP), the laboratory shall analyze at least two Proficiency

Testing (PT) samples for each combination of analyte-matrix-method that corresponds to its scope of accreditation. Laboratories that combine multiple methods into one Standard

Operating Procedure (SOP) (e.g., SOP that combines Method 624 volatiles and Method 8260 volatiles) can report those methods with a single PT sample provided the strictest Quality

Control (QC) criteria are applied. All other analyte-matrix-method combinations may require other applicable PT samples as discussed under Section 3.1.2 below.

The laboratory shall demonstrate successful participation for a minimum of one year in an

ISO/IEC 17043:2010(E) accredited PT program. The single blind studies must be related to regulatory or environmental programs, analytes, matrix types, and methods for each of the analytical disciplines (i.e., inorganic, organic, radiochemistry, biological, etc.) that each laboratory will perform in support of DOE sites. A laboratory is required to analyze PT samples in matrices containing analytes listed on the accreditation scope using methodology applicable to data they report under DOE contracts, where available. PT samples must be tested and evaluated in the same manner as regular environmental samples.

3.1.2 PT Samples for Initial Inclusion

PT providers will be required to maintain proficiency in an ISO/IEC 17043:2010(E) accredited

PT program for all analytes, matrices, and methods that are included in the laboratory’s scope of work as defined in the subcontracts issued by DOE sites. A laboratory must possess a radioactive materials license from the Nuclear Regulatory Commission, an Agreement State, or a DOE exemption authorized by the contract holder to receive PT samples that contain radiological materials.

Other programs (such as Drinking Water) require program-specific PT samples.

3.1.3 PT Samples not from an ISO/IEC 17043:2010(E) Accredited PT Provider

When PT samples cannot be obtained from an ISO/IEC 17043:2010(E) accredited PT provider, the laboratory shall obtain permission to use non- ISO/IEC 17043:2010(E) PT providers from their AB prior to analyzing the PT sample. The requirements and criteria from the AB and the PT provider must be met by the laboratory for the PT sample to be considered successful.

3.1.4 PT Samples for Analyte-Matrix-Method not from a PT Provider

When PT samples for an analyte-matrix-method combination cannot be obtained from any PT provider, and the analyte-matrix-method combination is required for a scope of accreditation, the laboratory shall submit this fact in writing to their DOECAP-AP Accreditation Body (AB).

Other measures (e.g., precision, bias, and selectivity) as outlined in the appropriate 2009 TNI

Standard Test Modules must be performed to satisfy the PT requirement until those PT samples are available.

3.1.5 Analysis Date of PT Samples

The PT sample analysis dates by the laboratory for initial DOECAP-AP accreditation shall be no more than 12 months old. The analysis date between PT samples shall be at least 7 calendar days apart if two or more successive PT samples are performed.

3.1.6 PT Study Determination

The success or failure of any analyte-matrix-method combination for a PT study shall be determined by the PT provider under the requirements of the governing regulatory or ISO/IEC

3.1.7 PT Samples Same as Regular Environmental Samples

PT samples must be tested and evaluated in the same manner as regular environmental samples. A laboratory shall employ the same quality control, sequence of preparation and analytical steps, and replicates as used when analyzing routine samples from DOE sites for the purposes of achieving accreditation.

3.2 Continued Participation

3.2.1 Maintaining Participation

The laboratory shall demonstrate continued proficiency throughout the term of the contract award. In addition, the client reserves the right to submit blind PT samples. Each laboratory shall continue to participate in all applicable rounds of external PT programs.

To maintain DOECAP-AP accreditation, the laboratory shall successfully analyze at least two

PT samples, where available, per calendar year for each analyte-matrix-method combination on their scope of accreditation. Each PT sample shall be analyzed approximately six months apart

(any time frame from four to eight months apart is considered acceptable) if two PT samples are analyzed.

3.2.2 Laboratory PT History

The laboratory shall maintain a history of at least two (2) successful PT rounds out of the most recent three (3) attempts for each analyte-matrix-method combination on their scope of accreditation.

3.2.3 Reporting Requirements to DOE Sites

The results of all PT programs will be utilized in the reports produced for DOE and the sites that have contracts with the laboratory. PT results from commercial PT studies will be provided to the Laboratory’s applicable DOE contract holder sites no later than 10 days of receipt of results from the PT provider from the most recent PT study.

3.2.4 Failure to Meet Criteria

Any applicable analyte for which individual laboratory results are entered as NR or “not reported” will not be considered an acceptable result unless it is a remedial PT study. The success or failure of any analyte-matrix-method combination for a PT study shall be determined by the PT provider under the requirements of the governing regulatory or ISO/IEC

If the laboratory fails two consecutive evaluations or two (2) out of three (3) attempts, the laboratory should not receive samples from DOE sites for analysis by the failed analyte-matrix-method combination until acceptable PT performance has been achieved. However, the decision to withhold sample shipments will be at the discretion of the individual DOE contract holder. Analyte-matrix-method combinations that do not meet the above criteria must be removed from the DOECAP-AP scope of accreditation by the Accrediting Body.

The laboratory can demonstrate proficiency in remedial PT studies by acceptable performance in an unscheduled evaluation by the same PT program or by participation in the next regularly scheduled study. The use of quick turnaround and remedial samples will be acceptable, but the

PT samples are included in the number of possible attempts at maintaining proficiency (i.e., receiving acceptable performance in two out of the last three rounds by analyte-matrix-method of proficiency testing reported). PT samples are required for corrective action to reestablish history of successful PT performance. The analysis dates of successive corrective action PT samples shall be at least 15 calendar days apart.

3.2.5 PT Samples Same as Regular Environmental Samples

Module 2

Volume 1, Module 2: Quality Systems General Requirements

1.0 INTRODUCTION, SCOPE, AND APPLICABILITY

1.1 Introduction

No additions or clarifications were made to this section. TNI and ISO/IEC 17025:2005(E) standards shall be followed.

1.2 Scope DoD/DOE (Clarification)

The following is a clarification of TNI section 1.2:

The Department of Defense (DoD) Environmental Data Quality Workgroup (EDQW) and the

Department of Energy (DOE) Consolidated Audit Program (DOECAP) participants developed the DoD/DOE Quality Systems Manual (QSM). This manual provides baseline requirements for the establishment and management of quality systems for laboratories performing analytical testing services for the DoD and the DOE. This manual is based on Volume 1 of The NELAC

Institute (TNI) Standards (September 2009), which incorporates ISO/IEC 17025:2005(E), General requirements for the competence of testing and calibration laboratories. Conformance to the requirements contained in this manual is mandatory for any laboratory that is 1) seeking or maintaining accreditation in accordance with the DoD Environmental Laboratory Accreditation

Program (ELAP) or 2) seeking or maintaining accreditation in accordance with the DOE

Consolidated Audit Program Accreditation Program (DOECAP-AP) requirements and all applicable qualifications in accordance with the DOECAP and DOE related contract awards for analytical services and industrial hygiene testing. Laboratories that comply with the requirements of this manual must also comply with the TNI standards (September 2009) and

ISO/IEC 17025:2005(E) unless superseded by this document. All references to the term

“accreditation” in this manual refer to the DoD ELAP and the DOECAP-AP.

This manual is presented in a format which is designed for use in conjunction with the TNI

(September 2009) and ISO/IEC 17025:2005(E) standards. Updated requirements from the

ISO/IEC 17025:2017 standard are referenced by grey boxes. DoD/DOE specific language is presented as text and appendices in the order in which topics are addressed in the TNI standards. DoD/DOE text contains additional requirements, clarifications, and guidance to supplement the TNI and ISO/IEC language. Information that may be beneficial to a laboratory, but is not required, is marked as guidance. To the extent possible, DoD and DOE requirements have been consolidated. Text or appendices that are unique to either DoD or DOE are marked as such.

The DoD/DOE QSM is international in scope and applies to all laboratories regardless of size or complexity. Nothing in this document relieves any laboratory from complying with more stringent contract specifications, host-nation final governing standards, or federal, state, tribal, and local regulations.

To ensure that laboratories are capable of generating data that will meet project-specific requirements, the EDQW and the DOECAP Data Quality Workgroup (DOE-DQW) strongly encourages the involvement of project chemists and laboratories during project-planning activities.

DOE Only (Clarification): Laboratories must follow the requirements of DOE Order 414.1B, C, or D as part of the laboratory contract. The DOECAP-AP will be an acceptable replacement to all references to the DOECAP program. DOECAP participation includes active participation in the DOECAP-AP.

2.0 NORMATIVE REFERENCES (ISO/IEC 17025:2005(E),

Clause 2)

3.0 TERMS AND DEFINITIONS

3.1 Additional Terms and Definitions

The following are DoD/DOE clarifications and additions to TNI section 3.1:

Accreditation: Refers to accreditation in accordance with the DoD ELAP and the DOECAP-AP as applicable.

Box 1

The following shall be implemented in addition to TNI section 1.2:

ISO/IEC 17025:2017(E) section 1

Box 2

The following shall be implemented in addition to TNI section 2.0:

ISO/IEC 17025:2017(E) section 2

Accreditation Body (AB): Entities recognized in accordance with the DoD ELAP and the

DOECAP-AP that are required to operate in accordance with ISO/IEC 17011, Conformity assessment: General requirements for accreditation bodies accrediting conformity assessment bodies. The AB must be a signatory, in good standing, to the International Laboratory

Accreditation Cooperation (ILAC) mutual recognition arrangement (MRA) that verifies, by evaluation and peer assessment, that its signatory members are in full compliance with ISO/IEC

17011 and that its accredited laboratories comply with ISO/IEC 17025.

Aliquot: A discrete, measured, representative portion of a sample taken for analysis.

Analytical Method: A formal process that identifies and quantifies the chemical components of interest (target analytes) in a sample.

Analysis: A combination of sample preparation and instrument determination.

Analyte: The specific chemicals or components for which a sample is analyzed; it may be a group of chemicals that belong to the same chemical family and are analyzed together.

Assessment (Clarification): Assessment is an all-inclusive term used to denote any of the following: audit, performance evaluation, peer review, inspection, or surveillance conducted on-site.

Blank (Clarification): Blank samples are negative control samples, which typically include field blank samples (e.g., Trip Blank, Equipment (rinsate) Blank, and Temperature Blank) and laboratory blank samples (e.g., Method Blank, Reagent Blank, Instrument Blank, Calibration

Blank, and Storage Blank).

Calibration Range: The range of values (concentrations) between the lowest and highest calibration standards of a multi-level calibration curve. For metals analysis with a single-point calibration, the low-level calibration check standard and the high standard establish the linear calibration range, which lies within the linear dynamic range.

Confirmation (Clarification): Includes verification of the identity and quantity of the analyte being measured by another means (e.g., by another determinative method, technology, or column). Additional cleanup procedures alone are not considered confirmation techniques.

Consensus Standard: A standard established by a group representing a cross-section of a particular industry or trade, or a part thereof.

Continuing Calibration Verification: The verification of the initial calibration. Required prior to sample analysis and at periodic intervals. Continuing calibration verification applies to both external standard and internal standard calibration techniques, as well as to linear and non-linear calibration models.

Correction: Action taken to eliminate a detected non-conformity.

Corrective Action: The action taken to eliminate the causes of an existing nonconformity, defect, or other undesirable situation in order to prevent recurrence. A root cause analysis may not be necessary in all cases.

Customer: Any individual or organization for which products or services are furnished or work performed in response to defined requirements and expectations.

Definitive Data: Analytical data of known quantity and quality. The levels of data quality on precision and bias meet the requirements for the decision to be made. Data that is suitable for final decision-making.

Demonstration of Capability (Clarification): A procedure to establish the ability of the analyst to generate analytical results by a specific method that meet measurement quality objectives

(e.g., for precision and bias).

Detection Limit (DL): The smallest analyte concentration that can be demonstrated to be different from zero or a blank concentration with 99% confidence. At the DL, the false positive rate (Type I error) is 1%. A DL may be used as the lowest concentration for reliably reporting a detection of a specific analyte in a specific matrix with a specific method with 99% confidence.

Deuterated Monitoring Compounds (DMCs): SIM specific surrogates as specified for GC/MS

SIM analysis.

Digestion: A process in which a sample is treated (usually in conjunction with heat and acid) to convert the target analytes in a sample to a more easily measured form.

Documents: Written components of the laboratory management system (e.g., policies, procedures, and instructions).

Environmental Data: Any measurements or information that describe environmental processes, locations, or conditions; ecological or health effects and consequences; or the performance of environmental technology.

Extracted Internal Standard Analyte: Isotopically labeled analogs of analytes of interest added to all standards, blanks and samples analyzed. Added to samples and batch QC samples prior to the first step of sample extraction and to standards and instrument blanks prior to analysis. Used for isotope dilution methods.

False Negative: A result that fails to identify (detect) an analyte or reporting an analyte to be present at or below a level of interest when the analyte is actually above the level of interest.

False Positive: A result that erroneously identifies (detects) an analyte or reporting an analyte to be present above a level of interest when the analyte is actually present at or below the level of interest.

Finding (Clarification): An assessment conclusion that identifies a condition having a significant effect on an item or activity. An assessment finding may be positive, negative, or neutral and is normally accompanied by specific examples of the observed condition. The finding must be linked to a specific requirement (e.g., this standard, ISO requirements, analytical methods, contract specifications, or laboratory management systems requirements).

Holding Times (Clarification): The maximum time that may elapse from the time of sampling to the time of preparation or analysis, or from preparation to analysis, as appropriate.

Improper Actions: Intentional or unintentional deviations from contract-specified or method-specified analytical practices that have not been authorized by the customer (i.e., DoD or DOE).

Incremental Sampling Method (ISM): Structured composite sampling and processing protocol having specific elements designed to reduce data variability and increase sample representativeness for a specified volume of soil under investigation.

Initial Calibration Verification (ICV): Verifies the initial calibration with a standard obtained or prepared from a source independent of the source of the initial calibration standards to avoid potential bias of the initial calibration.

Injection Internal Standard Analyte: Isotopically labeled analogs of analytes of interest (or similar in physiochemical properties to the target analytes but with a distinct response) to be quantitated. Added to all blanks, standards, samples and batch QC after extraction and prior to analysis.

Internal Standard: A known amount of standard added to a test portion of a sample as a reference for evaluating and controlling the precision and bias of the applied analytical method.

Laboratory Information Management Systems (LIMS): The entirety of an electronic data system (including hardware and software) that collects, analyzes, stores, and archives electronic records and documents.

Limits of Detection (LOD) (Clarification): The smallest concentration of a substance that must be present in a sample in order to be detected at the DL with 99% confidence. At the

LOD, the false negative rate (Type II error) is 1%. A LOD may be used as the lowest concentration for reliably reporting a non-detect of a specific analyte in a specific matrix with a specific method at 99% confidence.

Limits of Quantitation (LOQ) (Clarification): The smallest concentration that produces a quantitative result with known and recorded precision and bias. For DoD/DOE projects, the

LOQ shall be set at or above the concentration of the lowest initial calibration standard and within the calibration range.

Linear Dynamic Range (LDR): Concentration range where the instrument provides a linear response.

Measurement System (Clarification): A test method, as implemented at a particular laboratory, and which includes the equipment used to perform the sample preparation and test and the operator(s).

Measurement Uncertainty: An estimate of the error in a measurement often stated as a range of values that contain the true value within a certain confidence level. The uncertainty generally includes many components which may be evaluated from experimental standard deviations based on repeated observations or by standard deviations evaluated from assumed probability distributions based on experience or other information. For DoD/DOE, a laboratory’s Analytical

Uncertainty (such as use of LCS control limits) can be reported as the minimum uncertainty.

Operator Aid: A technical posting (such as poster, operating manual, or notepad) that assists workers in performing routine tasks. All operator aids must be controlled documents (i.e., a part of the laboratory management system).

Preservation (Clarification): Any conditions under which a sample must be kept in order to maintain chemical, physical, and/or biological integrity prior to analysis.

Qualitative Analysis: Analysis designed to identify the components of a substance or mixture.

Quality System Matrix (Clarification): The matrix definitions in the TNI standard shall be used for purposes of batch and quality control requirements and may be different from a field of accreditation matrix.

Quantitation Range: The range of values (concentrations) in a calibration curve between the

LOQ and the highest successfully analyzed initial calibration standard used to relate instrument response to analyte concentration. The quantitation range (adjusted for initial sample volume/weight, concentration/dilution and final volume) lies within the calibration range.

Quantitative Analysis: Analysis designed to determine the amounts or proportions of the components of a substance.

Records: The output of implementing and following management system documents (e.g., test data in electronic or hand-written forms, files, and logbooks).

Reporting Limit: A customer-specified lowest concentration value that meets project requirements for quantitative data with known precision and bias for a specific analyte in a specific matrix.

Selected Ion Monitoring (SIM): Using GC-MS, characteristic ions specific to target compounds are detected and used to quantify in applications where the normal full scan mass spectrometry results in excessive noise.

Signal to Noise Ratio (S/N): S/N is a measure of signal strength relative to background noise.

The average strength of the noise of most measurements is constant and independent of the magnitude of the signal. Thus, as the quantity being measured (producing the signal) decreases in magnitude, S/N decreases and the effect of noise on the relative error of a measurement increases.

Storage Blank: A sample of analyte-free media prepared by the laboratory and retained in the sample storage area of the laboratory. A Storage Blank is used to record contamination attributable to sample storage at the laboratory.

Surrogate: A substance with properties that mimic the analyte of interest. It is unlikely to be found in environmental samples and is added to them for quality control purposes.

Target Analytes: Analytes or chemicals of primary concern identified by the customer on a project-specific basis.

Test Method: A definitive procedure that determines one or more characteristics of a given substance or product.

Third Party: An entity who may be indirectly involved but is not a principal party to environmental testing (i.e., reference material provider, accrediting body, data validator, etc.).

Unethical Actions: Deliberate falsification of analytical or quality control results where failed method or contractual requirements are made to appear acceptable.

Validation: The confirmation by examination and provision of objective evidence that the particular requirements for a specific intended use are fulfilled.

3.2 Sources

No additions or clarifications were made to this section. TNI 2009 and ISO/IEC 17025:2005(E)

3.3 Exclusions and Exceptions

Box 3

The following shall be implemented in addition to TNI section 3.1:

ISO/IEC 17025:2017(E) section 3

4.0 MANAGEMENT REQUIREMENTS

4.1 Organization (ISO/IEC 17025:2005(E), Clause 4.1)

4.1.5 DoD/DOE Requirement

The following shall be implemented in addition to ISO Clause 4.1.5 j):

j) At a minimum, the following laboratory management staff (however named) shall be considered key managerial personnel:

i) Management (e.g., President, Chief Executive Officer, Chief Operating Officer, Laboratory Director);

ii) Technical Managers (e.g., Technical Director, Section Supervisors);

iii) Quality Managers;

iv) Support Systems and Administrative Managers (e.g., Laboratory Information

Management System (LIMS) manager, purchasing manager, project managers); and

v) Customer Services Managers.

4.1.7.1 DoD/DOE Requirement

The following shall be implemented in addition to TNI sections 4.1.7.1 a) through h):

i) implement, maintain, and improve the management system by using available tools such as audit and surveillance results, control charts, proficiency testing results, data analysis, corrective and preventive actions, customer feedback, and management reviews in efforts to monitor trends.

Box 4

The following shall be implemented in addition to ISO/IEC 17025:2005(E) Clause 4.1:

ISO/IEC 17025:2017(E) sections 4.1, 4.2, 5.3, and 5.4

Box 5

The following shall be implemented in addition to ISO/IEC 17025:2005(E) Clause 4.1.5:

ISO/IEC 17025:2017(E) sections 6.2.3, 6.2.4, and 6.2.5.d)

4.2 Management (ISO/IEC 17025:2005(E), Clause 4.2)

4.2.1 DoD/DOE Requirement

The following shall be implemented in addition to ISO Clause 4.2.1:

Copies of all management system documentation provided to DoD ELAP ABs, DOECAP-AP, or to personnel on behalf of DoD/DOE shall be in English.

4.2.2 DoD/DOE Requirement

4.2.3 DoD/DOE Requirement

The following shall be implemented in addition to ISO Clause 4.2.3:

Top management (including 4.1.5 j) i) through iii)) shall be responsible for:

a) defining the minimum qualifications, experience, and skills necessary for all positions in the laboratory;

b) ensuring that all laboratory technical staff have demonstrated capability in the activities for which they are responsible. Such demonstration shall be recorded;

c) ensuring that the training of each member of the technical staff is kept up-to-date (on-going) by the following:

i) each employee training file must contain a certification that the employee has read, understands, and is using the latest version of the management system records relating to his/her job responsibilities;

ii) training courses or workshops on specific equipment, analytical techniques, or laboratory procedures shall all be recorded; and

iii) review of analyst work by relevant technical managers on an on-going basis is recorded or another…