Lab Quality Manual

Laboratory Quality Manual
FOR THE OREGON DEPARTMENT OF

ENVIRONMENTAL QUALITY
DEQ91-LAB-0006-QMP
Version 5.0 – November 2004
Laboratory Division
1712 SW 11th Avenue
Portland, OR 97201
Phone: (503) 229-5983
Fax: (503) 229-6924
www.deq.state.or.us
This Page Intentionally Left Blank
Laboratory Quality Manual Oregon Department of Environmental Quality
DEQ91-LAB-0006-QMP November 2004
Version 5.0 Page iii
Concurrences:
Mary Abrams, Laboratory Division Administrator Date
Eugene Foster, Organic Section Manager Date
RaeAnn Haynes, Inorganic Section Manager Date
Dan Hickman, Technical Services Section Manager Date
Jeff Smith, Air Monitoring Section Manager Date
Greg Pettit, Watershed Assessment Section Manager Date
Paul McKay, Air Quality Assurance Officer Date
Ron Doughten, Land Quality and Agency Quality Assurance Officer Date
Chris Redman, Water Quality and Laboratory Quality Assurance Officer Date
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Laboratory Quality Manual Oregon Department of Environmental quality
Version 5.0 Page v
Table of Contents
Laboratory Quality Manual ............................................................................................................. i
Concurrences:.............................................................................................................................. iii
Table of Contents.......................................................................................................................... v
Acronyms and Abbreviations ...................................................................................................... vii
Glossary ......................................................................................................................................viii
1 Quality System ..................................................................................................................1
1.1 Introduction:...................................................................................................................1
1.2 DEQ's Quality Management Policy ...............................................................................2
2 Laboratory Management Structure....................................................................................4
2.1 Laboratory Quality Assurance Team .............................................................................4
2.2 Administration................................................................................................................5
2.3 Air Quality Monitoring ....................................................................................................5
2.4 Watershed Assessment ................................................................................................5
2.5 Inorganic Laboratory .....................................................................................................5
2.6 Organic Laboratory........................................................................................................6
2.7 Technical Services ........................................................................................................6
2.8 Personnel ......................................................................................................................6
3 Standard Operating Procedures......................................................................................12
3.1 Sampling .....................................................................................................................12
3.2 Sample Handling .........................................................................................................13
3.2.1 Sample Identification ...............................................................................................13
3.2.2 Sample Receipt .......................................................................................................13
3.2.3 Sample Integrity.......................................................................................................14
3.3 Test Methods and Method Validation..........................................................................15
3.3.1 Analytical SOPs.......................................................................................................15
3.3.2 Demonstrations of Capability...................................................................................16
3.3.3 Data Validation ........................................................................................................16
3.3.4 Estimation of Uncertainty of Measurement..............................................................17
3.3.5 Data Control ............................................................................................................17
4 Measurement Traceability ...............................................................................................19
4.1 Documentation ............................................................................................................19
4.2 Purchasing Services and Supplies..............................................................................19
4.2.1 Request for Purchase..............................................................................................20
4.2.2 Purchase .................................................................................................................20
Version 5.0 Table of Contents cont. Page vi
4.2.3 Receipt .................................................................................................................... 21

4.2.4 Labeling................................................................................................................... 21
4.2.5 Storage.................................................................................................................... 21
4.2.6 Use and Consumption............................................................................................. 21
5 Assuring the Quality of Analytical Data ........................................................................... 23
6 Equipment ....................................................................................................................... 24
6.1 Support Equipment ..................................................................................................... 24
6.2 Instruments used for the Determinative Step.............................................................. 25
6.3 Accommodation and Environmental Conditions ......................................................... 27
6.3.1 Laboratory Facility ................................................................................................... 27
6.3.2 Environmental Controls ........................................................................................... 28
7 Quality Assurance ........................................................................................................... 29
7.1 Control of Quality Documents ..................................................................................... 29
7.2 Analytical Records ...................................................................................................... 29
7.3 Data Reports and Verification Records....................................................................... 29
7.4 Client Correspondences.............................................................................................. 30
7.4.1 Analytical Work Submitted to the Laboratory .......................................................... 31
7.4.2 Complaints .............................................................................................................. 32
7.5 Quality Assurance Measures ...................................................................................... 32
7.5.1 Internal Audit ........................................................................................................... 32
7.5.2 Annual QA Report ................................................................................................... 33
7.5.3 Nonconformance Investigations and Corrective Action Reports ............................. 34
7.5.4 Preventative Measures ........................................................................................... 36
8 Reporting Results............................................................................................................ 38
Appendices
Appendix A: Demonstration of Capability .................................................................................. 41
Appendix B: 40 CFR Part 136, App. B....................................................................................... 42
Appendix C: Nonconformance Report ....................................................................................... 46
Appendix D: LIMS status codes................................................................................................. 50
Appendix E: Major Analytical Equipment ................................................................................... 51
Appendix F: QC definitions ........................................................................................................ 53
Appendix G: Analytical Methods ................................................................................................ 58
Appendix H: Laboratory Organizational Chart ........................................................................... 64
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Acronyms and Abbreviations

AR Analytical Reagent grade
CCB Continuing Calibration Blank
CCV Continuing Calibration Verification
CA Corrective Action
CAA Clean Air Act
CERCLA Comprehensive Environmental Response, Compensation and Liability Act
CWA Federal Water Pollution Control Act (Clean Water Act)
DAR Data Analysis Report
DAS Oregon Division of Administrative Services
DEQ Oregon Department of Environmental Quality
DOC Demonstration Of Capability
DQO Data Quality Objectives
EMT DEQ’s Executive Management Team
EQC Oregon’s Environmental Quality Commission
EPA Environmental Protection Agency
FIFRA Federal Insecticide, Fungicide and Rodenticide Act
LASAR Laboratory Analytical Storage and Retrieval (archive database for DEQ)
LCS Laboratory Control Sample
LIMS Laboratory Information Management System (active database)
LMT Laboratory Management Team
LQAO Laboratory Quality Assurance Officer
MB Method Blank
MDL Method Detection Limit
MRL Method Reporting Limit
NELAC National Environmental Laboratory Accreditation Conference
NELAP National Environmental Laboratory Accreditation Program
NIST National Institute of Standards and Technology
ORELAP Oregon Environmental Laboratory Accreditation Program
PCS Procurement & Contract Specialist
PDF Portable Document Format
PDR Property Disposition Request
QA Quality Assurance
QAO Quality Assurance Officer
QAPP Quality Assurance Project Plan
QAT Quality Assurance Team
QC Quality Control
QMP Quality Management Plan
RCRA Resource Conservation and Recovery Act
SAP Sampling and Analysis Plan
SDWA Safe Drinking Water Act
SOP Standard Operating Procedure
Version 5.0 Page viii
Glossary1
Accuracy: the degree of agreement between an observed value and an
accepted reference value. Accuracy includes a combination
of random error (precision) and systematic error (bias)
components which are due to sampling and analytical
operations; a data quality indicator. (QAMS)
Analyst: the designated individual who performs the "hands-on"
analytical methods and associated techniques and who is the
one responsible for applying required laboratory practices and
other pertinent quality controls to meet the required level of
quality. (NELAC)
Audit: a systematic evaluation to determine the conformance to
quantitative and qualitative specifications of some operational
function or activity. (EPA-QAD)
Batch: environmental samples that are prepared and/or analyzed
together with the same process and personnel, using the
same lot(s) of reagents. A preparation batch is composed of
one to 20 environmental samples of the same NELAC-defined
matrix, meeting the above mentioned criteria and with a
maximum time between the start of processing of the first and
last sample in the batch to be 24 hours. An analytical batch is
composed of prepared environmental samples (extracts,
digestates or concentrates) which are analyzed together as a
group. An analytical batch can include prepared samples
originating from various environmental matrices and can
exceed 20 samples. (NELAC Quality Systems Committee)
Chain of Custody Form: record that documents the possession of the samples from the
time of collection to receipt in the laboratory. This record
generally includes: the number and types of containers; the
mode of collection; collector; time of collection; preservation;
and requested analyses. (NELAC)
Clean Air Act: the enabling legislation in 42 U.S.C. 7401 et seq., Public Law
91-604, 84 Stat. 1676 Pub. L. 95-95, 91 Stat., 685 and Pub.
L. 95-190, 91 Stat., 1399, as amended, empowering EPA and
its delegates to promulgate air quality standards, monitor and
to enforce them. (NELAC/DEQ)
Comprehensive the enabling legislation in 42 U.S.C. 9601-9675 et seq., as
Environmental amended by the Superfund Amendments and Reauthorization
Response, Act of 1986 (SARA), 42 U.S.C. 9601et seq., to eliminate the
Compensation and health and environmental threats posed by hazardous waste
Liability Act sites. (NELAC)
(CERCLA/Superfund):
1
Sources in ( ) are presented at the end of the glossary.
Version 5.0 Glossary cont. Page ix
Conformance: an affirmative indication or judgment that a product or service

has met the requirements of the relevant specifications,
contract, or regulation; also the state of meeting the
requirements. (ANSI/ASQC E4-1994)
Federal Insecticide, the enabling legislation under 7 U.S.C. 135 et seq., as
Fungicide and amended, that empowers the EPA to register insecticides,
Rodenticide Act (FIFRA): fungicides, and rodenticides. (NELAC)
Federal Water Pollution the enabling legislation under 33 U.S.C. 1251 et seq., Public
Control Act (Clean Water Law 92-50086 Stat. 816, that empowers EPA and its
Act, CWA): delegates to set discharge limitations, write discharge permits,
monitor, and bring enforcement action for non-compliance.
(NELAC/DEQ)
Field Measurement: The determination of physical, biological, or radiological
properties, or chemical constituents that are measured on-
site, close in time and space to the matrices being
sampled/measured, following accepted test methods. This
testing is performed in the field outside of a fixed-laboratory or
outside of an enclosed structure that meets the requirements
of a mobile laboratory. (NELAC)
Holding Times The maximum times that samples may be held prior to
(Maximum Allowable analysis and still be considered valid or not compromised. (40
Holding Times): CFR Part 136)
Integrity: The quality or state of being complete or uncompromised.
(DEQ)
Legal Chain of Custody Procedures employed to record the possession of samples
Protocols: from the time of sampling until analysis, performed at the
special request of the client. These protocols include the use
of a Chain of Custody Form that documents the collection,
transport, and receipt of compliance samples by the
laboratory. In addition, these protocols document all
handling of the samples within the laboratory. (NELAC)
Must: Denotes a requirement that must be met (Random House
College Dictionary); to be distinguished from “shall” in that
“shall” implies a policy requirement and “must” implies a
standard requirement. (NELAC/DEQ)
National Institute of An agency of the US Department of Commerce’s Technology
Standards and Administration that is working with EPA, States, NELAC, and
Technology (NIST): other public and commercial entities to establish a system
under which private sector companies and interested States
can be accredited by NIST to provide NIST-traceable
proficiency testing (PT) to those laboratories testing drinking
water and wastewater. (NIST)
National Environmental A voluntary organization of State and Federal environmental
Laboratory Accreditation officials and interest groups purposed primarily to establish
Conference (NELAC): mutually acceptable standards for accrediting environmental
laboratories. A subset of NELAP. (NELAC)
Version 5.0 Glossary cont. Page x
National Environmental The overall National Environmental Laboratory Accreditation

Laboratory Accreditation Program of which NELAC is a part. (NELAC)
Program (NELAP):
National Voluntary A program administered by NIST that is used by providers of
Laboratory Accreditation proficiency testing to gain accreditation for all
Program (NVLAP): compounds/matrices for which NVLAP accreditation is
available, and for which the provider intends to provide
NELAP PT samples. (NELAC)
Negative Control: Measures taken to ensure that a test, its components, or the
environment do not cause undesired effects, or produce
incorrect test results. (NELAC)
NELAC Standards: The plan of procedures for consistently evaluating and
documenting the ability of laboratories performing
environmental measurements to meet nationally defined
standards established by the National Environmental
Laboratory Accreditation Conference. (NELAC)
NELAP Recognition: The determination by the NELAP Director that an accrediting
authority meets the requirements of the NELAP and is
authorized to grant NELAP accreditation to laboratories.
(NELAC)
Nonconformance: Event that does not meet laboratory requirements prescribed
by policies or procedures (see conformance). (DEQ)
Programs: Agency work units with the authority to implement state rules
and regulations created through the CAA, CWA, CERCLA,
FIFRA, RCRA, or SDWA.
Protocol: A detailed written procedure for field and/or laboratory
operation (e.g., sampling, analysis) which must be strictly
followed. (EPA-QAD)
Quality Assurance (QA): An integrated system of activities involving planning, quality
control, quality assessment, reporting and quality
improvement to ensure that a product or service meets
defined standards of quality with a stated level of confidence.
(QAMS)
Quality Assurance A formal document describing the detailed quality control
[Project] Plan (QAPP): procedures by which the quality requirements defined for the
data and decisions pertaining to a specific project are to be
achieved. (EPA-QAD)
Quality Control (QC): The overall system of technical activities whose purpose is to
measure and control the quality of a product or service so that
it meets the needs of users. (QAMS)
Quality Control Sample A sample used to assess the performance of all or a portion of
(QCS): the measurement system. QC samples may be Certified
Reference Materials, a blank matrix fortified by spiking, or
actual samples fortified by spiking. (NELAC)
Version 5.0 Glossary cont. Page xi
Quality Manual: A document stating the management policies, objectives,

principles, organizational structure and authority,
responsibilities, accountability, and implementation of an
agency, organization, or laboratory, to ensure the quality of its
product and the utility of its product to its users. (NELAC)
Quality System: A structured and documented management system describing
the policies, objectives, principles, organizational authority,
responsibilities, accountability, and implementation plan of an
organization for ensuring quality in its work processes,
products (items), and services. The quality system provides
the framework for planning, implementing, and assessing
work performed by the organization and for carrying out
required QA and QC. (ANSI/ASQC E-41994)
Quality System Matrix: These matrix definitions are an expansion of the field of
accreditation matrices and shall be used for purposes of batch
and quality control requirements (see Appendix D of NELAC
standards Chapter 5). These matrix distinctions shall be
used: (NELAC)
whole gas or vapor samples including those contained in
Air and Emissions:
flexible or rigid wall containers and the extracted concentrated
analytes of interest from a gas or vapor that are collected with
a sorbent tube, impinger solution, filter, or other device.
any aqueous sample excluded from the definition of Drinking
Aqueous:
Water matrix or Saline/Estuarine source. Includes surface
water, groundwater, effluents, and TCLP or other extracts.
any aqueous sample that has been designated a potable or
Drinking Water:
potential potable water source.
any aqueous sample from an ocean or estuary, or other salt
Saline/Estuarine:
water source such as the Great Salt Lake. Non-aqueous
Liquid: any organic liquid with <15% settleable solids.
any sample of a biological origin such as fish tissue, shellfish,
Biological Tissue:
or plant material. Such samples shall be grouped according
to origin.
includes soils, sediments, sludges and other matrices with
Solids:
>15% settleable solids.
a product or by-product of an industrial process that results in
Chemical Waste:
a matrix not previously defined.
Resource Conservation The enabling legislation under 42 USC 321 et seq. (1976),
and Recovery Act that gives EPA the authority to control hazardous waste from
(RCRA): the “cradle-to-grave”, including its generation, transportation,
treatment, storage, and disposal. (NELAC)
Safe Drinking Water Act The enabling legislation, 42 USC 300f et seq. (1974), (Public
(SDWA): Law 93-523), that requires the EPA to protect the quality of
drinking water in the U.S. by setting maximum allowable
contaminant levels, monitoring, and enforcing violations.
(NELAC)
Version 5.0 Glossary cont. Page xii
Sample Tracking: Procedures employed to record the possession of the

samples from the time of sampling until analysis, reporting,
and archiving. These procedures include the use of a Chain
of Custody Form that documents the collection, transport, and
receipt of compliance samples to the laboratory. In addition,
access to the laboratory is limited and controlled to protect the
integrity of the samples. (NELAC)
Section Manager: The individual designated as being responsible for a particular
area or category of scientific analysis. This responsibility
includes direct day-to-day supervision of technical employees,
supply and instrument adequacy and upkeep, quality
assurance/quality control duties and ascertaining that
technical employees have the required balance of education,
training and experience to perform the required analyses.
(NELAC/DEQ)
Shall: Denotes a requirement that is mandatory whenever the
criterion for conformance with the specification requires that
there be no deviation. This does not prohibit the use of
alternative approaches or methods for implementing the
specification so long as the requirement is fulfilled. (ANSI)
Should: Denotes a guideline or recommendation whenever
noncompliance with the specification is permissible. (ANSI)
Standard Operating A written document which details the method of an operation,
Procedures (SOPs): analysis or action whose techniques and procedures are
thoroughly prescribed and which is accepted as the method
for performing certain routine or repetitive tasks. (QAMS)
Standard Method: A test method issued by an organization generally recognized
as competent to do so. (NELAC)
Toxic Substances The enabling legislation in 15 USC 2601 et seq., (1976), that
Control Act (TSCA): provides for testing, regulating, and screening all chemicals
produced or imported into the United States for possible toxic
effects prior to commercial manufacture. (NELAC)
Traceability: The property that allows a measurement to be related to
appropriate standards, generally international or national
standards, through an unbroken chain of comparisons. (VIM-
6.12/DEQ)
United States The federal governmental agency with responsibility for
Environmental protecting public health and safeguarding and improving the
Protection Agency natural environment (i.e., the air, water, and land) upon which
(EPA): human life depends. (US-EPA)
Validation: The confirmation by examination and provision of objective
evidence that the particular requirements for a specific
intended use are fulfilled. (NELAC)
Version 5.0 Glossary cont. Page xiii
Verification: Confirmation by examination and provision of objective

evidence that specified requirements have been met.
(NELAC/DEQ)
NOTE: In connection with the management of measuring
equipment, verification provides a means for checking that
deviations between values indicated by a measuring
instrument and corresponding known values of a measured
quantity are consistently smaller than the maximum allowable
error defined in a standard, regulation or specification peculiar
to the management of the measuring equipment.
Verification leads to a decision either to restore in service, to
perform adjustment, to repair, to downgrade, or to declare
obsolete. In all cases, it is required that a written trace of the
verification performed shall be kept on the measuring
instrument’s individual record.
Sources:
40 CFR Part 136
American Society for Quality Control (ASQC), Definitions of Environmental Quality Assurance
Terms, 1996
American National Standards Institute (ANSI), Style Manual for Preparation of Proposed
American National Standards, Eighth Edition, March 1991
ANSI/ASQC E4, 1994
ANSI N42.23-1995, Measurement and Associated Instrument Quality Assurance for
Radiobioassay Laboratories
International Standards Organization (ISO) Guides 2, 30, 8402
International Vocabulary of Basic and General Terms in Metrology (VIM): 1984. Issued by
BIPM, IEC, ISO and OIML
National Institute of Standards and Technology (NIST)
National Environmental Laboratory Accreditation Conference (NELAC), July 1998 Standards
Random House College Dictionary
US EPA Quality Assurance Management Section (QAMS), Glossary of Terms of Quality
Assurance Terms, 8/31/92 and 12/6/95
US EPA Quality Assurance Division (QAD)
Webster’s New World Dictionary of the American Language
Version 5.0 Page 1 of 64
1 Quality System
1.1 Introduction:
The Oregon Department of Environmental Quality (DEQ) was formally established in 1969 as a
product of a 1938 citizen initiative known as the Water Purification and Prevention of Pollution
Bill. In 1970 the Environmental Protection Agency (EPA) was created thereby making available
federal funds for environmental programs. The DEQ receives a significant portion of its funding
through the EPA; consequently many of the DEQ’s programs are designed to meet EPA
requirements. To qualify for this federal funding the EPA has made specific requirements of the
recipients, such as having a Quality System, which must be documented in the organizations
Quality Management Plan (QMP). The scope of the QMP is defined by EPA’s memorandum
5360 A1.
The QMP is a policy statement describing how an EPA organization shall comply with the
requirements of EPA Order 5360.1 CHG 2. Quality systems encompass the management and
technical activities necessary to plan, implement, and assess the effectiveness of QA and QC
operations applied to environmental programs. The QMP provides the blueprint for how an
individual EPA Program Office, Region, and National Laboratory or Center EPA Quality Manual
for Environmental Programs will plan, implement, and assess its quality system for the
environmental work to be performed as part of its mission. QMPs are reviewed and approved by
the OEI. Approval is valid for a period of up to five years.2
The DEQ first wrote its Quality Management Plan in 1982 to meet the standards at the time.
The DEQ’s latest QMP can be found on Q-Net and is intended to meet EPA’s current (R-2)
standard. The QMP describes the DEQ’s policies, objectives, principles, authority responsibility
and implementation of the agency’s Quality Management system. EPA has signed and
approved the DEQ’s QMP allowing the EPA programs to grant funds and accept data from the
DEQ. EPA requires the QMP be signed by the agency’s senior management. DEQ’s Executive
Management Team (EMT), which includes the director, the deputy director, and division
administrators have signed the QMP giving their concurrence. This commitment by top
management is essential for the success of the agency’s Quality System.
The QMP describes the use of other Quality Systems documents including this manual. The
Laboratory Quality Manual (LQM) shall describe the policies and, where appropriate,
procedures for all personnel within the Laboratory Division to follow. The LQM is not new to the
Laboratory. Its history is similar to that of the QMP and was formerly titled the DEQ Laboratory
Quality Assurance Manual. The policies and procedures in the LQM shall guide laboratory
personnel in collecting, producing, maintaining, and reporting data of known quality. The LQM
is continuously evolving with the discovery of omissions or undocumented policies, changes in
the agency’s Quality System, and adoption of new quality standards. The Laboratory Quality
Assurance Officer is responsible for the review and revision of the LQM. Laboratory Division
personnel must keep abreast of changes in quality policy and procedures, and therefore, must
read the changes to the LQM with each revision.
The QMP also describes the agency’s commitment to use National Environmental Laboratory
Accreditation Conference (NELAC) standards to evaluate a laboratory’s ability to generate
quality data. This LQM is written to meet NELAC standards and will be reviewed and revised as
required by the adoption of revised NELAC standards. NELAC standards may be revised at the
annual meeting, which may require annual modifications to the Laboratory Quality Manual,
however as the standards become more refined fewer and fewer changes shall come about.
NELAC standards are adopted two years after they are approved at the annual meeting, thus
2
EPA Quality Manual for Environmental Programs 5360 A1, 5/5/2000 US EPA, pg 2-8.
Version 5.0 Quality System cont. Page 2 of 64
allowing laboratories and accrediting authorities the opportunity to make the appropriate
adjustments in their systems. NELAC 2002 was used for the revision of this DEQ LQM.
1.2 DEQ's Quality Management Policy

In 2002 and re-written in 2004, as part of an investment in environmental excellence, the DEQ
identified its Strategic Directions and defined the Agency's priority work. Incumbent to these
Strategic Directions and DEQ's vision to work cooperatively with all Oregonians for a healthy,
sustainable environment are four priorities:
• Deliver Excellence in Performance and Product;
• Protect Oregon's Water;
• Protect Human Health and the Environment from Toxics; and
• Involve Oregonians in Solving Environmental Problems.
To deliver excellence the DEQ has a policy that Agency activities shall result in products and
decisions of known and acceptable quality. Consequently, the Laboratory's management
practices are intended to document and ensure that all environmental data generated, stored,
reported, or used by DEQ is of known and adequate quality to fulfill the needs of the primary
data user. Moreover, data used by the Agency shall be accurate, precise, complete,
representative, comparable, and when required, legally defensible. This policy applies to data
generated both internally within DEQ through the direct efforts of Agency personnel, and data
that is generated external to the Agency, arising from regulated activities, contracts, inter-
agency agreements, grants, and/or cooperative agreements.3
Management and Staff Responsibilities: As a key action element described in the
agency’s Strategic Directions, the agency recognizes the importance of motivated DEQ
employees to deliver excellence in their work. Laboratory management shall play an active role
in supporting laboratory staff and providing a work climate that fosters excellent service and
high quality work. Personnel honesty is of utmost importance for producing data of know
quality. Laboratory staff shall perform their duties with the intention to meet the policies and
procedures in this Quality Manual. Personnel shall not receive incentive rewards where to do
so would mean that Quality Assurance (QA) policies and or procedures could not be followed,
nor shall staff receive punitive actions for failing to generate data by applying QA policies and
procedures. Laboratory management shall not attempt to coerce staff into reporting data of
uncertain quality as if it were known to be acceptable. Personnel should contact a Quality
Assurance Officer (QAO), should they feel that pressure to generate data is compromising
quality. The QAO shall document the event and conduct an internal audit of the allegations.
The identity of the person making the observation shall remain anonymous if so desired. It is
recommended that such issues be brought before the Laboratory Quality Assurance Team
(QAT). Personnel may contact any member of the QAT whom they feel most comfortable with
or a Union representative to discuss their concerns.
LQM Objectives: The objectives of the LQM are to document the laboratory’s quality policies
and procedures, and to provide a tool for ensuring personnel are both knowledgeable of and
committed to these policies and procedures. All laboratory personnel must read this document
and sign an attestation memo that they shall implement the policies and procedures contained
in the LQM in their work practices. These policies and procedures shall ensure:
• Laboratory personnel have appropriate training and supervision (Chapter 2 Laboratory Management
Structure);
3
“QUALITY MANAGEMENT PLAN FOR THE OREGON DEPARTMENT OF ENVIRONMENTAL
QUALITY”, introduction and chapter 1.1 DEQ’s Management Policy.
Version 5.0 Quality System cont. Page 3 of 64
• the implementation of proper procedures for sample collection, storage, preservation, sample
tracking, analysis, and reporting (Chapter 3 Standard Operating Procedures);
• where applicable data is traceable to acceptable reference standards (Chapter 4 Measurement
Traceability);
• the degree of precision, accuracy, and bias of the analyses is known and documented (Chapter 5
Assuring the Quality of Analytical Data);
• that analytical equipment is properly used, calibrated, and maintained (Chapter 6 Equipment);
• all items influencing the quality of data are properly documented (Chapter 7 Quality Assurance);
• data is reported in useful and comparable formats (Chapter 8 Reporting Results).
2 Laboratory Management Structure

The laboratory shall have managerial and technical personnel with the authority and resources
needed to carry out their duties and to identify the occurrence of departures from the quality
system or from the procedures for performing environmental tests, and to initiate actions to
prevent or minimize such departures. The laboratory shall have technical management who
shall have overall responsibility for technical operations and can allocate the necessary
resources to ensure the required quality of laboratory operations. The laboratory shall also
appoint a Laboratory Quality Assurance Officer (LQAO) who shall ensure NELAC standards are
implemented in the laboratory.
The laboratory’s organizational structure and its place in the agency supports this policy by
giving the laboratory autonomy with executive leadership.
The DEQ is organized into the Office of the Director and seven Regions/Divisions which report
to either the Director or Deputy Director. The Director is required to answer to the members of
the Environmental Quality Commission (EQC), who are appointed by the governor and serve as
an external oversight board. For a more in depth description of the Director’s Office and the
agency’s divisions other than the Laboratory Division refer to the agency’s QMP.
The Laboratory Division is organized into six structural groups under the direction of the
Laboratory Administrator. The Administration section of the laboratory is under the direct
supervision of the Laboratory Administrator as are the section managers for Air Quality
Monitoring, Watershed Assessment, Inorganic Laboratory, Organic & General Chemistry
Laboratory, and Technical Services. Each section manager is responsible for the proper
management of his/her section and compliance with the LQM. Even though the Air Quality
Monitoring and Watershed Assessment sections generate data while not physically in the
laboratory, they must also comply with the policies and procedures of the LQM. The Laboratory
Organizational Chart (Appendix H) illustrates the present structure of the laboratory. The
technical requirements and training documentation for each position are described in section 2.8
below.
Section managers are responsible for the training needs of each person within their sections.
Through the use of the laboratory’s personnel training database, managers shall monitor
required and received training. Section managers shall also submit to the LQAO documentation
of personnel receiving training; and, where pertinent, certificates of Demonstration Of Capability
(Appendix A). The LQAO shall maintain administrative files containing this documentation and
a signature log with initials and date. These files should not be confused with other personnel
files, which are maintained by the laboratory executive staff and the Human Resources Division.
The laboratory executive staff must maintain files containing personal information on
employees. This personal information is not available for QA review, whereas the QA
administrative files shall be available for quality audits. The LQAO shall routinely destroy
laboratory QA administrative documentation older than five years.
2.1 Laboratory Quality Assurance Team

Laboratory QA activities are processed through the laboratory Quality Assurance Team (QAT).
The QAT is made up the Quality Assurance Officers (QAOs) and representatives from each
section of the laboratory. The QAT may assist the QAOs with internal audits, review of
documents, and QA/QC policy. The QAT shall recommend QA decisions to the Laboratory
Management Team (LMT) and the Division Administrator, whereupon the Administrator shall
adopt or rescind the decision. The LMT shall support and abide by all adopted QA decisions.
The mission of the laboratory QAT is to continually review quality with respect to the functions of
the laboratory. The QAT shall meet routinely to discuss and implement action items, and to
Version 5.0 Laboratory Management Structure cont. Page 5 of 64
develop systems to help prevent quality related problems. Laboratory personnel are
encouraged to discuss Quality Management issues with the QAT members. When the QAT
recognizes the need to change or adopt new quality polices or practices, the QAT shall prepare
an action plan to ensure that the changes are implemented and monitored. The QAT meeting
minutes shall include the perceived need of a plan, the procedure for initiating the plan, and
application of controls to ensure the preventative measure is effective.
2.2 Administration
The administrative section of the laboratory provides support for the laboratory in the areas of
Human Resources/Accounting, special projects, and Quality Management.
An executive support specialist offers administrative support to all sections of the laboratory in
addition to the administrator (e.g. travel and time accounting) and serves as a liaison to PSU
facilities.
Special projects include updating monitoring strategies, assisting with laboratory and monitoring
operational analysis, legislative coordination for the Lab Division (including grant applications
and reports), and assistance to the Administrator on unanticipated requests from outside
stakeholders or colleagues.
The oversight of quality assurance issues is delegated to three QAOs. There is a QAO for each
DEQ program: Air Quality, Land Quality, and Water Quality. The QAOs provide technical
assistance in the development and implementation of QA project plans; audits monitoring
network; performs assessments of self-monitoring activities under air, NPDES, and RCRA
permits; participates in Oregon Laboratory Accreditation Program (ORELAP) activities; reports
to programs documenting project data quality; and ensures corrective action procedures are
followed when data quality criteria are not met. Additionally one Quality Assurance Officer shall
be assigned the responsibility of ensuring that NELAC standards are implemented at the DEQ
laboratory and is recognized in this document as the Laboratory Quality Assurance Officer
(LQAO).
2.3 Air Quality Monitoring

The Air Quality Monitoring section operates and maintains the DEQ ambient air
monitoring/sampling network, calibrates air monitors/samplers, collects samples, maintains
equipment, and reports air monitoring data to EPA. The Air Quality Monitoring (AQM) section
may audit ambient air monitoring and meteorological monitoring activities by permitted sources
and Prevention of Significant Deterioration applicants.
2.4 Watershed Assessment

Watershed Assessment staff collect data and samples for ambient water quality monitoring of
both surface and groundwater, for monitoring biological activity, and for groundwater monitoring
at solid waste sites. The Watershed Assessment section maintains field equipment and
instruments, provides technical assistance for the collection of water, soil, and sediment
samples, performs audits of self-monitoring programs, collects split samples, and reports on
audit findings and project studies.
2.5 Inorganic Laboratory

Inorganic personnel conduct analyses on Air / Emissions, Aqueous, Drinking Water,
Saline/Estuarine, Biological Tissue, Solids, and Chemical Waste samples for inorganic
constituents such as metals, nutrients, and particulate mass. They also provide technical
assistance in the preparation of QA project plans relating to sampling requirements, and
laboratory capabilities; and interpret inorganic analytical data.
2.6 Organic Laboratory

Organic personnel conduct analyses on Air / Emissions, Aqueous, Drinking Water,
Saline/Estuarine, Biological Tissue, Solids, and Chemical Waste samples for organic
constituents and physical properties. They also provide technical assistance relating to
preparation of QA project plans, sample collection requirements, and laboratory capabilities;
and interpret organic analytical data.
2.7 Technical Services

The Technical Services section maintains the laboratory computer network, Laboratory
Information Management System (LIMS), and the laboratory data stored in these systems.
Technical Services also responds to customer service and data interpretation requests. After
the Laboratory Administrator approves the final release of data, the Technical Services section
ensures the report recipient (programs and other agencies) receives the data in a usable format.
Technical Services ensures samples are received in compliance with requirements of the
Quality Assurance Project Plan (QAPP) and that sample integrity is maintained through the
completion of the analytical work or that data is flagged. Technical Services also maintains an
inventory control system for equipment and supplies; processes supply requisitions for the
laboratory; provides clerical support; and controls access to the laboratory.
2.8 Personnel
The DEQ laboratory hires employees with the necessary training and experience through the
recruiting procedures required by the State of Oregon. The minimum qualifications of agency
positions are defined by Oregon State Division of Administrative Services (DAS). The DEQ
must adhere to strict and consistent processing of all recruitments. A prospective employee
must complete a State application form where he/she lists his/her qualifications and certify the
information he/she gives as true and complete. All applications and recruitment materials are
kept in the Human Resource office in confidential files. These files are available for internal
review upon request. In order for an applicant to advance to the interview stage of a
recruitment, his/her application is first reviewed by the agency’s Human Resources department
to insure he/she meets the minimum qualifications for the classification as determined by DAS
(refer to Table 1). An applicant is required to meet the established minimum qualifications in
order to proceed in the recruiting process. The DEQ laboratory management shall assume that
any person who has been selected for the opportunity to interview for a particular position has
successfully met or exceeded the minimum qualifications required for that position.
Many of the skilled laboratory positions require special training. Management shall ensure
personnel receive the special training required for these positions. This training shall be
documented and submitted to the LQAO. During an internal audit the QAO shall review these
records to ensure personnel have had the training to perform their duties as required by
programs, NELAC standards, and laboratory policy.
Table 1 Minimum Qualification for Laboratory Personnel
Position Minimum Qualification

Laboratory Division Qualifications will be determined by the appointing authority based
Administrator (P E/Mgr G) on the duties and responsibilities of the position.
Four years of management experience in a public or private
organization which included responsibility for each of the
following:
a) development of program rules and policies;
b) development of long- and short-range goals and plans;
c) program evaluation; and
d) budget preparation.
Graduate level courses in management may be substituted for
one year of the required experience.
Quality Assurance Officer Three years of experience in the program area. At least one year
(NRS5, Chem3, NRS3) of the experience must be at a technical or professional level
performing activities in the program such as researching and
analyzing data, conducting investigations, applying pertinent laws
and regulations, OR coordinating and monitoring project activities;
AND a Bachelor's degree in chemistry or environmental
disciplines, OR three additional years of related (pertinent)
experience.
A Master's degree in chemistry or environmental disciplines will
substitute for up to one year of the required experience.
A Doctorate degree in chemistry or environmental disciplines will
substitute for up to two years of the required experience.
QAOs have day-to-day responsibility for agency program QA
needs and frequently function as a team leader to fulfill program
responsibilities, or frequently lead other staff and coordinate
actions to accomplish central projects or studies.
Section Manager (P E/Mgr Three years of management experience in a public or private
E) organization which included responsibility for each of the
following: a) development of program rules and policies, b)
development of long- and short-range goals and plans, c) program
evaluation, and d) budget preparation.
Graduate level courses in management may be substituted for
one year of the required experience.
Laboratory Section managers must have the technical expertise
for the sections they supervise. Experience in the field of
expertise may be used to qualify a candidate.

Senior Monitoring Three years of experience in the program area. At least one year
Specialist/Chemist, and of the experience must be at a technical or professional level
Toxics Coordinator (NRS4) performing activities in the program such as researching and
experience.
Senior Monitoring Specialist and Chemist have day-to-day
responsibility as a team leader to fulfill program responsibilities, or
frequently lead other staff and coordinate actions to accomplish
central projects or studies.
Lead Chemist (Chem3) Two years of experience independently performing analytical
chemistry procedures which included designing, developing, and
implementing analytical methods and procedures AND a
Bachelor's degree in Chemistry
Three additional years of pertinent experience may substitute for
the Bachelor's.
In general the lead chemist serves as a specialist with expertise in
a specialty area of chemistry involving the design, development,
and application of the state of the art analytical methods and
procedures to complex and unusual problems and may serve as a
team leader to fulfill program responsibilities.
Chemist (Chem2 & One year of experience independently performing analytical
Chem1) chemistry procedures and a Bachelor's degree in Chemistry.
Three additional years of pertinent experience may substitute for
the Bachelor's degree.

Monitoring Specialist Three years of experience in the program area. At least one year
(NRS3) of the experience must be at a technical or professional level
performing activities in a natural resource program such as
researching and analyzing data, conducting investigations,
applying pertinent laws and regulations, OR coordinating and
monitoring project activities; AND a Bachelor's degree in
environmental related disciplines, OR three additional years of
related (pertinent) experience.
A Master's degree in environmental related disciplines will
A Doctorate degree in environmental related disciplines will
Monitoring Specialists frequently function as a team leader to fulfill
program responsibilities.
Monitoring Technician Two years of experience in environmental work, AND a
(NRS2) Bachelor's degree in environmental related disciplines, or three
additional years of related (pertinent) experience; OR one year of
experience in environmental related disciplines, and a Master's
degree in environmental related disciplines; OR a Doctorate
degree in environmental related disciplines.
Project Coordinator Three years of experience in the program area. At least one year
(NRS5) of the experience must be at a technical or professional level
experience.
LIMS Coordinator (ISS5) Three years of professional consultative, technical, or
administrative experience which includes designing, constructing,
or analyzing information systems. Experience must include
activities in Laboratory Information Systems; AND either
(a) at least 30 quarter (20 semester) credits in computer science;
OR
(b) two more years of experience providing a knowledge of
information systems theory and principles;

Database Specialist (ISS4) Two years of professional information systems experience which
includes developing, maintaining, and installing information
systems, and analyzing systems. Experience must include
activities in database maintenance; AND either
(a) at least 30 quarter (20 semester) credits in computer science;
OR
(b) two more years of information systems experience;
Sample Tracker (NRS3) Three years of experience in the program area. At least one year
of the experience must be at a technical or professional level
experience.
Procurement & Contract Three years experience in the procurement of goods and services
Specialist (PCS1) through purchase orders and contract agreements, or tracking
and preparing simple or standard contracts or agreements
OR
A Bachelor's Degree in Business or Public Administration, or a
related degree that included course work in general business
management, contract or business law, accounting, finance or
economics.
Document Control Two years of general clerical experience, one year of which
Coordinator (OS2) included typing, word processing, or other experience generating
documents; OR an Associate's degree in Office Occupations or
Office Technology; OR graduation from a private school of
business with a Certificate in Office Occupations or Office
Technology AND one year of general clerical experience.
College courses in Office Occupations or Office Technology will
substitute for the required experience on a year-for-year basis.
Laboratory management may supplement the minimum
qualifications to require specific knowledge and skills as specified
in the Classification Specification, i.e. knowledge of database
structure and maintenance.

Data Clerk (OS2) Two years of general clerical experience, one year of which
included typing, word processing, or other experience generating
documents; OR an Associate's degree in Office Occupations or
Office Technology; OR graduation from a private school of
business with a Certificate in Office Occupations or Office
Technology AND one year of general clerical experience.
College courses in Office Occupations or Office Technology will
substitute for the required experience on a year-for-year basis.
Laboratory management may supplement the minimum
qualifications to require specific knowledge and skills as specified
in the Classification Specification, i.e. knowledge of Chemical
naming conventions.
3 Standard Operating Procedures

The Laboratory shall provide personnel with written instructions that shall be used to ensure the
correctness and reliability of test results. The laboratory shall write Standard Operating
Procedures (SOPs) for repetitive routine tasks, which shall describe the techniques and
procedures for an analysis or action.
Laboratory section managers shall ensure SOPs are written and controlled using the
laboratory’s Document Control procedure (DEQ02-LAB-0004-SOP). The Quality Assurance Team
(QAT) will help identify work requiring development of an SOP. The following activities must be
described in Laboratory SOPs. This list is not designed to be exhaustive. Additional activities
may also need to be documented in SOPs:
• Watershed Assessment and Air Quality Monitoring section managers shall ensure that
sample collection and field analysis procedures are written to cover their respective
fields.
• The Laboratory Quality Assurance Officer (LQAO) shall revise the Field Sampling
Reference Guide used for field operations typically performed by regional staff.
• The organic and inorganic section managers shall ensure SOPs are written for sample
analyses and data transfer to appropriate databases.
• Technical Services shall ensure SOPs are written and revised for a series of routine
work performed by the Technical Services section. Technical Services will make sample
storage, preservation, and tracking SOPs available on Q-net.
• Technical Services shall write SOPs for the control of electronic information within the
laboratory; i.e. posting documents on the web, securing servers for defined uses,
maintaining tables within LIMS, creating reports from LIMS, and the reporting of results.
SOPs shall be available to all Laboratory and Agency personnel. Hardcopies may be requested
through the LQAO and electronic version will be available whenever possible on Q-net.
3.1 Sampling
The DEQ laboratory primarily conducts analytical tests on samples collected by the different
regions of the agency and by the Laboratory sections of Watershed Assessment (WA) and Air
Quality Monitoring (AQM). WA has prepared a Mode of Operations Manual (MOM) to cover
sampling procedures and analytical work performed in the field. AQM staff have prepared
SOPs for each of the sampling techniques they use. Sampling procedures shall instruct
personnel on how to collect representative samples, record data, and when applicable submit
properly preserved samples to the laboratory for further analysis. Data recorded during
sampling should include the sampling procedure used, the identification of sampling equipment
and personnel, environmental conditions (if relevant), the time sample collection started and
stopped, the date, and the sampling location.
The LQAO shall maintain the Field Sampling Reference Guide, which instructs personnel
outside the laboratory on how to collect and submit samples to the DEQ laboratory. The
Technical Services section shall make these documents available on Q-Net.
The laboratory must have on file copies of Quality Assurance Project Plans (QAPPs) as
required by the agency’s QMP. The QAPP should describe the methods used to collect
samples, ensuring the quality of the data and, if appropriate, the statistics used to develop the
sampling procedures. The QAPP shall provide sampling information or the appropriate
template for writing a Sampling & Analysis Plan (SAP). SAPs are a subgroup of the larger more
encompassing QAPP. There are cases where the QAPP shall describe the elements within the
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SAP and thus a SAP may not be necessary for all samples. SAPs are also controlled
documents (refer to the agency’s QMP for more information). The SAP should primarily
describe the schedule for collecting samples, the location of the sample, and the requested test
methods. The laboratory should receive the SAP and/or QAPP before sampling begins so the
different sections of the laboratory can make the necessary arrangements to perform the work.
If the project coordinator requires a deviation from the QAPP, a SAP may describe the deviation
without revising the QAPP. Technical Services shall devise a system for ensuring that all
appropriate personnel are advised of SAPs and that they shall have access to SAPs.
3.2 Sample Handling

Technical Services shall receive samples submitted to the laboratory. The Technical Services
manager shall ensure the Sample Receiving SOP is controlled as with all other SOPs. The
procedure shall describe required documentation and information on the transportation, receipt,
handling, protection, storage, retention and/or disposal of samples, including all provisions
necessary to protect the integrity of the sample.
3.2.1 Sample Identification

Upon sample receipt, the sample tracker shall assign a sampling event number to the group of
samples packaged together. Each container is inspected to ensure the container identification
number appears on the form used to submit the samples. Typically labels are made of a
durable plastic material with pre-printed numbers or are engraved into the container. The
container number along with the sampling event number uniquely identifies each sample/sub-
sample received. The sample tracker logs the sampling event number and container number
into LIMS, which assigns an item number to each sample linking sample, sub-samples and
sample location. This combination of numbers is used in LIMS to minimize confusion regarding
the identity of samples at any time. The combined sampling event number, item number and/or
container number are used for the identification of all subsequent extracts and/or digestates to
link the sample with all related laboratory activities.
As the supply of containers diminishes over time new containers are purchased and label
numbers are engraved into them. The numbers assigned to the container should not exceed
four digits to minimize transcription errors. The laboratory has used several thousand
containers over the years and the numbering system has rolled over since its conception.
Because it is not clear whether the container was disposed of prior to reusing a number, it is
possible for the same container number to appear in the system at the same time. Technical
Services shall maintain a controlled log of container numbers to manage the process of
discarding old containers and labeling new containers. In the event that more than one sample
with the same container number is entered into LIMS at the same time, the LIMS system will
catch the problem and prompt the sample tracker to verify the numbers. The sample tracker
may append a suffix to the number or re-label the container to create a unique combination of
numbers.
3.2.2 Sample Receipt

LIMS shall track who received the samples and the date and time the sample is entered into the
database. This record will be the official sample receipt date and time. Because some methods
require short holding times it is important for the project coordinator to account for transportation
time from the shipper and the time it takes for the tracker to log in the sampling event. The
project coordinator shall discuss these details with the QAO during the development of the
QAPP.
Upon receipt of samples, the sample tracker shall fill out a "Sample Receipt Checklist" that will
identify the number of shipping containers, the internal temperature of those containers, the
condition of the samples, the status of preservation checks, and whether or not the samples
were shipped and received with a Chain-of-Custody form. Any abnormalities or departures from
acceptable conditions as described in the QAPP or SOPs shall be noted on the checklist. This
checklist may be used in lieu of the Nonconformance forms in Appendix C, however the
procedures in section 7.5.3 below must be followed to ensure the proper information is collected
and documented. The sample tracker must consult with the project coordinator and document
all correspondence to determine the course of action, i.e. to resample, void, or proceed with
sample analysis. The project coordinator’s instructions must be determined prior to proceeding
with the analyses. The sample tracker’s Sample Receiving procedure shall be provided to
project coordinators during the development of their QAPP so they may add any specific needs
for handling samples. The project coordinator shall either accept the sample trackers procedure
or address procedures in the QAPP for avoiding deterioration, contamination, loss or damage to
the sample during storage, handling, preparation and testing. Without explicit sample handling
procedures described in the QAPP, the laboratory shall assume that there is no deviation from
the tracker’s Sample Receiving SOP. Should the sample tracker discover special sample
handling instructions at the time of receipt, the sample tracker shall communicate the sample
handling deviation to laboratory managers using the proper Nonconformance documentation
procedures (refer to Appendix C: Nonconformance Report).
The laboratory uses a special Legal Chain Of Custody procedure for handling samples collected
for the use of enforcement investigations. This procedure documents the location of the sample
and who has removed it from its locked location to perform his/her work. The sample tracker
shall record the “Legal” status of the sample in LIMS. The tracker, Technical Services manager,
and the assistant to the laboratory director shall be the only personnel to have a key to the
locked “Legal” storage areas.
3.2.3 Sample Integrity

The sample tracker shall place all samples in specified storage areas. The sample tracker shall
ensure that these areas are maintained and the environmental conditions are monitored, and
recorded. The tracker’s Sample Receiving SOP shall describe how to check, record, and
identify the types of samples requiring the following prescribed preservation protocols:
1) Samples which require thermal preservation shall be stored under refrigeration which is
+/-2°C of the specified preservation temperature unless method specific criteria exist.
For samples with a specified storage temperature of 4°C, storage at a temperature
above the freezing point of water to 6°C shall be acceptable.
a) Samples that are hand delivered to the laboratory immediately after collection may
not meet this criterion. In these cases, the samples shall be considered acceptable if
there is evidence that chilling has begun such as arrival on ice.
2) Samples requiring pH preservation shall be checked either at the time of sample receipt
or by the laboratory analysts; the point at which preservation is checked will be
documented on the Sample Receipt Checklist. All preservation checks will be
electronically documented in the LIMS.
3) Samples shall be stored away from all standards, reagents, food and other potentially
contaminating sources. Samples shall be stored in such a manner to prevent cross
contamination.
a) Sample fractions, extracts, leachates and other sample preparation products shall be
stored as described above or according to specifications in the test method or QAPP.
b) Test method SOPs shall describe the process for the disposal of digestates,
leachates and extracts or other sample preparation products.
c) The Technical Services section shall maintain the SOP for the disposal of samples.
Samples identified as Hazardous Waste shall be collected for disposal at an
appropriate facility, refer to the laboratory’s Chemical Waste Management SOP
(DEQ04-LAB-0014-SOP).
4) After logging in samples the tracker shall notify appropriate personnel of the receipt of
samples with short holding times (for methods with holding times of less than or equal to
48 hours refer to the sample tracker’s Sample Receiving SOP). Chemists shall begin
these test methods within the cited holding times.
Personnel who find that any of the above sample integrity policies has been compromised shall
initiate the corrective action procedure described in this document and begin the completion of
the Nonconformance Report. In most cases the data shall be reported as an estimate with an
appropriate comment attached to the result.
3.3 Test Methods and Method Validation
3.3.1 Analytical SOPs

Appendix G lists the analytical test methods the laboratory performs and cites the EPA
reference test method. The laboratory shall have controlled (refer to section 2.8) written
Standard Operating Procedures (SOPs) for each of these test methods. Authors of test method
SOPs shall write or revise the SOP to conform to the cited procedure, but any revision shall not
alter the chemistry involved in the cited method. Copies of the cited reference materials shall be
controlled and retained for the same period as the referencing SOP. Laboratory SOPs shall
clarify ambiguities and explicitly identify options used in the referenced method. The author
shall clearly note any deviation from the referenced test method.
The DEQ laboratory shall attempt to use peer-reviewed and validated methods published by
international, national, or regional authorities. The laboratory shall ensure it uses the latest valid
edition of a standard unless it is not appropriate or possible to do so. Deviations from this policy
shall require discussions between the project coordinator, laboratory section managers, and the
QAO. When necessary, the Laboratory-specific SOP shall supplement the reference method
with additional details to ensure consistent application. The DEQ shall only use EPA
promulgated test methods for programs that require such methods. The QAOs shall ensure
QAPPs cite the appropriate analytical methodologies.
Test method SOPs shall instruct the reader on the use and operation of all relevant equipment,
and on the handling and preparation of samples (refer to Preparing Standard Operating
Procedures: DEQ04-LAB-0001-SOP for creating an acceptable SOP). During the annual
internal audit, the auditors shall cite, when necessary, the deficiency of failing to meet criteria
described in the Preparing Standard Operating Procedures. The corrective action plan for this
deficiency shall be to revise the SOP to meet the current NELAC standards and to set a
schedule for completing the revision.
There are occasions where projects require technical deviations from the laboratory’s
documented procedures. Deviation from cited methods shall occur only if the deviation is
documented in the QAPP. The deviation shall be technically justified, authorized, and accepted
by appropriate personnel (typically the signatories on the QAPP). The QAO shall ensure that
method deviations required by the project are documented in the QAPP and communicated to
all appropriate personnel, which includes personnel identified in the QAPP and all appropriate
sections of the laboratory. Test results that are reported using the altered procedure shall be
recorded and tracked in LIMS by creating a unique “Standard Parameter” for the new
procedure.
During the development of the QAPP, the QAO shall advise the project coordinator if test
methods appear to be inappropriate or out of date. If a decision is made to continue with an
undocumented procedure, the DEQ laboratory will then develop its own procedure. The QAO
shall assign the task of creating the new SOP to the appropriate laboratory section. The section
manager shall delegate the responsibility for developing the method and writing the SOP to
appropriate personnel.
The analytical sections of the laboratory shall play the most significant role in the development
and documentation of new test methods; however, they must maintain open communication
with the QAO and management. The development of new methods shall be a planned activity,
which will require routine meetings between analytical staff, management, and the QAO. The
meeting minutes shall become part of the SOP control document file. The meetings shall cover
the process of developing the method and its progress. QAT members shall put method
development on their meeting agenda to share the progress of their new methods with other
sections of the laboratory. New methods will be based on the laboratory’s best available
technologies and preferably on test methods published by reputable organizations or instrument
manufacturers. Communication between project coordinators and QAO is essential to ensure
laboratory procedures conform to program requirements.
3.3.2 Demonstrations of Capability

Prior to using a procedure, all test methods must be validated through completion of an Initial
Demonstration of Capability (IDOC). A summary of the IDOC data shall be included in the
"Method Performance" section of the analytical SOP. The IDOC should confirm the laboratory’s
ability to meet QC criteria cited in referenced methods. Ongoing QC should ensure that each
batch of data produced continues to meet expected quality. Continuing Demonstration Of
Capability (CDOC) studies are required annually and shall demonstrate the laboratory’s
continued proficiency to perform the analytical method. DOC records (refer to Appendix A) will
be kept on file for all personnel who perform analytical test methods. SOPs shall be reviewed
annually and DOC procedures shall be verified to comply with the current NELAC standards.
Details of the Laboratory's DOC procedures will be written by the LQAO.
3.3.3 Data Validation

Laboratory personnel will ensure that all reported data satisfies – at a minimum – the
appropriate analytical Quality Control requirements. The typical DEQ analytical procedure must
satisfy specific QC requirements, which are usually cited in the reference method. In the event
that data does not meet the requisite QC criteria, results will be reported with data qualifiers.
During the development of the QAPP the QAOs will discuss the laboratory's QC procedures and
establish if they are appropriate for the project needs. In many instances, the Laboratory's QC
requirements and control limits will meet or exceed project needs and the Laboratory's default
procedures will be used. However, if the project requires the reporting of data that falls outside
the Laboratory's default control limits, the laboratory shall develop and document procedures for
reporting such data in the QAPP. By default, data that falling outside the default control limits
will be reported as estimates ("est"), and the data flagged with in LIMS with the QA status code
of “B”. LIMS status codes (Appendix D) are used to track the quality of analytical results in the
Laboratory Analytical Storage and Retrieval (LASAR) database. This coding system allows the
secondary and LASAR data users to quickly and easily assess data quality using the
Laboratory's default QC criteria. The status code of "B" is used to mark data as failing to meet
the Laboratory's default QC standards. Data users should carefully review data and the
associated QC information before using it.
The Laboratory will not provide detailed data quality assessment services to the Agency by
default. Generally, Project Coordinators sending samples to the Laboratory shall be responsible
for the statistical validation of data for their projects. Project Coordinators submitting samples to
the lab should first identify their Data Quality Objectives (e.g. verifying a null hypothesis) and
establish the appropriate the statistical approach for assessing the data set. Laboratory
assistance with data quality assessments, can be arranged between the project coordinator and
a QAO or the Technical Services section manager. Data quality concerns should be reported to
the QAOs so that DQOs can be refined in future QAPPs. Project Coordinators are encouraged
to request QC data with the analytical report, so they can more readily evaluate the
effectiveness of the project.
3.3.4 Estimation of Uncertainty of Measurement

With adoption of the 2002 NELAC standards, the DEQ Laboratory is required to establish a
system for estimating measurement uncertainty. Analytical SOPs written or revised after
adoption of these standards (01 July 2004) shall discuss the sources of measurement
uncertainty. If rigorous, metrologically and statistically valid, calculations of uncertainty cannot
be described, the SOP shall attempt to identify all the major components of analytical
uncertainty and make a reasonable estimation of the expected uncertainty. Under no
circumstances should the Laboratory misrepresent the estimation of measurement uncertainty;
reasonable attempts must be made to establish the limits of measurement uncertainty for all
analytical methods. Reasonable attempts at estimation shall be based on knowledge of the
method performance and on the measurement scope, and shall make use of previous
experience and validation data.
When estimating measurement uncertainty, all uncertainty components which are important in a
given situation shall be taken into account using appropriate methods of analysis.
3.3.5 Data Control

Employees performing new functions shall have their work reviewed by their peers. Section
managers may assign this task to other staff members or review the work themselves. Typically
the frequency of review diminishes as personnel become more competent. However comfort
can lead to a level of complacency and a system of routine checks is needed.
Section mangers shall write a procedure for data control within their sections. Since different
analytical methods and programs require different recording procedures, a laboratory-wide
generic data control procedure is not practical. All data control procedures shall comply with
section 7.2 of this document (Analytical Records). The procedure shall assign responsibility for
the review of integrations, data transfer, and manual calculations; the frequency of these
reviews; and the implementation process for potential corrective actions.
As described in the Nonconformance Investigations and Corrective Action procedure an analyst
shall typically review data for transfer and calculation errors prior to completing the work lists in
LIMS. The lead chemists, section managers and QAO shall then examine quality control
measures prior to approving the data during the review processes.
Most of the analytical equipment used by the laboratory is controlled by computers. The
software on these computers must have sufficient documentation, which is adequate for its
intended use. Personnel purchasing new systems shall ensure they come with appropriate
documentation. Commercial off-the-shelf software (e. g. word processing, database and
statistical programs) in general use within the designed application range may be considered to
be sufficiently validated. Personnel shall maintain automated equipment to ensure they function
properly. The laboratory facility shall provide the necessary environmental and operating
conditions to maintain the integrity of data stored in these computer systems.
The Technical Services section shall develop a SOP for ensuring the data integrity of electronic
data. This SOP shall describe the process used to maintain, document, and store data ensuring
that it can not be altered, is transmitted correctly, and processing does not produce
misinformation. Data shall be stored such that security can be monitored and access controlled.
4 Measurement Traceability
The laboratory shall ensure analytical measurements are traceable to acceptable reference
standards.
4.1 Documentation
In order to ensure data is of known quality, laboratory staff must be able to document the source
and tolerance levels of reference standards, and reagents. To the best of its ability, the
laboratory shall use National Institute of Standards and Technology (NIST) traceable standards
and contract services that use NIST traceable standards. The laboratory must be able to show
a paper trail from the test result of a sample back to the NIST standard for the analyte and all
measurement devices used in the analysis. Analysts performing analytical work shall follow the
laboratory’s documentation procedures ensuring that analytical results are easily linked to
calibration data, which is linked to reference material certificates described in Purchasing
Services and Supplies section below.
There are occasions when certificates are not available in which case the analyst must validate
the suitability of the reference. The analyst should obtain approval from his/her section
manager prior to testing the suitability of a product, since the Laboratory should be able to
purchase materials with certificates. This suitability testing procedure must be documented and
approved by the Quality Assurance Team (QAT) or test method signatories. As a final measure
for verifying the suitability of uncertified materials, the analyst must evaluate the result of a
Laboratory Control Sample (LCS) using the material in question. Results of the suitability
testing shall be documented as other test method results, thus the first occurrence of the
product identification number in the analytical records will be that of the suitability test.
• Glassware, Chemicals, Reagent Water, Gases, and Reagents
The laboratory will purchase supplies of the highest quality needed to ensure minimal
interference or contamination with a procedure. As appropriate Chemists and Technicians will:
• use “Class A” volumetric glassware for the preparation and dilution of reagents,
standards, and samples;
• ensure non-volumetric glassware is of an appropriate quality;
• ensure compressed gases are of known purity and guaranteed by the supplier;
• ensure chemicals are dated on receipt, stored according to chemical properties, and
discarded when shelf life is exceeded (for chemicals where shelf life is defined);
• ensure solvents employed in organic analyses are “HPLC” or “Pesticide grade” and
stored in ventilated explosion-proof cabinets; and,
• ensure analytical reagents or solvents are never stored with samples awaiting analysis.
The analyst shall document reagent preparation. Documentation shall include the source of the
reagent, the mass or volume used, and dilution information. The test method SOP should
contain specific instructions for reagent preparation and documentation. Reagents shall be
prepared from “Analytical Reagent” grade (AR) or higher purity chemicals as required by the
method, and shall be stored as recommended in the method, or by the chemical manufacturer.
4.2 Purchasing Services and Supplies

For the purpose of this LQM only the purchasing procedures for products that have an effect on
data quality are discussed here. For example the purchases of paper and phone services are
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not directly related to data quality. Whereas the quality of chemical reagents, concentration of
standards, instrumentation, and instrument service contracts do have an impact on the quality of
data reported. In order to ensure the integrity of data, laboratory staff must follow these
procedures for purchasing services and supplies.
It is the responsibility of the Procurement & Contract Specialist (PCS) to purchase, receive,
label appropriate supplies, and to dispose of unused obsolete equipment and supplies by
following the State Surplus procedures and completing the Property Disposition Request (PDR)
forms. The Technical Services section manager shall ensure the PCS is properly trained and
instructed to apply the following Request for Purchase SOP to all chemicals, measuring
devices, and service contracts.
4.2.1 Request for Purchase

The PCS, analyst, and the section manager are responsible for the traceability of supplies. The
PCS shall maintain the Requisition database, which is used to track the purchase and receipt of
all orders.
The chemist or technician, who needs the supplies shall investigate purchase options and
request the purchase of appropriate supplies and/or services. Even though some laboratory
sections may designate an individual to complete the Requisition forms, the chemist/technician
requesting the supplies shall note the quality needed. Signatory authorities who sign test
method SOPs shall ensure the SOP specifies the quality of chemicals and instrument to be
used. Test method SOPs shall identify chemicals that need not come with certificates or are
unlikely to have such certification. Test method SOPs shall describe how these chemicals will
be evaluated to assess their suitability.
The purchaser of supplies or services in each section shall use the Requisition database, where
the purchaser may retrieve historical data to help determine viable vendors. The list of vendors
in the database is maintained by the PCS. Chemists and technicians using the products shall
offer feedback to the Technical Services section as to the quality of the product received from
the vendor. Technical Services shall document the feedback and link the comments to the
vendors within the Requisition database. This information shall be reviewed for the annual QA
report to management and for future consideration of a given vendor. Some programs may
require the use of specific products available through qualified vendors. The Requisition
database shall maintain an auditable link between product and vendor ensuring the use of
appropriate vendors for prescriptive program needs.
It is the responsibility of management to either concur with staff requests for purchase or
disapprove them. When the section manager signs the Requisition form he/she is agreeing with
the chemist’s assessment of the appropriate product quality.
4.2.2 Purchase
All purchases have a formal purchase approval process. Expenses over an amount set by the
Oregon State Division of Administrative Services (DAS) must be approved by DAS. Less
expensive orders may be approved by the DEQ’s accounting office or laboratory personnel.
The triggers, which identify who is to grant final approval of a purchase, change with time and
the PCS shall stay informed of the current policy.
Many purchases are performed using credit cards. Such purchases must be approved by the
credit card holder and the section manager. Since these purchases may occur without prior
consent, personnel should take caution and management shall inform personnel of the current
credit card policy. Personnel may be held responsible for inappropriate purchases.
To ensure products directly related to data quality are tracked; personnel must copy the
Requisition by printing it from the database or by filing out the paper form. Products that shall
be tracked are often of sufficient value to trigger the requirement to complete a Requisition;
however, laboratory staff may use petty cash for inexpensive supplies. Personnel must be
mindful of the requirement that certain products must be tracked and the PCS must have a copy
of the Requisition to ensure data for such products are entered into the system.
4.2.3 Receipt
Upon receipt of any product the laboratory receptionist shall notify the PCS of its arrival. The
PCS shall identify the product and locate a copy of the Requisition form and notify the staff
member who requested the purchase. The purchaser shall inspect the product for consistency
with the order and possible shipping damage. The purchaser shall also verify the quality of any
chemical received and verify that the appropriate certificate of analysis was sent. If the
purchaser finds no problems, he/she shall sign the receipt and return it to the PCS. The
recipient of contracted services shall request copies of certificates from the contractor to
maintain the laboratory’s traceability requirements. If there is a problem with the order the PCS
shall take appropriate steps to reverse the order or the analyst may attempt to verify the
suitability of the product (refer to section 4 Measurement Traceability).
4.2.4 Labeling
If the product is acceptable the PCS shall label the product with a unique identification number.
The identification number will be logged into the Requisition database and transcribed to the
Requisition form, receipt, and accompanying quality certificates. The PCS shall file the receipt
and Requisition form in the appropriate binder. The PCS shall forward quality certificates to the
LQAO, who shall file the certificate in the Quality Document file. The requisition binders and
Quality Document files shall be retained for at least five years.
4.2.5 Storage
The laboratory has very little storage space; personnel are encouraged to make accommodation
for purchases prior to receiving supplies. Chemical reagents and standards must be handled
such that their composition shall not be jeopardized. Some chemicals must be preserved and
should come with special instructions; chemists shall inform the PCS of special handling
procedures when completing their Requisition form. When the section manager signs the
Requisition form, he/she should also look for special handling instructions of which the PCS
should be aware.
Often Material Safety Data Sheet (MSDS) are packaged with chemicals. The purchaser should
forward MSDSs to the laboratory receptionist who will file them in the MSDS notebooks stored
in the centralized Safety area.
4.2.6 Use and Consumption

Personnel who find consumable materials or equipment that affect the quality of analytical data
without the appropriate laboratory identification label shall notify the PCS and obtain a new
label. Personnel shall transcribe the identification number of the chemicals and instrument
devices used during the analysis to secondary containers, logs, computer systems used for
tracking data output, and bench work sheets. LIMS may also be used to document the use of
these materials. Such documentation shall be adequate to verify the calibration of all measuring
devices used during the analysis that are critical in the computation of the result.
Equipment and supplies which are not the desired level of quality shall be taken out of service.
Instruments, which have served their purpose and are no longer of any use to the agency,
should be disposed of through the State Surplus procedures. Personnel should contact the
PCS for the current procedure, which shall include completing the PDR form and moving the
equipment to the holding area so that it can not be inappropriately put back into service.
Chemical supplies have a shelf life and shall not be used beyond the recommended holding
time unless they are tested and proven to still be suitable for use.
5 Assuring the Quality of Analytical Data

The laboratory shall define Quality Control (QC) measures and provide a process of data review
to ensure the degree of precision, accuracy, and bias of the analyses is known and
documented.
In addition to maintaining traceability to NIST or like standards to ensure the production of
quality data, the laboratory shall participate in Performance Evaluation studies, Inter-laboratory
split comparisons, and EPA triennial audits. The LQAO shall use the information collected from
these sources with the routine QC data to develop plans to prevent the deterioration of data
quality.
The multiple levels of review as described below in section 7.5.3.5 (Technical Corrective Action)
plays a significant role in reporting quality data. This review process shall ensure that all QC
measures of precision, accuracy, and bias are reviewed by qualified personnel. Test method
SOPs shall describe the QC measure to be taken by the analyst. Laboratory section managers
shall assign the responsibility of monitoring QC data to the appropriate chemists or technicians,
who shall evaluate calibration, Laboratory Control Samples (LCS), Matrix Spikes (MS), blanks,
surrogates, and duplicate measurements. Where applicable the chemist shall use statistical
techniques to summarize the QC data. During the internal audit of the test method SOP, the
auditor shall review the summarized QC data looking for trends. The chemist shall not rely on
the internal audit to discover trends in his/her QC data; he/she shall continually review his/her
QC data and use the Nonconformance Report form (Appendix C), should he/she discover
anomalies or exceed QC limits.
The lead or senior chemist/technician shall validate data per sampling event by reviewing
sample history, comparing intra-sample results, and investigating data anomalies. The section
manger shall review the comments of the chemists and lead chemist and the decision process
when necessary.
Personnel performing an internal audit shall review test method SOPs ensuring all necessary
QC measures listed in Appendix F are accounted for in the procedure. The auditor shall
consider the essential QC standards outlined in the current NELAC standard, mandated
methods or regulations (whichever is more stringent) to determine if any deficiencies exist. If
the test method SOP and cited documents do not described how to conduct the QC measures
described in Appendix F the auditor shall write a deficiency. Through the corrective action
process, the QAO and Laboratory Section Manager shall determine if the cited QC should be
included in the SOP.
Specific procedures for conducting each of the QC measures in Appendix F shall be developed
by the laboratory’s Quality Assurance Team (QAT). These procedures shall be entered into the
Document Control database, which shall be linked to the training database.
6 Equipment
The laboratory shall ensure analytical equipment is properly used, calibrated, and maintained
The laboratory is equipped with state-of-the-art analytical instrumentation for analysis of
environmental samples. Appendix E lists the major analytical instrumentation used in the DEQ
Laboratory (this list does not include field instrumentation). Instruments are maintained in
proper operating condition through service contracts on major equipment, and by following
maintenance and calibration schedules. No equipment shall be used without first verifying its
accuracy. Records of this initial verification and the ongoing maintenance performed on
equipment shall be recorded in controlled maintenance/calibration logs (refer to Analytical
Records section 7.2 below). Some equipment such as volumetric glassware may only require
the purchase receipt for documentation of its accuracy. Should the laboratory use equipment
that is not owned by the laboratory, the laboratory shall maintain and calibrate said instrument
as prescribed in this section of the LQM. Records and maintenance logs shall be retained by
the laboratory, even though the equipment may not be retained.
Calibration procedures must be included in the test method SOPs. Calibration requirements are
divided into three parts:
1) requirements for analytical support equipment,
2) requirements for standardizing reagents used for calculating concentration, and
3) requirements for instrument calibration, which is further divided into
a) initial instrument calibration and
b) continuing instrument calibration verification
6.1 Support Equipment

Support equipment may not be the actual test instruments, but are necessary to support
laboratory operations. These include but are not limited to: balances, ovens, refrigerators,
freezers, incubators, water baths, temperature measuring devices (including thermometers and
thermistors), thermal/pressure sample preparation devices and volumetric dispensing devices
(such as Eppendorf®, or automatic dilutor/dispensing devices) if quantitative results are
dependent on their accuracy, as in standards preparation and dispensing or dilution into a
specified volume.
Often this equipment is shared within the laboratory, however, not usually between sections.
The section manager shall ensure all support equipment used in his/her section shall be
maintained and in proper working order. Records of all repairs, maintenance activities including
service calls, and calibration data shall be recorded in appropriate logs. These logs shall be
controlled as described in section 7.2 (Analytical Records).
• Support equipment shall be calibrated or verified at least annually, using NIST traceable
references when available, over the entire range of use. The results of such calibration shall
be within the specifications required of the application of this equipment or:
i. the equipment shall be removed from service until repaired; or
ii. the laboratory shall maintain records of established correction factors to correct all
measurements.
• Raw data records shall be retained to document equipment performance.
• Prior to use on each working day, balances, ovens, refrigerators, freezers, and water baths
shall be checked in the expected use range, with NIST traceable references where
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available. The acceptability for use or continued use shall depend on the needs of the
intended analysis or application.
• Mechanical volumetric dispensing devices including burettes (except Class A glassware)
shall be checked for accuracy on at least a quarterly use basis. If these devices are not
used during the quarter it is not necessary to check their accuracy. Glass micro-liter
syringes are to be considered in the same manner as Class A glassware, but must come
with a certificate attesting to established accuracy or the accuracy must be initially
demonstrated and documented by the laboratory.
• For chemical tests the temperature, cycle time, and pressure of each run of autoclaves must
be documented by the use of appropriate chemical indicators or temperature recorders and
pressure gauges.
6.2 Instruments used for the Determinative Step

This section of the LQM lists and describes the use of equipment required for to perform the
analytical methods listed in Appendix G. It should be noted that typically all procedures the lab
performs will be developed from EPA reference test methods, which already describe the
calibration procedures summarized in this document. This document dictates the criteria for
selecting the correct options when further developing methods for laboratory use and writing the
SOPs. Each analytical test method SOP shall describe the essential elements for when and
how to perform the Initial Calibration, and the Continuing Calibration Verification as well as the
type of calibration to be used.
Unless the reference method specifies otherwise, a multipoint calibration curve shall be created
for the Initial Calibration. Single point calibrations may not be used except with approval from
the LQAO, the section manager, and when one of the following three conditions is satisfied:
• the method does not allow the use of multiple point calibrations;
• instrument manufacturers have validated calibrations techniques for the technology and
the promulgated test method cites the technique; or
• the method employs standardization with a single standard i.e. titration techniques.
When using multipoint calibrations, the analytical results must be calculated from the initial
instrument calibration using one of these three approaches:
• linear regression (the preferred option);
• second order regressions may be used if during the development of the analytical test
method it is demonstrated that a linear response cannot be routinely achieved and a
second order regression yields more appropriate results. Appropriate use of second
order regressions must be documented in the SOP. Third order regressions and greater
are not allowed; or
• a point to point calibration (i.e., a linear regression fit between the two nearest points)
may be used if the first and second order curves prove to be inappropriate for the test
method.
In each case raw data from the instrument and the knowledge of the standard concentrations
are used in the statistical method of least squares to create a calibration curve. The analyst
shall record and determine QC control limits for the correlation coefficients. Test method SOPs
shall provide the control limits for the coefficients and the number of calibration standards to
use. In the event that circumstances do not allow for the proper calibration, the analyst must
follow the Nonconformance Investigations and Corrective Action procedure (section 7.5.3) and
initiate the completion of the appropriate Nonconformance form. The test method SOP shall
also describe how raw data records are to be retained. Data records shall contain sufficient
information to permit the reconstruction of the initial instrument calibration, including:
• calibration date;
• test method;
• instrument;
• analysis date;
• analyte name (or analyst’s initials or signature);
• concentration and response of each standard;
• unique equation or coefficient used to convert instrument responses to analyte
concentration; and
• calibration assessment factor (i.e., r2 or other criteria).
Sample results shall be quantitated from the initial instrument calibration and may not be
calculated from any continuing instrument calibration verification unless otherwise specified in
the QAPP.
With the exception of those test methods that allow for a single point calibration at least three
calibration standards shall be used in the initial calibration not including the calibration blank or
a zero standard. The concentrations of the standards shall be distributed throughout the
calibration range. The lowest calibration standard shall be equal to or less than program
required reporting levels when appropriate and the analytical method reporting limit. If specific
programs are more prescriptive in establishing the initial calibration, those requirements shall be
followed. During the development of the laboratory method, the lowest calibration standard
(MRL) shall be determined by using a dilution of the stock standard that is one to five times
greater than the Method Detection Limit (refer to Appendix B: 40 CFR Part 136, App. B). If
blank samples tend to yield detectable contamination, the lowest calibration standard shall be
set to five to ten times greater than the MDL. Refer to the Laboratory's procedures for
establishing the Method Detection Limit and Method Reporting Limit for additional details.
For analytical methods that have been approved to use a single point calibration, the following
requirements must be satisfied:
1) the linear dynamic range (LDR) of the instrument must be established (and verified
annually) by analyzing a series of standards, beginning at the MRL and extending to the
highest concentration that will be reported without sample dilution;
2) a new calibration (with a calibration blank and single point calibration standard) must be
created for every analytical batch;
3) the calibration curve must be verified immediately following the initial calibration with two
second source quality control samples. One QCS must be analyzed at the MRL and the
second QCS must be analyzed at a second concentration that will not exceed 90% of
the single point standard concentration;
4) Sample concentrations within an analytical batch that exceed the single point calibration
concentration must be handled with one of the following procedures:
a) analysis of a reference material at or above the sample value that meets established
acceptance criteria for validating the linearity;
b) sample dilution such that the result falls below the single point calibration
concentration; or
c) use of an appropriate data qualifier and comment explaining the qualifier flag.
For analytical methods that do not require an initial calibration with every analytical batch, a new
initial calibration shall be prepared whenever there is sufficient change in instrument setup or
reagents used to cause a quantitative change in instrument response, or when QC failures
initiate the Corrective Action procedure from which it is determined the instrument should be
recalibrated. Immediately following the initial calibration a sample called an Initial Calibration
Verification (ICV) shall be run to verify the quality of the calibration. The ICV will be prepared
from a second source standard when possible and meet the same quality as the primary
calibration standard. The SOP shall cite the control limits set on the ICV.
If it is necessary to report data generated from calibrations that do not meet control limits or the
ICV fails to fall within the acceptable range and it is not possible to rerun samples, the analytical
results shall be reported as estimates with comments explaining the problem.
6.3 Accommodation and Environmental Conditions
6.3.1 Laboratory Facility

The DEQ laboratory is equipped with sufficient power resources to operate instruments and
equipment safely for the work noted above. Space is at a premium so personnel must employ
good “house keeping” procedures to accommodate other work performed in common areas.
When appropriate the test method SOP shall describe “house keeping” procedures. Personnel
must communicate with the Quality Assurance Team (QAT) and management should they
recognize limits of the PSU facility that hamper the progress of producing quality data. As with
all other observations and findings, management shall ensure that this communication is
documented. The Nonconformance form shall be completed and an internal audit initiated if
appropriate.
The laboratory is structurally organized to isolate similar work to be accomplished in general
work areas. Personnel working in these areas are naturally familiar with similar cleaning
procedures, sample handling procedures, and instrument requirements. This division helps to
ensure that sample integrity and instrument response won’t be compromised. Special care is
taken to ensure that cross contamination won’t occur. In particular the Volatile Organic
Compounds (VOCs) analysis is easily contaminated by work performed on non-volatile
organics. Clean VOC work shall be performed in L-71 A and organic extractions that use
solvents, which have VOC contaminants, shall be performed in L-63. Special care is also taken
for the analysis of metals by ICP/MS, which is capable of measuring very low levels of metal
contamination. The normal laboratory environment will create contamination problems for tests
performed by ICP/MS, thus a special clean hood is used for ICP/MS tests.
In addition to the structural requirements for analytical testing and calibration procedures, the
laboratory shall maintain work areas with sufficient access and entryways to the laboratory:
a) sample receipt area(s);
b) sample storage area(s);
c) chemical and waste storage area(s); and,
d) office space for data handling and data storage
Access to the laboratory is controlled by requiring all visitors report to the receptionist and sign
in. The receptionist shall page the appropriate personnel, who shall inform the guest of our
safety policy, evacuation routes, and location of work areas. The laboratory is divided into an
upper and lower floor. Each floor has a main hallway that divides most desk spaces from the
calibration and analytical test methods areas. Special safety rules, which also help preserve
data quality, are required in the calibration and analytical areas. Personnel are required to read
the laboratory’s Chemical Hygiene Plan (CHP: DEQ04-LAB-0025-SFTY), which covers the
safety procedures necessary for the work performed at the laboratory. Documentation that
personnel have read the CHP shall be kept in the LQAO’s administrative file.
6.3.2 Environmental Controls

Where applicable test method SOPs shall specify requirements for controlling the environment
of the laboratory. The laboratory shall monitor, control and record environmental conditions as
required by the relevant specifications, methods and procedures or where the environment
influences the quality of the result e.g., the weighing of Air Quality particulate samples requires
a temperature and humidity controlled environment and virtually all samples are stored in a
refrigerator. The temperature and humidity of the Air Quality room is monitored and
documented, this process is documented in the Air particulate weighing procedure. Although it
may not be documented in a particular procedure, the temperature of the refrigerator is
maintained and documented because sample storage temperature is known to influence the
quality of numerous test methods.
7 Quality Assurance
The laboratory shall provide a system to ensure all events influencing data quality are
documented.
7.1 Control of Quality Documents

The laboratory must maintain control of all documents that form the laboratory’s Quality System
to ensure personnel use and have access to the most recent versions of quality documents and
SOPs. The laboratory’s document control procedure (DEQ02-LAB-0004-SOP) can be found on
Q-Net and in the agency’s QMP. This procedure describes the process the laboratory shall use
to develop, write, approve, and store controlled documents. The approval process shall ensure
QA objectives are met and that the laboratory’s Quality Assurance Team (QAT) has input.
The author, technical editor, and QAO shall sign controlled documents of manuals, policies, and
procedures. The page header of controlled quality documents shall contain the document title,
control number, the version number, the effective date, and page numbers. Controlled
documents are identified by the signatures and colored title page. The QAO shall ensure the
controlled copy is stored in a locked file cabinet. Photocopies of the signed document and re-
printed electronic documents are not controlled. It is the responsibility of the document holder to
ensure he/she has the most current document. The QAO shall ensure electronic copies of
controlled documents are available on Q-Net and notify the appropriate personnel when
revisions are posted.
Section managers shall maintain database documentation identifying personnel who are
required to keep current with specific controlled documents. Section managers shall submit to
the LQAO records of attestations that employees will follow the policy and procedures described
in controlled documents.
7.2 Analytical Records

As a public agency the laboratory must also follow state policies for maintaining records.
It is the policy of the State of Oregon to assure the preservation of records essential to meet the needs of
the state, its political subdivisions, and its citizens, and to assure the prompt destruction of records without
continuing value.
All instrument logs, sample preparation logs, standard/reagent logs, bench work sheets, and
data output records from electronic instruments used to generate analytical data must be
retained for at least five years. To ensure the laboratory meets this requirement all chemists
and field technicians must read and sign memos of attestation for document and record control
procedures.
The document control coordinator shall assign control numbers to logs and notebooks prior to
use. The document control coordinator shall create control numbers in a database and enter
pertinent data describing the content, version, author, and date of the document or records log.
Once the logs and/or notebooks are full, the chemists and technicians must return the records
to the document control coordinator for archiving. Analytical records shall be archived for a
period of five years since the last entry in the log. Refer to the agency’s Archiving procedures,
for storage and retrieval of archived records.
7.3 Data Reports and Verification Records

Technical Services (TS) is responsible for maintaining the integrity of analytical data generated
by the laboratory division. The Technical Services section manages analytical data through the
use of LIMS. As data progresses through the system from entry to review to reporting, LIMS
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adjusts the status code of the result, which restricts what can be done to the data. Chemists or
technicians enter data into LIMS and may make corrections to data up until they submit their
work for review. Senior chemists review data and may send the data back to the chemist for
rework. LIMS users can not alter data during the review process. Once the results are reported
and approved for all tests performed on a set of samples, Technical Services shall print an
analytical report. The DEQ laboratory shall release the analytical report after the QA Officer and
Laboratory Administrator review and sign the document. The release process is completed
when Technical Services sends a copy of the report (either electronically or paper) to the
primary recipient. Up until that point the report may be edited without an erratum. However,
after the report is sent to the primary recipient it must not be altered. Subsequent changes in an
analytical report must be made through an erratum. Should an error in the report be detected
following the release of the report an erratum must be prepared (refer to DEQ03-LAB-0002-
SOP for this procedure).
As with other controlled documents the colored title page and the signatures on the analytical
report identifies the report as the official controlled copy. Reprinted electronic reports and
photocopies of the analytical report are not controlled. Technical Services shall ensure that
PDF copies of the controlled report are available through electronic means. Data users may
receive PDF copies of the report through e-mail or retrieve them out of Q-Net. Although the
PDF is not the official copy, Technical Services shall ensure the electronic copy of a report is
equally maintained. Technical Services shall store electronic copies of the original reports and
subsequent errata in a secure server location. The process of maintaining an official controlled
document on paper and a secure electronic copy offers a backup system for system failures in
the controlled document procedure.
During data review, lead chemists/technicians, senior chemists/technicians, managers, QAO,
and the Division Administrator may question the validity of data and initiate an audit. Technical
Services is responsible for tracking the audit request, findings, and corrective action. The
auditor shall identify what prompted the question in a memo addressed to personnel involved in
the corrective action and the QAO. The title of the memo shall contain the sampling event
number.
Documentation of this audit must be retained per NELAC 2002 5.4.12.2.4 d, and 5.4.12.2.5.f.
Although data may be altered during specific steps of the review process all changes are
tracked through the LIMS audit trail.
7.4 Client Correspondences

As noted earlier the Director has placed commitment to Delivering Excellence in Performance
and Product in the agency’s Strategic Directions. Responding to laboratory client needs is a
top priority for achieving this goal. The laboratory’s primary clients are the agency’s programs,
who in turn have clients of their own. Ultimately it is the public who is our client.
The laboratory shall cooperate with agency personnel in an attempt to clarify work requests and
to monitor the laboratory’s performance in relation to the work performed. Agency personnel
should contact the laboratory’s Technical Services manager for information on projects and for
retrieving data. The public has access to data stored in the Laboratory Analytical Storage and
Retrieval (LASAR) database. All requests from the public for laboratory data should be directed
to the Technical Services manager, who shall follow agency policy and procedures for assisting
the public in retrieving such data. Not all data shall be available immediately to the public, such
as data collected for criminal enforcement or determined confidential for national security. The
Technical Services section shall write an analytical report SOP, which shall ensure client
confidentiality in these cases. This SOP shall follow the laboratory’s document control policy.
7.4.1 Analytical Work Submitted to the Laboratory

Quality Assurance Project Plans
The process of developing QAPPs as prescribed in the agency’s QMP enables the laboratory to
review work prior to receiving samples, and to support the laboratory’s ability to produce a
client-defined product. During the development of the QAPP project coordinators shall involve
the QAO, who shall ensure the QAPP addresses laboratory requirements as well as the client’s
interests. The QAPP must meet the QMP policy and structure requirements, which is modeled
after EPA’s R5 QAPP procedure. The R5 procedure is available on EPA’s web page.
Personnel developing a QAPP are encouraged to review these procedures as well as the
agency’s QMP.
The QAOs shall approve all agency QAPPs and ensure that QAPPs include:
• test method requirements:
1) The QAO shall ensure test methods to be performed are well documented. Agency
personnel who are writing QAPPs should review the current test method SOPs , which are
posted on Q-Net.
2) Special projects may require deviations from test method SOPs or new SOPs. The QAPP
shall describe test methods in full detail if there is no SOP available. The QAO shall
discuss test method proposals with the appropriate section manager and personnel
ensuring, the laboratory has the resources and capabilities to make such adjustments.
The laboratory shall validate the new procedure as described in section 3.3.1 of this
document.
3) If the DEQ laboratory opts not to develop a special test method, it may subcontract the
work to other laboratories with the appropriate capabilities. Subcontracting agreements
shall be covered in the QAPP.
• reporting levels required for the project,
• contaminant action levels to be used for decision making,
• the projects accreditation requirements and the laboratory’s current status,
1) The QAO shall track the accreditation status of subcontracted laboratories. If appropriate
the QAO shall qualify data and ensure the DEQ analytical report includes the appropriate
comments.
2) The QAPP shall specify if and how analytical data should be flagged when there are
changes in accreditation status.
• QC measures to be taken,
• procedures to control nonconforming work, i.e. deviations from the QAPP,
1) Refer to section C1 of “EPA Requirements for Quality Assurance Project Plans EPA
QA/R-5”.
2) The Nonconformance procedure in the QAPP shall describe the process for finding
deficiencies in meeting QAPP requirement.
a) The Nonconformance procedure shall identify management responsibility for taking
action, such as halting work until a corrective action plan is determined, and identifying
the authority responsible for resuming work.
b) The QAO and project coordinators shall review QAPPs during the project and they shall
have the capacity to make amendments to the QAPP.
c) If deficiencies are found in DEQ laboratory work, the Nonconformance Investigations
and Corrective Action procedure (section 7.5.3) shall be used to document and find
solutions for the Nonconformance work.
• procedures for amending the QAPP
1) The QAO and project coordinator shall review and approve amendments.
7.4.2 Complaints
It is not in the scope of the LQM to address all viable complaints that come to the laboratory.
The LQM shall focus on issues that relate to data quality. The laboratory shall respond to
inquiries of data anomalies and complaints of report format or content, response time, and
laboratory policy using the Nonconformance Investigations and Corrective Action procedures
described in section 7.5.3. Complaints that are related to personnel conduct, and agency policy
are handled by laboratory management and the DEQ Human Resources Division.
Agency personnel tend to contact the sample tracker, whereas the receptionist usually receives
calls from the public. The receptionist and the sample tracker shall attempt to direct the caller to
the appropriate employee; however complaints are often difficult to decipher and will be referred
to the Technical Services manager or the laboratory Administrator as the default. All laboratory
staff members shall ensure the complaints they receive are discussed with the appropriate
section manager. If an employee feels uncomfortable with bringing a complaint to his/her
supervisor he/she may contact a QAO, the Technical Services section manager, or the
Laboratory Division Administrator.
Laboratory personnel should not attempt to resolve complaints without informing management.
Section managers shall assess whether the root causes of the complaint puts the integrity of
laboratory work into question. If the section manager determines there is a QA problem, the
manager shall ensure the Internal Audit procedures below are initiated immediately.
A complaint does not necessarily mean nonconforming work has occurred; however, complaints
must be investigated to determine whether or not an error has occurred. The laboratory must
also control records of complaints received. Thus, whenever a complaint is received, the
section manager shall file a Nonconformance report with the Technical Services section. The
Technical Services section manager shall assign a Nonconformance investigation to unbiased
personnel who will determine the validity of the complaint and assess whether the event that
generated the complaint violated laboratory policy or failed to follow procedures. The QAO
team shall participate in the investigation when necessary to guarantee an unbiased evaluation.
Technical Services shall track complaints received by recording pertinent information about the
complaint such as: description, date, staff assigned to investigate, action taken, and date
resolved.
7.5 Quality Assurance Measures

The LQAO shall maintain procedures for identification, collection, indexing, access, filing,
storage, maintenance and disposal of quality and technical records. Quality records shall
include reports from internal audits and management reviews as well as records of corrective
and preventative actions. Records may be kept on either paper or electronic media.
7.5.1 Internal Audit

The LQAO shall establish an internal audit schedule, and at least annually, conduct internal
audits of the laboratory’s activities to verify operations continue to comply with the LQM. The
internal audit program shall address all elements of the LQM, including test method activities. It
is the responsibility of the LQAO to plan and organize audits as required by the schedule and
requested by management. The QAO team shall audit the technical operations of the
laboratory, since the QAOs are independent of this laboratory function. Management shall
assign other staff members to audit QA activities, which may include members of the QAT.
Personnel shall not audit their own activities except when insufficient resources are available
and the QAO team is satisfied the individuals involved can carry out an effective audit.
When audit findings cast doubt on the laboratory’s operational effectiveness or on the
correctness or validity of the laboratory's work, the laboratory shall take timely corrective action.
The LQAO shall retain documentation that the project coordinator was notified in writing of
findings showing the laboratory results may have been affected.
The audit team shall use the Oregon Laboratory Accreditation Program (ORELAP) database to
record assessment findings, from which an Audit report will be printed and submitted to the
section managers. The section manager shall ensure that a corrective action plan for his/her
section will be written within 30 days of receiving the report. The LQAO and section manager
shall negotiate reasonable time frames for completion of corrective action procedures. The
LQAO shall record the scheduled completion date of the corrective action procedure in the
database. The LQAO will then monitor and routinely report on the status of the corrective
action. Subsequent internal audits shall verify and record the implementation and effectiveness
of the corrective action taken.
The LQAO shall review NELAC required administrative files. These files should contain
documentation of training requirements, training received, Demonstration of Capability, and
personnel conduct with respect to compliance to the laboratory data integrity policy. Discovery
of potential personnel issues shall be handled in a confidential manner until such time as a
follow up evaluation, full investigation including union representation if requested, or other
appropriate actions have been completed and the issues clarified. All investigations that result
in finding of inappropriate activity shall be documented and shall include corrective actions
taken and all appropriate notifications to clients. Any disciplinary actions taken shall be
documented and stored in the Human Resources Division’s personnel files which are not
accessible to the general public. All documentation of these investigations and actions taken
shall be maintained for at least five years.
7.5.2 Annual QA Report

The LQAO shall schedule and prepare an annual Laboratory Quality Assurance report for the
Laboratory Division Administrator to review. The report shall cover the status of the laboratory's
quality system and the laboratory’s analytical activities to ensure the continuing suitability and
effectiveness of the system, and to introduce necessary changes or improvements. The report
will be completed by 31 January and shall take account of QA activities and concerns that
occurred during the previous calendar year, including:
1. the suitability of policies and procedures;
2. reports from managerial and supervisory personnel;
3. the outcome of recent internal audits;
4. corrective and preventative actions;
5. assessments by external bodies;
6. the results of interlaboratory comparisons or proficiency tests;
7. changes in the volume and type of work;
8. client feedback;
9. complaints;
10. other relevant factors, such as quality control activities, resources and staff training.
The Division Administrator shall comment on the Annual QA Report and if necessary set a
corrective action schedule and assign responsibility. The LQAO shall maintain a file of the
Annual QA Reports, the Division Administrator’s responses and applicable corrective action
plans. The LQAO shall also ensure all section managers receive a copy of this file. The
corrective action assigned by the Division Administrator shall be monitored as described in the
Corrective Action procedure below (section 7.5.3).
7.5.3 Nonconformance Investigations and Corrective Action Reports

Whenever personnel suspect or identify deviations from the policies or procedures within the
LQM, monitoring activities, analytical test method SOPs, or failed QA/QC, they must initiate a
Nonconformance investigation. The procedure for documenting Nonconformance events and
the subsequent corrective action shall encompass all measures taken to rectify QA/QC
problems, which include but are not limited to:
• documentation or evidence of the presumed problem;
• identification of the SOPs not conforming to the LQM;
• a description of how the SOP was not being followed as written; and
• impediments to following the SOP.
Nonconformance Investigations shall be documented using the Nonconformance report form (or
equivalent) in Appendix C to record the description of the incident, personnel involved in the
investigation, deadlines, Corrective Action (CA) taken, and the dates for completing each event.
Section managers may develop their own Nonconformance form for reporting failed QC, which
shall be approved by the QAT prior to use. The Technical Services section shall develop a
system to capture this information and track the status of these investigations. Technical
Services shall also maintain these records for at least five years.
This corrective action procedure is referenced throughout this document and shall be used for
all incidences where non-routine work occurs and alternative documentation strategies have not
been identified. Although external audits may require a specific format for the corrective action
plan, the laboratory shall track the actions taken using the Nonconformance report form or until
an alternate electronic Nonconformance information system is developed and implemented.
7.5.3.1 Cause Analysis

Cause Analysis is the initial step in any corrective action that is initiated in response to a
Nonconformance Investigation. The Cause Analysis shall start with an investigation to
determine the root cause(s) of the problem. Personnel who initiated the Nonconformance
Investigation may offer opinions on the possible the root cause. Even if the root cause can not
be determined, the investigation and the Nonconformance report must be completed.
Personnel shall begin the process by filling in the applicable fields of the Nonconformance form
and forwarding it on to their supervisor or lead worker, who will then evaluate the problem and
assign the investigation to appropriate staff. The investigation shall begin with employees
whom appear to be most directly related to the Nonconformance.
If the manager determines the Nonconformance is not related to his/her section, he/she shall
forward the report onto the appropriate manager. The section manager shall immediately bring
deviations from the LQM or the QAPP to the attention of the QAO team, who shall conduct
these Nonconformance investigations. The QAO shall ensure the project coordinator is
involved with the corrective action plan. Generally, Nonconformance Investigations will be
handled by the appropriate laboratory sections:
• Technical Services section shall investigate and perform corrective actions that relate to
LIMS functions, sample receipt, sample integrity, and complaints;
• the analytical sections of the laboratory shall conduct the investigation and complete the
necessary corrective actions for deviations from analytical test methods and failed QC
measures within their sections; and,
• the monitory sections shall investigate nonconformance events related to sample
collection, continuous monitoring, and other field operations;
Cause analysis should be conducted through data review and QA audits. The data review
process may reveal a Nonconformance which is of a technical nature and a suite of corrective
action procedures to follow (refer to Technical Corrective Action section 7.5.3.5).
Section managers may delegate the responsibility of reviewing data and assigning corrective
action tasks to whom ever they choose in their staff. Since it is the managers’ prerogative to
assign investigations and corrective action tasks as they see fit, each section shall write
procedures for Data Control, which will describe who is responsible for implementing corrective
action procedures for data quality problems.
7.5.3.2 Corrective Action Selection and Implementation

One the root of the problem has been identified through Cause Analysis, potential solutions
shall be proposed an implemented through a Corrective Action Selection and Implementation
process. Corrective actions shall be appropriate to the magnitude and risk of the problem. The
section manager shall collaborate with the LQAO to identify potential corrective action
procedures and to select and implement action(s) most likely to eliminate the problem and to
prevent recurrence. The section manager shall record these corrective action options on the
Nonconformance report.
Once it has been identified, the appropriate corrective action must be implemented. The first
step in implementation will often be the revision or amendment of the relevant Laboratory policy
or procedure.
The QAT shall document and ensure implementation of any required changes in the LQM or
laboratory policy resulting from corrective action investigations. Section managers shall
approve changes in analytical data and in SOPs with QAO concurrence.
7.5.3.3 Monitoring of Corrective Actions

The LQAO or his/her designee shall monitor the effectiveness of corrective actions taken. The
Nonconformance report system shall provide sufficient information to assess the effectiveness
of corrective action procedures. The Nonconformance report must associated with the
appropriate documents through the control numbers described in section 2.8 above. The
success and performance of the implemented corrective action plans will be a routine part of the
annual Internal Audit (section 7.5.1).
7.5.3.4 Additional Audits

Where the identification of Nonconformances or departures from QAPP, SOP, or LQM casts
doubt on the laboratory's compliance with its own policies and procedures, the laboratory shall
ensure the appropriate activities are audited in accordance with the Internal Audit procedures as
soon as possible.
7.5.3.5 Technical Corrective Action and Data Review Process

Corrective action taken in the course of day to day validation of data may require less of a
formal cause analysis than the corrective action taken for the response to an internal audit.
Test method SOPs shall provide procedures for correcting problems which may occur during
the analytical process. Moreover, to help avoid inadvertent departures from quality policies and
procedures analytical data shall be reviewed at several levels.
1) Chemists/Technicians producing analytical data shall review their work ensuring sample
and batch QC measures meet acceptable limits. Chemists shall follow their SOPs to
correct any failed QC and repeat the analysis provided there is sufficient sample. If the
analysis can not be repeated within the recommended sample holding time, the chemist
must attach a comment to the result in LIMS and report the value as an estimate or void
the result. Typically chemists shall void results only due to analytical failures and not to
sample or batch QC limit failures. However, the failure to meet multiple QC limits may
lead to the action of voiding the result.
a) Sample QC measures may include but are not limited to:
i) Matrix Spike
ii) Matrix Spike Duplicate
iii) Duplicate analysis
b) Batch QC measures may include but are not limited to:
i) Method Blank
ii) Laboratory Control Sample
iii) Continuing Calibration Verification
iv) Calibration coefficients
As noted previously, if a chemist believes he/she has identified a questionable
procedure or feels his/her SOP does not meet the policy or procedures detailed in the
LQM, he/she is obligated to bring his/her concerns forward. He/she may contact a QAO,
a QAT member, his/her section supervisor, or the Laboratory Administrator.
2) Senior chemist/Lead Chemist/Lead Monitoring Specialists
a) The lead or senior chemist/technician shall validate data by reviewing sample
history, comparing intra-sample contaminants, and investigating data anomalies.
The lead chemists shall confer with chemists to evaluate any question he/she may
have about the data and may send the results back to the chemist for rework. As
above this process is controlled through the DAR approval process. The chemist
shall verify the transcription of data from the original source to LIMS, and if
necessary and possible, retest the sample.
3) The section manager shall review the decision process, which the chemist/technician
used to qualify the data and either approve the outcome or send the results back for
rework. The procedure for reworking results through LIMS is described in the DAR
SOP. This procedure will ensure NELAC 2002 5.4.12 Control of Records and 5.4.13
Internal Audits are followed.
4) The QAO shall review analytical data packets for completeness and sign analytical
reports certifying the controlled document is in compliance with the laboratory’s quality
policy. The QAO shall re-work analytical reports that do not comply with these policies.
If a quality control measure fails, all samples associated with the failed quality control
measure shall be reported with the appropriate data qualifier(s).
In addition to verifying precision and accuracy of analytical data, QC procedures
described in test method SOPs shall document the process for obtaining QC data. An
independent QAO shall review and sign all controlled documents, for which he/she is not
the author to help ensure that QC collection is documented. During review of the
controlled documents, problems may arise that warrant the creation of a
Nonconformance report. The QAO should solicit an investigation from personnel not
related to the issues.
7.5.4 Preventative Measures

Preventative measures are a pro-active process to identify opportunities for improvement rather
than a reaction to problems or complaints. The agency’s QMP addresses how the Quality
Systems shall continue to grow and improve (chapter 10 of the QMP); the laboratory shall
comply with this goal. It is the QAT’s responsibility to assess and implement the laboratory’s
preventative measures (refer to section 2.1 Laboratory Quality Assurance Team).
8 Reporting Results
The laboratory shall report data in useful and comparable formats.
The Technical Services section of the laboratory has the responsibility of creating analytical
reports. Technical Services shall ensure that all projects entered into LIMS and assigned a
sampling event number shall be reported in a standard format, creating an official report record.
The report shall accurately, clearly, unambiguously, and objectively depict the results for
requested measurements. The intent of the report design is to minimize the possibility of
misunderstanding or misuse of data.
Technical Services shall ensure the integrity of the official report by applying the document
control procedures as described in section 7.3 (Data Reports and Verification Records). Even
though project coordinators may only use data stored in an electronic database, Technical
Services shall create an official paper report for document control.
Analytical reports shall be generated from LIMS and converted to a PDF, which shall be printed
on a color printer. Each page of the report shall have the title of the report, the sampling event
name and number prominently displayed at the top of the report. The report footer shall contain
the name of the PDF file, date and time the report was printed, and the page number with the
total number of pages in the PDF. The analytical report shall contain the following sections:
• Title page w/
1) Primary Report Recipient,
2) Report Date,
3) Laboratory Demographics, and
4) Approval Signatures.
• Narrative page w/
1) Sampling Event narrative when present,
2) List of Report Recipients,
3) List of Sample Collectors, and
4) List of Analytical Laboratories involved in the analyses.
• Sampling Event Summary page w/
1) Project ID linking the Sampling Event to the QAPP,
2) List of Sampling Sites w/
a) Item number,
b) Site ID,
c) Sample Description,
d) Matrix,
e) Sample Date,
f) Sample Time, and
g) Endnote references
• Analytical Results w/
1) Sample identification w/
a) Item Number,
b) Site ID,
c) Sample Description,
d) Sample Date, and
e) Sample Time
2) Analytical Parameter w/
a) Method reference,
b) Lower Reporting Limit,
c) Result,
Version 5.0 Reporting Results cont. Page 39 of 64
d) Unit,
e) Date and Time of sample preparation for test methods with holding time less than 72
hours, and
f) Endnote references
• Endnotes
• Electronic scanned sample collection form
The Technical Services section shall attach the following original forms and reports to the official
analytical report, although they may not be included in the electronic data packet.
• The original sample collection form
• QC reports
• Subcontracted analytical reports
Project coordinators may make special requests to scan documents which could then be
attached to the electronic document.
Technical Services shall transcribe pertinent data to LIMS from the sample collection form and
subcontracted analytical reports, which shall appear in the official report as well.
The analyst entering data into LIMS shall report results associated with failed QC as estimates
and enter a comment explaining his/her decision to qualify data as an estimate. Through the
Data Analysis Report (DAR) approval process management shall scrutinize the data and
identify which comments will be reported. LIMS will generate endnotes from the approved
comments and insert them in the appropriate section of the report.
The Technical Services section shall develop a system for tracking and reporting references to
sampling methods. As noted previously Watershed Assessment and Air Quality Monitoring
have documented procedures for collecting samples. References to these procedures shall be
included in analytical reports where appropriate.
The QAO shall complete the sampling event narrative portion of the analytical report. This
section shall be used to clarify QC measures and to offer opinions or interpretations of the data
by the QAO.
Project coordinators shall identify in the QAPP or SAP the report recipients and how they will
receive the analytical report. Typically agency personnel will receive an e-mail notice with a link
to the PDF. Reports may be emailed as a PDF, or photocopied and mailed. LIMS allows the
sample tracker to modify the list of report recipients at the time of sample entry. Staff may add
or delete personnel to and from the list of people receiving the analytical report. The project
coordinator shall be notified of changes to the recipient list. The laboratory shall only send
analytical reports to personnel listed as recipients. Laboratory personnel shall instruct the public
to request copies of an analytical report from the project coordinator, thus ensuring the project
coordinator is made aware of the potential use of their data.
APPENDICES
Appendix A: Demonstration of Capability

Certification Statement
Date: Page of
Laboratory Name: Oregon Department of Environmental Quality
Laboratory Address: 1712 SW 11th Avenue, Portland OR 97201
Analyst(s) Name(s):
Matrix:
(Examples: laboratory pure water, soil, air, solid, biological tissue)
Method:
Method number, SOP#, Rev#, and Analyte, or Class of Analytes or Measured Parameters
(Examples: barium by 200.7, trace metals by 6010, benzene by 8021, etc.)
We, the undersigned, CERTIFY that:
1. The analysts identified above, using the cited test method(s), which is in use at this facility for the
analyses of samples under the National Environmental Laboratory Accreditation Program, have met the
Demonstration of Capability.
2. The test method(s) was performed by the analyst(s) identified on this certification.
3. A copy of the test method(s) and the laboratory-specific SOPs are available for all personnel on-site.
4. The data associated with the demonstration capability are true, accurate, complete and self-explanatory
(1).
5. All raw data (including a copy of this certification form) necessary to reconstruct and validate these
analyses have been retained at the facility, and that the associated information is well organized and
available for review by authorized assessors.
Technical Director’s Name and Title Signature Date
Quality Assurance Officer’s Name Signature Date

Appendix B: 40 CFR Part 136, App. B

Environmental Protection Agency
[49 FR 43261, Oct. 26, 1984; 50 FR 692, 695, Jan. 4, 1985, as amended at 51 FR 23702, June 30, 1986]
DEFINITION AND PROCEDURE FOR THE DETERMINATION OF THE METHOD DETECTION LIMIT -
REVISION 1.11
Definition
The method detection limit (MDL) is defined as the minimum concentration of a substance that can be
measured and reported with 99% confidence that the analyte concentration is greater than zero and is
determined from analysis of a sample in a given matrix containing the analyte.
Scope and Application
This procedure is designed for applicability to a wide variety of sample types ranging from reagent (blank)
water containing analyte to wastewater containing analyte. The MDL for an analytical procedure may vary
as a function of sample type. The procedure requires a complete, specific, and well defined analytical
method. It is essential that all sample processing steps of the analytical method be included in the
determination of the method detection limit.
The MDL obtained by this procedure is used to judge the significance of a single measurement of a future
sample.
The MDL procedure was designed for applicability to a broad variety of physical and chemical methods.
To accomplish this, the procedure was made device- or instrument- independent.
Procedure
1) Make an estimate of the detection limit using one of the following:
a) The concentration value that corresponds to an instrument signal/noise in the range of 2.5 to 5.
b) The concentration equivalent of three times the standard deviation of replicate instrumental
measurements of the analyte in reagent water.
c) That region of the standard curve where there is a significant change in sensitivity, i.e., a break in
the slope of the standard curve.
d) Instrumental limitations.
It is recognized that the experience of the analyst is important to this process. However, the analyst must
include the above considerations in the initial estimate of the detection limit.
2) Prepare reagent (blank) water that is as free of analyte as possible. Reagent or interference free water
is defined as a water sample in which analyte and interferant concentrations are not detected at the
method detection limit of each analyte of interest. Interferences are defined as systematic errors in the
measured analytical signal of an established procedure caused by the presence of interfering species
(interferant). The interferant concentration is pre-supposed to be normally distributed in representative
samples of a given matrix.
3)
a) If the MDL is to be determined in reagent (blank) water, prepare a laboratory standard (analyte in
reagent water) at a concentration which is at least equal to or in the same concentration range as
the estimated method detection limit. (Recommend between 1 and 5 times the estimated method
detection limit.) Proceed to Step 4.
b) If the MDL is to be determined in another sample matrix, analyze the sample. If the measured level
of the analyte is in the recommended range of one to five times the estimated detection limit,
proceed to Step 4.
Version 5.0 : 40 CFR Part 136, App. B cont. Page 43 of 64
If the measured level of analyte is less than the estimated detection limit, add a known amount of
analyte to bring the level of analyte between one and five times the estimated detection limit.
If the measured level of analyte is greater than five times the estimated detection limit, there are two
options.
i) Obtain another sample with a lower level of analyte in the same matrix if possible.
ii) The sample may be used as is for determining the method detection limit if the analyte level does
not exceed 10 times the MDL of the analyte in reagent water. The variance of the analytical
method changes as the analyte concentration increases from the MDL, hence the MDL
determined under these circumstances may not truly reflect method variance at lower analyte
concentrations.
4)
a) Take a minimum of seven aliquots of the sample to be used to calculate the method detection limit
and process each through the entire analytical method. Make all computations according to the
defined method with final results in the method reporting units. If a blank measurement is required
to calculate the measured level of analyte, obtain a separate blank measurement for each sample
aliquot analyzed. The average blank measurement is subtracted from the respective sample
measurements.
b) It may be economically and technically desirable to evaluate the estimated method detection limit
before proceeding with 4a. This will: (1) Prevent repeating this entire procedure when the costs of
analyses are high and (2) insure that the procedure is being conducted at the correct concentration.
It is quite possible that an inflated MDL will be calculated from data obtained at many times the real
MDL even though the level of analyte is less than five times the calculated method detection limit.
To insure that the estimate of the method detection limit is a good estimate, it is necessary to
determine that a lower concentration of analyte will not result in a significantly lower method
detection limit. Take two aliquots of the sample to be used to calculate the method detection limit
and process each through the entire method, including blank measurements as described above in
4a. Evaluate these data:
i) If these measurements indicate the sample is in desirable range for determination of the MDL,
take five additional aliquots and proceed. Use all seven measurements for calculation of the MDL.
ii) If these measurements indicate the sample is not in correct range, re-estimate the MDL, obtain
new sample as in 3 and repeat either 4a or 4b.
5) Calculate the variance (S²) standard deviation (S) of the replicate measurements as follows:
[ILLUSTRATION GOES HERE]
ER31AU93.074
2
n ⎛ n
⎞
∑ X - ⎜⎜
2
i
⎝
∑
i=1
X i ⎟⎟
⎠
/n
2 i=1
S =
n-1
S = (S ) 2 1/2
where: Xi for i = 1 to n, are the analytical results in the final method reporting units obtained from the
n sample aliquots and Σ refers to the sum of the X values from i = 1 to n.
6)
a) Compute the MDL as follows:
MDL = t(n-1, 1-α = 0.99) (S)
where:
MDL = the method detection limit
t(n-1, 1-α = 0.99) = the students' t value appropriate for a 99% confidence level and a standard
deviation estimate with n-1 degrees of freedom. See 1.
S = standard deviation of the replicate analyses.
b) The 95% confidence interval estimates for the MDL derived in 6a are computed according to the
following equations derived from percentiles of the chi square over degrees of freedom distribution
(χ²/df).
LCL = 0.64 MDL
UCL = 2.20 MDL
where:
LCL and UCL are the lower and upper 95% confidence limits respectively based on seven
aliquots.
7) Optional iterative procedure to verify the reasonableness of the estimate of the MDL and subsequent
MDL determinations.
a) If this is the initial attempt to compute MDL based on the estimate of MDL formulated in Step 1, take
the MDL as calculated in Step 6, spike the matrix at this calculated MDL and proceed through the
procedure starting with Step 4.
b) If this is the second or later iteration of the MDL calculation, use S² from the current MDL calculation
and S² from the previous MDL calculation to compute the F-ratio. The F-ratio is calculated by
substituting the larger S² into the numerator S²A and the other into the denominator S²B. The
computed F-ratio is then compared with the F-ratio found in the table which is 3.05 as follows: if
S²A/S²B < 3.05, then compute the pooled standard deviation by the following equation:
[ILLUSTRATION GOES HERE]
ER31AU93.075
1/2
⎡ 6 S 2A + 6 S 2B ⎤
S pooled = ⎢ ⎥
⎣ 12 ⎦ 1
if S²A/S²B > 3.05, re-spike at the most recent calculated MDL and process the
samples through the procedure starting with Step 4. If the most recent calculated MDL does not permit
qualitative identification when samples are spiked at that level, report the MDL as a concentration between
the current and previous MDL which permits qualitative identification.
c) Use the Spooled as calculated in 7b to compute the final MDL according to the following equation:
MDL = 2.681 (Spooled)
where 2.681 is equal to t(12, 1-α = .99)
d) The 95% confidence limits for MDL derived in 7c are computed according to the following equations
derived from percentiles of the chi squared over degrees of freedom distribution.
LCL = 0.72 MDL
UCL = 1.65 MDL
where LCL and UCL are the lower and upper 95% confidence limits respectively
based on 14 aliquots.
TABLES OF STUDENTS' t VALUES AT THE 99 PERCENT CONFIDENCE LEVEL
Students' t: Table I.
Number of replicates Degrees of freedom t(n-1, 1-α = 0.99)
(n-1)
7 6 3.143
8 7 2.998
9 8 2.896
10 9 2.821
11 10 2.764
16 15 2.602
21 20 2.528
26 25 2.485
31 30 2.457
61 60 2.390
∞ ∞ 2.326
Reporting
The analytical method used must be specifically identified by number or title and the MDL for each analyte
expressed in the appropriate method reporting units. If the analytical method permits options which affect
the method detection limit, these conditions must be specified with the MDL value. The sample matrix
used to determine the MDL must also be identified with MDL value. Report the mean analyte level with the
MDL and indicate if the MDL procedure was iterated. If a laboratory standard or a sample that contained a
known amount analyte was used for this determination, also report the mean recovery.
If the level of analyte in the sample was below the determined MDL or exceeds 10 times the MDL of the
analyte in reagent water, do not report a value for the MDL.
Appendix C: Nonconformance Report

ID number:
Nonconformance recorded by: Date:
Description:
(Attach separate sheets if needed)
If applicable complaint’s name & phone number:
Data impacted:
Sampling Event(s) Item(s) Container(s) Test(s)/Contaminant
Root cause:
Possible Corrective Action (CA):
Assigned to: Target Date:
CA taken:
Management review: Date:
Quality Assurance Officer's audit: Date:
Subsequent or follow up CA refer to:

Non-conformance report ID number
Version 5.0 Nonconformance Report cont. Page 47 of 64
Technical Corrective Action

SECTION:
WA, AQM, Inorganic, or Organic/General Chem.
To From Date
Case Number Case Name
The review process has revealed the possible problems noted below. Please check bottle numbers, calculations,
dilution factors, and data entry for errors. Rerun samples if necessary to resolve the problem(s). If needed, reanalyze
another aliquot from another sample container to check for contamination, container or site mix-ups, etc. Complete
this report and return it when finished. This rework is a priority task.
New Result Data Correction
Item Number Date Bottle Number Test Result
Site Name
Bottle Number
Alternate Bottle
N b
Standard Parameter Initial Result Verified? Yes No
Initial Test Result Reason Code for Change
Expected Test Result Comments:
Problem Code

Site Name
Bottle Number
Alternate Bottle Number
Problem Code

Site Name
Bottle Number
Alternate Bottle Number
Problem Code
Problem Codes Change Codes
A – Field Duplicate Difference a – Data transfer
B – Disagreement with history b – Data transfer error
C – Disagreement with other tests c – Dilution or correction factor error
D – Irregular Field Blank d – Bottle Number mix-up
E – Disagreement with Ion Balance e – Other (describe)
F – Other (describe)
FIELD/LAB QUALITY CONTROL CHECK

Event Number Event Name
Item Number Date Sampled
Field Data Laboratory Data
Test Meter ID Result Units Bottle Number Test Date Result Units Confirms Field Data
pH SU SU Yes No
Alkalinity mg/L mg/L Yes No
Turbidity NTU NTU Yes No
Conductivity µmhos/cm µmhos/cm Yes No
Comments:

pH SU SU Yes No
Comments:

pH SU SU Yes No
Comments:

pH SU SU Yes No
Comments:
Corrective Action: Analyze a confirmation sample if the Laboratory Alkalinity, Conductivity, or Turbidity
disagrees with the Field results by more than 20% RPD or if the pH value disagrees with the Field results
by more than +/-0.5 units. When one or both samples are < 5 times the MRL compare the results using +/-
1 MRL for the average. If one or both of the Turbidity samples are < 10 NTU, then compare the results
using +/- 1 MRL for the average + 1 NTU. Another sample container may be required to check for the
possibility of site/sample confusion of container handling or cleaning problems. If the discrepancy is
verified, have the analysis assigned and run all the samples for the entire sampling event.
The Relative Percent Difference (RPD) is calculated using the following equation:
Xs − Xd
RPD = × 100%
[Xs + Xd ] / 2
Where: Xs = field result and
Xd = lab result
The units for Xs must equal those of Xd
Example 1: Given two duplicate results of 18 and 23:
23 − 18 5
RPD = × 100% = × 100% = 24%.
[18 + 23] / 2 20.5
Therefore, the Quality Control Check would fail. The Laboratory RPD results are over the expectable RPD
of 20%.
Example 2: Given two duplicate results of 5 and 7:
The Quality Control Check calculation = (5 + 7)/2 = 6. Therefore, the Acceptance window is 6 ± 1 MRL.
Therefore, the Quality Control Check would pass. The Laboratory results are within the calculated range of
5 to 7.
Example 3 (for Turbidity): Given two duplicate results of 5 and 9, the Quality Control Check calculation =
(5 + 9)/2 = 7. The acceptance window is 7 ± 2. Therefore, the Quality Control Check would pass. The
Laboratory results are within the calculated range 5 to 9.
Appendix D: LIMS status codes

LIMS table: XLU STATUS
STATUS STATUS DESCRIPTION
A+ Data of known Quality. Presented by DEQ meeting current QC limits as established by the
Laboratory's Quality Systems Manual.
A Data of known Quality. Submitted by entities outside of DEQ meeting current QC limits for
external data as established by the DEQ Laboratory.
B Data of suspect Quality. Data may not meet established QC but is within marginal acceptance
criteria or data value may be accurate, however controls used to measure Data Quality
Objective elements failed i.e. batch failed to meet blank QC limit.
C Data of unacceptable Quality. Values are discarded (Void) typically due to analytical failure.
D No sample collected or no reportable results, typically due to sampling failure.
E Data of unknown quality. No QA information is available, data could be valid however there is
no evidence to prove either way (Educational Only, Very Questionable/Poor QA/QC).
F Exceptional Event. "A" Quality data but not representative of sampling conditions as required
by the project plan.
Appendix E: Major Analytical Equipment

Organic Analytical Section
• GC/MS/DS:
• Allocated to semi-volatile analyses a HP 5989 Mass Spectrometer Engine with HP 6890
series II GC and HP data system.
• Allocated to volatile analyses a HP 5972 Mass Spectrometer Detector with HP 6890 GC
and HP data system. Capillary/packed column GC with HP Purge Trap Concentrator
and a Varian Archon vial autosampler.
• Allocated for Air toxics HP 5971A Mass Spectrometer Detector with 5890 series II GC
and HP data system. Capillary/packed column.
• GCs:
• HP 6890 series II Plus, FID & NPD, HP 3365 Chemstation data system.
• Varian 6890 series II Plus; Capillary/packed column, PID and FID dedicated for SUMMA
canister analysis.
• HP 5890 series II; TCD & OI PID/FID; HP 3365 Chemstation data system. With OI 4560
Purge & Trap and 4551 vial autosampler.
• HP 5890 series II; two ECDs; HP 3365 Chemstation data system.
• HP 6890 series II; two ECDs.
• HPLC:
• Agilent Series 1100 equipped with HP Diode Array UV/Vis and Programmable
Fluorescence Detectors with an HP Chemstation.
• Chromatography Data Stations:
• HP 1405 Timeserver and LAN hardware
• Agilent 1100 LC/MSD Chemstation A.09.03
• Agilent Environmental Chemstation G1701DA
• Total Organic Carbon (TOC) Analyzer:
• Tekmar/Dohrman Apollo 9000
• COD Reactors:
• 3 x HACH COD Reactors.
• Total Organic Halogen (TOX) Analyzer:
• Mitsubishi TOX-10Σ, Aimed AutoAOX autosampler.
• Spectrophotometers:
• HACH DR/3000
• Fluorometer:
• Turner Designs TD-700
• Analytical Balances:
• Mettler PM4600 Delta Range semi-micro
• 2 x Mettler AT261 semi-micro
Inorganic Analytical Section
• Atomic Absorption Spectrophotometer (AAS):
• Varian AA-400. GTA-96 Graphite tube atomizer.
• Varian AA-400. Zeeman Graphite tube atomizer.
• CETAC M6000 Mercury Analyzer.
Version 5.0 Major Analytical Equipment cont. Page 52 of 64
• Microwave Digestor
• CEM MDS-2100
• Autoanalyzer:
• Lachat Flow Injection Ion Analyzer: Nitrate + Nitrite, Nitrite, Chloride, TK-N, and Sulfate
modules.
• Alpchem: Fluoride & Ammonia.
• Ion Chromatographs:
• Dionex Model 120, autosampler and Peaknet software
• Dionex 600 upgraded with CDM detector, gradient pump, SRS suppresser, AS40
autosampler, and Peaknet software.
• X-Ray Fluorescence Spectrometer:
• Fisons KEVEX EDX771
• Amperometric Titrator:
• Wallace & Tiernan Titrator
• Spectrophotometers:
• Bausch & Lomb: Spectronic 21
• Perkin Elmer Model Lambda 20 Spectrophotometer
• Hach DR/700
• Inductively Coupled Plasma (ICP):
• Simultaneous Perkin Elmer Optima 3000 DV
• Inductively Coupled Plasma Mass Spectrometry (ICP/MS):
• Thermo Elemental Model VG PQ Excel
• Analytical Balances:
• Sartorius A200S
• Mettler H15
• H6 w/filter weighing chamber
• Mettler H15, H18
• Sartorius 1712MP8
• Ohaus Balance, E4000D
• Microbalances:
• Cahn C30 - Range 1 µg to 3gm
• ATI Cahn C-44
• Optical Microscope:
• Zeiss Standard 18, Polarizing Trinocular with 35-mm camera
• Spencer Binocular stereo scope
• Olympus CH2 Phase Contrast microscope
Appendix F: QC definitions
QC Class QC LIMS Frequency Description/Corrective Action

Analytical Instrument Blank IB 1/analytcial Instrument Blank: a clean sample (e.g., distilled water) processed through the instrumental steps of the
batch measurement process; used to determine instrument contamination. (EPA-QAD)
QC sample is measured prior to batch analysis. If QC fails to meet assigned control limits and the problem
can not be corrected all reported results within the batch shall be flagged with the appropriate data qualifier.
Analytical Internal Standard IS 100% per Internal Standard: pure analyte(s) added to a sample, extract, or standard solution in known amounts and
SOP used to measure the relative responses of other method analytes that are components of the same sample
or solution. The internal standard must be an analyte that is not a sample component. (EPA Method 200.8)
The relative response of this QC element is used to adjust reported results of other analytes. Statistical
analysis of the relative response may prove useful for evaluating maintenance schedules.
Analytical Reagent Blank RB 1/ Reagent Blank: (method reagent blank): a sample consisting of reagent(s), without the target analyte or
preparation sample matrix, introduced into the analytical procedure at the appropriate point and carried through all
batch subsequent steps to determine the contribution of the reagents and of the involved analytical steps. (QAMS)
QC sample is measured prior to batch analysis. If QC fails to meet assigned control limits and the problem
can not be corrected all reported results within the batch shall be flagged with the appropriate data qualifier.
Calibration Continuing CCB per SOP Continuing Calibration Blank: Reanalysis of the calibration blank or equivalent matrix repeated through the
Calibration Blank analytical batch to establish instrumental bias, drift, and/or carry-over. (DEQ)
QC sample is measured during the batch analysis. If QC fails to meet assigned control limits and the
problem can not be corrected all reported results bracketed between the RB and CCB or between CCBs
shall be flagged with the appropriate data qualifier.
Calibration Continuing CCV beginning Continuing Calibration Verification: Reanalysis of the initial calibration standards during the course of a
Calibration and end of calibration batch used to demonstrate continued instrument performance. At a minimum, a CCV must be
Verification analytical repeated at the beginning and end of each analytical batch. The concentration of the CCV shall be varied
batch within the established calibration range. However, if an internal standard is used, only one CCV must be
analyzed per analytical batch. (DEQ)
If QC fails to meet assigned control limits and the problem can not be corrected, all reported results
bracketed between the ICV & CCV or between CCV’s shall be flagged with the appropriate data qualifier.
Version 5.0 Appendix F: QC definitions cont. Page 54 of 64

Calibration Quality Control ICV Immediately Quality Control Sample: an uncontaminated sample matrix spiked with known amounts of analytes from a
Sample (QCS) or following source independent from the calibration standards. It is generally used to establish intra-laboratory or
Initial Calibration initial analyst specific precision and bias or to assess the performance of all or a portion of the measurement
Verification calibration system. (EPA-QAD)
When used as the Initial Calibration Verification (ICV), the QCS is used to verify the initial instrument
calibration and should be the first sample analyzed in the analytical sequence. (NELAC/DEQ)
If the QC fails to meet control limits and the problem can not be corrected all reported results within the
analytical batch shall be flagged with the appropriate data qualifier.
Field Automated AP 1/ quarter Changed from Field Control Standard:
Precision
Used in air sampling. The operator generates a known concentration of the target analyte and analyzes it
through the equipment. Similar to a CCV sample, but used to assess field operations. (DEQ)
If QC fails to meet assigned control limits and the problem can not be corrected, all reported results
bracketed between the ICV & CCV or between CCV’s shall be flagged with the appropriate data qualifier.
Field Equipment Blank EB per Equipment Blank: a sample of analyte-free media which has been used to rinse common sampling
sampling equipment to check effectiveness of decontamination procedures. (NELAC)
expedition
If blank fails QC limits estimate target limits for the sampling event.
or per
QAPP
Field Field Audit FA per QAPP Field audit: verification of field measured parameters through the use of a secondary method. (DEQ)
Field Field Duplicate FD 10% Field Duplicate: discrete samples taken from the same field location and processed and analyzed
samples independently by the laboratory. The original sample is identified by space and time. The field duplicate is
collected collected at the same location and within a reasonable lapse of time. (DEQ)
during a
sampling
expedition
Field Laboratory LRB per SOP Changed from Lab Stored Blank.
Retained Blank
Laboratory Retained Blank: a sample of analyte-free matrix that remains in the laboratory and is used as
comparison with the blanks carried to the field. (DEQ)
Field Manual Precision MP 10% sample Changed from Co-located Sampler.
sites
Used in air sampling. A secondary sample collected from a location. Similar to a Field Duplicate. Multiple
sampling devices run simultaneously within close proximity. (DEQ)

Field Sample S 100% Sample identified by space and time. Space is defined by decimal latitude carried to five decimal places and
by longitude carried to five decimal places and elevation used in a vertically integrated sample. Time is
defined by the time zone using a 24 hour clock to the nearest minute. Start and stop time must be recorded
for composite samples.
Field Transfer Blank TSFB per QAPP Transfer Blank: a sample of analyte-free matrix which has been carried to the field and transferred to a
sample bottle in the field. (DEQ)
Field Transport Blank TNPB per QAPP Transport Blank: a sample of analyte-free media which has been carried to the field and returned to the
laboratory. (DEQ)
Operations Automated AA Used in air sampling. Generally a gas from a secondary source analyzed on-site by a secondary auditor.
Accuracy Very similar to a 2nd source QC in many respects. (DEQ)
Operations Blind Sample BLND Blind Sample: a sub-sample for analysis with a composition known to the submitter. The analyst/laboratory
may know the identity of the sample but not its composition. It is used to test the analyst’s or laboratory’s
proficiency in the execution of the measurement process. (NELAC)
Operations Certified CRM Certified Reference Material (CRM): a reference material one or more of whose property values are certified
Reference by a technically valid procedure, accompanied by or traceable to a certificate or other documentation which
Material is issued by a certifying body. (ISO Guide 30 - 2.2)
Operations Inter-Lab Split SPLT Changed from Split: Samples split with an external laboratory.
Sample
Laboratory audit or Split sample: verification of field and/or laboratory performance through the collection
and analysis of field duplicate samples by an alternate laboratory. (DEQ)
Operations Manual Accuracy MA Used in air sampling. A secondary auditor collects audit samples on equipment using equipment with known
properties, essentially the collection of an audit sample. (DEQ)
Operations Proficiency Test PT Proficiency Test Sample (PT): a sample, the composition of which is unknown to the analyst and is provided
Sample to test whether the analyst/laboratory can produce analytical results within specified acceptance criteria.
(QAMS)
Operations Reference RM Reference Material: a material or substance one or more properties of which are sufficiently well established
Material to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning
values to materials. (ISO Guide 30-2.1)

Operations Reference RS per QAPP Reference Standard: a standard, generally of the highest metrological quality available at a given location,
Standard from which measurements made at that location are derived. (VIM-6.08)
Preparation Dilution DR as required Dilution: additional measurement made from a diluted sample aliquot. Used with the undiluted sample or
other dilutions to establish analytical precision, evaluate matrix interferences, and/or bring the analyte
concentration to within the instrument's calibration range. (DEQ)
Preparation Laboratory LCON per SOP Confirmation: verification of the identity of a component through the use of an approach with a different
Confirmation scientific principle from the original method. These may include, but are not limited to:
Second column confirmation
Alternate wavelength
Derivatization
Mass spectral interpretation
Alternative detectors or
Additional cleanup procedures. (NELAC)"
Preparation Laboratory LCS 1/ analytical Laboratory Control Sample (also known as laboratory fortified blank, spiked blank, or QC check sample): a
Control Sample batch sample matrix, free from the analytes of interest, spiked with verified known amounts of analytes or a
material containing known and verified amounts of analytes. It is generally used to establish intra-laboratory
or analyst specific precision and bias or to assess the performance of all or a portion of the measurement
system. (NELAC)
The LCS requirements for analytical QC may be satisfied through the use of a Quality Control Sample
(QCS).
Preparation Laboratory LCSD Laboratory Control Sample Duplicate: a sample matrix, free from the analytes of interest, spiked with verified
Control Sample known amounts of analytes or a material containing known and verified amounts of analytes. It is used with
Duplicate the LCS to establish intra-laboratory or analyst specific precision and bias when more traditional methods are
unavailable. (DEQ)
Preparation Laboratory LD 10% / Changed from Analytical Replicate.
Duplicate preparation
Laboratory Duplicate: aliquots of a sample taken from the same container under laboratory conditions and
batch
processed and analyzed independently. (NELAC)
Preparation Matrix Spike MS Matrix Spike (spiked sample or fortified sample): a sample prepared by adding a known mass of target
analyte to a specified amount of matrix sample for which an independent estimate of Target analyte
concentration is available. Matrix spikes are used, for example, to determine the effect of the matrix on a
method's recovery efficiency. (QAMS)

Preparation Matrix Spike MSD Matrix Spike Duplicate (spiked sample or fortified sample duplicate): a second replicate matrix spike
Duplicate prepared in the laboratory and analyzed to obtain a measure of the precision of the recovery for each
analyte. (QAMS)
Preparation Method Blank MB 1/ Method Blank: a sample of a matrix similar to the batch of associated samples (when available) that is free
preparation from the analytes of interest and is processed simultaneously with and under the same conditions as
batch samples through all steps of the analytical procedures, and in which no target analytes or interferences are
present at concentrations that impact the analytical results for sample analyses. (NELAC)
Preparation Standard SRM per QAPP Standardized Reference Material (SRM): a certified reference material produced by the U.S. National
Reference Institute of Standards and Technology or other equivalent organization and characterized for absolute
Material content, independent of analytical method. (EPA-QAD)
Preparation Surrogate SS 100% per Surrogate: a substance with properties that mimic the analyte of interest. It is unlikely to be found in
SOP environment samples and is added to them for quality control purposes. (QAMS)
Appendix G: Analytical Methods
ANALYTE Standard EPA, iv EPAv, vi, vii SW-846viii TECHNIQUE

Methodsi, ii, iii
METALS
Aluminum 3120 B 200.7 200.7 6010 ICP
Antimony 3113 B 204.2 200.9 7041 AA FURNACE
Antimony 3120 B 200.7 6010 ICP
Arsenic 3113 B 206.2 200.9 7060 AA FURNACE
Arsenic 3114 B,4.d 206.3 7061 AA HYDRIDE
Arsenic 3120 B 200.7 200.7 6010 ICP
Barium 3120 B 200.7 200.7 6010 ICP
Beryllium 3113 B 210.2 200.9 7091 AA FURNACE
Beryllium 3120 B 200.7 200.7 6010 ICP
Boron 3120 B 200.7 6010 ICP
Cadmium 3113 B 213.2 200.9 7131 AA FURNACE
Cadmium 3120 B 200.7 200.7 6010 ICP
Calcium 3120 B 200.7 200.7 6010 ICP
Chromium 3113 B 218.2 200.9 7191 AA FURNACE
Chromium 3120 B 200.7 200.7 6010 ICP
+6
Chromium 218.5 COPRECIPITATION
Cobalt 3113 B 219.2 7201 AA FURNACE
Cobalt 3120 B 200.7 6010 ICP
Copper 3120 B 200.7 200.7 6010 ICP
Iron 3120 B 200.7 200.7 6010 ICP
Lanthanum 200.7 6010 ICP
Version 5.0 Appendix G: Analytical Methods cont. Page 59 of 64

Methodsi, ii, iii
Lead 3113 B 239.2 200.9 7421 AA FURNACE
Lead 3120 B 200.7 6010 ICP
Lithium 3120 B 200.7 6010 ICP
Magnesium 3120 B 200.7 200.7 6010 ICP
Manganese 3120 B 200.7 200.7 6010 ICP
Mercury 3112 B 245.1 245.1 6010 Manual Cold Vapor
Molybdenum 3120 B 200.7 6010 ICP
Nickel 3120 B 200.7 200.7 6010 ICP
Potassium 3120 B 200.7 6010 ICP
Selenium 3113 B 270.2 200.9 7740 AA FURNACE
Selenium 3114 B 270.3 7741 AA HYDRIDE
Selenium 3120 B 200.7 6010 ICP
Silica 3120 B 200.7 200.7 6010 ICP
Silver 3113 B 272.2 200.9 AA FURNACE
Silver 3120 B 200.7 200.7 ICP
Sodium 3120 B 200.7 200.7 6010 ICP
Strontium 3120 B 200.7 6010 ICP
Thallium 279.2 200.9 7841 AA FURNACE
Thallium 3120 B 200.7 6010 ICP
Tin 200.7 6010 ICP
Titanium 6010 ICP
Tungsten 6010 ICP
Vanadium 3120 B 200.7 6010 ICP

Methodsi, ii, iii
Zinc 3120 B 200.7 200.7 6010 ICP
Zirconium 6010 ICP
NON METALS
BOD5 5210 B Winkler-Azide Modification
CBOD5 5210 B Winkler-Azide Mod./Inhib
Dissolved Oxygen 4500-O C 360.2 Winkler-Azide Modification
Dissolved Oxygen 4500-O G 360.1 Membrane Electrode
Bromide 4110 B 300 Ion Chromatography
-
Chloride 4500-Cl C 325.1 Auto Ferricyanide
Chloride 4110 B 300.0 Ion Chromatography
Chlorine 4500-Cl D 330.1 Amperometric Titration
Chlorine 4500-Cl G 330.5 DPD Colorimetric
Fluoride 4500-F E 340.3 Auto Complexone
Ammonia-Nitrogen 4500-NH3 H 350.1 Auto Phenate
Total Kjeldahl Nitrogen 351.2 S-Auto Block Digestion
Nitrate-Nitrogen 4500-NO3 F 353.2 Auto Cadmium Reduction
Nitrite-Nitrogen 4500-NO3 F 353.2 Auto colorimetric
Nitrite-Nitrogen 4110 B 300.0 Ion Chromatography
Ortho Phosphate-P 4500-P E 365.2 Colorimetric Ascorbic Acid
Ortho Phosphate-P 4110 B 300.0 Ion Chromatography
Total Phosphate-P 4500-P E,5 365.2 Colorimetric Ascorbic Acid
Sulfate 4500-SO42 F 375.2 375.2 Auto Methylthymol Blue

Methodsi, ii, iii
Sulfate 4110 B 300.0 300.0 Ion Chromatography
PHYSICAL PARAMETERS
Acidity 2310 B 305.1 Titration
Alkalinity 2320 B 310.1 Titration
Color 2120 C 110.3 Colorimetric Pt/Co
Conductivity 2510 B 120.1 Wheatstone Bridge
Flash Point 1010 Pensky-Martens closed-cup
+
pH 4500-H 150.1 150.1 Electrometric
Filterable (TDS) 2540 C 160.1 Gravimetric, 180oC
Nonfilterable (TSS) 2540 D 160.2 Gravimetric, 103-105oC
Total (TS) 2540 B 160.3 Gravimetric, 103-105oC
Volatile 160.4 Gravimetric, Ignition @ 550oC
Temperature 2550 B 170.1
Turbidity 2130 B 180.1 Nephelometric
ORGANICS
Adipates 625 525.2 8270 GC/MS
BTEX 602 5020A GC/PID
Chlorinated Pest/PCB 608 508 8081 Solvent Extr., GC/ECD
PCB as DCBP 508A Solvent Extr., GC/ECD
Chlorinated Herbicides 515.1 8150A Solvent Extr., GC/MS
EDB, DBCP 504.1 GC/ECD

Methodsi, ii, iii
Herbicides 515.1 8150A Solv, Ext., derivation, GC/MS
Hydrocarbon ID (HCID) 8015 modified GC/FID
Pentachlorophenol 625 525.2 8270B GC/MS
PAHs 610 525.2 8270, 8310 Solv, Extr., GC/MS
Phthalates 625 525.2 8270 Extr., GC/MS
PPOE,BNA 625 525.2 8270 Extr., GC/MS
Trihalomethanes 624 524.2 8260 P&T, GC/MS
VOCs/VOAs 624 524.2 8260 P&T, GC/MS
N-P Pesticides 8141A GC/NPD
Miscellaneous
Chemical Oxygen Demand 5220 D 410.4 Colorimetric (Chromate)
Chlorophyll a/Pheophytin a 10200-H 445 Fluorometric
Cyanide, Total/Amenable 4500-CN E 352.2 9010 Colorimetric
MBAS (Surfactants) 5540 C 425.1 Methylene Blue Active Substance
NW-TPH: Gas
NW-TPH: Diesel
NW-TPH: Oil
Gas
Diesel
Oil
Oil and Grease 1664ix Gravimetric (Hexane)
Particulate Fall Out (PFO) Gravimetric
x
Percent Fat Hexane Extraction/Gravimetric

Methodsi, ii, iii
Phenolics 420.1 9066 Colorimetric (Pyrine)
xi
Sediment Sizing Gravimetric
Total Organic Halides (TOX or AOX) 1650
Total Organic Carbon 5310 B 415.1 Persulfate Oxidation/NDIR Detection
Total Organic Carbon (Soil)xii Walkley/Black Titration
i
Approved Waste Water Methods promulgated in 40 CFR Part 136 appear in “Bold”.
ii
Approved Drinking Water Methods promulgated in 40 CFR Part 141 appear in “Italic”.
iii
Standard Methods for the Examination of Water and Wastewater, 18th Edition, APHA, AWWA, WPCF, 1994.
iv
Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020, Revised 3/83.
v
300.0: Methods for the Determination of Inorganic Substances in Environmental Samples, EPA-600/R-93-100, August 1993.
vi
200.7 & 200.9: Methods for the Determination of Metals in Environmental Samples - Supplement I, EPA-600/R-94-111, May 1994.
vii
Five hundred series: Methods for the Determination of Organic Compounds in Drinking Water, EPA-600/4-88-039, December 1988. Methods for the Determination
of Organic Compounds in Drinking Water - Supplement I, EPA-600/4-90-020, July 1990. Methods for the Determination of Organic Compounds in Drinking
Water - Supplement II, EPA-600/R-92-129, August 1992.
viii
Test Methods for Evaluating Solid Waste: SW-846, Third Edition, USEPA, November 1986.
ix
Chuck Clarke, Regional Administrator for EPA, Region 10 has sent a letter of approval for an alternate test procedure. EPA will recognize results from Method 1664, Hexane
Extractables for all Oil and Grease analyses performed on samples that originate in Region 10.
x
DEQ Method Revised 2/3/98.
xi
DEQ Method developed 3/12/1987
xii
DEQ Method Developed 8/29/1989
Version 5.0 Appendix H: Organizational Chart Page 64 of 64
Division
Administrator:
Mary Abrams
Special Projects: Executive Support Specialist: Air Quality QAO: Land Quality QAO: Water Quality QAO:
Rick Hafele Sylvia Herrley Paul McKay Ron Doughten Chris Redman
Air Quality Monitoring Watershed Assessment Technical Services Manager: Inorganic Laboratory Manager: Organic & General Chemistry
Manager: Manager: Dan Hickman RaeAnn Haynes Laboratory Manager:
Jeff Smith Greg Pettit Eugene Foster
Senior Air Senior Air Senior Surface Senior Surface

Water Water Project LIMS Senior Lead Lead Senior
Monitoring Monitoring
Monitoring: Monitoring: Coordinator: Coordinator: Chemist: Chemist: Chemist: Chemist:
Specialist: Specialist:
Larry Caton Larry Marxer Steve Mrazik Jeff Jones Bill Karen Yates James Yates Rich Koenig
Mark Hansen Kathleen
Schuckman Calzaretta
Lead Surface Lead Surface Database

Senior Air Air Water Water Lead Specialist: Lead Lead GC Chemist: Lead
Monitoring Monitoring Monitoring: Monitoring: Chemist: John Koestler Chemist: Chemist: Julie Sievers Chemist:
Specialist: Specialist: Dave Gilbey Mike Mulvey Ted Haigh Ben Jones Linda McRae Paul
Anthony Ron Schoenlaub
Surface Water Lead Surface Database
Barnack Cunningham
Monitoring: Water Specialist:
Greg Coffeen Monitoring: Sample Rob Keller Chemist: Chemist: GC Chemist: Chemist:
Air Air Doug Drake Tracker: George Liliana Estegenet Rick Rother
Monitoring Monitoring Surface Water Bob McCoy DiDomenico Echeverria Belete
Specialist: Monitoring: Lead Surface Data Clerk:
Specialist:
Al Bogner Josh Jackson Water Mikina Moore
Lance
Hochmuth Monitoring:
Surface Water Analytical Chemist: Chemist: Extraction Chemist:
Aaron
Air Sampling Monitoring: Reports: Data Clerk: Lizbeth Rachel Webb Chemist: Kirk Keyes
Borisenko
Air Technician: Sarah Miller Deanna MaryJane Garcia Sarah
Monitoring Shanique Lead Surface Jones Gilles Romero
Specialist: Young Surface Water Water
Bob Jones Monitoring: Monitoring:
Alan Hamel Shannon Hubler Public Data Chemist: Chemist: Chemist: Chemist:
Air Sampling Relations: Verification: Ken Aldrich George Chris Moore Alem
Air Sampling Technician: Lead Ground Lead Surface Richard Sigrid Yousif Gebretasadik
Technician: Christopher Water Water Kokich Schwind
Holly Stewart McGarry Monitoring: Monitoring:
Rich Myzak Steve Hanson
Network Document Chemist: Chemist: Toxics
Administrator Control: Gordon Kenzin Fultz- Coordinator: Chemist:
Air Sampling Air Sampling Ground water Surface Water
Nelly Bernuy- Vacant Seele Wahl Fenix Grange Matt
Technician: Technician: Monitoring: Monitoring:
Garcia Lowrance
Keith Iding Keith Kilcoin Dave Cole David Huff
Ground water Surface Water

Air Sampling Air Sampling Monitoring: Monitoring: Procurement Receptionist:
Technician: Technician: Michael Won Kim & Contracts: Therese
Bill Becker Trina Ritchey Tichenor Paula Ingelby
D’Alfonso

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Laboratory Quality Manual

FOR THE OREGON DEPARTMENT OF

Mary Abrams, Laboratory Division Administrator Date

Eugene Foster, Organic Section Manager Date

RaeAnn Haynes, Inorganic Section Manager Date

Dan Hickman, Technical Services Section Manager Date

Jeff Smith, Air Monitoring Section Manager Date

Greg Pettit, Watershed Assessment Section Manager Date

Paul McKay, Air Quality Assurance Officer Date

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4.2.3 Receipt .................................................................................................................... 21

Acronyms and Abbreviations

Conformance: an affirmative indication or judgment that a product or service

National Environmental The overall National Environmental Laboratory Accreditation

Quality Manual: A document stating the management policies, objectives,

Sample Tracking: Procedures employed to record the possession of the

Verification: Confirmation by examination and provision of objective

1.2 DEQ's Quality Management Policy

2 Laboratory Management Structure

2.1 Laboratory Quality Assurance Team

2.3 Air Quality Monitoring

2.4 Watershed Assessment

2.5 Inorganic Laboratory

2.6 Organic Laboratory

2.7 Technical Services

Table 1 Minimum Qualification for Laboratory Personnel

Position Minimum Qualification

Position Minimum Qualification

Position Minimum Qualification

Position Minimum Qualification

Position Minimum Qualification

3 Standard Operating Procedures

3.2 Sample Handling

3.2.1 Sample Identification

3.2.2 Sample Receipt

3.2.3 Sample Integrity

3.3 Test Methods and Method Validation

3.3.1 Analytical SOPs

3.3.2 Demonstrations of Capability

3.3.3 Data Validation

3.3.4 Estimation of Uncertainty of Measurement

3.3.5 Data Control

4.2 Purchasing Services and Supplies

4.2.1 Request for Purchase

4.2.6 Use and Consumption

5 Assuring the Quality of Analytical Data

6.1 Support Equipment

6.2 Instruments used for the Determinative Step

6.3 Accommodation and Environmental Conditions

6.3.1 Laboratory Facility

6.3.2 Environmental Controls

7.1 Control of Quality Documents

7.2 Analytical Records

7.3 Data Reports and Verification Records

7.4 Client Correspondences

7.4.1 Analytical Work Submitted to the Laboratory

7.5 Quality Assurance Measures

7.5.1 Internal Audit

7.5.2 Annual QA Report

7.5.3 Nonconformance Investigations and Corrective Action Reports