Exhibit D - Scope of Work and Technical Specifications.pdf

Exhibit D, Scope of Work and Technical Specifications Rev 0, October 17, 2018

Attachment 1

Subcontract No. 250953

DATED: August 31, 2018, Rev. 0

Exhibit “D”

Scope of Work and Technical Specifications for

Off-Site Analytical Laboratory Services

CONTENTS

1.0 INTRODUCTION AND BACKGROUND

2.0 STATEMENT OF WORK

2.1 General Requirements

2.1.1 Sample Throughput Requirements

2.2 Corrections to Electronic Data and Hard Copy Deliverable

2.2.1 Requirements 7

2.3 Radioactive Materials License

2.3.1 Requirements 7

2.4 Analysis Requests

2.4.1 Work Orders 8

2.5 Time Definitions

2.5.1 Requirements 8

2.6 Request for Reanalysis

2.6.1 Incomplete Reports and Errors

2.6.2 Nonstandard Analyses

2.7 Personnel Requirements

3.1 General Data-Quality Objectives (DQO)

3.1.1 Methods, Quality Control, and Documentation

3.2 Certification and Accreditations

3.2.1 Requirements

3.3 SUBCONTRACTOR Laboratory Quality Assurance Plan

3.3.1 Specific Requirements

3.3.2 STANDARD OPERATING PROCEDURES (SOP) Support for the LQAP

3.4 Performance Evaluation Sample Analysis Requirement

3.4.1 Analytical Requirements

3.4.2 Proficiency

3.5 Systems and Internal Audit Requirements

3.5.1 Annual Systems Audits

3.5.2 On-Site Data Package Review

3.5.3 Internal Audits

3.6 Participation in Inter-Laboratory Comparison Studies

3.6.1 Required Intercomparison Programs

3.6.2 Reporting Intercomparison Results

3.7 Employee Training and Documenting Employee Proficiency

3.7.1 Training in Radiation Safety Practices and Techniques

3.8 SUBCONTRACTOR Instrumentation, Equipment, and Reagent Maintenance

3.8.1 Instrument Logs and Response Checks

3.8.2 Balances, Volumetric Pipettes, and Sample Storage Refrigerators

3.8.3 Reagent Water Production

3.8.4 Control of Standards

3.8.5 Glassware

3.8.6 Incident Tracking

3.9 Analytical and Quality Assurance Standard Operating Procedures

3.9.1 Control of SOPs

3.9.2 Availability of SOPs

3.9.3 Analyst Familiarity with SOPS

3.10 Sample Receipt and Storage Requirements

3.10.1 Chain-of-Custody Forms

3.10.2 Acknowledgment of Sample Receipt

3.10.3 Documentation of Anomalies

3.10.4 Communication of Anomalies

3.10.5 Sample Retention

3.10.6 Sample Disposal

3.10.7 Return of Shipping Coolers

3.11 Analytical Holding-Time Requirements

3.11.1 CONTRACTOR Holding Times

3.11.2 Definition

3.11.3 Matrix Types

3.11.4 Meeting Holding Times

3.11.5 Violations

3.12 SUBCONTRACTOR Data Verification and Review Requirements

3.12.1 Worksheet Review

3.12.2 Report Review

3.13 SUBCONTRACTOR Record Maintenance Requirements

3.13.1 Case Files

3.14 Corrective Action for Out-of-Control Events

3.14.1 Requests for CARs

3.14.2 Delivery of CARs

3.14.3 QPR Requirement Contents

3.15 Good Automated Laboratory Practices

3.15.1 Integrity of Software and Information

3.15.2 SUBCONTRACTOR Management

3.15.3 Personnel

3.15.4 QA

3.15.5 Electronic Data

3.15.6 Software

3.15.7 Security

3.15.8 Hardware Communications Components

3.15.9 Comprehensive Testing

3.15.10 Records Retention

3.15.11 Facilities

3.15.12 SOPs

3.16 Records for Method Development and Initial Demonstration of Proficiency

3.16.1 Records Tracking and Retrieval System

4.0 SPECIFICATIONS: ANALYTICAL AND QC REQUIREMENTS

4.1 Standard Preparation and Instrument Calibration Requirements

4.1.1 Working Standards

4.1.2 Calibration

4.2 Sample Analysis Requirements

4.2.1 Worksheet Requirements

4.2.2 Sample Preparation

4.2.3 Initial Dilution of Samples

4.2.4 Analytical Techniques and SOPS

4.3 Detection Limits, Reporting Requirements, and QC Exemptions

4.3.1 MDL Determination

4.3.2 PQLs

4.3.3 Reporting Conventions

4.3.4 Radiochemistry Detection Limits

4.3.5 QC Exemption for Filters

4.3.6 QC Exemption for Physical Parameters

4.3.7 Batch QC Requirements

4.3.8 Additional Requirements for Fluoride Run by IC

4.3.9 Elevating the MDL for a Particular Analyte

4.4 General Inorganic Analytical QC Requirements

4.4.1 Exemption from Reanalysis

4.4.2 Calibration Verification for ICV and CCV samples

4.4.3 Calibration Blanks

4.4.4 Preparation Blanks

4.4.5 Interference Check Samples

4.4.6 Serial Dilution

4.4.7 Linear Range Verification

4.4.8 Laboratory Control Samples

4.4.9 Replicate Analyses

4.4.10 Spiked Sample Analyses

4.4.11 Reporting Limit Verification Analyses

4.4.12 Perchlorate Analysis

4.4.13 Uranium Isotope Analysis

4.5 Organic Analytical and QC Requirements

4.5.1 Methods of Analysis

4.5.2 Required Target Analytes and Target MDLS

4.5.3 Instrument Calibration

4.5.4 Calibration Acceptance Criteria

4.5.5 Low-Concentration Soil VOC Analysis Calibration

4.5.6 Quantitation of Optional Compounds

4.5.7 Sample Preparation

4.5.8 Blank Analysis

4.5.9 MS and MSD Analyses

4.5.10 LCS Analysis

4.5.11 Second-Column or GC-MS Confirmation

4.5.12 Process Artifacts

4.5.13 Method-Specific Analytical Requirements

4.6 Radiochemistry Analytical QC Requirements

4.6.1 Radiological Safety Plan

4.6.2 Calibration Verification

4.6.3 Preparation Blanks

4.6.4 Laboratory Control Samples

4.6.5 Replicate Analyses

4.6.6 Spiked Sample Analyses

4.6.7 Chemical Recovery Requirements for Radionuclides

4.6.8 Blank Subtraction

4.6.9 Target MDAs

4.6.10 Counting Instrument Calibration Requirements

4.6.11 Reporting Nontarget Radionuclides in Gamma Spectroscopy

4.6.12 Reporting K-40 for Soils in Gamma Spectroscopy

4.6.13 Gross Alpha/Beta Planchette Flaming

4.7 Asbestos Analysis

4.7.1 Accreditation

4.7.2 Staff Qualifications

4.7.3 Quality Control

4.8 Low-Level Tritium

4.8.1 Prescreen Samples

4.8.2 Method

4.9 Bioassay/Bioaccumulation and Phytotoxicity

4.9.1 Method

4.10 Dissolved Organic Carbon Fractionation

4.10.1 Method

4.11 Particle-Size Analyses

4.11.1 Method

4.12 PCB Congeners

4.12.1 Method

5.0 ANALYTICAL DATA DELIVERABLE REQUIREMENTS

5.1 Analytical Data Packages

5.1.1 Analytical Data Package Contents and Format

5.1.2 “Partial” Analytical Reports

5.1.3 “Full” Analytical Reports

5.1.4 Reporting Forms for Analytical Results

5.1.5 “Less Than” Results

5.1.6 Analytical Uncertainties and Detection Limits

5.1.7 EDD Format

5.1.8 Reporting Conventions

5.1.9 QC Deliverables

5.1.10 General Inorganic Chemistry and Radiochemistry Data Qualifiers

5.1.11 Organic Chemistry Data Qualifiers

5.1.12 Completeness

5.1.13 Significant Figures

5.1.14 Chromatographic Data Presentation Guidelines

5.2 Analytical Data Deliverable Deadlines

5.2.1 Turnaround Times

5.2.2 “Full” Report Deliverable Deadlines

5.2.3 Reporting PE Results

5.2.4 Reporting Results for More Than One Analytical Category

6.0 REQUIRED DELIVERABLES AS STATED IN EXHIBIT “I”

7.0 REFERENCES

8.0 ATTACHMENTS

9.0 ACRONYMS, ABBREVIATIONS, AND GLOSSARY

ATTACHMENT 1 GENERAL INORGANIC PARAMETERS

ATTACHMENT 2 RADIOCHEMICAL PARAMETERS AND MINIMUM DETECTABLE ACTIVITIES

ATTACHMENT 3 ORGANIC PARAMETERS

ATTACHMENT 4 ANALYTICAL and INVOICING ELECTRONIC DATA DELIVERABLE

ATTACHMENT 5 ANALYTICAL SAMPLE FLOW

ATTACHMENT 6 CHAIN OF CUSTODY FORM

1.0 INTRODUCTION AND BACKGROUND

This Exhibit D sets forth the requirements for off-site analytical services to be provided by a multi-services laboratory (SUBCONTRACTOR). Multi-services means the SUBCONTRACTOR has the capability to perform general inorganic, organic, and radiochemical analyses. Samples obtained for chemical analysis in support of CONTRACTOR activities may consist of any type of environmental media including, but not limited to, soil, waste, groundwater, surface water, domestic supply water, air filters, demolition debris, biota, sludge, organic liquids, swipes, gas canisters, and bioassay samples. Samples may also be acquired for airborne-asbestos and bulk-asbestos testing. Most samples are also routinely screened for radiological contaminants per U.S. Department of Transportation regulations. The SUBCONTRACTOR must be qualified to handle radioactive samples (many samples will contain low levels of radioactivity).

Expected isotopes are Pu, Am, U, Th, 90Sr, and 3H, although others are occasionally present. The maximum level of radioactivity expected is 100 nCi/g, although the vast majority of samples have levels much lower than 2 nCi/g.

The following sections detail specific quality assurance (QA) protocols, analytical practices and procedures, analytical quality control (QC) requirements, deliverable formats, and schedule requirements.

Collectively, these conventions have been established to ensure CONTRACTOR data-quality objectives

(DQOs) are met and the data obtained from the analytical SUBCONTRACTOR are derived using consistent guidelines. The SUBCONTRACTOR is to conduct work under the SUBCONTRACTOR’S approved Quality Assurance Program.

2.0 STATEMENT OF WORK

2.1 Sample Throughput Requirements

The SUBCONTRACTOR shall have the capacity to process up to 1200 samples per week without missing specified turnaround time or data-quality requirements of this subcontract. The CONTRACTOR

Sample Management Office (SMO) will determine what samples are shipped to which

SUBCONTRACTOR based on volume and the analytical needs of the CONTRACTOR.

2.2 Electronic Data Deliverable and Analytical Data Package Deliverables

2.2.1 Deliverable Levels

The SUBCONTRACTOR shall provide a U.S. Environmental Protection Agency– (EPA-) defined Level IV report that includes raw data; or a Department of Defense (DOD)/Department of Energy (DOE) Quality

Systems Manual (QSM) Stage 4 report. The SUBCONTRACTOR meets turn-around time when the

SUBCONTRACTOR successfully loads the electronic data deliverable (EDD) into the CONTRACTOR database. The CONTRACTOR must receive the analytical data package PDF deliverable at the same time as the EDD has been loaded under normal turn-around time. Both of these deliverables and the transmittal form are fully described in Section 5.

Each NEW SUBCONTRACTOR’s first complete set of deliverables as defined in Section 5.0 will undergo

CONTRACTOR QA/QC review and comment prior to consent to proceed with additional work.

2.2.2 Corrections to EDD and Analytical Data Package Deliverables

Corrections to any EDD and analytical report PDF deliverable must be performed within 48 hours of formal request for correction. Corrective actions requiring a longer time period shall be addressed by a formal corrective action plan submitted to the CONTRACTOR Subcontractor Technical Representative (STR) within 4 days of formal request for correction by the CONTRACTOR STR. Content of the corrections and re-submissions are fully described in Section 5.3.3.

2.3 Radioactive Materials License Requirement

The SUBCONTRACTOR shall have a current Radioactive Materials License for handling at least 1.5 Ci that is appropriate to the materials expected to be received under this subcontract.

2.4 Analysis Requests

2.4.1 Work Orders, Standard Analyses Requests

The CONTRACTOR SMO will schedule the shipment and analysis of samples, grouped in a work order, directly with the SUBCONTRACTOR or approved Secondary SUBCONTRACTOR. In the event samples are sent directly to the Secondary SUBCONTRACTOR, the Secondary SUBCONTRACTOR shall notify the SUBCONTRACTOR by phone or email when it has received samples from the CONTRACTOR. The analytical request form that accompanies the samples will include the CONTRACTOR’s request number and other information that details the samples submitted and the analyses requested. If the

SUBCONTRACTOR does not receive the samples on the next business day, if any discrepancies are found between the samples received and the analytical request, if any sample containers are broken, if the chain-of-custody seal has been broken, or if insufficient sample volumes are available for analysis, the SUBCONTRACTOR shall notify the CONTRACTOR SMO and STR immediately by phone or e-mail of any such occurrences and document the occurrence in the case narrative of the hard-copy data package. Attachment 5 describes the analytical sample flow.

2.4.2 Secondary SUBCONTRACTOR Laboratory

If, for any reason, the SUBCONTRACTOR finds it necessary on occasion to utilize a Secondary

SUBCONTRACTOR to perform analyses, the Secondary SUBCONTRACTOR must meet all the qualifications stated within this document.

The SUBCONTRACTOR must:

(1) Contact the CONTRACTOR STR (email is acceptable) and describe the reason necessitating a

Secondary SUBCONTRACTOR Laboratory.

(2) Obtain prior approval for the change from the CONTRACTOR STR.

(3) Submit the SUBCONTRACTOR Deviation Disposition Request Form 2178.

2.4.3 Requests for Reanalysis

2.4.3.1 Incomplete Reports and Errors

If a suspected analytical error is identified by comparison with historical data, if QC data are either missing or outside the control limits, or if the data are unusable for any reason, the CONTRACTOR STR reserves the right to request delivery of the missing documentation or the reanalysis of any or all samples within the work order. If some results in a sample have met the acceptance criteria, reanalysis requests will be for the affected parameters only, rather than the entire analytical suite.

2.4.3.2 Reimbursement for Reanalysis Costs

The CONTRACTOR STR will request reanalyses by telephone and confirm the request in writing (e-mail is acceptable). Payment for reanalyses requested by the CONTRACTOR STR shall be made according to the following guidelines (see Exhibit “C,” Form A, Schedule of Quantities and Prices):

(a) The CONTRACTOR shall not pay for requested reanalyses due to reported QC data failures.

(b) Reanalyses that are requested because of a suspected significant error, and that confirm the original results within reasonable analytical error, shall be paid for by the CONTRACTOR. The

CONTRACTOR STR will seek input from the SUBCONTRACTOR regarding reanalysis confirmation in light of sample inhomogeneity or other special considerations.

(c) Reanalyses that are requested because of a suspected significant error, and that indicate that an analytical or reporting error was made in the first analysis, shall be paid for by the

SUBCONTRACTOR.

2.5 Nonstandard Analyses

The CONTRACTOR STR may find it necessary on occasion to request an analysis that is not listed in

Exhibit C but is still within the Scope of work of this subcontract.

2.6 Time Definitions

References to days, weeks, or months are defined as calendar days, weeks, and months. Turnaround times shall be considered as all calendar days, inclusive of weekends and holidays, and commences upon date of receipt by SUBCONTRACTOR. This applies to all turnaround time agreements, including rushed or accelerated analysis. Turnaround times ending on a national holiday shall be delivered the following absolute calendar day.

2.7 Personnel Requirements

Group leaders of the laboratory group shall have the following required minimum qualifications: B.A. or

B.S. in a science, technology, engineering, or mathematics field and at least three years of direct analytical experience in the discipline that they are managing (organic or inorganic or radiological).

Analytical instrument operators shall have two years of experience operating the equipment they are using.

2.8 Primary Contacts and Communication

2.8.1 SUBCONTRACTOR Primary contact person

The SUBCONTRACTOR shall assign a project manager to be the primary contact person for issues relating to the analysis of CONTRACTOR samples.

2.8.2 CONTRACTOR Contact

The CONTRACTOR shall assign a Site Technical Representative (STR) to be the primary contact person for issues relating to the analysis of CONTRACTOR samples.

Subcontract No. 250953

Page 10 of

2.8.3 Communication

Open communication between the CONTRACTOR and SUBCONTRACTOR is crucial to developing a mutually satisfactory business relationship. The SUBCONTRACTOR technical representatives are encouraged to seek guidance in advance of performing work when any questions arise and to comment on any analytical approach they may believe to be flawed

3.0 QUALITY ASSURANCE REQUIREMENTS NOTE: Quality Assurance (QA) requirements are also detailed in Exhibit H of this subcontract.

3.1 General Data-Quality Objectives (DQO)

3.1.1 Methods, Quality Control, and Documentation

3.1.1.1 The CONTRACTOR STR will sometimes find, through application of U.S. Department of

Energy (DOE) “SAFER” process for DQOs, that the QC or other requirements in this document may need to be relaxed or tightened to suit particular project needs. Individual project needs that necessitate requirements different from those discussed in this document will be negotiated on a case-by-case basis through the CONTRACTOR STR and Contract

Administrator.

3.1.1.2 Project-specific DQOs are developed by the CONTRACTOR. However, industry-standard promulgated methods, such as USEPA SW-846 (Third Edition), Clean Water Act approved analytical methods, Occupational Safety and Health Administration (OSHA) methods, American Society for Testing and Materials (ASTM) methods, and American Public Health

Association (APHA) methods (Standard Methods) will be used when available. The analytical requests submitted to the SUBCONTRACTOR will specify which methods apply. In the absence of specific direction from the CONTRACTOR, the SUBCONTRACTOR must employ a suitably sensitive analytical method that meets all project-specific quantitation levels. The

SUBCONTRACTOR shall assume, unless otherwise requested, that (1) air filters shall be analyzed by approved National Institute of Occupational Safety and Health (NIOSH) methods, and (2) tissue samples shall be analyzed using SW-846 methods, with samples prepared as specified in section 4.2.2.7 of this document. Where industry-standard methods do not address particular analytes, performance-based methods can be used with prior written (or e-mail) approval from the CONTRACTOR STR. All QC requirements specified shall be met, even if they exceed those specified in a particular requested method.

3.1.1.3 All methods should be the most current promulgated versions. Before implementation, the method must be proven by industry acceptance. The CONTRACTOR STR must give permission to update to the current version.

3.1.1.4 The SUBCONTRACTOR shall prepare complete documentation for every activity to facilitate review and enhance defensibility of the data. Documentation requirements include records for sample receipt/login, preparation, handling, digestion, extraction, sample or extract cleanup, standards preparation, sample analysis, data review, data reporting, raw supporting data, and records retention.

3.1.1.4 For cases in which the specific QA and QC protocols found in this document, or the

DOD/DOE QSM, or Chapter 5 of the National Environmental Laboratory Accreditation

Conference (NELAC) standards cannot be extended to the requested parameters, then professional judgment shall be employed in adhering as closely as possible to the spirit of those protocols. This means that the SUBCONTRACTOR shall extend all standard documentation and QC practices to parameters, methods, and analytical techniques that are not covered in these documents, where possible. The SUBCONTRACTOR shall formulate an approach to performance and documentation of analytical procedures in light of the fact that it is the general goal of the National Nuclear Security Administration (NNSA) Service Center to obtain legally and technically defensible data. Specific analytical and QC requirements are discussed in detail in section 4.0 of this document.

3.2 Certification and Accreditations Requirements

The SUBCONTRACTOR shall be accredited by NELAC and the State of Utah and shall have successfully passed a DOE Consolidated Audit Program (DOECAP) audit which includes CONTRACTOR representation. The SUBCONTRACTORS performing analyses in support of industrial hygiene programs must be American Industrial Hygiene Association (AIHA) certified, and the SUBCONTRACTORS supporting personnel monitoring programs must be DOE Laboratory Accreditation Program– (DOELAP-) approved. All accreditations and certifications shall remain current and on file.

3.3 SUBCONTRACTOR Laboratory Quality Assurance Plan

3.3.1 Specific Requirements

The SUBCONTRACTOR and any Secondary SUBCONTRACTORS accepted for participation in the program shall have a Laboratory Quality Assurance Plan (LQAP) that contains sections or references addressing all of the items listed below.

3.3.1.1 Title page with provision for approval signatures and dates of revision

3.3.1.2 Table of contents

3.3.1.3 Laboratory organizational structure and key personnel responsibilities

3.3.1.4 Personnel training, with required training, frequency, and methods of records maintenance specified

3.3.1.5 Sample receipt, custody, and management of CONTRACTOR sample practices. This section shall specify a formal vehicle for notifying the SUBCONTRACTOR’S analytical group of holding times near expiration in order to minimize occurrences of expiration before analysis. This section shall also specify how SUBCONTRACTOR personnel will recognize N3B samples and any special conditions for analysis required by this document.

3.3.1.6 Facilities and equipment, including a description of security procedures, sample storage practices, chemical safety data sheets, and a list of equipment available at the laboratory. Equipment lists shall include acquisition dates and maintenance schedules.

3.3.1.7 List of all laboratory analytical procedures by method number and matrix. The

SUBCONTRACTOR policy shall require that controlled copies of standard operating procedures (SOPs) be available to the analysts.

3.3.1.8 General instrument calibration and calibration verification policies, including documentation of calibration standards, coefficients resulting from linear or higher-order polynomial regression calculations, calibration curve correlation coefficients, and the associated acceptance criteria.

The issues below shall be addressed as applicable to the type of analyses being performed.

(a) Procedures shall require that linear regression calibration curve correlation coefficients (r2) for general inorganic chemistry be 0.995.

(b) Conformance with organic chemistry method calibration requirements shall be required. If linear regressions are used in calibration for organic methods, the LQAP or SUBCONTRACTOR SOPs must specify a minimum correlation coefficient or coefficient of determination of 0.995. If higher- order polynomials are used, the SUBCONTRACTOR must obtain prior approval from the CONTRACTOR STR and must follow the applicable guidance in SW-846 method 8000.

(c) Calibration frequency, methodologies, and documentation practices for radiochemistry counting instruments shall be discussed.

(d) Evaluation practices and criteria for nonzero intercepts shall be addressed. Procedures shall require that linear curves for both organic and inorganic data have initial calibration Y-intercept absolute values ≤3 times the method detection limit (MDL). Second-order calibration models

(quadratic fit) shall not be used.

3.3.1.9 MDLs for general inorganic chemistry and organic chemistry. The section addressing MDLs shall specify detection-limit determination methodologies and shall include both empirical MDL verification and examination of the method-blank populations for each analyte. Minimum MDL study requirements are discussed in greater detail in section 4.3.1 of this document. Minimum detectable activity (MDA) calculation requirements for radiochemistry are given in section

4.3.4 of this document.

3.3.1.10 Default criteria for QC sample type, analysis frequency, data acceptance, and corrective actions for failures in daily QC practices. Where QC acceptance criteria are not given in this document or in the applicable method, laboratory acceptance criteria shall be established statistically with a minimum of 20 data points by QC type, method/technique, and matrix.

Control limits shall be established at the 3-sigma (3) confidence level. Where data are insufficient to statistically establish acceptance criteria, an approved fixed limit will be temporarily applied. This section shall also discuss the QC data review processes employed by the SUBCONTRACTOR. The SUBCONTRACTOR performing radiochemical analyses shall specify default minimum tracer and carrier recovery criteria in the LQAP. QC data requirements and acceptance criteria for the CONTRACTOR work are discussed in detail in section 4.0 of this document.

3.3.1.11 A description of the corrective action report (CAR) process. A copy of a CAR form shall be provided in the LQAP. The process shall include tracking and documentation of completion of all corrective actions.

3.3.1.12. A description of SUBCONTRACTOR document-control procedures, including archiving and archive retrieval.

3.3.1.13 An outline of the process for data review and approval with signature authorities. Provision shall be made for peer, supervisory, or QA review of all chemist worksheets. In addition, the

LQAP shall outline document flow, including review steps, from chain of custody (COC) to the final analytical report.

3.3.1.14 A discussion of the SUBCONTRACTOR’s holding time policies and processes for preservation of sample bottles, sample preservation checks, and documentation of preservation checks.

Holding times and preservation techniques can be found in the applicable method.

3.3.1.15 A discussion of the frequency and method of conducting and documenting internal audits. In addition, the LQAP shall specify the frequency and contents of QA reports to management.

3.3.1.16 A list of approvals and certifications from states and external agencies. The LQAP shall specifically require client notification when accreditations or certifications are revoked or suspended.

3.3.1.17 Specific SUBCONTRACTOR policies regarding rounding and the number of significant figures to be used in reporting analytical results. Also, the LQAP or an SOP shall require that leading zeroes be used for numbers less than one, and that units accompany all numbers that are not dimensionless. (The significant figures requirements for this document can be found in section

5.1.13.) Additionally, the LQAP or an SOP shall define appropriate error correction practices and require the use of indelible ink for records.

3.3.1.18 A description of procedures for material procurement, quality inspection, inventory, and storage.

3.3.1.19 A discussion of methods for verifying the agreement of electronic data files with hard-copy reports, including both EDDs and electronic reproductions of reports.

3.3.2 STANDARD OPERATING PROCEDURES (SOP) Support for the LQAP

The CONTRACTOR reserves the right to review SUBCONTRACTORS SOPs at any given time during the term of this subcontract. The LQAP sections addressing some of the issues listed above shall refer to detailed SUBCONTRACTOR SOPs. Complete and comprehensive descriptions of all the listed processes are not required in the LQAP when the specific process details are outlined in

SUBCONTRACTOR SOPs. However, the supporting SOPs shall be referenced in the LQAP.

3.4 Performance Evaluation Sample Analysis Requirement

3.4.1 Analytical Requirements

SUBCONTRACTOR shall perform the analysis of site performance evaluation (PE) samples as described in Section 3 of the QSM, Version 5.1. In addition to the PE testing outlined in the QSM, CONTRACTOR reserves the right to provide additional PE samples to the SUBCONTRACTOR. The analytical and deliverable requirements for CONTRACTOR-provided PE samples are the same as all CONTRACTOR SMO samples. Payment for the analysis of CONTRACTOR-provided PE samples shall be made according to the fees specified in Exhibit C. The analytical techniques and SOPs used in the analysis of all PE samples shall be the same as those used in routine analysis of the CONTRACTOR samples.

3.4.2 Proficiency

The CONTRACTOR SMO will provide a summary of analytical results and theoretical values for each

CONTRACTOR-provided PE round to each lower tier SUBCONTRACTOR after all the data for that round are in. Any requests for a CAR necessitated by SUBCONTRACTOR PE sample failures will accompany the summary report. Initial responses to CAR requests, including the projected schedule for completion, shall be due no later than 2 weeks from the date of the request. The CONTRACTOR STR reserves the right to request accelerated delivery of CARs if circumstances make this necessary.

3.4.3 Failure to meet Criteria

As per Section 3.2.2 of the QSM, Version 5.1, the CONTRACTOR STR reserves the right to decide to withhold sample shipments based on any PE Failure to Meet Criteria event

3.5 Systems and Internal Audit Requirements

3.5.1 Annual Systems Audits

The SUBCONTRACTOR shall undergo a DOECAP quality systems audit at least once a year. DOECAP audits will serve as a key performance indicator for verifying or denying the acceptability of an analytical

SUBCONTRACTOR to provide analytical services for DOE. Acceptability will be based primarily on the ability of the SUBCONTRACTOR to produce data of known, adequate, and consistent quality. A formal audit report will be issued following this activity. Responses to audit reports will be submitted to DOECAP as specified in the DOECAP requirements documents. Laboratories not scheduled for DOECAP audits will be scheduled for oversight activities as appropriate for their scope of work.

A CONTRACTOR STR systems review may be conducted at the SUBCONTRACTOR facility at the discretion of the CONTRACTOR. The purpose of this review is to verify SUBCONTRACTOR compliance with the LQAP and the specifications of this document. In addition, recommendations may be made to

SUBCONTRACTOR personnel regarding possible quality improvements. CONTRACTOR will issue a formal report or request for corrective action to SUBCONTRACTOR following this activity.

SUBCONTRACTOR shall respond to a request for corrective action within 30 days from the date of issue unless a more rapid turnaround is specified by CONTRACTOR in order to safeguard data quality.

3.5.2 On-Site Data Package Review

Data package reviews may be conducted at the SUBCONTRACTOR’S facility at the discretion of the

CONTRACTOR STR. The focus of these reviews shall be to verify subcontract compliance and deliverable accuracy, ensure that raw data and supporting documentation are maintained in retrievable form, and review ancillary documentation not included in deliverables. The data package to be reviewed will be chosen at the time of the review activity. CONTRACTOR will issue a formal report or corrective action request following this activity. SUBCONTRACTOR shall respond to a request for corrective action within 30 days from the date of issue unless a more rapid turnaround is specified by CONTRACTOR in order to safeguard data quality.

3.5.3 Internal Audits

The SUBCONTRACTOR shall perform internal QA audits at least annually.

3.5.4 External Surveillance/Observations

The CONTRACTOR reserves the right to visit the SUBCONTRACTOR’s facility to assure conformance to the technical requirements of this subcontract. This includes the review of review raw data including but not limited to logbooks, bench sheets, calibration records, continuing calibration verification samples

(CCV), continuing calibration blanks (CCB), interference check samples (ICS), initial calibration verification samples (ICV), and initial calibration blanks (ICB), RAD spectra, ICSA from metals analysis, instrument printouts and other related documentation. Reasonable advanced notice (minimum 24 hours) in writing shall be provided to the SUBCONTRACTOR prior to a visit.

3.6 Participation in Inter-Laboratory Comparison Studies

3.6.1 Required Intercomparison Programs

The SUBCONTRACTOR performing inorganic or organic analyses shall participate in two single-blind, single-concentration performance testing (PT) studies per year, where available, for item (a) below. The

SUBCONTRACTOR performing radiochemical analyses shall participate in two single-blind, single-concentration PT studies per year, where available, for item (b) below. The SUBCONTRACTOR performing airborne silica, asbestos, metals, and/or organics analyses shall participate in item (c) below.

The SUBCONTRACTOR performing lead in paint analyses shall participate in item (d) below. The

SUBCONTRACTOR performing National Pollutant Discharge Elimination System (NPDES) analyses shall participate in item (e) below.

(a) Commercial vendor programs designed to meet the requirements given in the Proficiency

Testing section (Chapter II) of the NELAC standard currently in effect.

(b) Mixed Analyte Performance Evaluation Program (MAPEP), U.S. Department of Energy, Idaho

Operations Office, Idaho Falls, Idaho

(c) Proficiency Analytical Testing (PAT) Program, AIHA

(d) Environmental Lead Proficiency Analytical Testing Program (ELPAT), AIHA.

(e) Discharge Monitoring Report–Quality Assurance Study (DMR-QA), EPA Office of Enforcement and Compliance Assurance.

3.6.2 Reporting Intercomparison Results

The SUBCONTRACTOR shall report results of the intercomparison studies to the CONTRACTOR STR quarterly. This report is due with the delivery of the SUBCONTRACTOR’s QPR. All results received by the SUBCONTRACTOR since the last quarterly report and more than 1 week before the due date shall be included in this deliverable. Results received less than 1 week before the due date will be held for inclusion in the next quarter’s deliverable.

3.7 Employee Training and Documenting Employee Proficiency

3.7.1 Training in Radiation Safety Practices and Techniques

The SUBCONTRACTOR personnel who are involved in receiving, processing, and/or managing CONTRACTOR samples shall be trained in radiation safety practices and techniques.

3.8 SUBCONTRACTOR Instrumentation, Equipment, and Reagent Maintenance

3.8.1 Instrument Logs and Response Checks

3.8.1.1 The SUBCONTRACTOR shall have an SOP that specifies the requirements for maintaining logbooks. These requirements shall specifically address QA protocols for error correction as well as schedules for peer, supervisory, or QA review of logbooks. In addition, the use of indelible ink to make logbook entries shall be explicitly required.

3.8.1.2 The SUBCONTRACTOR shall maintain an instrument logbook for all major instruments used to acquire data for the CONTRACTOR samples. Each instrument logbook shall be clearly labeled to indicate its association with a particular piece of laboratory equipment.

3.8.1.3 The SUBCONTRACTOR performing general inorganic analysis of CONTRACTOR samples shall have an SOP requiring that instrument response checks or other appropriate instrument performance checks are performed daily. The requirements shall include recording the results of such checks in the associated instrument maintenance log.

3.8.1.4 The SUBCONTRACTOR performing organic analysis of CONTRACTOR samples shall have an SOP requiring that instrument logs contain a brief description of run failures and the file names for analysis runs. Reanalysis run entries, including those for necessary dilutions, or for cross-contamination from other samples, shall reference the original run to facilitate review.

Instrument logs for GC-MS volatiles shall reference the port used for each run where multiple ports exist.

3.8.1.5 The SUBCONTRACTOR performing radiochemical analysis of CONTRACTOR samples shall record the data file names and dates for all calibration activities in the associated instrument logs. Procedures shall also require that the gas flow proportional counter (GFPC), alpha spectrometry, gamma spectroscopy, or alpha scintillation detector used to count each sample be logged.

3.8.2 Balances, Volumetric Pipettes, and Sample Storage Refrigerators

3.8.2.1 The chemical and geotechnical analysis SUBCONTRACTOR shall have a calibration SOP for analytical balances. The SOP shall specify that balances be checked daily (on all business days) against certified standards and that balances not accurate to within at least ±1% be recalibrated or removed from service. The SUBCONTRACTOR shall maintain logbooks in which the daily analytical balance calibration checks are recorded.

3.8.2.2 The chemical analysis SUBCONTRACTOR shall have an SOP that requires daily temperature monitoring (on all business days) for refrigerated sample storage areas and the corrective action that will be initiated if a measurement falls outside the required range. The

SUBCONTRACTOR shall maintain logbooks for sample storage refrigeration units in which the daily temperature checks are recorded.

3.8.2.3 The chemical analysis SUBCONTRACTOR shall have a calibration SOP for volumetric pipettes, other than glass pipettes, that deliver 100 L or more. This SOP shall specify that

(1) pipettes be checked daily (on all business days) by weighing deionized (DI) water, and

(2) pipettes failing to deliver to within ±1% accuracy be recalibrated or removed from service.

3.8.3 Reagent Water Production

3.8.3.1 The chemical analysis SUBCONTRACTOR shall have an SOP for reagent water or DI water production and system maintenance. This SOP shall outline specific control criteria for reagent or DI water quality, require daily water quality measurement (on all business days), and give specific corrective actions to be taken for out-of-control events.

3.8.3.2 Daily records of water quality shall be kept in logbooks designated for that purpose.

3.8.4 Control of Standards

3.8.4.1 The chemical analysis SUBCONTRACTOR shall have an SOP outlining policy on shelf life, labeling, and stock maintenance for reagents, stock solutions, intermediate dilutions, and working standards. The SUBCONTRACTOR shall maintain standards preparation logs and standard certificates of analysis in an orderly manner to facilitate retrieval.

3.8.4.2 The SOP shall specify a shelf life no greater than 1 year for stock solutions prepared by

SUBCONTRACTOR from salts or metals.

3.8.4.3 The SOP shall specify a shelf life of no greater than 1 year for intermediate dilutions and vendor-supplied stock solutions, other than radionuclide solutions, when the constituent concentrations are 1 mg/L or higher. General inorganic analyte solutions with constituent concentrations less than 1 mg/L shall be defined as working standards.

3.8.4.4 The 1-year shelf life shall not apply to neat materials or unopened ampoules containing solutions of organic compounds. The manufacturer’s expiration date, if any, shall apply to neat materials and unopened ampoules containing organic standard solutions.

3.8.4.5 The SOP shall limit the shelf lives of opened ampoules and intermediate dilutions containing organic standard solutions to no greater than those given below. Shorter shelf lives given in the

EPA methods shall supersede the specified guidelines.

Analyte Shelf Life

Volatile Organic Compounds (VOCs) 7 days for gases

180 days for non-gases

Total petroleum hydrocarbons (TPH) 180 days for purgeable (gasoline range organics [GRO])

365 days for extractable (diesel range organics [DRO])

Pesticides/polychlorinated biphenyls (PCBs)/herbicides

180 days

Semivolatile Organic Compounds (SVOCs) 365 days

High explosives (HE) 365 days, 1000 ppm, stock 30 days, all intermediate dilutions Daily prep, all working standards

3.8.4.6 The SOP shall specify that working standards for volatiles and general inorganic analyses, other than multielement radial viewing inductively coupled plasma atomic emission spectroscopy (ICPAES) working standards, be prepared fresh daily. The SOP shall require that

ICPMS and axial viewing ICPAES working standards having concentrations less than 1 ppm be prepared fresh daily.

3.8.4.7 The SOP shall specify that multielement radial viewing ICPAES working standards be prepared fresh at least once a month.

3.8.4.8 The SOP shall specify that anion and nutrient stock solutions be kept in refrigerated storage.

Refrigerated storage for standards is subject to the requirements of section 3.8.2.2 of this document.

3.8.4.9 For radiochemistry, the SOP shall limit radionuclide solution shelf lives to a maximum of

5 years or five half-lives, whichever is less. The SOP can allow verification of expired standards against National Institute of Standards and Technology (NIST) traceable standards or require that they be discarded. Reverification is allowed if the following criteria are met.

(a) At least three verification measurements of a standard shall be used to determine the mean value and standard deviation of the verification results.

(b) The 2-sigma (2) value defining the 95% confidence interval shall not exceed 10% of the mean value of the three verification measurements.

(c) The certificate value (NOT including any uncertainty) shall lie within the 95% confidence interval determined from the mean and 2 standard deviations of the three measurements. However, if the interval defined is narrower than the mean ±5% of the mean, a ±5% acceptance criterion may be used.

(d) The methodology used, performance requirements, and documentation practices must be discussed in the SOP.

3.8.4.10 The SOP shall require that stock solutions and intermediate dilutions prepared in the laboratory be logged in a standards preparation log. The SOP shall give specific guidelines on what information is to be included in log entries. Expiration dates for solutions prepared from multiple sources shall coincide with the earliest expiration date of the starting materials.

3.8.4.11 Minimum labeling requirements for stock solutions and intermediate dilutions that are intended for long-term use shall be addressed in the SOP and shall include the following information:

Preparer’s initials

Date of preparation

Matrix

Concentration of constituents, unless too many are contained to be listed on the label

Expiration date

Unique standard name that is traceable to a standards preparation log

3.8.4.12 The SOP shall require that organic analysis calibration standards be prepared using high-purity solvents that were accompanied by manufacturers’ certificates of analysis when purchased.

3.8.4.13 The SOP shall require that standards for atomic spectroscopy be prepared in ASTM Type I water. The applicable ASTM standard for Type I water is the older standard that specifies a

16.67-Mcm resistivity control criterion. Preparation water need not meet the newer

18.0-Mcm criterion.

3.8.4.14 The SOP shall require that standards for radiochemistry and wet chemistry be prepared using

ASTM Type II water, at a minimum. It must also require using dead water for radiochemical analyses method blanks.

3.7.4.15 The SOP shall specify that expired standards be segregated and labeled as expired while awaiting disposal.

3.8.4.16 Vendor-supplied solutions that are used as primary calibrants shall be NIST-traceable where possible.

3.8.5 Glassware

3.8.5.1 The SUBCONTRACTOR shall have an SOP for cleaning glassware.

3.8.5.2 All volumetric glassware used to make standard and sample dilutions in CONTRACTOR work shall be ASTM Class A glassware. Dilutions may also be accomplished by automation or by using pipettes and/or balances that are controlled in accordance with the applicable provisions of this document.

3.8.5.3 The SUBCONTRACTOR shall have a SOP on screening glassware for low-level tritium.

3.8.6 Incident Tracking

The SUBCONTRACTOR shall have a system for recording and tracking incidents involving breakage of reagents and client samples. This system is needed to help explain unexpected “hits” in samples that were analyzed during periods when the ambient air may have been contaminated. The tracking system shall be implemented through facilities, health and safety (H&S), QA, or other

SUBCONTRACTOR groups.

3.9 Analytical and Quality Assurance Standard Operating Procedures

3.9.1 Control of SOPs

The SUBCONTRACTOR shall maintain controlled copies of approved SOPs for each analytical method or general procedure performed by SUBCONTRACTOR personnel. The SUBCONTRACTOR shall set and demonstrably adhere to a schedule of periodic review for SOPs. Changes in the SUBCONTRACTOR

SOPs that affect the analysis or documentation of CONTRACTOR samples shall be transmitted in writing to the CONTRACTOR STR for approval before implementation. Geotechnical SUBCONTRACTOR may use the most recent ASTM methods instead of SOPs, provided that there are no deviations from the method in practice.

3.9.2 Availability of SOPs

Controlled copies of SOPs shall be readily available to all personnel performing analytical work in support of the CONTRACTOR. This shall be accomplished either by issuing a copy to each analyst, electronically posting SOPs, or making a library of SOPs accessible to analysts. Electronically posted SOPs shall be

“read only” files. Policies for notifying SUBCONTRACTOR staff members of SOP updates shall be defined.

3.9.3 Analyst Familiarity with SOPS

Analyst familiarity with SOPs shall be documented to ensure that the contents of QA and analytical

SOPs are effectively communicated to personnel performing analysis of CONTRACTOR samples.

SUBCONTRACTOR procedures shall require that method training and QA indoctrination be performed and documented in training files.

3.10 Sample Receipt and Storage Requirements

3.10.1 Chain-of-Custody Forms

3.10.1.1 CONTRACTOR samples received by the SUBCONTRACTOR will be accompanied by a COC form. A typical COC form is included as Attachment 7. Sample custody will be transferred to the SUBCONTRACTOR at the time of sample receipt, after which the SUBCONTRACTOR will be responsible for maintaining unbroken COC. By definition, a sample is in custody if it is (1) in one’s possession, (2) in view, or (3) in a controlled access area.

3.10.1.2 At the time of sample receipt, the COC form will have been partially completed by the sampling team and will indicate the SUBCONTRACTOR’s name, delivery order number, sample IDs, sample matrix, bottle volume, collection dates and times, date shipped, and method of shipment.

3.10.1.3 Individual sample bottles are labeled with the sample identification (ID), sampling date and time, preservation method, sampler's identity, and comments.

3.10.1.4 The SUBCONTRACTOR’s sample custodian receiving the samples shall verify that the information listed on the COC form is correct and accurately describes the contents of the shipment.

3.10.2 Acknowledgment of Sample Receipt

3.10.2.1 At the time of receipt, the SUBCONTRACTOR’s sample custodian shall sign and date the COC form in indelible ink to acknowledge sample receipt and accept custody. The sample custodian shall note discrepancies between the samples listed on the COC and those actually received on the COC form and sample login worksheets.

3.10.2.2 The SUBCONTRACTOR shall include all airbills in the case file where possible and shall record all freight-carrier tracking numbers on the login records when the airbills cannot be removed intact.

3.10.3 Documentation of Anomalies

3.10.3.1 The SUBCONTRACTOR’s sample custodian shall note on the COC form and sample login worksheets any irregularities observed with the shipment, temperature, preservation, condition, or custody seals of samples received. Login worksheets shall specifically identify any samples affected by such irregularities.

3.10.3.2 The pH of all preserved aqueous sample fractions that require specific pH preservation shall be checked during sample login.

3.10.3.3 The allowable temperature range for samples requiring cooling for preservation is ≤6°C. The actual temperature of sample shipments shall be noted on login worksheets.

3.10.3.4 If no anomalies are encountered for a sample shipment, a brief statement of that fact shall be provided on login worksheets and in the case narrative.

3.10.3.5 If samples requiring preservation arrive unpreserved or inadequately preserved, the

SUBCONTRACTOR must contact the CONTRACTOR SMO for instruction regarding whether to proceed with the analysis. If the SUBCONTRACTOR is instructed to adjust the sample pH, metals samples must be held for 16 hours and radionuclide samples must be held for 24 hours before an aliquot is withdrawn for analysis.

3.10.4 Communication of Anomalies

3.10.4.1 A SUBCONTRACTOR representative shall notify the CONTRACTOR SMO immediately by telephone or e-mail of any irregularities noted during the sample receiving process. In addition, the SUBCONTRACTOR shall notify the CONTRACTOR SMO immediately if a sample shipment does not include sufficient sample volumes to meet the QC requirements of this document. Any problems with a sample shipment that adversely affect data quality shall be described in the case narrative that accompanies the report of analytical results for that delivery order.

3.10.5 Sample Retention

The SUBCONTRACTOR shall retain and store all CONTRACTOR samples associated with a specific delivery order for a period of 90 days after issuing the analytical report for that delivery order. Where sample retention is required in excess of 90 days, CONTRACTOR will notify SUBCONTRACTOR in writing.

3.10.6 Sample Disposal

3.10.6.1 The SUBCONTRACTOR shall lawfully dispose of all CONTRACTOR samples after the 90-day sample storage requirement is fulfilled if the exception given immediately below does not apply.

3.10.6.2 If given the nature of the samples, the SUBCONTRACTOR has no outlet for disposal then samples may be returned to the CONTRACTOR SMO with prior approval.

3.10.6.3 If samples are to be returned to the CONTRACTOR SMO, the SUBCONTRACTOR shall provide notification that includes an inventory of samples to the CONTRACTOR SMO at least

2 weeks before shipping. The SUBCONTRACTOR is solely responsible for the lawful shipping and payment of shipping for samples sent back to the CONTRACTOR.

3.10.6.4 The SUBCONTRACTOR shall not return extracts or digestates to the CONTRACTOR SMO.

3.10.7 Return of Shipping Coolers

The SUBCONTRACTOR shall initiate the shipment of sample coolers with blue ice back to the

CONTRACTOR SMO within 7 days of receipt.

3.10.8 Laboratory-supplied sample containers

The CONTRACTOR SMO may wish to use laboratory-supplied sample containers for some projects.

The schedule of prices provided in the laboratory’s proposal shall include separate prices for pre-cleaned sample containers, having the appropriate preservative, for each analysis covered in the proposal.

Container and preservative requirements are given in Attachment 5. This also includes sample media for industrial hygiene samples.

3.11 Analytical Holding-Time Requirements

3.11.1 CONTRACTOR Holding Times

Requirements for analytical holding times are specified in the applicable method.

3.11.2 Definition

Holding times are calculated in days or hours, according to the time units used in the approved method holding-time requirements. If the method-specified holding time is given in hours, then the analysis must be complete before the end of the last hour of the holding…