ASB LOQAM
Effective Date: April 24,2018
ANALYTICAL SERVICES BRANCH
LABORATORY OPERATIONS
and
QUALITY ASSURANCE MANUAL
U.S. ENVIRONMENTAL PROTECTION AGENCY
SCIENCE AND ECOSYSTEM SUPPORT DIVISION
REGION 4
980 COLLEGE STATION ROAD
ATHENS, GEORGIA 30605-2700
Concurrences and Approvals:
(1) Name: Dannv France Phone: 706-355-8738
Title: Branch Chief, Analytical Services Branch
Signature ^ ' Date:
(2) Name: JeffrevYlendel Phone: 706-355-8839
Title: Section Chief. Inorganic Chemistry Section
Signature: Date: ?//*-
(3) Name: Flovd Wellborn Phone: 706-355-8567
Title: Section Chief. Organic Chemistry Section
Signature: Date:
(4) Name: Stacie Masters Phone: 706-355-8847
Title: Laboratory Quality Manager
Signature: .vi&V/ Date:
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DISCLAIMER
The mention of trade names or commercial products in this manual is for
illustration purposes only and does not constitute endorsement or
recommendation for use by the Environmental Protection Agency.
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Analytical Services Branch
Ethics Policy
"// shall be the policy of the Region 4 Laboratory to conduct all business
with integrity and in an ethical manner. It is a basic and expected
responsibility of each staff member and each manager to hold to the
highest ethical standard ofprofessional conduct in the performance of all
duties and to adhere to EPA's Principles of Scientific Integrity, dated
November 24,1999."
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Table of Contents
Chapter 1 INTRODUCTION
1.1 Purpose
1.2 Mission of the EPA Regional Laboratory
1.3 Operations Policy
1.4 Accreditation and Certification
1.5 Hierarchy
Chapter 2 PERSONNEL/FACILITIES/EQUIPMENT
2.1 Organization
2.2 Educational Experience and Training Requirements
2.3 Roles and Responsibilities
2.4 Facilities
2.5 Equipment
Figure 2-1 Analytical Services Branch Organization Chart
Figure 2-2 Science and Ecosystem Support Division Organization Chart
Chapter 3 SAMPLE SCHEDULING, HANDLING, STORAGE AND DISPOSAL
3.1 Introduction
3.2 Sample Collection
3.3 Sample Scheduling
3.4 Sample Receipt
3.5 Sample Logging and Storage
3.6 Custody
3.7 Review of Custody Records
Table 3-1 Recommended Preservation & Holding Times
Chapter 4 GENERAL LABORATORY PRACTICES and PROCEDURES
4.1 Good Lab Practices
4.2 Document Control/File Management
4.3 Laboratory Apparatus and Instruments
4.4 Laboratory Supplies
4.5 Laboratory Hazardous and Non-Hazardous Waste Handling and Disposal
Procedures
4.6 Laboratory Cleanliness
Chapter 5 PERFORMANCE QUALITY CONTROL and DATA HANDLING
5.1 Introduction
5.2 Terminology
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5.3 Essential Quality Control Requirements
5.4 Data Handling
5.5 Data Reporting
5.6 Data Management and Data Security
5.7 Annual Analytical Performance Summary
5.8 QC Study Plan
5.9 Complaints/Inquiries
5.10 Corrective Actions
5.11 Preventive Actions and Improvements
5.12 Control of Nonconforming Testing Work
5.13 Annual Management Review
Table 5-1 Critical values of the studentized deviation
Table 5-2 Critical values of the Q in Dixon's Q-test
Chapter 6 METHODOLOGY
6.1 General
6.2 Method Information
6.3 Minimum Reporting Limits
6.4 Land Disposal Restrictions
Table 6-1 Levels of Concern for Various Programs
Figure 6-1 Decision Tree for Analysis of Samples for Land Disposal Restriction
Table 6-2 Capability for Potable Waters - Inorganics
Table 6-3 Capability for Potable Waters - Organics
Table 6-4 Metals Analyte List Minimum Reporting Limits by Matrices
Table 6-5 Nutrients and Classicals Analyte List Minimum Reporting Limits by
Matrices
Table 6-6 Volatile Organics (VOAs) Target Analyte List Minimum Reporting
Limits by Matrices
Table 6-7 Semivolatile Organics (SemiVOAs) Target Analyte List Minimum
Reporting Limits by Matrices
Table 6-8 Routine Pesticide Target Analyte List Minimum Reporting Limits by
Matrices
Table 6-9 Special Request Pesticide Target Analyte List Minimum Reporting
Limits by Matrices
Table 6-10 Carbamate Pesticide Target Analyte List Minimum Reporting Limits
by Matrices
Table 6-11 Herbicides Target Analyte List Minimum Reporting Limits by
Matrices
Table 6-12 Per- and Polyfluoroalkyl Substances (PFAS) Target Analyte List
Minimum Reporting Limits by Matrices
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CHAPTER 1
Purpose, Policy, Accreditation and Hierarchy
1.1 Purpose
The purpose of this manual, entitled Laboratory Operations and Quality Assurance Manual
(LOQAM), is to document the quality assurance policies and procedures of the USEPA,
Region 4 Analytical Services Branch (ASB) laboratory. A defined system of quality
assurance practices and operational policies (a quality system) is essential for ensuring that
data generated from analytical processes are well-defined and defensible. While the design
and development of a quality assurance program is a management function, each individual
staff member shares the responsibility for maintaining knowledge of the quality system and
for following established quality control procedures. Meeting the International Organization
for Standardization (ISO) 17025 standard, "General requirements for the competence of
testing and calibration laboratories", and continually improving quality system effectiveness
is a principle objective of the laboratory.
1.2 Mission of the EPA Regional Laboratory
The mission of ASB is to provide environmental data for decision making in EPA's media
programs for protecting the environment and human health. This is achieved by
maintaining a fully equipped environmental laboratory and a technically skilled, properly
trained and dedicated staff that produces physical, biological, and chemical data of a
known and defensible quality. ASB provides environmental data at the request of the
customer within the Agency. All requests for analyses must originate with an EPA
manager or staff person with the authority to request services from ASB. As an EPA
laboratory, ASB is not permitted to operate as a fee-for-service laboratory.
1.3 Operations Policy
It is a basic policy of ASB to conduct all activities with four guiding principles: (1) Safety
(2) Data Integrity and Laboratory Ethics (3) Quality and (4) Service. All of these items
must be present for successful operations
1.3.1 Safety The primary consideration in all laboratory operations must be safety. There is
no assignment for which safety should ever be compromised. Safety takes priority over all
considerations and it is the responsibility of each staff person to have a clear understanding
of the basic safety rules and, in particular, how to safely perform operations within their area
of responsibility. It is the responsibility of each individual to maintain a constant vigilance
over safe operations and to notify their supervisor, Safety and Health Manager and the
branch Safety Officer of any unsafe conditions. ASB employees must never initiate an
action, procedure, or method if they are unsure of the appropriate safety procedures. If unsure
of the safety of any method, procedure, or operational activity, it is the responsibility of each
employee to contact their supervisor to obtain additional information or instructions on the
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proper safety procedures. Refer to the Safety, Health and Environmental Management Policy
and Procedures Manual (SHEMP) for safety and health policies and procedures.
1.3.2 Data Integrity and Laboratory Ethics It is the policy of the Region 4 Laboratory to
conduct all business with integrity and in an ethical manner. It is a basic and expected
responsibility of each staff member and manager to hold to the highest ethical standard of
professional conduct in the performance of all duties and to adhere to EPA's Principles of
Scientific Integrity (1999) and the Scientific Integrity Policy (2012). The quality system of
the branch has data integrity and ethical behavior at its very foundation. It is absolutely
essential that every employee of the branch understand and adhere to these ethical standards
in order to preserve the basic integrity of all work products. Data integrity, defined in its
most simple terms as "the state of being unimpaired", concerns the ability to define and
defend that the entire analytical process has been "unimpaired" and performed in
accordance with appropriate practices and procedures. The ability to defend the integrity of
the data is through complete documentation of actions and activities which includes, but is
not limited to such items as: maintaining chain of custody and security of the samples; clear
documentation of the activities performed in the preparation and analysis of the samples
according to SOPs and in the final data reduction, review, and reporting; and maintaining
complete and clear files of these records.
1.3.3 Quality It is the policy of ASB that all data generated is of the quality required to
meet or exceed the data quality objectives (DQOs) of each project as determined by the
customer. Managers and analysts of the branch share the responsibility of ensuring that
analytical methods, instruments, analyte detection and quantitation are such that the data
produced is scientifically sound and well documented. It is of utmost importance that the
quality of all data produced by ASB be well defined and communicated to the customer.
This policy is implemented by:
1.3.3.1 Having in place and following a complete and systematic process of
quality control activities to assist in defining data quality;
1.3.3.2 Ensuring that data quality is documented and communicated to the customers
of the data by assigning appropriate qualifiers according to prescribed procedures; and
1.3.3.3 Having a peer review process to verify that data are generated in accordance
with sound and appropriate technical procedures and to ensure that all activities
associated with the analyses, calculations and data reduction are complete and accurate.
1.3.4 Service ASB is a service organization and as such, management and staff
must maintain an awareness of customer needs and regulatory requirements as
related to satisfaction with work products. Service is built upon the following two
important principles.
1.3.4.1 Communication between the laboratory's staff and its clients is
required to fully define a project's measurement and DQOs and to assist the
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customer in understanding analytical capabilities and limitations.
Communications also enhance the ability to learn of emerging needs and to
plan accordingly. ASB management and staff must be proactive in initiating
these discussions and will make every effort to inform customers of the
advantages and disadvantages of requested methods and quality control
procedures. Laboratory management reserves the right to determine the most
appropriate analytical methodology and quality control procedures based on the
DQOs, if provided by the customer.
1.3.4.2 Timeliness Timing of final work products and reports are often critical and are a
vital part of the overall service performed. While it is ASB's policy to never
compromise safety, integrity or quality for the sake of timeliness, timeliness is often the
most important factor contributing to customer satisfaction. All staff must maintain a
high degree of attention toward providing the data in a timely manner as established by
project objectives. In the event circumstances result in late reports, the customer must be
contacted, kept up-to-date on the issues surrounding the late data, and kept abreast of the
progress of project completion.
1.4 Accreditation and Certification
1.4.1 EPA issued a policy directive on February 23, 2004 that all Agency laboratories shall
maintain competency by documenting and maintaining a quality system which meets the
requirements of EPA Order CIO 2105.0, (formerly 5360.1 A2) May 2000. The policy
requires EPA laboratories to participate in an appropriate, recognized laboratory
accreditation program when available.
1.4.2 ASB is ISO/IEC 17025:2005 accredited. Refer to certificate number AT-1691 and
scope for specific accreditation information. The laboratory is also Drinking Water certified
by the Office of Ground Water and Drinking Water (OGWDW) and is certified to the current
Drinking Water methodologies and the Fifth Edition of the Manual for the Certification of
Laboratories Analytical Drinking Water (EPA 815-R-05-004, January 2005).
1.4.3 ASB's objective is to seek and maintain accreditation and certification for the methods
and analytes that it performs on a routine basis. A list of the methods for which ASB is
currently accredited and certified is available from the Laboratory Quality Manager (LQM).
ASB will not use an accrediting organization's logo (such as the ANAB logo) on data reports
and does not conduct any advertising which might show an accrediting organization's logo.
A statement indicating the accrediting body and the accreditation status of individual tests
will be included on all test reports issued by ASB.
1.5 Hierarchy
This manual describes the policies that are the basis of ASB's quality system. Specific
technical and procedural details are contained in methods and technical and administrative
SOPs. On occasion, an analytical method or procedure may require deviation from some
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of the policies contained in this manual for specific technical reasons. These deviations
will be documented in the individual SOPs. As such, instructions in SOPs and regulatory
program requirements take precedence over this manual on those occasions.
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CHAPTER 2
Personnel, Facility and Equipment
2.1 Organization
Below is a listing of all ASB Staff and their major area(s) of responsibility. The ASB
organizational structure is shown in Figure 2-1. Figure 2-2 depicts ASB as it fits into the
total operation of the Science and Ecosystem Support Division (SESD). In the event that the
Branch Chief, Section Chief, or Laboratory Quality Manager (LQM) is absent for a period
of a week or more, the appropriate management official within the branch or section shall
appoint a deputy to act on behalf of the individual who is absent. Staff signatures and
initials are kept on file by the LQM.
2.1.1 Analytical Services Branch Personnel
Immediate Office
Name
Danny France
Scott Sivertsen
Stacie Masters
Mike Beall
Alva Eisenman
Marilyn Maycock
Principal Duties
Branch Chief
Senior Technical Advisor
Laboratory Quality Manager
Sample Custodian (SEE Employee)
Divisional Document Control (SEE Employee)
Senior Technical Advisor
Inorganic Chemistry Section
Name
Jeffrey Hendel
Daniel Adams
Pam Betts
Curtis Callahan
Anthony Carroll
Megan DeJesus
Earnest Walton
Terri White
Kayle Whiten
Principal Duties
Section Chief-Technical Director Inorganic Analyses
Nutrients, Classicals, Final Data Review/Production
Classicals, ASB Safety Officer
Nutrients, Classicals
Mercury, Hexavalent Chromium, Lead Bioavailability
Metals ICP
Metals ICP-MS
Metals ICP, Final Data review/Production
Nutrients, Classicals
Organic Chemistry Section
Name Principal Duties
Floyd Wellborn Section Chief-Technical Director Organic Analyses
Diana Burdette Semivolatiles, LC-MS/MS
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Jason Collum
Sam Dutton
John Giles
Sallie Hale
David Spidle
Kristin Trapp
Stephanie Wimpey
Francine Vancuron
Pesticides/PCBs, SESD Chemical Hygiene Officer
Pesticides/PCBs
Extraction, Semivolatiles, LC-MS/MS
Volatiles (Air)
Monitored Natural Attenuation
Volatiles (Air)
Volatiles, Property Officer, ChemShare Coordinator
LC-MS/MS
2.2 Educational. Experience and Training Requirements
2.2.1 EPA operates its hiring procedures under the federal government's Office of
Personnel Management (OPM) regulations. OPM issues qualification and classification
standards for all general schedule (GS) positions. Typically, ASB's professionals and
technicians fall within the 1300 - Physical Sciences Group, Job Family Standards for
Professional Work and Technical Work (See http://www.opm.gov/aualifications/index.asp
and https://www.opm.gov/policv-data-oversight/classification-qualifications/classifying-
general- schedule-positions/#url=l 300. V The OPM qualification and classification
standards describe the educational and experience requirements which a potential employee
must meet to satisfy the OPM requirements for a specific job series and grade. Before a
laboratory employee is hired, EPA's Shared Service Center for Personnel Management
verifies that the applicant meets the OPM education and experience requirements for the
appropriate GS series and grade. After the verification process is complete, ASB managers
are allowed to hire an applicant who meets the OPM requirements from a certificate of
eligible candidates.
2.2.2 Prior to hiring a contract employee, an EPA Contracting Officer or Contracting
Officer's Representative, in consultation with ASB management, will describe to the
contractor in general terms the educational and experience requirements needed to
perform the work. Contractor employees' experience and education are verified by the
contractor's human resources department.
2.2.3 SESD has developed a set of required training sessions for each employee; they are
specified in the SESD Employee Training SOP. Documentation of training is maintained
by sign-in forms or certificates, and are maintained by the LQM in ASB's training files.
An ongoing goal of ASB's training program is to ensure that personnel are aware of the
importance of their activities and how they contribute to the overall mission and goals of
the Agency.
2.3 Roles and Responsibilities
2.3.1 Branch Chief
2.3.1.1 Has overall management responsibility, including hiring, budgeting, and policy
development for the branch, and mission. The Branch Chief also has ultimate
responsibility for the development, implementation, approval, and continued operation
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of the branch quality assurance system.
2.3.1.2 Assigns the authority and responsibility for day-to-day management of the
quality system is the LQM and assures that communication takes place regarding the
effectiveness of the quality system.
2.3.1.3 Delegates authority and responsibility for the daily oversight of quality control
activities in ICS and OCS to the Section Chiefs.
2.3.1.4 Provides leadership promoting a work culture that stresses the importance of
safety, integrity, data quality, timeliness and customer service.
2.3.1.5 Assures that qualified analysts and support staff are assigned to the laboratory
and that all staff are properly trained to perform their duties.
2.3.1.6 Is authorized to offer opinions and interpretations.
2.3.1.7 Makes overall decisions relating to staffing, personnel management,
work assignments, laboratory capability and capacity in consultation with
laboratory supervisors and staff.
2.3.2 Laboratory Quality Manager (LQM) - also referred to as the Quality Assurance
Manager (QAM)
2.3.2.1 Is independent from all laboratory operations, reports directly to the ASB
Chief and has the delegated responsibility and authority for the implementation,
management, and maintenance of the quality system for the laboratory.
2.3.2.2 Ensures compliance with all laboratory accreditation requirements.
2.3.2.3 Coordinates the branch-wide QA/QC activities.
2.3.2.4 Initiates and leads annual internal audits within the branch.
2.3.2.5 Works with Section Chiefs in determining the adequacy of corrective
and preventive actions.
2.3.2.6 Performs periodic spot checks (in addition to or in conjunction with the annual
internal audits) of project files to ensure that all proper documentation and QC
activities were performed. The spot checks shall be documented and any problems
communicated with the appropriate Section Chief and technical staff.
2.3.2.7 Maintains QA files with appropriate documentation to include, but not limited
to:
2.3.2.7.1 Managerial and supervisory reports;
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2.3.2.7.2 Documents requiring LQM signature/approval;
2.3.2.7.3 Outcomes of internal and external audits (reports,
CA/PA/Improvements, etc.);
2.3.2.7.4 Results of inter-laboratory comparisons or proficiency tests;
2.3.2.7.5 Records for measurement traceability for testing equipment
(i.e., weights/thermometers/volumetric syringes); and
2.3.2.7.6 Records and Documentation
2.3.2.7.6.1 Demonstration of Competency (DOC) and Continuing
Demonstrations of Proficiency (CDOP);
2.3.2.7.6.2 Method Detection Limits (MDLs) and Limits of Detection (LODs);
2.3.2.7.6.3 Instrument Detection Limits (IDLs);
2.3.2.7.6.4 New method/technology validation studies;
2.3.2.7.6.5 Special Issue Studies reports;
2.3.2.7.6.6 Summaries of updates for acceptance limits in Element® for spikes,
replicates, surrogates, and other QC data;
2.3.2.7.6.7 Trend reports produced by the sections;
2.3.2.7.6.8 Signature and initials of all employees;
2.3.2.7.6.9 Training files to include internal and external training, cross
training, certifications, etc.; and
2.3.2.7.6.10 Corrective Action and Preventive Action reports.
2.3.2.8 Performs periodic verification of primary standard prep and external verification
of the standards. (As a separate check or in conjunction with the periodic internal
audits.)
2.3.2.9 Reviews and approves all branch SOPs and QA manual updates and submits to
Branch Chief for final approval.
2.3.2.10 Initiates and coordinates external proficiency test studies for all branch
analytical operations.
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2.3.2.11 Advises branch management concerning QA/QC issues.
2.3.2.12 Is authorized to give opinions and interpretations.
2.3.3 Section Chief
233.1 Serves as the Technical Director of the section and oversees its day-to-day
activities including analysis of samples within the quality system and production of data
within each analytical group.
23.3.2 Ensures that a final overview of each work product (e.g., data, written reports)
is performed so that all quality control information is complete, properly utilized,
documented and maintained within the various analytical work units of the section.
2333 Reports final data produced by the section to the customer or delegates
to authorized staff.
233.4 Monitors all section work activities with the help of Group Leaders
where designated.
233.5 Ensures that appropriate actions are taken as a result of QC indicators.
Ensures that appropriate corrective actions are instituted within the analytical work
groups as a result of internal and external audits.
233.6 Reviews and approves all section specific technical document and LOQAM
updates.
233.7 Monitors and coordinates section workload and acceptance of work.
233.8 Ensures that individual project files are generated and maintained in
accordance with branch policies and other appropriate file management requirements.
233.9 Authorized to offer opinions and interpretations on analyses under their technical
direction as well as authorize other qualified individuals under their supervision to offer
opinions and interpretations on specific technical areas.
233.10 Communicates with customers to ensure that needs are met and to solicit
feedback on ASB's services.
233.11 Ensures compliance with all laboratory accreditation requirements.
2.3.4 Analytical Staff
23.4.1 General staff are responsible for:
2.3.4.1.1 Having a general knowledge of the branch and divisional policies
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and procedures including health and safety, data integrity, and waste disposal;
2.3.4.1.2 Having a working knowledge of analytical methodologies used within
their work areas;
2.3.4.1.3 Having a working knowledge of all policies, procedures, and QC
activities within their respective work areas and ensuring that documentation of
work performed is complete, accurate, and that analytical data are properly
reported;
2.3.4.1.4 Notifying their immediate supervisor of any issues/problems with any
work products; and
2.3.4.1.5 Maintaining and following appropriate SOPs for their work areas.
2.3.4.2 Group Leader (if designated by the Section Chief) At the discretion of the
Section Chief, the Organic or Inorganic Section may be comprised of work groups. If
applicable, each analytical work group may have a Group Leader appointed by the
Section Chief. This is not a supervisory position; however, Group Leaders are
assigned technical responsibilities to assist the Section Chief and may be called upon
to assist the Section Chief with work scheduling issues. The Section Chief will fill the
role of the Group Leader during periods for which there is no one so designated.
2.3.4.2.1 Serves as the primary technical contact on analytical issues or
questions pertaining to their specific expertise.
2.3.4.2.2 Provides daily direction of the technical activities within their work
unit; ensures that QA/QC actions are in accordance with sound technical
practices and follows policies and procedures of the LOQAM.
2.3.4.2.3 Ensures that appropriate corrective actions are taken based on
quality indicators from the analyses within their work unit.
2.3.4.2.4 Communicates regularly with LQM and other Group Leaders on
technical issues and problems.
2.3.43 Primary Analyst/Technician Defined as the staff analyst or technician
performing a test on a given date and time. Typically, the primary analyst performs
initial data reduction and transfer of data to the Element®. However, this task may also
be performed by another analyst competent to perform the analysis. The primary
analyst/technician shall ensure that:
2.3.4.3.1 Appropriate analytical methodologies and standard operating procedures
are followed;
2.3.4.3.2 Appropriate QC activities are performed as designated by the
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method, SOPs, and/or the LOQAM;
2.3.4.3.3 Analytical activities are properly documented as specified by the
method, SOPs, and/or the LOQAM;
2.3.4.3.4 Appropriate actions are taken when QC indicators do not meet
established criteria and assures that necessary corrective action is
implemented;
2.3.4.3.5 Individual analytical data points are completely and accurately
recorded;
2.3.4.3.6 Data qualifier flags and explanatory footnotes are properly placed;
and
2.3.4.3.7 All appropriate items on the data review/verification checklist are
properly documented.
2.3.4.4 Secondary Analyst (Data Verification) may be the Group Leader or another
staff analyst that is qualified to perform data review for the analysis being checked. It
is the responsibility of the secondary analyst to perform a thorough review of all
important details associated with the data being verified. The Secondary Analyst shall
ensure that:
2.3.4.4.1 Appropriate analytical methodologies and SOPs were followed;
2.3.4.4.2 Appropriate QC activities were performed as designated by the method,
SOP, and/or the LOQAM;
2.3.4.4.3 Analytical activities were properly documented as specified by the method,
SOP, and/or the LOQAM;
2.3.4.4.4 Appropriate actions were taken as a result of QC indicators; and
2.3.4.4.5 Analytical data qualifiers were accurately recorded and that all qualifier
flags and explanatory footnotes are properly placed on the data.
2.3.5 Deputies (Acting Chief or LQM) who are acting on behalf of Chiefs or LQM
assumes the duties and responsibilities of that individual under the quality system. Any
deputy will be notified of their temporary assumption of duties and responsibilities and must
be familiar with and capable of executing the applicable requirements of the quality system.
2.3.6 Environmental Services Assistance Team (ESAT) Laboratory Support -
Analytical support is often obtained through the ESAT contract as funding permits. The
ESAT team is located on site within the ASB laboratory areas with space assigned
specifically to them. Work is assigned by EPA Contract Officers to ESAT staff through
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technical direction documents following all contractual rules and regulations. ESAT
personnel are expected to be familiar with the LOQAM, follow its policies and practices, and to
follow analytical SOPs approved by EPA management.
2.3.7 ASB Staff - ESAT Work Assignments
23.7.1 Select ASB staff may submit technical direction requests to ESAT through the
ESAT Tracking System. ESAT assignments may require communication with the
Section Chief to assure that the ESAT workload is evenly distributed. Under the
existing contract, only the EPA Contract Officer to ESAT or Alternate may issue work
to ESAT.
23.12 ASB staff that submit technical direction requests must follow all rules and
regulations of the contracting process. ASB staff are also responsible for receiving the
work products that are generated by ESAT staff and performing an appropriate review
of the work performed.
2.3.73 Each data package should be reviewed at a minimum to ensure that:
2.3.7.3.1 Appropriate analytical methodologies and SOPs were followed;
2.3.7.3.2 Appropriate QC activities were performed as designated by the method,
SOP, and/or the LOQAM;
2.3.7.3.3 Analytical activities were properly documented as specified by the
method, SOP, and/or the LOQAM;
2.3.7.3.4 Appropriate actions were taken as a result of QC indicators;
2.3.7.3.5 Recording of all individual analytical data points aiecomplete and
accurate and data qualifier flags and explanatory footnotes are properly placed;
2.3.7.3.6 Project file contains, or references, location of all necessary information
including raw data, calibrations, extraction logs, standards, run logs, and dilutions;
and
2.3.7.3.7 Data have been entered and verified in Element® and, if qualified, contain
the appropriate remarks to show reason(s) for qualification.
Note: Divisional Director, Deputy Director and Regional Quality Assurance Manager
(RQAM) Roles and Responsibilities are outlined in the SESD Quality Management Plan
(QMP). Please refer to the most recent version of the QMP for more information.
2.4 Facilities
The total facility consists of approximately 55,000 net usable square feet, a little less than a
third of which is occupied by ASB. Operation and maintenance of the facility is the
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responsibility of the lessor through the Government Services Administration (GSA). SESD
(not within ASB) has one or more staff members dedicated to facility issues, coordinating
maintenance and operations with GSA and the lessor. The facility has adequate
accommodations to perform testing procedures in the laboratory area. The laboratory will
ensure the facility and environmental conditions relevant to the procedure will be
monitored as required.
2.5 Equipment
2.5.1 Inventory ASB maintains a list of analytical instrumentation on the LAN.
2.5.2 Maintenance/Service Proper maintenance of laboratory instrumentation is a key
ingredient to both the longevity of the useful life of the instrument, as well as providing
reliable analyses. Maintenance and service requires an alert analytical staff that recognizes
the need for equipment maintenance coupled with support services provided either by
in-house staff or by vendor technicians. All staff members have the responsibility for
ensuring that all primary maintenance is carried out on instrumentation in accordance with
manufacturer's recommendations and schedules as practical.
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Figure 2-1
Analytical Services Branch Organization Chart
y
Immediate Office
Danny France, Chief
Scott Sivertsen (Technical Advisor)
Stacie Masters (LQ.M)
Mike Beall (SEE)
Alva Eisenman (SEE)
Marilyn Maycock (Technical Advisor)
L
A
r
inorganic Section
Jeffrey Hendel, Chief
D. Adams
C. Callahan
P. Betts
E. Walton
A. Carroll
T. White
M. DeJesus
K. Whiten
J
r
Organic Section
Floyd Wellborn, Chief
D. Burdette
D. Spidle
J. Collum
K, Trapp
S. Dutton
S. Wimpey
J. Giles
F. Va neuron
S. Hale
L
J
Page 14 of 100
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Figure 2-2
Science and Ecosystem Support Division — Athens, Georgia
Quality Assurance and
Technical Services Branch
Chief
r
Quality Assurance Section
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Chapter 3
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CHAPTER 3
Sample Scheduling, Handling, Storage and Disposal
3.1 Introduction
Complete documentation of the sample collection and handling process is an extremely
important aspect of producing defensible laboratory data. Chain-of-custody procedures
provide a record of sample traceability, accountability, and serve to validate sample
integrity. All samples for analysis received by ASB are controlled with documented
custody procedures.
3.2 Sample Collection
3.2.1 Procedures ASB staff does not perform field sampling activities, therefore the
sampling activities are covered under the project specific Quality Assurance Project
Plans.
3.2.2 Containers and Holding Times Selection of sample container types and
preservation techniques are guided by the methods being applied. Guidance is available
in such references as Standard Methods for the Examination of Water and Wastewater,
ASTM, EPA Methods for Chemical Analyses of Water and Waste, 40 CFR 136, 40 CFR
141 and others. Table 3-1 includes sample containers, analysis, sample matrices,
preservatives, and recommended holding times. ASB will accept smaller aliquots of
samples than referenced in Table 3-1; however, when reducing sample volumes, the
volume of preservative must also be reduced to achieve the same final concentrations of
preservative in the sample.
3.3 Sample Scheduling
3.3.1 Initial Scheduling ASB uses an in-house laboratory information management
system (LIMS), called R4LIMS for project scheduling. Each project that is entered into
R4LEMS is assigned a unique project number that is used throughout its life for
tracking, reporting, and filing.
3.3.2 Sample Acceptance
Review of Requested Analyses The ASB Section Chiefs routinely review
requested projects through R4LEMS to determine whether to accept the requested
project, or if the project should be contracted outside the laboratory through a
national contract such as the Superfund Contract Laboratory Program (CLP). When
projects are entered into R4LIMS requesting analysis, ASB management has the
first right of refusal of the work. The laboratory will not accept samples that arrive
without first being requested and scheduled in R4LEMS prior to receipt. If this
situation occurs, laboratory management will contact the project requestor and/or
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their management to determine if the samples must be analyzed and what priority
will be assigned. Normally all samples in support of criminal investigation projects
will be analyzed within the ASB laboratories or sent to the National Enforcement
Investigations Center (NEIC) for analysis. R4LIMS shows scheduled projects in
grey until they have been officially accepted by ASB. Scheduling of the samples
generally includes an estimate of numbers, matrices, requested analyses and turn-
around time (TAT) requirements. The standard TAT for the laboratory from the time
samples are received until results are reported is 35 calendar days for routine
analyses and 45 calendar days for projects with TCLP requirements. When a project
requires samples to be received by the laboratory over multiple days, the TAT is
calculated based on the last day samples are received by the laboratory for the
particular project. Communication of special project requirements are noted in
R4LIMS Project Notes.
3.3.2.1 Sample Acceptance Responsibility and Considerations The acceptance of
samples into the ASB laboratory is the responsibility of the Section Chiefs, Branch
Chief, or designated alternate(s). Factors considered by ASB management when
accepting samples for analysis include whether laboratory and staff have the
necessary skills, expertise, and instrumental capability to perform the environmental
tests requested, a demonstration of competency is on file and the laboratory has
accreditation for a specific method/analyte/technology when an accredited test result
is requested. If the consideration of the above factors indicates any deficiency, lack
of accreditation, or inability to perform the work, laboratory management will notify
the data requestor, either verbally or in writing, and resolve any differences in
methodology, quality control, or scope of work to be performed.
3.3.2.2 Special Project Needs Occasionally, the laboratory receives requests to
perform analyses for non-routine analytes or matrices. As a support laboratory for
various EPA programs, the laboratory must maintain the flexibility to accept and
perform analyses using methods and for analytes for which it is not accredited. The
region's Emergency Response program is an example where the laboratory may be
called upon to perform unique analyses in order to protect public health or the
environment. If the laboratory is requested to perform analyses for non-accredited
methods, the data requestor will be informed that the laboratory may not have all
quality control requirements in place to meet accreditation requirements. Any
limitations on data usability will also be explained to the customer.
3.3.2.3 Potable Water On occasion, ASB receives requests for the analysis of
potable water samples. Most requests are not in support of the Safe Drinking Water
Act (SDWA) found at 40 CFR Part 141. If there is any doubt as to whether the
request is in support of SDWA regulations, the Section Chief or designee will
contact the requestor to determine the purpose of the analysis.
3.3.2.3.1 If the request is in support of SDWA regulations, analyses must be
performed by approved methods found at 40 CFR Part 141. Tables 6-1 and 6-2
list primary drinking water contaminants, including analytical method
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requirements. As indicated in Table 6-2, ASB does not analyze the full list of
primary drinking water contaminants. If the requestor requires the analysis of a
primary contaminant which ASB does not analyze, the Regional Sample Control
Coordinator (RSCC) will assist the requestor in locating a laboratory that has the
capability and proper accreditation.
3.3.2.3.2 If the request is not in support of SDWA regulations, then ASB may
choose to use alternate methods which meet the project's data quality
objectives.
3.3.2.4 NPDES These analyses requested in support of the National Pollutant
Discharge Elimination System (NPDES) regulations at 40 CFR Part 136 require
the use of approved methods.
3.3.2.5 Request for Use of Specific Analytical Methods The usual procedure for
booking samples for analysis includes information from the requestor as to the
Minimum Reporting Limits (MRL) required for the project (either routine levels, or
special request). ASB chooses an appropriate analytical method to meet the client's
needs in consideration of the Data Quality Objectives (DQO). On occasion, ASB
may receive a request to use a specific analytical method. These requests typically
initiate a conversation with the requestor as to the ultimate DQOs and whether the
specified method is the most appropriate choice for the requestor's needs.
3.3.2.6 Documenting Communication in R4LIMS and Element® Workorder
Notes Communication between the project leader and ASB personnel should be
documented. This includes documenting in Element® or the project file any special
requests or clarification to requests, changes to the project.
3.3.2.6.1 When negotiating the terms of the initial project request,
documentation of verbal or written (email) communication should be
included in R4LIMS project notes.
3.3.2.6.2 After samples are received, all changes to the Element® Workorder
must be approved by the appropriate ASB manager (or designee) and
documented by the SCC in the Element® Workorder notes. Refer to SOP ASB
105G for more procedures related to sample receipt.
3.3.2.7 Quick Turn-Around Analyses If laboratory capacity allows; a quick
turnaround time can be accepted. It is important that the SCC monitors R4LIMS for
receipt documentation and communicates any issues to managers and analysts so
that analyses may begin as soon as possible in order to accommodate the request. In
able to accommodate the quick-turn requests, distribution of results will be handled
in one of two ways.
3.3.2.7.1 Preliminary results will be reported to the customer within the
requested timeframe, followed by final reporting at a later date.
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33.2.1.2 Final results that have gone through the necessary QA/QC checks will
be reported.
3.3.3 Canceled Projects/Samples On occasion, whole projects, samples, or analyses
can be cancelled due to funding, broken bottles, etc. Project Notes or Element® will be
used for documenting the reasons for cancelled projects, samples or analyses. Lost
samples or containers will be noted in Element® and the affected analyses will be
reported as "Not Analyzed".
3.4 Sample Receipt
3.4.1 Sample Acceptance Policy Samples requested for analysis within ASB are
typically from internal Agency sampling organizations, contractors, or states directly
supporting EPA Region 4 Programs. As such, it would be a rare circumstance that a
sample directed for analysis within ASB would be refused based on issues related to
field sampling (e.g., temperature, improper containers, etc.). Any sampling anomalies
for a specific project must be evaluated on individual merit for the impact upon the
results and the data quality objectives of the project. If possible, the decision will be to
proceed with the analyses with proper documentation and communication of the
sampling anomaly and any known or suspected impacts on data quality.
Documentation of the issue and the final decision for action shall be included in the
project file.
Due to waste handling and sample disposal considerations, ASB's policy is not to
provide storage for samples which have been or are to be analyzed by other
laboratories. Exceptions to this policy may be made on a case-by-case basis by
laboratory management.
3.4.2 Sample Receiving Procedure Detailed sample receiving procedures are
documented in the most current revision of SOP ASB 105G, Sample Receiving and
Custody.
3.4.3 Sample Receipt Guidelines for Analyses with Short Holding Time
Requirements Some organic and inorganic analyses such as waters requiring analysis
for semivolatiles, pesticides/PCBs TSS, TDS, Unpreserved Nitrate or Nitrite, BOD, and
unpreserved volatiles require expedited shipping to SESD due to the short holding
times. Therefore, the following sample shipping guidelines should be observed by field
sampling organizations.
3.4.3.1 Semivolatiles, Pesticides/PCBs, TSS, TDS, and unpreserved VOA
waters Water samples collected during the week must be shipped to the lab
within 48 hours of collection in order to meet the required holding time.
Observation of Federal holidays should be considered when planning sampling
projects.
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3.4.3.2 VOA soils These samples generally must be shipped (or "walked in") daily
to meet the 48-hour holding time. However, if the soils are collected in 40-mL
vials (with or without water/methanol) and then frozen at -7 to -20°C in the field,
quick delivery is not necessary. Freezing coring devices in the field does not
extend the 48-hour holding time.
Note: Dry ice cannot be used to freeze the samples because the temperature in the
cooler may be < -20 °C.
3.4.3.3 Unpreserved Nitrate or Nitrite and BOD These samples should be
shipped (or "walked in") daily to meet the 48-hour holding time.
3.4.3.4 Short Hold Samples Held in the Field: ASB does not guarantee holding
times for short-hold samples that are held in the field and not shipped promptly to
the laboratory on the aforementioned schedules.
3.4.4 Acceptance of Samples Known to Contain Listed RCRA Dioxin-Containing Waste
3.4.4.1 Environmental samples (biota, soil, sediment, groundwater, and surface
water) known or suspected to be contaminated with listed RCRA dioxin-
containing hazardous waste will not be accepted by ASB. This policy has been
implemented because of the special waste handling and disposal restrictions
placed upon listed RCRA dioxin-containing hazardous waste.
3.4.4.2 If capacity is available, ASB will accept other environmental samples
including those samples suspected of being contaminated with polychlorinated
dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), as long
as the suspected PCDD and PCDF contamination is not due to listed RCRA
dioxin-containing wastes.
3.4.4.2.1 Scheduling Samples When project leaders schedule samples known or
suspected to contain dioxin into R4LIMS for routine analyses, the requestors are
required to indicate whether the samples are or are not contaminated with listed
RCRA dioxin-containing wastes. Because the laboratory has limited, if any,
knowledge of site or facility history, it is the project leaders' responsibility to
determine whether samples are contaminated with the listed RCRA-dioxin
containing wastes. A waste is determined to be a hazardous waste if it is
specifically listed on the F or K lists found in title 40 of the Code of Federal
Regulations (CFR) in Section 261. Prior to scheduling samples, review the
hazardous waste criteria information at the following link to determine if the
samples will be acceptable by ASB:
Defining Hazardous Waste: Listed. Characteristic and Mixed Radiological
Wastes I Hazardous Waste I US EPA
3.4.4.2.2 The documents cited in references 1 and 2 are located on the SESD
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LAN and may be consulted for additional information on the management of
RCRA wastes.
'Management of Contaminated Media, EPA Region 4, September 7, 1999
Management of Remediation Wastes under RCRA, EPA 530-F-98-026, October 1998
3.4.5 Sample Disposal ASB will depend on the Project Lead, Sample Control Coordinator,
samplers' knowledge of site conditions concerning listed RCRA dioxin containing
wastes. Environmental samples containing dioxin but which do not contain dioxin listed
wastes do not require disposal as RCRA hazardous wastes. Such samples will be
disposed as ordinary environmental samples unless they are hazardous by other RCRA
characteristics or are a listed waste.
3.5 Sample Logging and Storage
3.5.1 Assignment of Numbers Each sample (and container) is assigned a
unique identification by Element® based on the following pattern.
3.5.1.1 EYYWWNN-AN-L where EYYWWNN represents a 'Work Order' number,
analogous to an R4LEMS project number and -AN-L is a sample number within the
work order.
3.5.1.2 The letter E is a non-changing designation for samples analyzed by the ASB lab.
3.5.1.3 YY is a two-number designation for the calendar year.
3.5.1.4 WW is a two-letter designation for the week of the calendar year (01 through 52).
3.5.1.5 NN is a two-number designation (01 through 99) representing an
incremental number of the work order received for that week. The sample number
-AN- is a two- digit sample number (01 through 99) or alpha character (AA
through ZZ) and -L is a unique letter designation assigned to each container
received from a particular sampling location.
3.5.2 Storage of Samples When all numbers are assigned; sample bottles are secured
within the custody room walk-in coolers or freezer. Other specifically designated
sample storage locations are used by the ASB laboratory such as dedicated refrigerators
for VOA samples in the VOA laboratory. Metals do not require storage in a refrigerator.
3.5.2.1 The temperatures of designated storage areas are continuously monitored
using a certified wireless temperature sensor which interfaces with a data logger
controlled through software located on the DicksonOne website. The system is
Cloud-based and the units are connected via WiFi. The software records and sends
e-mail and text message alerts if the temperature exceeds the specified range.
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3.5.2.2 The acceptable temperature range for the coolers is above freezing to 6°C.
The freezer should maintain < -10°C. A temperature excursion outside acceptance
criteria may result in initiating a corrective action to determine if the excursion was
a systematic issue. The Custody Room coolers and freezer are additionally
monitored by security personnel outside regular business hours.
3.6 Custody
3.6.1 Custody records for all samples received by ASB are maintained within Element®.
Reports can be generated on each Workorder which details the custody for each sample
container.
3.6.2 Custody Room Access Key card entry controls access to the main custody room
area. Entry is coordinated with the facility representative by each Branch Chief
submitting request for all staff authorized for entry. It is the responsibility of the
facility representative to ensure that authorized names are properly entered into the
computer.
3.6.3 Custody Room Housekeeping The sample custodian or designee monitors all
areas of the custody room to ensure it is maintained in a clean, orderly and secure
manner. Areas needing attention shall be brought to the attention of the Section Chief
(Organic or Inorganic) for which the area is designated for use. Facility cleaning staff do
not routinely enter the custody room. The custody room is cleaned only by special
coordination and scheduling through the facility representative.
3.6.4 Documentation of Custody Documentation of sample custody is accomplished
by the use of custody seals placed on the sample coolers that are secured by field
sampling personnel, a COC form initiated at the time of sample collection, field log
books, individual analysis logs, the Element® and sample disposal memos and records.
The original field custody form, along with a computer printout of the requested
analytical tests (workorder printout), is maintained in the SESD Project files. A copy of
the field custody form and a copy of the computer print-out are sent to the project team
personnel responsible for sample collection associated with a specific project. It is the
project leader's responsibility to check the computer print-out against the COC record
for accuracy as it relates to analyses requested for the project and the sampling station
identification information.
3.6.5 Assuming Custody for Sample Analysis ASB utilizes Element® to perform
sample check-out, check-in to/from their storage locations. To receive samples for
analysis, an analyst must assume custody of the samples (including those 'aliquoted' in
the custody room such as frozen tissue). When the need for the sample container is
complete, custody is relinquished by setting the location of the container to "disposed"
in Element® and returning it back to the original storage location.
3.6.6 Tracking Custody of Sample Extracts, Digestates and/or Leachates
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3.6.6.1 ASB will track the custody of the extracts, digestates and/or leachates
throughout the prep and analysis of the samples.
3.6.6.2 The custody of the extracts, digestates and/or leachates are transferred from
the prep area personnel to the analytical personnel by using the bench sheet. There
are areas at the end of each bench sheet that track the custody of the samples as they
move through the analytical process. The prep analyst signs in the "relinquished
by" area and the receiving analyst signs in the "received by" area. If the analyst
transfers custody of the samples prior to disposal, the analyst should relinquish
custody by signing the bench sheet in the same manner as described above.
3.6.6.3 Batch IDs are assigned automatically by Element® and are in the
format 'YYMMnnnn' where:
3.6.6.3.1' YY' is a two-digit number identifying the year of the batch,
3.6.6.3.2 'MM' is a two-digit number identifying the month and
3.6.6.33 'nnnn' is a four-digit number representing the incremental
batch created that month.
3.6.6.4 If a batch of samples requires re-extraction or re-digestion, the samples are
re- batched within Element®.
3.6.6.5 Batch IDs are also used for tracking QC data associated with a batch. That is,
any method blank, LCS data or matrix QC data associated with a particular batch of
samples is assigned a unique ID associating it with the batch.
3.6.6.6 Transfer of Custody from ASB: On occasion, after ASB has assumed
custody of the samples, there may be requests for samples to be transferred to other
individuals or organizations. Samples shall only be removed from ASB custody by
transferring official custody using appropriate COC forms and notations in
Element®. All custody transfers of this nature must be coordinated through the
sample custodian or designee.
3.7 Review of Custody Records
Review of custody records will be performed by the LQM or designee(s). These reviews performed
prior to the inclusion of documents in the project file. For a list of the custody records that must to be
included in the project file, refer to ASB SOP 105G.
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Table 3-1
Recommended Preservation & Holding Times
Soil/Sediment1
Water12
and Waste Water
Waste
Tissue
Analytical
Group
Pres3
Hold'
Pres3
Hold'
Pres3
Hold'
Pres3
Hold'
Amf
Container
Type5
Amf
Container
Type5
Amf
Containe
r Type5
Amf
Container
Type5
Inorganics
Acidity
NA
NA
Ice-4°C
500 mLP.FP
Fill completely
and cap tightly
14 days
NA
NA
NA
NA
Alkalinity
NA
NA
Ice-4°C
500 mLP.FP
Fill completely
and cap tightly
14 days
NA
NA
NA
NA
BOD5
NA
NA
Ice-4°C
2LP.FP
48 hrs
NA
NA
NA
NA
BOD - Long Term
NA
NA
Ice-4°C
1 gal(x2)15 P, FP
48 hrs
NA
NA
NA
NA
Bromide
NA
NA
Ice-4°C
500 mLP.FP
28 days
NA
NA
NA
NA
Chloride
None
8 oz G
Not
specified
None
500 mLP.FP
28 days
NA
NA
NA
NA
Chlorine -
Residual
NA
NA
None
500 mLP
Immediate
NA
NA
NA
NA
Chromium VI
(hexavalent)
Ice-4°C 8 oz
G
Extract -
1 month
Analysis
- 4 days7
Filter immed.9
Ice-4°C
1LP.FP
Buffer to extend
HT3
24 hrs
28 days
if
buffered
3
No
ne
8oz
G
Extract-
1 month
Analysis -
4 days7
NA
NA
Cyanide
Ice-4°C
8 oz G
14 days
NaOH to
pH>12,
ascorbic acid8,
Ice-4°C
500 mLP.FP
14 days
No
ne
8oz
G
Not
specified
NA
NA
Dissolved P, total
NA
NA
Filter immed.9
Ice-4°C
H2S04 to pH<2
500 mLP.FP
28 days
NA
NA
NA
NA
Fluoride
None
8 oz G
Not
specified
None
500 mLP
28 days
NA
NA
NA
NA
Grain Size
None
8oz G
Not
Specified
NA
NA
NA
NA
NA
NA
Hardness (calc)
NA
NA
NA
Separate bottle not
required,
calculated from
the metals scan
NA
NA
NA
NA
NA
Mercury, Routine
Ice-4°C
8 oz G
28 days29
HNOsto pH<2 1L
P, FP
28 days29
No
ne
8oz
G
180 days
Freeze, 5
g 8 oz G,
A1
foil or plastic
Not
specifie
d
Mercury - TCLP
None
8 oz G
28 days
56 days10
None
1LP, FP or
1 gal. P, FP, G
if multiphase
(>0.5% and
<10%solids)
28 days
56 days10
None
8oz G or
1 gal P,
Gif
multipha
se
(>0.5%
28 days
56 days10
NA
NA
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Table 3-1
Recommended Preservation & Holding Times
Soil/Sediment1
Water1,2
and Waste Water
Waste
Tissue
Analytical
Group
Pres3
Hold'
Pres3
Hold'
Pres3
Hold'
Pres3
Hold'
Amf
Container
Type5
Amf
Container
Type5
Amf
Containe
r Type5
Amf
Container
Type5
and
<10%
soli
ds)
Mercury - UTL
Ice-4°C
8 oz G
90 days
HC1 to pH<2 1L
FP (bottles
require
prescreening
and special
handling)
90 days
No
ne
8oz
G
Not
specified
Freeze, 5
g 8 oz G,
A1
foil or
plastic
Not
specifie
d
Metals, except
mercury
None 8 oz G
6 months
HNO,topH<2 1L
P, FP
180 days
6 months
No
ne
8oz
G
6 months
Freeze, 15
g 8 oz G,
A1
foil or
plastic
Not
specifie
d
Dissolved Metals,
except mercury
NA
NA
Filter immed9,
HNO,topH<2 1L
P, FP
180 days
6 months
NA
NA
NA
NA
Metals - TCLP
(except mercury, see
above)
None
8 ozG
180 days
360 days11
None
1L P, FP or
1 gal., P, FP, G
if multiphase
(>0.5% and
<10% solids)
180 days
360 days11
None
8 oz G or
1 gal. P, G
if
multiphase
(>0.5%
and <10%
solids)
360 days11
NA
NA
Nitrate (requires
two containers: one
unpreserved and a
2nd preserved)
Ice-4°C
8 oz G
Not
specified
Ice-4°C
500 mL P, FP
AND 2nd container
Ice- 4°C,
H2SO4 to pH<2 500
mL
48 hrs
NA
NA
NA
NA
Nitrite
Ice-4°C
8 oz G
Not
specified
Ice-4°C
500 mL P, FP
48 hrs
NA
NA
NA
NA
Nutrients
(ammonia, TKN,
NO3+NO2 -N,
total phosphorus)
Ice-4°C
8 oz G
Not
specified
Ice-4°C,
H2SO4 to pH<2
500 mL/ parameter
or 1L total P,FP
28 days
NA
NA
NA
NA
Ortho-P
NA
NA
Ice-4°C
500 mL P, FP
48 hrs
NA
NA
NA
NA
Orlho-P (when
equating dissolved
with Ortho-P)
NA
NA
Filter immed9,
Ice-4°C
500 mL P, FP
48 hrs
NA
NA
NA
NA
pH
None 8 oz G
Not
specified
None
500 mL P, FP
Immediate
except 24
hrs for
RCRA12
None 8 oz
G
24 hrs for
aqueous,
otherwise
not specified
NA
NA
Solids Series (TS,
TSS, TDS, TVSS,
etc.)
NA
NA
Ice-4°C
1L P, FP
7 days
NA
NA
NA
NA
Sulfates
Ice-4°C
8 oz G
Not
specified
Ice-4°C
500 mL P, FP
28 days
NA
NA
NA
NA
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Table 3-1
Recommended Preservation & Holding Times
Analytical
Group
Soil/Sediment1
Water1,2
and Waste Water
Waste
Tissue
Pres3
Amf
Container
Type5
Hold'
Pres3
Amf
Container
Type5
Hold'
Pres3
Amf
Containe
r Type5
Hold'
Pres3
Amf
Container
Type5
Hold'
TOC
Ice-4°C
8 oz G
Not
Specified
Ice-4°C,
H2S04 to pH<2
500mL P, FP
28 days
NA
NA
NA
NA
Dissolved TOC
NA
NA
Filter immed',
Ice 4°C,
H2S04 to pH<2
500mL, P, FP
28 days
NA
NA
NA
NA
Organics
TCLP Extractables
(Pesticides,
Herbicides,
Semivolatiles)
Ice-4°C 8 oz G
61 days13
Ice-4°C
1 L (x2 per
fraction)15 G/A
61 days13
None 8 oz
G
61 days13
NA
NA
For multi-phase samples, extra sample volume must be collected for TCLP analysis.
Extractables
(Pesticides/PCBs
, Herbicides,
Semivolatiles)
Ice-4°C
8 ozG
54 days14
Ice-4°C
1 L (x2 per
fraction)15 G/A
47 days16
None 8 oz
G
54 days14
Ice &
Freeze 30
g A1 Foil
Not
specified
Extractables/
Pesticides/PCBs
- residual
chlorine present
NA
NA
Ice-4°C
3 ml of 10 %
sodium
thiosulfate per
gallon
HCL, (pH,2)
1 L (x2 per
fraction)15 G/A
44 days17
NA
NA
NA
NA
Flashpoint
NA
NA
NA
NA
None
8 oz G
Not
specified
NA
NA
Methane/Ethane/
Ethene
NA
NA
HCL (pH<2),
Ice-4°C
40 mL(x3)15 G/S
14 days
NA
NA
NA
NA
Org Halide
(TOX)
Ice-4°C
8 oz G
28 days
Ice-4°C
H2SO4 to pH<2 1
LG/A
28 days
NA
NA
NA
NA
Perfluorocarbons
NA
NA
Ice-4-15°C lab
ambient+ 10-40
% acetonitrile
125-mL
Polypropylene
(x2)
194 days27
NA
NA
NA
NA
Carbamates
NA
NA
Ice-4°C 60-mL
G/A(x2)
14 days28
Phenols (analyzed
as semivolatile
compounds)
Ice 4°C
8 oz G
54 days14
Ice-4°C
1 L(x2)15 G/A
47 days16
None
8 ozG
54
days14
Ice & Freeze
30 g A1
Foil
Not
specified
Volatile Organics
Volatile Organics
Method 5035A
Ice-4°C
5 g (x3)18E
or equivalent1'
48
hours
iced/14
days
frozen20
NA
NA
Ice-4°C
8-oz G26
14
days21
NA
NA
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Table 3-1
Recommended Preservation & Holding Times
Soil/Sediment1
Water1,2
and Waste Water
Waste
Tissue
Analytical
Group
Pres3
Hold'
Pres3
Hold'
Pres3
Hold'
Pres3
Hold'
Amf
Container
Type5
Amf
Container
Type5
Amf
Containe
r Type5
Amf
Container
Type5
Volatile Organics
Method 5035A
Ice-4°C
5 g (x3)18
into tared 40- mL
VOA
vials19
48 hours
iced/14
days
frozen2
0
NA
NA
NA
NA
NA
NA
Volatile Organics
Method 5035A
Ice-4°C
5 g (x3)18
into tared 40- mL
VOA
vials containing 5
mL water19,22
48
hours
iced/14
days
frozen20
NA
NA
NA
NA
NA
NA
Volatile Organics
Method 5035A
-7 to -20°C
5 g (x3)18
into tared
40- mL VOA
vin1cl'» 22
14 days
frozen
NA
NA
NA
NA
NA
NA
Volatile Organics
Method 5035A
-7 to -20°C
5 g (x3)18
into tared
40- mL VOA
vials containing 5
mL water19,22
14 days
frozen
NA
NA
NA
NA
NA
NA
Volatile Organics
Method 5035A
Ice-4°C
5 g (x3) into tared
40-mL VOA vials
containing
5 mL
methanol19
14 days
NA
NA
NA
NA
NA
NA
Volatile Oiganics
no residual chlorine
present
NA
NA
Ice^°C
40 mL (x3)ls
G/S
7 days
NA
NA
NA
NA
Volatile Organics
no residual chlorine
present
NA
NA
0.2 mL 1+1 HCL
(pH<2), Ice-4°C 40
mL (x3)ls G/S
14 days
NA
NA
NA
NA
Volatile Oiganics
residual chlorine
present
NA
NA
3mg Na2S203, 0.2
mL 1+1 HC1
(pH<2), Ice-4°C
40 mL (x3)15G/S
14 days23
NA
NA
NA
NA
Volatile Oiganics
TCLP
Ice-4°C
2 oz G
28 days24
NA
Ice 4°C
40 mL (x3)lsG/S
NA
28 days24
Ice-4°C
8 oz G26
If <10%
solids, 4x
Boz G
28 days24
NA
NA
Volatile Oiganics
in Air
Preservation: closed,
leak fiee valve with
tightened cap.
Amount: preferably
10 to 14psia
Container:
passivated 6-liter
canister
General Notes:
NA = Not applicable
Pres = Preservation Immed = Immediate
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Footnotes:
1 ASB's policy is that where the sample preservation is specified at 4°C, the acceptable temperature range for samples during shipping and
storage is from above the freezing point of water to 6°C.
2
Consult 40 CFR Part 136 Table II: Required Containers, Preservation Techniques, and Holding Times for latest NPDES requirements.
3 Preservatives:
Tee - Sufficient ice must be placed in the shipping/transport container to ensure ice is still present when the samples are received at
the lab. HC1HCL- Hydrochloric Acid used as a preservative must be present at concentrations < 0.04% by weight (pH about 1.96 or
greater) as specified in 40 CFR 136.3, Table II, footnote 3. The proper amount of HQ is added to the sample container at the
laboratory prior to sampling.
HiSO< - Sulfuric Acid used as a preservative must be present at concentrations < 0.35% by weight (pH about 1.15 or greater), as
specified in 40 CFR 136.3, Table n, footnote 3.
NaOH - Sodium Hydroxide) used as a preservative must be present at concentrations <0.080% by weight (pH about 12.30 or
less), as specified in 40 CFR 136.3, Table n, footnote 3.
HNOi - Nitric Acid used as a preservative must be present at concentrations < 0.15% by weight (pH about 1.62 or greater), as
specified in 40 CFR 136.3, Table n, footnote 3.
Chromium VI buffer - A concentrated buffer is used to extend the holding time for hexavalent chromium samples from 24 hours to
28 days and uses constituents as allowed by EPA guidance found at: http://water.eDa.eov/scitech/methods/cwa/auestions-cr6.cfln.
The sample preservation buffer is prepared by carefully dissolving 330 g ammonium sulfate and 50 g sodium hydroxide in about 500
mL of deionized water. The solution is allowed to cool and 260 mL of 29% ammonium hydroxide is added and solution is diluted
with deionized water to a final volume of 1L. In house studies revealed that the equivalent of 1% of buffer volume is needed to
preserve samples to attain the pH range (pH 9.3 to 9.7,10 mL buffer for a 1 L sample) as specified in 40 CFR 136.3 Table IL Adding
preservative to sample bottles prior to shipment to the field is recommended to minimize sampler contact with the buffer.
NA - Not Applicable. No sample preservation is required.
4 Amount: The amounts listed must be considered approximate requirements that are appropriate for most media. If a particular medium
to be sampled is very light, more sample volume may be required to obtain the necessary mass for the analysis.
s Container Type:
G = Glass
P = Polyethylene
FP = Fluoropolymer
E = Coring device
C = Cubitainer
S = Septum Seal
A = Amber
W = Whirl-Pak ™
GF/F = Glass Fiber Filter PP = Polypropylene
6 Holding Time - Stated in days unless marked otherwise. A holding time of "immed" (immediate), indicates that the sample is to be
analyzed within 15 minutes (40 CFR 136 Table II). "Not Specified" indicates no holding time is specified in the method or by the
relatedprogram.
7Chromium VI (hexavalent) -1 month until extraction, 4 days to analysis of extract. Store at 4"2°C until analyzed (SW-846, Table 3-1).
8 Use ascorbic acid only if the sample contains residual chlorine. To test for residual chlorine, place a drop of sample on potassium iodide-
starch test paper. If the test paper turns blue, residual chlorine is present. Add a few crystals of ascorbic acid and re-test until the paper no
longer turns blue. Add an additional 0.6 grams of ascorbic acid for each liter of sample.
9 Filter on-site. Use 0.45 |im-filter for dissolved parameters.
10 TCLP Mercury - 56 days: 28 days to TCLP extraction plus 28 days to analysis of extract (SW-846, Method 1311, Section 8.5).
11 TCLP Metals - 360 days: 180 days to TCLP extraction plus 180 days to analysis of extract (SW-846, Method 1311, Section 8.5).
12
pH - Aqueous RCRA samples only - a 24-hour holding time from receipt is allowed.
13 TCLP Extractables - 61 days: 14 days to TCLP extraction, 7 days to solvent extraction, 40 days to analysis of extract (SW-846, Method
1311, Section 8.5).
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14 Extractables - 54 days: 14 days to extraction, 40 days to analysis of extract (SW-846, Table 4-1).
15 Collect double volume for MS/MSD analyses at one station per 20 or one per project if < 20 samples in project or Sample Delivery
Group (SDG).
16 Extractables, water, no residual chlorine present - 47 days: 7 days to solvent extraction, 40 days to analysis of extract (SW-846, Table 4-1).
17 Extractables - Drinking water, residual chlorine present: 14 days to extraction, 30 days to analysis of extract (EPA525.2).
IS
Collect triple volume (9 vials) for MS/MSD analyses at one station per 20 samples or one per project if <20 samples in project or SDG.
19 Volatile Organics Soil Samples - A separate 2-ounce glass container or 40-mL vial is needed in order to determine percent solids
for soil samples. Alternatively, an extra coring device will suffice. Do not freeze percent solids container!!
20 Volatile Organics Soil Samples - Contents of coring device must be analyzed or transferred to VOA vial containing organic-free water
and preserved within 48 hours. Preservation is accomplished by sealing and freezing the VOA vial. The sample must be analyzed
within 14 days of collection date. Soil samples received in VOA vials must be analyzed within 48 hours or frozen and analyzed within
14 days of collection date. Refer to Method 5035A, July 2002, Table A1 for additional details.
21 Wastes are dissolved in methanol at the analytical lab.
22 One 40-mL vial should be empty so that a methanol extraction can be performed if a high-level VOA is needed. Alternately, one tared
40-mL vial may contain 5 mL methanol.
23 Volatile Organics Waters -14 days for acid preserved, 7 days if not preserved (40 CFR136 Table II).
24 TCLP Volatile Organics - 28 days: 14 days to TCLP extraction plus 14 days to analysis of extract, or 7 days to analysis of
extract if not preserved following extraction.
25 Collect in 50-mL plastic centrifuge tube. Keep sample in the dark. Freeze for up to 24 days.
26 Waste samples collected for volatile analysis are transported in secondary containment.
27 Perfluorocarbons - Water: 14 days to preparation, 180 days to analysis of extract.
28 Sampled to analyzed
29 Holding time for routine mercury by Method 200.8, is 28 days from sample collection to digestion and 28 days from digestion to analysis.
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CHAPTER 4
General Laboratory Practices
4.1 Good Laboratory Practices
4.1.1 Policy Following good laboratory practices in all aspects of the organization's
operations is intrinsic to the production of quality analytical data. Recognizing the
necessity of maintaining control over general laboratory operations, the subsequent
sections outline provisions for maintaining quality in all laboratory practices and
procedures.
4.1.2 Corrections to Records
4.1.2.1 Corrections to hardcopy records shall be made using a single line-out with
the date and the signature or initials of the analyst making the corrections. No
changes shall be made with any technique that obliterates the original such as
erasures or correction fluid. All records and corrections shall be in ink. Pencil shall
not be used on analytical records. When corrections are due to reasons other than
transcription errors, the reason for the correction shall be documented.
4.1.2.2 Corrections to final data must be done by reprinting and re-transmitting
through Element®, the final data report forms with the corrected results. Corrected
results shall be transmitted with a case narrative explanation that the report is to
correct data previously reported. The original report name should be included in the
case narrative. An official copy of all corrected data, along with the original data,
must be retained in the project file and must contain clear documentation as to why
the corrections were necessary.
4.1.3 Following SOPs/LOQAM It is the policy of the ASB that the laboratory's SOPs
and LOQAM be followed by all ASB staff and by ESAT contractors. Documentation
will be maintained in each employee's training file that he/she has read, understood and
agreed to follow the latest version of SOPs and LOQAM. Significant deviations from
the LOQAM or SOPs shall be coordinated with the appropriate Section Chief, Branch
Chief (if necessary) and Laboratory Quality Manager (LQM); the rationale for the
deviation shall be clearly documented and included in the project file. When it is
determined prior to receipt of samples that standard procedures will need to be modified
for a specific project, these proposed deviations will be documented in R4LIMS project
notes for review by the project leader.
4.1.4 Method Modifications Method modifications, where allowed by regulation, are
encouraged as new technologies are developed which result in analytical efficiencies,
pollution prevention and increased precision and accuracy. Restrictions apply to the
modification of Safe Drinking Water Act (SDWA) and National Pollutant Discharge
Elimination System (NPDES) methods. Methodology in support of the Safe Drinking
Water Act (40 CFR Part 141) shall not be modified unless specified in the individual
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method. Permitted modifications are documented in memos from OGWDW or approval
as an Alternate Test Procedure (ATP). When these modifications are used, ASB's SOP
should state that an allowed modification is being utilized, and reference the specific
memo allowing the modification.
4.1.5 Manual Peak Integration Some of the analytical techniques utilized by ASB
employ a chromatogram that displays time versus signal, which when integrated,
provides an area count that is used to calculate concentration of a target analyte.
4.1.5.1 Analysts are required to review the automated electronic data processing
(i.e., integration) for accuracy and consistency with appropriate data reduction
techniques. Some electronic reductions can result in incorrect actions by the system
software, and for these instances a manual override and correction of the electronic
processing is appropriate. Examples of this may be such items as integration of an
incorrect peak or misplacement of the baseline in peak integration due to poor peak
shape or interferences. Guidance related to manual integrations is documented in
individual workgroup Data Review Guidelines or technical SOPs. When a manual
override of the electronic process is performed, most of the current commercially
available software packages provides an automated notation on the quantitation
report showing that a modification to a peak occurred. When a manual modification
of a peak occurs, the analyst shall provide documentation for the file to include a
hard-copy representation of the before and after correction, the action taken and
why. The action should be concurred by the Secondary Review Analyst or Section
Chief, and include an initial and date of the review of the modification on the data
review form. Manual override actions are appropriate only to correct inaccuracies
and shall be done in accordance with sound analytical procedures. The software
option for denoting a manual integration in the quantitation report must always be
activated. There shall be no manipulation of the software to conceal an electronic
correction that is used to report results.
4.1.6 Checklists-Primary Analyst/Secondary Analyst Review Analytical data
reduction activities for both the primary analysis and the secondary review shall be
documented using the appropriate data review checklist. Checklists are designed for the
procedure(s) being performed. The individual data review checklists for organic and
inorganic analyses are maintained on SESD's local area network drive (LAN) as
controlled documents.
4.2 Document Control/File Management
4.2.1 It is the policy of ASB to maintain complete and accurate records which document
all laboratory activities in a readily accessible and understandable manner. These
records shall include, but are not limited to: equipment identifier, analytical methods
and related activities such as sample receipt, preparation, data verification and transfer
of custody. Additionally, it is the policy of ASB that all documents issued as part of
ASB's Quality System shall be controlled in the following way.
4.2.1.1 All documents are reviewed and approved by an authorized approving
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official prior to being issued. Approving officials are Section Chiefs, Branch Chief
or the LQM. The SESD Deputy Director serves as the approving official for all
SESD quality system documents.
4.2.1.2 Authorized revisions shall be available to all personnel at the point-of-use.
4.2.1.3 A master list shall be maintained which identifies the current
revision (or equivalent) and its distribution status.
4.2.1.4 Documents shall be periodically reviewed for suitability or needed revisions.
4.2.1.5 Obsolete documents shall be removed from the point(s)-of-issue (or
marked as obsolete).
4.2.1.6 SOPs that are expired, but have not been updated or reviewed will stay in
effect until the new version is effective.
4.2.1.7 Archived documents shall be marked as such.
4.2.1.8 ASB's procedures for document control are detailed in SESDPROC-
1000- Document Control.
4.2.2 Internal Chain-of-Custody (COC) ASB analysts check samples in/out of the
Custody Room or designated storage location through Element® (see SOP ASB 105G).
Custody of extracts and digestates are tracked on Element® - generated bench sheets,
which are included in the project file.
4.2.3 COC Receipt Form The sample custodian/designee receives a COC record
from the field samplers with every shipment of samples (see ASB SOP 105G).
4.2.4 Instrument/Maintenance/Analysis/Preparation Logbooks Each analysis area
maintains records using logbooks which are kept within the laboratory work areas when
active or in the appropriate records archive. All entries in instrument, sample
preparation and other logs are made legibly in ink at the time of the observation or
performance of the operation. When full, these logbooks shall be archived using the
appropriate form and given to the LQM. The logbooks will be transferred to the SESD
Records Room. If a logbook is discontinued prior to using all the pre-printed pages, a
single line shall be drawn through the first vacant page and a note added stating that the
logbook has been discontinued. This note shall be dated and initialed by the analyst.
4.2.4.1 Instrument/Analysis Logbooks Instrument logs shall indicate the
unique instrument ID, date of analysis, analyst and samples which have been
analyzed. The logbook shall contain or reference a record of which options or
analytical conditions were used for analysis. Where appropriate, instrument
acceptance criteria (e.g., tune criteria, sensitivity checks) should be noted in the
logbook. Electronic records, including spreadsheets which contain original
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measurements, may be used to create logbooks if all the required information
can be captured by the instrumental software; however, a sequential analysis log
must still be created and maintained. This is accomplished by printing a copy of
the electronic record and including it in a notebook. These sequential logs must
also include failed runs, or sequences which were abandoned prior to
completion. When a pre-determined number of pages has been accumulated
(e.g., 50 pages), the individual records are combined into a single bound
logbook and retained as specified above. Any electronic records must accurately
reflect actual analytical information. For analyses with holding times <72
hours, or when time-critical or method-specified times are included in the
analysis, the time of analysis must also be recorded.
4.2.4.2 Preparation Logbooks Preparation logs shall document all information to
reconstruct the preparation of samples, reagents, and standards, and should include,
but not limited to: weights, volumes, lot number of digestion tubes, balance used,
weights used, reagents/standards used, preservation checks, units and any cleanup
procedures. Electronic traceability via Element® is an acceptable option for
documentingstandard preparation. If Element® is used as the standard prep log, it is
subject to all the requirements of this section.
4.2.4.3 Instrument Maintenance Logbooks Each major instrument shall have a
maintenance logbook. At a minimum, instrument serial number, software version,
in- service date (if known) and unique name shall be included in the log.
Maintenance, service and repair records are maintained in these logbooks.
Preventive maintenance schedules should be noted in the log, or in a separate
maintenance log. Active logbooks are maintained within the laboratory where the
instrument is located and should be maintained with the instrument throughout its
useful life. At such time the instrument is removed from service the logbook is
transferred with the appropriate form to the LQM, and then to the SESD Records
Room. When a service or maintenance call is completed by the vendor, the analyst
should place a copy of the documentation or transcribe the details for the work that
was performed on the instrument in the logbook. The original work order invoice
should be provided to the Program Support Section for payment.
4.2.4.4 Other Some analytical methods are manual and do not use analytical
instrumentation to generate a result (e.g., solids). For these methods, ASB relies on
spreadsheets or other calculating software for recording/documenting original
observations made, such as weights. All spreadsheets or other calculating software
used within ASB as logbooks or used in support of data generation will be validated
and controlled. All cells, except informational input cells, will be locked to prevent
alteration of a formula or essential static information, such as the unique identifier.
The entire spreadsheet will be password-protected. The password will be assigned by
the LQM at the time of posting. Copies of any spreadsheet used must be obtained
from the password protected official, posted version on the LAN. Prior to posting
and use, all calculations in spreadsheets will be hand-validated by the responsible
party and submitted through the Section Chief to the LQM for approval and posting.
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4.2.5 ASB Laboratory Operations and Quality Assurance Manual The most
current version of the ASB LOQAM is maintained electronically by the LQM. The
manual is available to all EPA and ESAT staff as "read-only" on the LAN at
K:\ASB\Current Documents\QA Manual. While hard copies of the manual may be
printed, it is the responsibility of each individual to ensure that they are using the most
current version. The ASB LOQAM shall be maintained as described below.
4.2.5.1 The quality manual will be reviewed in total at least once each year. The
Section Chiefs will solicit feedback from their section and incorporate all changes
into the proposed version, which is reviewed by management and the LQM. The
annual total review of the manual shall be completed as near as possible to the
anniversary of the most recent fully reviewed manual date.
4.2.5.2 The annual review and versions of less comprehensive reviews, as described
in section 4.2.5.3 below, that are in use for any given period of time will be tracked
by date. Revisions resulting from less than total review of the manual do not reset
the annual review clock. The next full review shall commence at an appropriate date in
order to maintain the annual full review schedule described in section 4.2.5.1 above.
4.2.5.3 To keep the manual as up to date as possible, changes may be made at any
time deemed appropriate during the calendar year. When this occurs, the redline
strikeout version of the manual will be kept as a record of the changes. The original
signed copy will be maintained by the LQM. Signatories for the change
authorization will be Organic and Inorganic Section Chiefs, LQM, and the Branch
Chief. The effective date of the change will be the signature date of the Branch
Chief.
4.2.6 Standard Operations Procedures/Methods SOPs shall be written based on
agency guidance EPAQA/G-6 "Guidance for the Preparation of Standard Operating
Procedures for Quality Related Documents". Detailed policies and procedures for the
preparation, review and change of both administrative and technical SOPs are found in
SESDPROC-lOO-Document Control. Technical SOPs for the various methods in use in
each laboratory may be placed within the laboratory for reference purposes; however,
the official copy of each SOP resides on the LAN in the K:\ASB\Current
Documents\SOPs folder.
4.2.7 Project Files
4.2.7.1 A project file is all pertinent information and documentation related to a
group of samples that are associated with a unique identifier (project number)
assigned by the division's R4LEMS software. Each analytical project has a "project
file" which contains when possible, originals of all the information. In some
instances, such as bound logbooks, it will be necessary to make copies; however, it
is essential that the copy placed in the file be the exact copy of the original.
4.2.7.2 The project file contains all data (or copies thereof) used to produce the final
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data report. For example, if an analytical run is not used because of a calibration
failure, it need not be retained in the project file. However, if the failed run was
used to determine the level of dilution required by a sample in the final run, it
should be maintained. See SOP ASB 118G for the required elements needed for a
complete project file.
4.2.7.3 If corrections are deemed necessary to original project file documents after
the project file has been completed, the primary analyst or data reporter will ensure
that a copy of the corrected documents are placed in the file. If the final data
reports, either in part or in total, must be corrected or clarified and reported again, a
new final report shall be generated for transmittal of the correction, explaining the
nature of the correction and placed into the project file along with the corrected
data.
4.2.7.4 The analytical information is maintained by analysts while the analyses are
in progress. Each completed data packet is transferred to the secondary reviewer for
review, submitted to the Section Chief or designee for final reporting, and
ultimately transferred to the SESD records room for inclusion into the project file. It
is absolutely essential that the hard copies placed into project files exactly reflect
the electronic data produced for the project. Forensic accreditation policy requires
that the complete project file to be paginated, therefore ASB includes an inventory
checklist that accounts for each page of the project file. It is agency policy that hard copy
project files are the official record and e-data files are not required to be maintained.
Ultimate retention and disposal of all records will be in accordance with Agency record
management rules and regulations as detailed in the "Records Management Standard
Operating Procedures, Science and Ecosystem Support Division."
NOTE: While data work-up is in progress, raw data may be logged out of the
SESD facility for review at a teleworking location. A log will be maintained in the
project file indicating which data package(s) were removed from the SESD
facility, the responsible party and the return date. Under no circumstances will
any portion of a project file be removed from the SESD facility for teleworking
purposes after the data has been reported, unless authorized by the Branch Chief.
If any data is maintained in electronic-only format (such as PDF), it shall be stored
to allow retrieval of the information for at least five years after completion of the
project. Any software supporting electronic-only data must be also available for the
same period of time, even if the software/instrumentation has been removed from
routine service.
4.2.8 Confidentiality of Data
4.2.8.1 ASB does not, under normal operations, accept samples considered to
require the use of Confidential Business Information (CBI) procedures. Therefore,
most of the information generated by ASB is accessible under the Freedom of
Information Act (FOIA). The exception is data from all criminal investigation
projects; it is not subject to release and will not be reported to anyone other than
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project managers leading the criminal investigations or to individuals that are
authorized by ASB management. Criminal projects are so noted when logged into
R4LIMS.
4.2.8.2 Data transmittal memos contain a confidentiality notice stating the data is
only for the use of the specific individual addressee(s). ASB does not release data to
anyone other than the project manager or those approved by the project manager to
receive results.
4.2.9 General Correspondence All general written correspondence (e.g., memos,
letters) from ASB technical staff to any party external to ASB, but internal to SESD
shall be reviewed and approved by the respective section chief and shall have the
section chief as a "THRU" signatory. All correspondence external to the Division shall
also include the Branch Chief as a "THRU" signatory. Correspondence related to a
specific project shall be filed in the project file. General correspondence shall be
forwarded to the LQM for filing according to the ASB Divisional File Plan.
4.2.10 Training Files A training file shall be maintained for each ASB and contract
staff member by the LQM. The file shall contain all training documentation, including
conference and seminar participation. Training files may be maintained in hard copy,
electronic format, or a combination of both. Refer to SESDPROC-1003.
4.2.11 QA/QC Records ASB maintains project specific records in the project file.
Proficiency records, method development records and managerial reports are
examples of QA/QC records maintained by the LQM Refer to SESDPROC-1001.
4.2.12 Document/Forms Revisions Many forms and documents (e.g., SOPs, data
review check lists, extraction/preparation log forms, etc.) are generated within ASB
and handled as controlled documents. All forms will be controlled by the LQM, or
designee in the appropriate subdirectory on the LAN at K:\ASB\Current
DocumentsYFormsV These forms shall be reviewed and revised as necessary at the
same frequency detailed in SESDPROC-IOOO. Changes to controlled forms are
authorized by the Branch Chief or Section Chiefs by sending an email to the LQM
denoting approval and with a copy of the changes. The LQM also has the ability to
approve branch related forms for posting on the LAN. The LQM, or designee is
responsible for posting the modified and approved form to the LAN, and to notify all
appropriate staff. It is the responsibility of each staff memberto ensure the current
version as listed on the K: drive is being used. Specific document control procedures
are detailed in SESDPROC-IOOO.
4.2.13 Records Management/Disposition ASB records will be managed in
accordance with the Records Management Standard Operating Procedures of the
Science and Ecosystem Support Division. In the event that the SESD and ASB
organizations are eliminated, all records would be maintained as required by U.S.
government regulations for records retention in force at the time of the discontinuation.
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4.3 Laboratory Apparatus and Instruments
4.3.1 General Policy It is the policy of ASB that all laboratory apparatus and
instruments meet or exceed any method-specified tolerances to ensure results are
reported within acceptable uncertainty levels. Environmental Management System goals
(e.g., reduction in chemical use or more energy efficiency) should be considered when
evaluating new equipment for purchase, but may not always be the deciding factors. All
equipment will be determined to be clean, free of contaminants and operational and will
be calibrated prior to use as per manufacturer's instruction or procedures detailed in the
technical SOPs. If any equipment becomes defective or is suspected of being defective,
it will either be removed from the work area or marked as out-of-service. The defective
equipment will be separated from equipment currently in use. Equipment will be utilized
by authorized personnel and user manuals will be available for review either in
electronic or hard copy formats. In general, all ASB laboratory apparatus and
instruments remain under the control of ASB at all times. However, if equipment leaves
the direct control of ASB (e.g., loaned to another agency), it shall be verified to be
operating properly prior to being placed back into service at ASB. SESDPROC-1009
details equipment management procedures.
4.3.2 Incubators Each incubator within ASB will be monitored by an automatic
temperature recorder.
4.3.3 Water Baths Monitor and record temperature in the preparation and or analysis
log at least once each working day while in use or as specified by the published method
or technical SOP. Verification of operation within the correct temperature range maybe
documented in an alternate fashion if it can be demonstrated that the unit did not exceed its
minimum or maximum permissible level (e.g., with a min/max temperature record). Drain and
clean water baths periodically as recommended by manufacturer, by methods or by accepted
practice. Be sure to check temperature variations when water baths are loaded to capacity and
document this check in the preparation/analysis log or temperature log, whichever is
appropriate. When an automatic temperature recorder is used, it is designated as the official
record; any other thermometers in use are for convenient quick checks.
4.3.4 Refrigerators/Freezers/Drying Ovens
4.3.4.1 Check and document the temperature each working day that the refrigerator,
freezer or drying oven is "in use". "In use" shall be defined as when the unit
contains materials for which a specified temperature is required by method, policy,
or procedure. Verification of operation within the correct temperature range may be
documented in an alternate fashion if it can be demonstrated that the unit does not
exceed its minimum or maximum permissible level (e.g., with a min/max
temperature record). If a unit is not being used for this purpose, it should be so
noted in the temperature record log and daily checks will not be necessary. If a
piece of equipment never requires temperature checks, a sign will be placed on the
unit stating it isn't used for maintaining required temperatures. In order to place a
unit back into use, a current temperature measurement must be taken for verification
that it is at the proper temperature. This must be documented in the temperature
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recording log indicating that the unit has been placed back into active service and
daily checks must resume. Alternatively, temperature checks for an apparatus which
is not used on a daily basis (e.g., drying ovens for percent moisture determinations)
may be recorded directly into analysis log(s). When an automatic temperature
recorder is used, it is designated as the official record; any other thermometers in
use are for convenient quick checks.
4.3.4.2 Due to the relatively small volume of refrigerators, freezers and ovens it is
expected that the units will go outside of normal operating temperatures for a period
of time after loading, unloading or other activities where the door may be open to
the ambient environment. Additionally, freezers may undergo defrost cycles where
the temperature is above the maximum for a period of time during the cycle. These
deviations are unavoidable and will not trigger an out-of-control situation. To
account for these normal temperature variations, a recovery time of 45 minutes is
allowed for units equipped with automatic temperature recording devices.
Exceedances lasting longer than 45 minutes will trigger an alert which will require
evaluation and potential corrective action. The evaluation will include consideration
of the material under temperature control, as well as the intent of the temperature
control. For example, while a method or manufacturer may include instructions for
refrigeration of the material, it is recognized that the material is usually shipped at
ambient temperature, brought to room temperature before use and/or left on
autosamplers at room temperature for several hours before analysis. In these cases, it
is obviously the intent of the refrigeration requirement to maintain a colder than
ambient temperature for long term storage to prevent degradation over time rather
than to maintain a specific temperature for all times. As such, temperature
exceedances for these types of materials would be allowed as long as the device
returns to normal operating temperature. Temperature exceedances will be
monitored for trends to indicate whether a device requires service or replacement.
4.3.4.3 Outdated materials in refrigerators and/or freezers are properly disposed of
when no longer needed.
4.3.4.4 Do not store food in any laboratory refrigerator or freezer. Drying ovens
should never be used to warm food or for drying eating utensils.
4.3.5 Autoclaves
4.3.5.1 Check and document the temperature each time the unit is in use
and/or as required in the published methods or technical SOPs.
4.3.5.2 At a minimum, record the date, sterilization time, and temperature for each cycle.
4.3.6 Balances A list of ASB balances and the unique identification assigned to each
balance is located on the LAN. All balances are serviced/calibrated annually (± 30
days).
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4.3.6.1 Accuracy Balance accuracy shall be validated with NIST-traceable weights
at the time of use, or on the same day of use, against the following criteria.
4.3.6.1.1 Method-or SOP-specified criteria take precedence over other criteria.
4.3.6.1.2 If a method specifies the accuracy of a balance to be used in the
procedure, (e.g. a balance capable of weighing to the nearest 0.01 g), the
accuracy check at the time of use should be within ±1 in the final place. The
accuracy check should bracket the targeted weight of the material being
weighed.
4.3.6.1.3 In the absence of method specified accuracy criteria, the accuracy
of the balance at the time of use should meet the criteria stated in
SESDPROC-1011, Equipment Certifications.
4.3.6.1.4 The unique identification of the balance and the check weight
shall be documented for each weighing.
4.3.6.2 Verification The verification should be documented in the appropriate
analysis log. Weights are verified annually and should meet the specifications
stated in SESDPROC-1011. This is required on an annual basis with re-
certification coordinated by the LQM.
4.3.6.3 Maintenance Clean and level balances as required and continue annual
maintenance services contract and records of the maintenance performed.
Analytical balances should be used in areas that are subjected to minimal
vibrations or influences from static electricity as appropriate.
4.3.7 Thermometers Unless otherwise specified by regulatory methodology, it is the
policy of ASB to use only non-mercury containing thermometers in all laboratory
operations. All thermometers used within ASB will be NIST-traceable. Certification of
thermometers is required on an annual basis and re-certification is coordinated by the
LQM as detailed in SESDPROC-1011. Analytical equipment with built-in
thermometers will have a specific procedure outlined in SESDPROC-1011 following
the manufacturers' instructions for performing the calibration.
4.3.8 Mechanical Dispensing Devices
4.3.8.1 Mechanical volumetric dispensing devices (except Class A glassware) shall
be checked for accuracy on an annual basis. Glass (iL syringes are exempt from this
requirement; however, syringes used for volumetric dispensation must have been
demonstrated for accuracy as documented by the manufacturer. Acceptance criteria
are located in SESD-PROC-1011.
4.3.8.2 Autotitrator dispensing accuracy is verified through analytical quality
control samples (e.g., laboratory control sample) and are not checked as mechanical
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dispensing devices. The liquid is dispensed in microliter quantities and are too small
to be accurately checked gravimetrically.
4.3.9 Records of NIST Traceability
4.3.9.1 Records of NIST-traceability for thermometers, weights, and mechanical
dispensing devices (as applicable) shall be maintained by the LQM. All staff
members are responsible for ensuring that they coordinate with the LQM each time
new supplies for these items are ordered and/or any time a recertification of any of
these items occurs. Staff will ensure that the LQM is furnished originals of any
documentation received with new purchases or recertification. The accuracy of
check weights and thermometers is verified on an annual basis using NIST-
traceable reference standards.
4.3.9.2 Records received from the vendor will be retained for all standards to ensure
traceability and to keep relevant information intact. These records include the
vendor, Certificate of Analysis (CO A), date of receipt, any recommended storage
conditions, expiration date and a cross reference to the Element® ID assigned to the
standard. CO As for purchased standards are maintained in individual laboratories
for a minimum of five years after the date of last use.
4.3.9.3 ASB will maintain vendor certificates verifying suitability of use (i.e.
cleanliness and volume) of products. For examples, digestion tubes and GC vial
CO As will be maintained in a binder in individual laboratories or similar manner.
4.3.10 Major Instrumentation
4.3.10.1 Major instrumentation includes, but is not limited to, the Inductively Coupled
Plasma; ICP/Mass Spectrometer (ICP/MS); Gas Chromatograph/Mass Spectrometer
(GC/MS); Gas Chromatograph (GC); Liquid Chromatograph/Mass Spectrometer/Mass
Spectrometer (LC/MS/MS); Ion Chromatograph (IC), Mercury analyzers, Auto-
analyzers; Accelerated Solvent Extractors; Gel Permeation Chromatography (GPC).
4.3.10.2 Major instrumentation shall be maintained in accordance with
manufacturers' recommendations and operational guidance. Maintenance records
shall be kept updated on each instrument. Additional details on maintenance,
calibration and troubleshooting procedures are contained in technical SOPs.
4.3.10.3 A list of all major instrumentation, including unique IDs, is maintained
by the LQM on the LAN.
4.4 Laboratory Supplies
4.4.1 General
4.4.1.1 Laboratory supplies shall be maintained in an uncluttered, clean, and
organized fashion. Supplies are monitored so that they are ordered before depletion
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occurs which could cause work stoppages due to lack of supplies routinely kept in
the laboratory. Supplies are pre-screened for suitability of use as detailed in ASB
SOP 122G-Screening of Supplies.
4.4.1.2 Contract personnel cannot order supplies with EPA funds, but are still
responsible for monitoring supplies that they use. Contractors may fill out an order
form and submit it to an EPA staff member or Section Chief. Alternatively, if it is
customary in a work area to maintain a list of supplies needing to be purchased (a
list that is monitored by EPA personnel) the contractor may use this avenue for
ordering supplies as needed.
4.4.1.3 A list of suppliers that have furnished acceptable supplies and services is
maintained by the LQM, or designee on the LAN. Additional vendors may be added
to this list if their supplies and services prove to be acceptable. The approved
supplier list is evaluated quarterly, accreditations dates are updated, first-time use
updated, unacceptable supplies noted and suppliers removed from the list, etc.
Supply vendors that maintain ISO accreditation (and meet Guide 34 requirements for
reference material producers) are placed on the acceptable supply list unless previous
experience with the supplier has been unacceptable.
4.4.2 Labware
4.4.2.1 Labware used in laboratory operations must be high quality borosilicate
glass, polymethylpentene, or Nalgene™ (Plastic). Volumetric Labware must be
Class "A" quality.
4.4.2.2 Labware shall be cleaned in accordance with individual SOPs and
manufacturer's instructions.
4.4.2.3 If a new washing compound or cleaning application is instituted within
the laboratory, tests shall be performed to ensure that the labware is free of
interferences before placement in service.
4.4.3 Chemicals, Reagents, Solvents, Standards, Gases
4.4.3.1 The quality of chemicals, reagents, solvents and gases is determined by the
sensitivity and specificity of the methods being used. Grades of materials for
analyses of lesser purity than specified by a method will not be used. When specific
grades of materials are not specified by the method, analytical reagent grade
materials should be used. ASB will purchase standards from vendors with ISO
17025 and Guide 34 accreditation, if possible.
4.4.3.1.1 Suitability of routine reagents is documented through method blanks.
A clean method blank documents that all reagents used in the associated batch
are suitable for use. A contaminated method blank requires technical corrective
action to determine whether the contamination is the result of unsuitable
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reagents, analytical system, or contamination introduced in the sample handling
process.
4.4.3.1.2 Records shall be maintained to document the purity of any material
requiring additional verification of its suitability for use in a test method
(e.g., suitability of acid for ultra-trace mercury analysis). Hard copies of
Certificates of Analysis are kept in a binder in the laboratory for five years
after the expiration or consumption of the material.
4.4.3.1.3 If any consumables, supplies or services evaluated through the above
procedures prove to be unsuitable for use, the personnel making that
determination shall document the issue in an email to the LQM. The
documentation should include a description of the item, the deficiency and the
vendor. Where possible, a copy of the purchase request should be transmitted to
the LQM. The LQM, or designee, will compile all occurrences of unsuitable
consumables, supplies or services and determine what further action may be
necessary.
4.4.3.2 Reagents, chemicals, solvents, and standard reference materials (excluding
high- demand items) should be purchased in small quantities to minimize extended
shelf- storage past its expiration date.
4.4.3.3 All reagents, chemicals, solvents, and standard reference materials should
be labeled with a received, opened and/or prepared date, and discarded when
expired, or when evidence of deterioration is detected. All standards received will
be entered into Element® for tracking purposes.
4.4.3.3.1 All materials should have an expiration date recorded on the original
container. For those materials received without a manufacturer's expiration date,
an expiration date of 1 year from the date the container was initially opened will
be applied to these materials; however, they should be monitored for
deterioration and replaced if evidence of deterioration or contamination is
present. Unopened containers will be evaluated based on the date the container is
opened.
4.4.3.3.2 Materials prepared and used within the same day (or discarded the
same day as prepared) are required to have identification of the contents on the
container and HMIS labeling. Expiration dates may be documented on the
container similarto 'Expires Daily' or 'Expires Today'.
4.4.3.3.3 Intermediate materials that are immediately consumed or promptly
added to another labeled container do not need any identification. These
intermediate preparations must be labeled if they are not consumed or added to
the labeled container within 15 minutes of the preparation of the intermediate.
The personnel making these intermediate preparations must have possession of
the material and must label it if he or she leaves the material unattended. The use
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of an intermediate standard or material to prepare a working standard or material
must be documented in the appropriate preparation logbook or Element®.
4.4.3.3.4 Records shall be maintained on reagent, standard and reference
material preparation. These records shall indicate traceability to purchased stocks
or neat materials, reference to the method of preparation, date of preparation,
expiration date and preparer's initials. A unique ID shall be assigned to each
prepared reagent and standard. Procedures for achieving traceability are
documented either in the individual method SOPs or stand-alone documents for
procedures which may apply across a variety of methods. The unique ID and
expiration date shall be recorded on each standard, reference material and
reagent container. A cross-reference to the Element® ID shall be recorded in
standard preparation records and on the Certificate of Analysis.
Note: Reagents which are not deemed critical to the success of the analysis, ones
which do not contribute to the quality of the test, do not have to be tracked. For
example, acids and solvents used in rinsing glassware prior to use typically
would not require reagent traceability.
4.4.3.3.5 Expired Stock Standard It is ASB's policy to allow for reverification
of analytical standards as described below. Verification of an expired material
will be performed by comparison with the same material from a second source
that is within the original vendor supplied expiration date. (Materials may also be
verified prior to expiration.) Successful verification must be documented on the
standard container and certificate of analysis by crossing through the vendor
assigned expiration date, assigning a new expiration date one year from the date
of verification, and adding the initials of the person who performed the
verification. Depending on the size of the container and label there may not be
room to add a new expiration date along with initials. In those cases, it may be
necessary to add an additional sticker or label (firmly secured) with the new
expiration date clearly marked. It is not necessary for a complete history of
expiration dates to be on the container itself. The certificate of analysis (CO A)
must also include the new recertification date, the analyst's initials, the analysis
with which the standard was recertified (i.e., the project number or other analysis
identification) and the initials of the Section Chief or LQM to show he or she
reviewed the verification information and concurs that the material is still stable.
The COA must show a complete history of all recertifications. The revised COA
is rescanned into Element®.
Note: Reagents, including purchased concentrated acids, may be recertified
following the procedure described above.
4.4.3.3.6 Acceptance Criteria for Verifying Expired Calibration Standards
The stability of the expired calibration standard is considered to be verified if:
4.4.3.3.6.1 The ICAL prepared using the expired standard meets method
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acceptance criteria and
4.4.3.3.6.2 A calibration check standard prepared from a second-source that
has not exceeded expiration meets the Calibration Verification Check
standard (ICV or however named) acceptance criteria in the relevant
technical SOP.
4.4.3.3.6.3 If an expired standard material fails the verification test, it may be
repeated. If it fails a second time, the expired standard material must be
replaced or with the Section Chiefs approval, failing analytes must be
properly qualified.
4.4.3.4 Storage of large quantities of some chemicals is required in the Hazardous
Materials (HAZMAT) Facility. This includes such items as concentrated acids and
organic solvents. See the SHEMP for chemical storage procedures in the HAZMAT
building.
4.4.4 Procurement of Chemicals and Chemical Inventories
4.4.4.1 Chemical inventories within SESD must be controlled and monitored.
These controls are particularly critical for P-Listed hazardous chemicals which
must be tracked from the point of purchase to final disposal. The documentation of
the chemical inventories is the responsibility of the SESD CHO who is on the staff
of the ASB.
4.4.4.2 Only persons who have been trained in the proper handling of P-Listed
chemicals will be authorized to use them. The training will be conducted by the
CHO and/or the Safety, Health and Environmental Manager (SHEM) or a designee.
Each individual taking the training will be required to sign documentation
confirming that they have completed the training and that they understand the proper
procedures for ordering, use, storage, and disposal. The CHO will coordinate with
the LQM on the maintenance of the files for training on P-List chemicals handling.
4.4.4.3 All P-Listed chemicals will be tracked using the "Chemical Tracking Form"
that is maintained on the LAN at K:\ASB\Current Documents\Forms\Branch\ and
following the procedure as outlined below. The CHO will maintain the files of the
Tracking Forms.
4.4.4.4 Ordering of Chemicals See SESDPROC-1008 for chemical
purchasing procedures.
4.4.4.5 Receipt of Chemicals The CHO will be listed on the purchase request as the
person to receive all laboratory chemicals delivered to SESD. If the CHO is not
available for an extended period of time, the CHO's designee will serve as an
alternate to receive, track and distribute chemicals.
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4.4.5 Laboratory Pure Water
4.4.5.1 The laboratory pure water system consists of a deionization supply
enhanced in individual laboratories by exchange modules and other modules
capable of supplying high quality (18 megaohm-cm) water suitable for the
application.
4.4.5.2 Change system modules annually, as recommended by the manufacturer, or
more frequently as indicated by water quality. Modules should be labelled with the
date of installation.
4.4.5.3 Water purity is verified by the analysis of laboratory blanks and is
determined acceptable for specific analyses as prescribed in the individual
technical SOPs. Metals analysis for drinking water requires ASTM Type I water.
4.4.5.4 HMIS labeling is not required for containers of DI water.
4.5 Laboratory Hazardous and Non-Hazardous Waste Handling and Disposal Procedures
4.5.1 Procedures for Satellite Hazardous Waste Accumulation Many laboratory
operations necessitate the generation of hazardous wastes (e.g., solvents, acids, etc.)
which are required to be near the point of generation. RCRA regulation (40 CFR
262.34(c)(1)) permits satellite accumulation areas of hazardous waste or acutely
hazardous wastes at or near the point of generation. In-laboratory "satellite"
accumulation of such waste should be carefully controlled by the laboratory analyst(s)
working with the SHEM to avoid creating an unsafe situation and also comply with
RCRA satellite storage requirements. Laboratory managers or designees shall conduct
periodic walk-through inspections to ensure the proper compliance of satellite waste
accumulation procedures. The biannual safety inspection by a Safety Officer serves this
purpose.
4.5.2 Satellite Storage - Acutely Hazardous Wastes (P-Listed Wastes) Acutely
hazardous wastes are those listed in 40 CFR 261.31-261.33 and must be accounted for
separately from regular wastes. See the current version of the "SHEMP, Procedures
and Policy Manual" for procedures that apply to satellite accumulation of acutely
hazardous waste in ASB.
4.5.3 P-Listed Chemicals When any unused chemical and/or the empty containers)
for a P-Listed Chemical are ready for disposal, the analyst must notify the SHEM and
coordinate transfer of the items to the SHEM. [Special note: If a P-Listed chemical is
transferred as a single component to other containers (and remains as a single component in
the new container), then each container becomes "P-Listed" for disposal purposes and must be
tracked and accounted for.]
4.5.4 Disposal of Outdated or Waste Chemicals/Chemical Containers It is the
individual analyst's responsibility to ensure that all appropriate procedures are followed
when disposing of outdated chemicals, chemicals that are no longer in use, or empty
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containers of spent chemicals. As a general policy, no chemicals or solvents shall be
disposed of by evaporation or by pouring down the sink, with the exception of dilute
acid and bases that are accounted for in SESD's waste stream. The SHEM should be
consulted to verify appropriate procedures.
4.5.5 Non-P-Listed Chemicals Follow all Standard Procedures for disposal as
specified in the "SHEMP, Procedures and Policy Manual" and the SESDPROC-1010,
Maintaining a Chemical Inventory System. Any questions about disposal of unused
chemicals should be referred to the appropriate supervisor or the SHEM.
4.5.6 Waste Minimization ASB is an active participant in pollution prevention
activities. Each staff member is responsible for monitoring and identifying the waste
stream generated by the analyses they perform and for seeking ways to minimize the
wastes generated. Ideas to minimize waste generation should be brought to the
attention of the employee's supervisor. All appropriate solid wastes are recycled.
Currently SESD has a recycling program for cardboard, aluminum cans, glass, mixed
paper, Styrofoam and plastics. This accounts for a large amount of the total waste
stream generated by ASB and SESD.
4.5.6.1 Branch management is responsible for ensuring that staff adhere to all
Region 4 recycling, waste handling, and disposal requirements for all laboratory
operations. This includes the implementation of procedures (i.e., technical and/or
management) designed to minimize the generation of hazardous wastes.
4.5.6.2 Waste minimization should be a prime consideration of initial experimental
design and investigation planning. The degree to which waste minimization is
achieved ultimately impacts the operation and cost effectiveness of our overall
hazardous waste management program.
4.6 Laboratory Cleanliness
Each analyst is responsible for keeping the lab clean and orderly. The work area should
be cleaned after each use in a timely manner to prevent the accumulation of used
glassware, chemical spillage, or other conditions which may create unsafe working
conditions.
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CHAPTER 5
Performance Quality and Data Handling
5.1 Introduction
Every component of environmental data acquisition from sample collection through
final data reporting, has associated with it degrees of uncertainty. This laboratory does
not attempt to quantify absolute uncertainty, since it includes both sampling and
analytical error. The purpose of a laboratory quality assurance program is to determine
when the analytical measurement uncertainty has exceeded acceptance limits for
precision and bias, and to notify the end user of the exceedances. The operating
procedures and quality control checks practiced in this laboratory and outlined in this
manual are implemented to minimize the analytical error associated with data
generation and to identify situations when the acceptance limits for precision and bias
data quality indicators are not met. Analyses are performed in support of EPA
Programs such as RCRA, Superfund, NPDES, Drinking Water, Air Toxics, CERCLA,
and other initiatives. The methods used for analysis are based primarily on EPA-
approved methods, some of which are guidance (e.g., most RCRA methods).
Modifications may have been made to increase quality, efficiency, or to support
specific requests of the various programs. Drinking water methods will not be modified
or altered unless allowed by the method itself or approved under the alternative test
procedure implemented by the Office of Water.
5.2 Terminology
5.2.1 Acceptance Criteria/Limits: specified limits placed on characteristics of a
quality control item as defined in required methods. These limits are either
statistically defined by historical method performance or by specific method
requirements.
5.2.2 Accuracy: 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.
5.2.3 Analyst: 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.
5.2.4 Analytical Uncertainty: a subset of Uncertainty of Measurement that
includes all laboratory activities performed as part of the analysis.
5.2.5 Assessment: evaluation process used to measure or establish the
performance, effectiveness, and conformance of an organization and/or its systems
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to defined criteria.
5.2.6 ASTM Type 1 Water; Type I grade of reagent water; prepared by
distillation or other equal process, followed by polishing with a mixed bed of ion
exchange materials and a 0.2-|im membrane filter. Feedwater to the final polishing
step must have a maximum conductivity of 20 (iS/cm at 298°K (25°C), resistivity
>18 MO-cm at 25°C, TOC <50 ppb, sodium <1 ppb, chloride <1 ppb, and total
silica <3 ppb.
5.2.7 Audit: systematic evaluation to determine the conformance to
quantitative and qualitative specifications of some operational function or
activity.
5.2.8 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 1-20 field samples of the same matrix, meeting the above mentioned
criteria. An analytical batch is composed of prepared field samples (extracts, digestates
or concentrates) which are analyzed together as a group. An analytical batch, i.e.,
sequence, can include prepared samples originating from various environmental matrices
and can exceed 20 environmental samples. However, all prepared or method-specified
QC samples must be analyzed at the correct frequency (e.g., method blank every 20 field
samples).
5.2.9 Bias: consistent deviation of measured values from the true value caused by
systematic errors in a procedure.
5.2.10 Blank: an artificial sample designed to monitor the introduction of
artifacts into the analytical process. The blank is subjected to the usual
analytical and measurement process to establish a zero baseline or background
value.
5.2.10.1 Bottle Blank: empty bottle filled with a volume of analyte-free media in the
laboratory and analyzed for contaminants. Results are typically reported in (ig/bottle
or mg/bottle.
5.2.10.2 Equipment Rinse Blank: sample of analyte-free media which has been
used to rinse common sampling equipment to check effectiveness of
decontamination procedures.
5.2.10.3 Field Blank: blank prepared in the field, (or in some cases, prepared in the
lab and carried to the field) by filling a clean container with analyte-free media and
appropriate preservative, if any, for the specific sampling activity.
5.2.10.4 Instrument Blank: analyte-free media processed through the instrumental
steps of the measurement process; used to determine the presence of instrument
contamination.
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5.2.10.5 Method Blank: media similar to the batch of associated field samples
(when available) in which no target analytes or interferences are present at
concentrations that impact the analytical results for sample analyses. Processed
simultaneously with and under the same conditions as the field samples through all
steps of the preparation and analytical procedures.
5.2.10.6 Reagent Blank (method reagent blank): analyte-free media
consisting of reagent(s), without the target analyte or sample matrix,
introduced into the analytical procedure at the appropriate point and carried
through all subsequent steps to determine the contribution of the reagents and
involved analytical steps.
5.2.11 Blind Sample: 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.
5.2.12 Calibration: determination, by measurement or comparison with a standard, of
the correct value of each scale reading on a meter, instrument, or other device. The
levels of the applied calibration standard should bracket the range of planned or
expected sample measurements.
5.2.13 Calibration Curve: graphical relationship between the known values,
such as concentrations, of a series of calibration standards and their instrument
response.
5.2.14 Calibration Method: defined technical procedure for performing a calibration.
5.2.15 Calibration Standard: substance or reference material used to
calibrate an instrument.
5.2.16 Certified Reference Material (CRM): reference material, one or more of whose
property values are certified by a technically valid procedure, accompanied by or
traceable to a certificate or other documentation which is issued by a certifying body.
5.2.17 Chain of Custody (COC): 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.
5.2.18 Check Standard: reference standard used to verify the concentration
of the calibration standard; obtained from a source independent of the
calibration standard.
5.2.19 Confirmation: verification of the identity of a component through the use of
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an approach with a different scientific principle from the original method. These may
include, but are not limited to: second column confirmation, alternate wavelength,
derivatization, mass spectral interpretation, alternate detectors or additional cleanup
procedures.
5.2.20 Conformance: 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.
5.2.21 Continuing Calibration Verification (CCV): analysis of an analytical
standard or reference used to verify the calibration curve.
5.2.22 Corrective Action: action taken to eliminate the causes of an existing
nonconformity, defect or other undesirable situation in order to prevent
recurrence.
5.2.23 Formal Corrective Action: higher level corrective action that includes a multi-
step process of describing the issue, performing a root cause analysis leading to a
proposed action, acceptance and closure.
5.2.24 Data Audit: qualitative and quantitative evaluation of the documentation and
procedures associated with environmental measurements to verify that the resulting
data are of acceptable quality (i.e., that they meet specified acceptance criteria).
5.2.25 Data Quality Objective (DQO): statement of data quality required from an
investigation as established by the end user during the planning phase of a project
requiring laboratory support. The DQO is a qualitative and/or quantitative statement of
the quality of data required to support specific decisions or regulatory actions.
5.2.26 Data Reduction: process of transforming raw data by arithmetic or statistical
calculations, standard curves, concentration factors, etc., and collation into a more
useable form.
5.2.27 Deficiency: unauthorized deviation from acceptable procedures or practices,
or a defect in an item.
5.2.28 Demonstration of Competency (DOC): procedure to establish the ability of
the method and/or analyst to generate acceptable accuracy.
5.2.29 Dissolved: terminology used in analytical reporting referring to a field
sample that has been filtered prior to preservation and arrival.
5.2.30 Document Control: act of ensuring that documents (and revisions thereto) are
proposed, reviewed for accuracy, approved for release by authorized personnel,
distributed properly and controlled to ensure use of the correct version at the location
where the prescribed activity is performed.
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5.2.31 Estimated Value: calculated value based on a reasonable approximation of the
true value.
5.2.32 Field of Accreditation Matrix: these matrix definitions shall be used when
accrediting a laboratory (see Field of Accreditation).
5.2.32.1 Drinking Water: any aqueous sample that has been designated a
potable or potential potable water source.
5.2.32.2 Non-Potable Water: any aqueous sample excluded from the definition of
Drinking Water matrix. Includes surface water, groundwater, effluents, water
treatment chemicals, and TCLP or other extracts.
5.2.32.3 Solid and Chemical Materials: includes soils, sediments, sludges, products
and by-products of an industrial process that results in a matrix not previously
defined.
5.2.32.4 Biological Tissue: any sample of a biological origin such as fish tissue,
shellfish, or plant material. Such samples shall be grouped according to origin.
5.2.32.5 Air and Emissions: whole gas or vapor samples including those contained
in 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.
5.2.33 Holding Time: period of time (usually in hours or days) from sample collection
until sample preparation or analysis. Initial time is when a grab sample is collected or
the time the last aliquot of a composite is collected; final time is when sample
preparation or analysis begins. This time requirement can be expressed in various units
(i.e., hours, days, weeks, etc.). Holding times are evaluated in the same units as
specified. For those analyses with both a preparation and analytical holding time, the
LIMS calculates the analytical holding time from the beginning of the sample
preparation time.
5.2.34 Initial Calibration Curve (ICAL): calibration curve with concentrations
bracketing the range of interest performed at the beginning of the analytical process and
again each day prior to sample analysis or at a frequency required by a specific method.
5.2.35 Initial Test Method Evaluation (ITME): procedure for establishing an
authorized method in a specific lab through a formal validation study to include an
evaluation of a method's precision and bias. The ITME can include a method detection
limit (MDL) determination and an evaluation of the minimum reporting limit (MRL),
where applicable.
5.2.36 Internal Standard: known amount of standard added to a test portion of a
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sample as a reference for evaluating and controlling the precision and bias of the applied
analytical method.
5.2.37 Laboratory Control Sample (LCS): 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.
5.2.38 Laboratory Control Sample Duplicate (LCSD): replicate LCS prepared in
the laboratory and analyzed to obtain a measure of the precision of the recovery for
each analyte.
5.2.39 Laboratory Replicate Analyses: measurements of the variable of interest
performed identically on two or more sub-samples of the same samples within a
short time interval. A laboratory duplicate is a subset of laboratory replicates.
5.2.40 Laboratory Duplicate: aliquots of a sample taken from the same container
under laboratory conditions and processed and analyzed independently.
5.2.41 Management System Review: qualitative assessment of an organization's
overall quality system and the effectiveness of its implementation.
5.2.42 Marginal Exceedance (ME): term that is used to describe an LCS recovery
that is beyond the LCS control limit (three standard deviations), but within ME limits
which are between three and four standard deviations from the mean. Data is
reviewed for exceedance of the marginal exceedance limits solely for the purpose of
determining if the need for technical corrective action exists.
5.2.43 Matrix: substrate of a test sample.
5.2.44 Matrix Spike (spiked sample or fortified sample): sample prepared by
adding a known mass of target analyte to a specified amount of matrix sample for
which an independent estimate of the target analyte concentration is available.
Matrix spikes are used to determine the effect of the matrix on a method's recovery
efficiency.
5.2.45 Matrix Spike Duplicate (spiked sample or fortified sample duplicate):
second replicate matrix spike prepared in the laboratory and analyzed to obtain a
measure of the precision of the recovery for each analyte.
5.2.46 May: denotes permitted action, but not required action.
5.2.47 Measurement Quality Objective (MQO): desired sensitivity, range,
precision, and bias of a measurement.
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5.2.48 Method: a body of procedures and techniques for performing an activity (e.g.
sampling, chemical analysis, quantification), systematically presented in the order in
which they are to be executed.
5.2.49 Method Detection Limit: minimum concentration of a substance (an analyte)
that can be measured and reported with a 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.
5.2.50 Minimum Reporting Limit (MRL): concentration level below which the
variance of the results for a particular analyte (element or compound) exceeds the
acceptable quality control criteria. This value corresponds to the lowest quantitative
point on the calibration curve or the lowest demonstrated level of acceptable
quantitation. The MRL is sample-specific and accounts for preparation weights and
volumes, dilutions, and moisture content of soil/sediments.
5.2.51 Must: denotes required action.
5.2.52 Non-target Analyte: compound that is detected by an analytical system, but
is not specifically targeted by the method as a parameter. In this instance, there
would not be a calibration standard used to calibrate the analytical system
specifically for this analyte. (This most often occurs with analyses for organic
parameters.) The identification (qualitative analysis) of the non-target analyte is
generally based on a comparison to known or published information (e.g., spectra
from published libraries) and is usually considered tentative or provisional. The
amounts reported are calculated relative to known concentrations of other reference
materials and are reported as estimated or qualified. These analytes are also often
referred to as tentatively identified compounds (TICs).
5.2.53 Organic Free Water: reagent water without organic compounds that might
interfere with the extraction or analysis of samples.
5.2.54 Outlier: observation (or subset of observations) which appears to be
inconsistent with the remainder of that set of data.
5.2.55 Precision: degree to which a set of observations or measurements of the same
property, obtained under similar conditions, conform to themselves; a data quality
indicator. Precision is usually expressed as standard deviation, variance or range, in
either absolute or relative terms.
5.2.56 Preliminary Data: produced prior to undergoing a complete QA/QC review
and may be subject to change as a result of the review process. Upon request, a
preliminary draft report of the data requested will be submitted to the project leader
via e-mail in PDF format, prior to the data being subject to the complete review
process.
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5.2.57 Preservation: refrigeration and/or reagents added before (e.g., 50% HC1) or
at the time of sample collection to maintain the chemical and/or biological integrity
of the sample. Preservation may also take place after sampling in certain situations.
5.2.58 Preventive Action: proactive process to identify opportunities for
improvement rather than a reaction to the identification of problems or complaints.
5.2.59 Proficiency Test Sample (PT): a sample, the composition of which is
unknown to the analyst, which is provided to test whether the analyst/laboratory can
produce analytical results within specified acceptance criteria.
5.2.60 Pure Reagent Water: water (defined by national or international standard) in
which no target analytes or interferences are detected as required by the analytical
method.
5.2.61 Quality Control Sample: sample used to assess the performance of all or a
portion of the measurement system. QC samples may be Certified Reference
Materials, a quality system matrix fortified by spiking, or actual samples fortified by
spiking.
5.2.62 Quality System: defined system of quality assurance practices and
operational policies.
5.2.63 Quantitation Limits: levels, concentrations, or quantities of a target variable
(e.g., target analyte) that can be reported at a specified degree of confidence.
5.2.64 Range: difference between the minimum and maximum of a set of values.
5.2.65 Raw Data: any original factual information from a measurement activity or
study recorded in a laboratory notebook, worksheets, records, memoranda, notes, or
exact copies thereof necessary for reconstruction and evaluation of the report of
activity or study. Raw data may include photography, computer printouts,
magnetic/digital media, and recorded data from automated instruments. If exact
copies of raw data have been prepared (e.g., tapes transcribed verbatim, data copied
and verified accurate by signature), the exact copy or exact transcript may be
submitted.
5.2.66 Reference Material: material or substance one or more properties of which
are sufficiently well established to be used for the calibration of an apparatus, the
assessment of a measurement method, or for assigning values to materials.
5.2.67 Reference Method: method of known and documented accuracy and
precision issued by an organization recognized as competent to issue said method.
5.2.68 Reference Standard: standard, generally of the highest metrological quality
available at a given location, from which measurements made at that location are
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derived.
5.2.69 Reporting Limit: also known as the Minimum Reporting Limit (MRL) in
ASB.
5.2.70 Sample: particular aliquot of a certain matrix (soil/sediment, water, air, etc.)
collected at a specific location, date, and time (grab or composite). This aliquot could
be distributed over several different size or type of containers depending on the
analytical and/or preservation requirements.
5.2.71 Scope of Accreditation: accredited work organized on the certifying
statement by category, sub-category and technique.
5.2.72 Second-Source Material: term typically applied to a QC sample used to
verify a standard curve. Second source refers to a stock standard obtained from a
different vendor than that used for the calibration standards. Alternatively, if a
second vendor is not readily available, a different lot number from the same vendor
may be used if the vendor verifies that the lots were prepared independently from
different source material.
5.2.73 Selectivity: the capability of a test method or instrument to respond to a target
substance or constituent in the presence of non-target substances.
5.2.74 Sensitivity: capability of a method or instrument to discriminate between
measurement responses representing different levels (e.g., concentrations) of a
variable of interest.
5.2.75 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.
5.2.76 Should: denotes a guideline or recommendation whenever noncompliance
with the specification is permissible.
5.2.77 Significant Figures The number of digits in a reported result that are known
definitely as justified by the accuracy of the analysis with one additional figure that
may have some degree of uncertainty. For example, an analyst would be certain of
the "75" in a result reported at "75.6" mg/L, but may be uncertain as to whether the
".6 "should be ".5" or ".7" because of unavoidable uncertainty in the analytical
procedure. Digits beyond this last figure are not significant. In the example, analysts
reporting to 3 significant figures would report "75.6". Only figures justified by the
accuracy of the analysis (significant figures) shall be reported. (Based on Standard
Methods (SM) for the Examination of Water and Wastewater, 22nd edition)
5.2.78 Spike: known mass of target analyte added to a blank sample or sub-sample;
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used to determine recovery efficiency or for other quality control purposes.
5.2.79 Standard Reference Material (SRM): certified reference material produced
by the U.S. National Institute of Standards and Technology or other equivalent
organization and characterized for absolute content, independent of analytical
method.
5.2.80 Target Analyte: individual analyte specifically targeted for analysis by using
a method designed and validated for the analyte. The method includes calibration
standards and other quality control parameters to calibrate and document the ability
of the analytical system to successfully analyze for the analyte.
5.2.81 Technical Corrective Action: any action taken to address instrument or
quality control specifications at the time an exceedance is noted. Technical
corrective actions are proactive and preventative in nature and do not require a root
cause analysis as they do not impact data quality.
5.2.82 Technical System Review: assessment of analytical procedures, record
keeping, data verification, data management and other technical aspects within an
organization.
5.2.83 Tentatively Identified Compound (TIC): see Non-Target Analyte.
5.2.84 Traceability: property of a result of a measurement where it can be related to
appropriate standards, generally international or national, through an unbroken chain
of comparisons.
5.2.85 Uncertainty of Measurement (Uncertainty): parameter, associated with the
result of a measurement that characterizes the dispersion of the values that could
reasonably be attributed to the measurand (object being measured). Uncertainty
differs from error in that it takes the form of a range of values as opposed to error
which is the difference from the true value and is represented by a single value.
5.2.86 Verification: confirmation by examination and provision of evidence that
specified requirements have been met.
5.2.87 Work Cell: a group of analysts that share responsibility for a specified
analysis.
5.3 Essential Quality Control Requirements
5.3.1 Demonstration of Competency (DOC) ASB requires all analysts to
demonstrate initial competency (prior to independent analysis of environmental
samples) or with method or instrumental changes that could impact method
performance. Extraction Laboratory analysts may participate in extraction
procedures prior to completing a DOC provided they are performing the work with
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another analyst with an active DOC for that extraction method. Analyst DOCs are
specific to the method only, demonstrating the analyst's ability to successfully
perform the method. Procedures for performing a DOC are detailed in SOP ASB
110G: Standard Operating Procedure for Initial Test Method Evaluations and
Establishing Demonstrations of Competency and SESD PROC-1003 Training and
Demonstrations of Competency.
5.3.2 Continuing Demonstrations of Proficiency (CDOP) An analyst's continued
proficiency with a test method will be evaluated through the completion of a CDOP.
Performance of the CDOP is required every four years at a minimum. Detailed
procedures for documenting an analysts' CDOP are detailed in SOP ASB 110G and
SESD PROC-1003.
5.3.2 MDL Studies ASB performs MDL studies as part of the ITME and upon
change in instrumentation; they are verified on an ongoing basis, in accordance with
40CFR Part 136 Appendix B as detailed in ASB SOP 119G. ASB only reports non-
detects at the MDL by special request.
533 Instrument Calibration
533.1 Initial Calibration Curve (ICAL) All instrumentation utilized in the
preparation or analysis of environmental samples will be calibrated prior to use.
The calibration curve shall bracket the range of expected concentrations for the
analytes being evaluated. Calibration frequency and acceptance criteria will
follow method and/or technical SOP requirements. Calibration standards shall be
prepared using the same, or equivalent, type of acid or solvent and at the
expected concentration as the samples following sample preparation. ASB
requires purchased standards to be prepared in accordance with ISO guide 34
specifications. Traceability shall be to a national standard, when commercially
available.
Any data above the calibration range shall be diluted or considered to have an
increased quantitative uncertainty and shall be reported with a qualifier, where
applicable. For Metals samples analyzed by ICP, a linear range study is
performed and verified with each analysis. Samples exceeding the calibration but
within the linear range are reported unqualified provided the linear range check
standard is within the ±10% acceptance criteria.
533.2 Initial Calibration Verification (ICV) ICALs shall be verified with a
second source standard, on the frequency prescribed in the published method or
technical SOP. Traceability shall be to a national standard, when commercially
available. For test methods where a second source is not available (e.g., technical
toxaphene). ASB allows for verification of the calibration through the use of
alternative quality controls. In these instances, the technical SOP will describe
the verification requirements.
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5.3.3.3 Continuing Calibration Verification (CCV) In addition to the initial
calibration verification, ASB requires verification of the calibration over time to
assess instrument performance throughout the course of the analysis of samples.
A standard solution (either primary or second source is acceptable) will be
analyzed prior to analysis of a batch containing environmental samples and at the
frequency prescribed in the published method or technical SOP.
5.3.4 Acceptance Criteria All methods in use must have acceptance criteria against
which all QC results are evaluated. When method-specific acceptance criteria are not
specified or available, in-house acceptance criteria must be developed using a
minimum of 20 results, but no more than 30 results. After the initial limits are
determined, they should be updated again as needed or as soon as practical. It is the
policy of ASB that bias and precision limits are set at three standard deviations from
the mean of the dataset. Technical SOPs will detail the acceptance criteria for all
applicable QC elements required by the published method. Interim limits for bias
and precision will be established based on guidance in the published method or
equivalent. If there are no existing guidelines for limits, arbitrary limits will be
established.
5.3.4.1 Setting Interim Bias (Recovery) Limits ASB allows for the use of interim
limits for bias until sufficient data is available to establish limits based on
historical data. Interim Limits for bias will be calculated using the most recent
seven valid spiked results. If seven data points are not available, Interim limits for
bias will be established based on guidance in the published method or equivalent.
If there are no existing guidelines for limits, arbitrary limits will be established and
used until such time that seven spike values are generated and interim limits can be
calculated. Limits for inorganic analyses should be set at 85-115% and limits for
organic analyses at 70-130%.
5.3.4.2 Setting Interim Precision Limits Interim limits for precision are set at an
RPD or RSD of 20. At the discretion of the Technical Director or LQM, interim
RPD limits of 50 may be set for complex matrices such as soil, tissue or waste.
5.3.5 Method Blanks ASB requires one method blank per batch of up to 20
environmental samples per matrix type per sample preparation method, or as
specified by the published method. The method blank is utilized to assess potential
contamination of the associated sample batch.
5.3.6 Laboratory Control Samples (LCS) For every batch of up to 20
environmental samples per matrix type per sample preparation method, or as
specified in the published method, ASB requires an LCS to be carried through the
entire analytical process. ASB uses the LCS to assess the performance of all or a
portion of the measurement system. ASB also assesses the LCS results for organic
analysis as a mechanism for determining if technical corrective action is through the
use of marginal exceedances. A marginal exceedance report is generated from
Element® and included with each project file. The report identifies any compounds
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in the LCS standard that exceed 4 standard deviations of the mean % recovery.
Action is required based on the number of exceedances versus the number of
compounds spike din the LCS standard as follows:
*Greater than 90 analytes in LCS, 5 analytes allowed within ME limits
*From 71-90 analytes within LCS, 4 analytes allowed within the ME limits
*From 51-70 analytes within LCS, 3 analytes allowed within the ME limits
*From 31-50 analytes within LCS, 2 analytes allowed within the ME limits
*From 11-30 analytes within LCS, 1 analytes allowed within the ME limits
*Less than 11 analytes in LCS, no analytes allowed within ME limits
5.3.7 Matrix Spike (MS) Frequency of the analysis of MS samples shall be
determined as part of the systematic planning process (e.g., DQOs) or as specified by
the required reference method. Unless otherwise allowed by the technical SOP, a
minimum of at least one MS should be prepared per batch of up to 20 samples for all
methods amenable to performing a MS. The matrix spike analysis is used to assess
the performance of the method by measuring the effects of interferences caused by
the sample matrix and reflects the bias of the method for the particular matrix in
question. ASB uses the acceptance criteria for evaluating a MS as defined in the
published method. If no acceptance criteria are provided, QC limits will be
established using historical data. ASB does not qualify any batch results based on the
MS analysis. Only the sample spiked is qualified if QC results are outside of the MS
limits for that sample.
5.3.8 ASB expresses bias as percent recovery (%R) and calculated bias for both LCS
and matrix spikes using the following formulas:
Bias
Spike Reference Reference Materials
Or
%R= ^(100) %R= ^ (100)
Where: X = Concentration in unspiked sample.
Y = Measured concentration
Z = Concentration in spiked sample.
T = True concentration of spike added or of analyte in reference material.
5.3.9 Surrogate Spike Recovery of the surrogate standard is used to monitor for
unusual matrix effects, gross sample processing errors, etc. and is evaluated by
determining whether the measured concentration falls within an established
statistical acceptance limit. Surrogate spiking compounds are added, when
appropriate, to each sample just prior to preparation, i.e., extraction or purging.
Surrogate standards are normally utilized in organic analyses. Sample results with
surrogate limits that fall outside acceptance criteria are qualified appropriately.
Acceptance limits are defined by the technical SOP. Surrogate recoveries are
compared to the method-specified acceptance limits within Element®.
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5.3.10 Proficiency Test Sample (PT sample) ASB will participate in independent
Proficiency Testing Studies as required for accreditation or more often as deemed
necessary by ASB management or the LQM. Performance in these studies further
indicates the effectiveness of the laboratory's day-to-day quality control procedure.
ASB's current Forensic and ISO 17025 accreditation requires the entire scope of
accreditation to be covered with a PT every four years. In addition, the laboratory
should participate in one PT per calendar year. The results of the PT studies must be
reported to the accrediting body prior to the annual accreditation visit. The
laboratory will create and maintain a four-year PT plan that consists of each PT that
will be performed that calendar year. The accrediting body will review the plan
during the annual assessment. When the laboratory receives a performance score of
'not acceptable' a formal corrective action and makeup PT shall be performed for the
analytes that were deemed unacceptable prior to the next scheduled PT.
5.3.11 Standard Reference Materials (SRM) and Certified Reference Materials
(CRM) These reference materials will be utilized to determine method/analytical
performance as deemed appropriate.
5.3.12 Minimum Reporting Limit (MRL) Verification Standard A standard at or
near(0.5X- 2X) the MRL that has been processed through all steps (preparation and
analysis) of the method used to verify the performance of the measurement system at
the lower end of the calibration curve.
5.3.13 Precision Refers to the level of agreement among repeated measurements of
the same analyte or property. Results may be compared to historical ASB limits or
the acceptance criteria in the published method. Precision is expressed as relative
percent difference (RPD).
5.3.14 Matrix Duplicate Analyses At a minimum, either a matrix duplicate or MS
duplicate (see below) shall be prepared with each batch of up to 20 environmental
samples as required by the published method, where the method is amenable to
spiking. The results from matrix duplicates are designed to assess the precision of
analytical results in a given matrix. ASB does not qualify any batch results based on
the matrix duplicate analysis. Only the sample which was duplicated is flagged if QC
results are outside of the matrix duplicate limits for that sample.
5.3.15 Laboratory Control Sample Duplicate (LCSD) ASB does not routinely
analyze an LCSD unless mandated by the published method, SOP, project specific
DQOs or if precision of the analysis is not determined through the analysis of a
matrix duplicate or spike duplicate. Acceptance criteria for the LCSD results are
compared to established limits for that specific matrix if available. If precision
results from an LCS/LCSD pair are outside of established acceptance criteria, all
results for that analyte in the batch, both detects and non-detects, are qualified as
estimated "J" with an appropriate explanatory qualifier.
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5.3.16 Matrix Spike Duplicates (MSD) MSDs will be included in each sample
batch as specified by the published method where sufficient sample is received for
performing the analysis. The results from MSDs are utilized to assess the precision
of the analytical results in a given matrix. Results are compared to established limits
for that specific matrix if available. ASB does not qualify any batch results based on
the MSD analysis. Only the sample which was spiked is flagged if QC results are
outside of the matrix spike duplicate limits for that sample.
5.3.17 Internal Standards ASB uses internal standards for the evaluation of
instrumental drift as well as suppressions or enhancements of instrument response
caused by the sample matrix, as required by the applicable published method.
Internal standards are added to all calibration standards and QC samples (method
blank, MS/MSD, LCS/LCSD, MRL verification) at the same concentration as the
samples following preparation. The acceptance criteria in the method will be
observed.
5.3.18 Bottle blanks, equipment rinse blanks and other in-house QC analyzed for
the field branches and supply screening will be performed with a reduced level of
QC due to the nature of the matrix which is reagent water.
5.4 Data Handling
5.4.1 Holding Time Sample preparation and analysis will be performed with the
recommended holding times specified in the published method or technical SOP. If analyses
are performed outside defined recommended maximum holding times, results will be "J"-
qualified and an appropriate Element® explanatory qualifier will be added. For analyses that
have a preparation/extraction step, holding times for each segment of the analysis must be
evaluated. If any segment of the holding time is exceeded (i.e., time elapsed prior to
extraction or time elapsed prior to analysis of the extract), ASB will consider the holding
time for that sample to have been exceeded.
5.4.2 Minimum Reporting Limit (MRL) ASB includes a standard at the MRL as the
lowest standard in the calibration curve, or, where applicable (i.e., ICP analysis where
the calibration curve consists of a blank and a high level standard), analyzes a low level
check standard at the MRL following calibration. Results are considered to be within
acceptable quantitative accuracy if analyses are performed within the appropriate
quantitation range as defined by the calibration curve. Results reported outside these
limits will be qualified with the "J"-flag or otherwise as appropriate. A remark
describing the reason for the qualifier will be added to the report.
5.4.3 Reporting data between the MDL and MRL As a matter of routine practice,
ASB's reporting level policy is as follows.
5.4.3.1 Organic Chromatographic/Mass Spectral Data Because
chromatographic/mass spectral analyses use both retention time and a spectral
match, there is qualitative evidence for the presence of target analytes at
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concentrations between the MDL and the MRL.
5.4.3.1.1 Non-detects are reported to the MRL.
5.4.3.1.2 Positive detects between the MDL and the MRL are reported with
a 'J' and explanatory qualifier.
5.4.3.1.3 Any requests for non-detects to be reported as less than the MDL must
be approved by the Section Chief or LQM who will verify that a current MDL
study is in place that will meet the needs of the data user.
5.4.3.2 All other data
5.4.3.2.1 Non-detects are reported to the MRL.
5.4.3.2.2 Any detects between the MDL and the MRL are reported as less
than the MRL.
5.4.3.2.3 All requests for results to be reported between the MRL and MDL must
be approved by the Section Chief or LQM who will verify that a current MDL
study is in place that will meet the needs of the data-user.
5.4.4 Units
5.4.4.1 Sediment/Soil All soil/sediment samples shall be reported on a dry-weight
basis unless otherwise specified by the published method or technical SOP.
Soil/sediment samples are reported in mg/kg or (ig/kg units.
5.4.4.2 Waste (aqueous and non-aqueous) Reported on a wet-weight basis
unless otherwise specified by the sample requestor.
5.4.4.3 RCRA Wastewaters as defined at 40 CFR 268.2(f) analyzed in support of
Land Disposal Restrictions constituents (40 CFR 268.48) are reported inmg/L.
5.4.4.4 Tissue samples Reported on a wet-weight basis unless otherwise specified
by the sample requestor. Tissue samples are reported in mg/kg or (ig/kg units.
5.4.4.5 Water sample Water samples include groundwater, surface water, potable
water, etc. and are reported in (ig/L or mg/L.
5.4.4.6 Air sample Air samples including VOA samples are reported in ppbv or fig/m .
5.4.5 Significant Figures Because the accuracy and/or uncertainty of every procedure
is not always precisely known, it is the general practice of ASB to report analytical
results to 2 significant figures, with the exception of PT samples which are reported to
3 significant figures.
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5.4.6 Rounding Rules
5.4.6.1 Manual Rounding Where manual data entry is performed, ASB will round
entries to achieve a final result with 2 significant figures. Round numbers by
dropping digits that are not significant. If the digit 6, 7, 8, or 9 is dropped, increase
preceding digit by one unit; if the digit 0,1, 2, 3, or 4 is dropped, do not alter
preceding digit. If the digit 5 is dropped, round off preceding digit to the nearest
even number; thus 2.25 becomes 2.2, and 2.35 becomes 2.4. Use only the digit
beyond the last significant figure for rounding. Rounding should be performed only
after arriving at the final result in the calculation.
5.4.6.2 Rounding in LIMS Element® follows the above rounding rules when
all digits following the 5 are zero. Any numbers transferred to Element® with
digits following the 5 that are not zero are interpreted as a result greater than 5
and thus are rounded up.
5.4.6.3 Values that are below the MRL, but are equal to the MRL after rounding
are reported as detects. For example, if the MRL is 0.5 and the unrounded result is
0.4986, Element® will round the result to 0.50 and report the value as detected at
0.50.
5.4.7 Determination of Outliers - Student f-test or Dixon's Q-test
5.4.7.1 Data points may not be discarded as outliers without a proper explanation or
valid justification. This applies to all data points collected (e.g. LCS, MDL, linear
curves, DOC, duplicates, etc.). Justifiable reasons for removing outliers include:
5.4.7.1.1 Known and documented laboratory error and
5.4.7.1.2 Use of an appropriate statistical outlier test.
5.4.7.2 Standard deviation from the mean - typically useful for large data sets
5.4.7.2.1 Calculate the mean and the standard deviation of all the data. Database
outliers are established by summarizing all the data in the database and then
applying one standard deviation beyond the statistical confidence level required.
For example, assuming the statistical confidence level required is 95% (2
standard deviations around the mean), any result greater than 3 standard
deviations around the mean would be an outlier.
5.4.7.3 Studentized deviation from the mean - Mest
5.4.7.3.1 Including the suspect extreme value (possible outlier), calculate the
sample mean (x) and the standard deviation (5) of the data.
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5.4.7.3.2 Calculate the ratio
\suspect value — x\
tcctlc = ~
5.4.7.3.3 Apply the following decision rule.
5.4.7.3.3.1 If tcaic is greater than the critical value (&77&ca/) at a given level of
confidence, then the suspect value should be removed.
5.4.7.3.3.2 Critical values of t (tawcai) as a function of sample size, n, at the 95%
level of confidence (level of significance, a= 0.05) are given in Table 5-1.
5.4.7.3.4 Example
MDLrep
Lead (}xg/L)
1
40.3
2
41.0
3
40.1
4
38.0
5
40.7
6
41.3
7
41.1
For the extreme low value, the calculated value of t is:
\smpev(-X\ 138.0-4035711
calc
&
The critical value of fis 2.02 for a = 0.05 and n = 7. The calculated value of t, 2.09, is
greater than the critical value of t (e.g., /cak> /critical). Thus the suspect value is an
outlier and should be removed.
5.4.7.4 Dixon's Q test
5.4.7.4.1 Sort the n data values in ascending order:
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which is one of the extreme values.
5.4.7.4.4 Calculate the value of Q:
I suspect value — nearest neighbor \
Qcalc = ' 1
range of entire data set
\xl~ x21 Ixn~ xn-i\
(xn~ xl) (xn~ xi)
5.4.7.4.5 Apply the following decision rule:
5.4.7.4.5.1 If the calculated value of Q (Qcaic) is greater than the critical
value of Q (Qcnticai) at a given level of confidence, then the suspect value is
an outlier and should be removed from the data set.
5.4.7.4.5.2 Critical values of Q as a function of sample size, n, at the 95%
level of confidence (level of significance, a = 0.05) are given in Table 5-2.
5.4.7.4.5.3 Example
MDL Rep
Lead (|ig/L)
1
40.3
2
41.0
3
40.1
4
38.0
5
40.7
6
41.3
7
41.1
The data sorted in ascending order are:
MDL Rep
Lead (|ig/L)
4
38.0
3
40.1
1
40.3
5
40.7
2
41.0
7
41.1
6
41.3
For the extreme low value, the calculated value of Q is:
|38.0—40.1|
Qcaic= z r = 0.636
V (41.3-38.0)
The critical value of Q is 0.568 for a=0.05 and for n=7. The calculated value
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of Q, 0.636, is greater than the critical value of Q (e •g. Qcalc ¦> Qcritica l). Thus,
the suspect value is an outlier and should be removed.
5.4.8 Uncertainty Where available, ASB utilizes well-recognized test methods which
specify limits to major sources of uncertainty (e.g., a balance accurate to ± 0.1 g) and
provide data reporting instructions so that the reported results do not give the wrong
impression of the uncertainty. ASB provides customers QC data with each final report
(both specific batch QC and acceptance criteria) to communicate an estimate of the
uncertainty associated with the final results of the dataset. Where applicable, a statement
on the estimated uncertainty of measurement will be included, such as when it is
relevant to the validity of the test result, when requested by the customer or when the
uncertainty may affect compliance to a regulatory limit.
5.4.9 If requested to provide a more rigorous estimate of the uncertainty of a test
result, the analyst in consultation with the Section Chief and LQM will use one of the
following two options.
5.4.9.1 Estimation of Uncertainty using Laboratory Control Samples (adapted
from: Georgian, 2000, Environmental Testing and Analysis). This method uses the
limits of historical LCS data to estimate results to a 99% confidence interval using
the following equation:
Uncertainty = 10oQ-) ^1 +
Where: c = measured concentration of the analyte
L = the half width of the control range, that is, (UCL-LCL)/2
R = mean historical LCS recovery
Because the LCS is a measure of the performance of the entire analytical process,
including instrument calibration, this is ASB's preferred method of estimating
uncertainty because it can estimate the uncertainty of the entire analytical process
with actual analytical results.
5.4.9.2 Standard Methods 1030B Measurement Uncertainty
5.5 Data Reporting
All accredited analytical data generated by ASB will be entered into and reported
from Element®.
5.5.1 Analytical Data Qualifiers Added to data in an effort to best describe the
quality of the data to the end-user. These qualifiers, based on the QC criteria
specified in the published method or technical SOP, are applied during data reduction
by primary analysts.
5.5.2 Report Narrative Additional explanatory remarks about the data can be added
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by the Section Chief (or designee) in the Report Narrative section of the data report.
Analysts will add any necessary explanatory remarks about their analyses in the 'Work
Order Notes' section of Element® and the Section Chief (or designee) will summarize
any pertinent information that needs to be transmitted to the data user in the final report
through the report narrative.
Note: Though the Report Narrative is identified as such on the Final Report, in
Element® on the reporting screen, it is called the Work Order Case Narrative.
5.5.3 Chemical Abstract Service (CAS) Registry Numbers and EPA Identifiers
(EPA ID) Each analyte reported from Element® is also reported with the analyte's
corresponding CAS number. For some analytes reported by ASB (e.g., BOD), a CAS
number does not exist. In these cases, a custom EPA ID number is assigned and
reported with the specific analyte. EPA's Substance Registry System (SRS) is the
source of CAS numbers and EPA IDs reported with all data. The SRS database is
located at: http://www.epa.gov/srs. ASB will assign a unique internal 'R4' code to any
analyte for which there is neither a CAS number nor EPA ID available in EPA's SRS.
5.5.4 Opinions and Interpretations ASB rarely, if ever, offers opinions and
interpretations of the reported data. However, if included with a laboratory report, the
basis upon which the opinion or interpretation was made shall be included in the
report. Any opinions or interpretations shall be clearly marked as such.
5.5.5 Demonstration of MRL or sample calculation ASB will demonstrate one
MRL or sample calculation per batch of samples as part of the data review and
validation procedure.
5.5.6 Reporting Preliminary Data ASB does not report preliminary data on a routine
basis; however, upon request of the project leader, preliminary data may be released by
the Section Chief (or designee). All preliminary data released shall be in the form of a
Draft report from Element®. The report must contain a narrative indicating that the data
presented is preliminary, has not been completely reviewed and should not be utilized
for any decision-making purposes.
5.5.7 Re-Reporting of Data ASB receives requests for re-reporting of data due to
corrections to sample locations or stations, etc. In those instances, the request will come
through the R4COCCorrections mailbox to the LQM. The LQM will forward the
requests to the sample custodian and the appropriate Section Chief. Once corrections are
complete, the Section Chief (or designee) will issue a new report. The new report will
contain a narrative indicating that the data has been re-reported and the reason, and a
statement that the new submission replaces the previous reported results. A copy of the
new report along with any additional supporting documentation will be added to the
project file.
5.6 Data Management and Data Security
5.6.1 Data is managed using both R4LIMS and Element®. R4LIMS is used for project
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scheduling and Element® is used for analytical data management. R4LIMS is an in-
house developed Sybase PowerBuilder® application. All data is stored in an Oracle
database residing on an SESD Windows 2003 Server. Console-level access to the
Oracle Server is limited to the SESD LAN Administrator, the Region 4 LAN
Administrator, and the R4LIMS Database Administrator (DBA) who is an SESD
computer specialist responsible for R4LIMS application development and database
administration.
5.6.1.1 Backups of the Oracle database (and the entire LAN) to magnetic tape are
performed Monday through Saturday evenings using a redundant network backup
system. One backup is conducted remotely from the ERD computer center and
another locally from the SESD computer center. After successful backups, the daily
tapes located at SESD are placed in a fire-proof media safe and a copy of the Friday
evening backup is rotated to the Atlanta EPA office for offsite storage. Detailed
backup procedures can be Backups of the Oracle database (and the entire LAN) to
magnetic tape are performed Monday through Saturday evenings using a redundant
network backup system. One backup is conducted remotely from the ERD computer
center and another locally from the SESD computer center. After successful
backups, the daily tapes located at SESD are placed in a fire-proof media safe and a
copy of the Friday evening backup is rotated to the Atlanta EPA office for offsite
storage.
5.6.1.2 Detailed backup procedures can be found in the 'ADP Disaster Recovery
Plan for Region 4' dated June 10, 2004 (and any future updates). The custodian of
this document is the Region 4 Information Security Officer in the Atlanta office. An
electronic copy is available from the Athens LAN administrator, and a hard copy is
located in the safe in room B107.
5.6.2 Direct access to the Oracle database table space is restricted to authorized EPA IT
staff only. Access is limited and on an as-needed basis. The Contract Programmer only
has rights to a development database and not the active R4LIMS database. The SESD
LAN Administrator and R4LIMS DBA have unrestricted rights to the database.
5.6.2.1 End-user access to the database is controlled through the compiled
R4LIMS Powerbuilder application, Element® DataSystem and the
Adobe/Macromedia Coldfusion® web server (currently limited to read-only
access of "public"data).
5.6.2.1.1 All R4LIMS and Element® application users are required to log-in to
the system using an R4LIMS or Element® application USERID and
PASSWORD. An R4LIMS PUBLIC account and the Coldfusion web server,
both with limited access as described later, are the only exceptions to this
requirement. Otherwise, access is controlled by USERID, with varying rights
assigned to each user.
5.6.2.1.2 Access to the EPA network and an account in R4LIMS or Element® is
required for access to data for entry or reporting purposes. Rights are assigned to
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each R4LIMS or Element® user upon request by their supervisor. Telephone
requests will not be accepted. Rights are assigned by the ASB R4LIMS
coordinator, the SESD LAN Administrator, or the R4LIMS DBA.
5.6.2.1.3 Users are restricted to certain functions within R4LIMS and Element®
based on their need and job function. Immediate supervisors generally have
rights equivalent to or greater than their subordinates, as deemed appropriate.
The R4LIMS DBA has the overall responsibility for security and functionality of
both databases. The ASB R4LIMS coordinator has the responsibility of security,
accuracy, and integrity of the data in the database.
5.6.2.1.3.1 Project log entry in R4LIMS is restricted to the Sample
Custodian (or those officially trained as such), the Region 4 Superfund
Division technical liaison, project leaders and their supervisor, the LQM,
and other project custodians as deemed necessary.
5.6.2.1.3.2 Modifications to project log entries are restricted to sample
custodians and the LQM after the project has been entered.
5.6.2.1.3.3 Sample logging in Element® is restricted to the sample
custodians (or those officially trained as such), the LQM and Section
Chiefs.
5.6.2.1.3.4 Data entry in Element® is restricted to those users who have
been given analyst rights.
5.6.2.1.3.5 Reporting of final data is restricted to Section Chiefs and
their designees.
5.6.3 After data has been reported it cannot be modified without the status of the data
being set from 'Reported' to a lower level by the LQM (or someone with QA
Administrator rights in Element®) or designee. A searchable audit trail which tracks
any change to the data or analyses in the database is maintained within Element®.
5.7 Annual Analytical Performance Summary
Control charts for each analysis are compiled and reviewed on a quarterly basis, as
applicable, and any significant trends are documented in the LQM's Quarterly QA
Report. Review of the control charts may initiate either Corrective Actions or
Preventive Actions as appropriate. On an annual basis, the LQM will note any
highlights from the Quarterly Reports as well as document all methods for which limits
and/or MDLs have been updated.
5.8 OC Study Plans
5.8.1 A QC Study Plan is developed when planning a non-routine MDL/DOC study,
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developing a new method, evaluating a new/modified analytical method, or addressing
a non- routine QC issue/problem for corrective action. The most recent form for
documenting this QC Study Plan is located in a subdirectory on the SESD LAN. For
routine studies with a limited focus, a QC Study Plan is not required. The decision to
develop a QC Study Plan will be made by the project leader in consultation with the
LQM and Section Chief.
5.8.2 For studies requiring a QC Study Plan, the appropriate analysts will convene to
discuss the issue, define the objective(s), and develop the study procedure. The LQM
may be involved in the study planning depending on the nature and complexity of the
issue. The final QC Study Plan will be approved by the LQM, Section Chief, and where
appropriate, peer- reviewed by other analysts. A report summarizing the study results
will be prepared for the LQM's comments as needed. At times, it may be appropriate to
update a Study Plan as the study progresses. Changes should be communicated to all
participants as needed.
5.9 Complaints/Inquiries
All complaints shall be reviewed by management. Those which are identified as
departures from ASB's policies or procedures will enter the corrective action process.
All others will be considered as opportunities for improvement. The customer will be
informed of the resolution, which shall be maintained by the LQM.
5.10 Corrective Actions
ASB requires resolution of non-conforming work through the corrective action process.
The process will include a root cause analysis. Corrective actions can be initiated by
any staff member; however, it is the responsibility of the LQM to track, monitor and
perform any follow-up action needed in relation to the corrective action. The corrective
action procedure is detailed in SESDPROC-1006- Complaint Resolution and Control
of Non-Conforming Work.
5.11 Preventive Actions and Improvements
Preventive Actions consist of proactive processes to prevent problems or complaints
and are used as opportunities for improvement. The preventive action procedure is
detailed in SESDPROC-1006.
5.12 Control of Nonconforming Work
ASB mitigates nonconforming work through the corrective action process.
Nonconforming work is defined as any work which does not meet stated laboratory
standards, either with respect to mode of execution or outcome, i.e., data quality.
Nonconforming work can be identified at various times during the analytical process.
The procedure for correcting nonconforming work is detailed in SESDPROC-1006
5.13 Annual Management Review
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ASB conducts an annual Management Review, where the effectiveness and
conformance to the accreditation standards of the quality management system are
assessed and reported to upper level Divisional management. The review also provides
an opportunity to plan for any needed improvements to the quality system. The review
is documented and maintained by the LQM and covers the ASB's overall quality
objectives, to include at a minimum the items outlined in the ISO 17025 standard,
Section 4.15.
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TABLE 5-1
Critical values of the studentized deviation t for testing whether a single
point should be rejected as an outlier (a = 0.05, two-sided test).1
Sample Size, n
Critical Value (tcritfcai)
3
1.15
4
1.48
5
1.71
6
1.89
7
2.02
8
2.13
9
2.21
10
2.29
11
2.36
12
2.41
13
2.46
14
2.51
15
2.55
16
2.59
17
2.62
18
2.65
19
2.68
20
2.71
21
2.73
22
2.76
23
2.78
24
2.80
25
2.82
1 Pearson, E. S.; Hartley, H.O., Eds, Biometrika Tables for Statisticians,
Vol. I, 3rd ed., Cambridge University Press, London, 1966.
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TABLE 5-2
Critical values of the Q in Dixon's Q-test for testing whether a single
point should be rejected as an outlier (a = 0.05, two-sided test).1
Sample Size, n
Critical Value (Qcnticai)
3
0.970
4
0.829
5
0.710
6
0.625
7
0.568
8
0.526
9
0.493
10
0.466
11
0.444
12
0.426
13
0.410
14
0.396
15
0.384
16
0.374
17
0.365
18
0.356
19
0.349
20
0.342
21
0.337
22
0.331
23
0.326
24
0.321
25
0.317
1 Rorabacher, D. B., "Statistical treatment for rejection of deviant values
of Dixon's 'Q' parameter and related sub-range ratios at the 95%
confidence level,' Anal. Chem. 1991, 63, 139-146
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CHAPTER 6
Methodology
6.1 General
The analytical methods used by ASB are guided by DQOs of specific projects and by
program requirements. Occasionally, matrices and samples present analytical
challenges or are not amenable to a standardized methodology. Deviations from SOPs
are documented by the analyst and stored in the project files. In Element®, methods are
associated with an analysis name. Analysis names include an analyte or group of
analytes and Element® identifies a specific analytical method for each analysis name.
6.2 Method Information
Each time an analysis is performed, the appropriate method ID is assigned to analysis
logs and bench sheets within Element®. This establishes a definitive record of the
technique used to prepare and analyze each sample. Details on method applications and
limitations are found within the technical SOPs. (Any reference to an analytical method
refers to the version of ASB's SOP that was in place at that time for the specific
method.) Acceptance criteria for precision and bias are documented in Element® and
stored within the database for all analyses.
6.3 Minimum Reporting Limits
Reporting units and MRL tables for routine target analytes analyzed by ASB are
maintained within Element® for each matrix and method. The metals,
classical/nutrients, volatiles, semivolatiles, pesticides/PCBs and perfluorinated
compounds MRL values are summarized in Tables 6-3 through 6-11 respectively of
this chapter. Any needs for specific quantitation (reporting) or detection levels should
be requested as detailed in the section on 'Scheduling' in Chapter 3 or through direct
communication with the ASB Section Chief(s). The MRLs listed in the tables are those
which are routinely achievable. However, sample-specific MRLs may be higher or
lower. Some factors which may influence MRLs are listed below.
6.3.1 The amount of sample used (either volume or weight) will raise or lower
specific MRLs.
6.3.2 Dilutions due to high amounts of target analytes or matrix interferences will
raise sample-specific MRLs.
6.3.3 Solid samples corrected for percent moisture content and reported on a dry-weight
basis will have higher MRLs.
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6.4 Land Disposal Restrictions fLDRt
6.4.1 During field investigations for the Resource Conservation and Recovery Act
(RCRA) program, samples may be collected and analyses requested to determine
whether the medium being sampled meets the treatment standards under LDR. The
RCRA LDR program is intended to ensure that hazardous waste cannot be placed on the
land until the waste meets specific treatment standards to reduce the mobility or toxicity
of its hazardous constituents. Requirements are covered in 40 CFR Part 268 and are
quite complex. Analyses supporting the LDR regulations must meet certain MRLs in
order to demonstrate whether the sample being tested has met the applicable treatment
standard. The levels of concern for LDR regulations are presented in Figure 6-1.
6.4.2 When placing requests for LDR, sufficient lead-time (a minimum of 30 days)
will be needed. LDR analyses require special reporting conventions that are not
routine for ASB's LEVIS. The laboratory needs to prepare for additional analyses
required for sample characterization and to ensure that results are reported in
accordance with RCRA Land Ban requirements. Project leaders should consult ASB
Section Chiefs when planning such projects.
6.4.3 Figure 6-1 is a flowchart which provides a decision tree applicable to LDR
samples. In addition to following the flowchart, analysts should consult their Section
Chief and/or the LQM when analyzing samples for LDR purposes.
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Table
5-1 Levels of Concern for Various Programs
PARAMETER
DRINKING WATER
40 CFR 141.13 and 141.62
MCLs
RCRA TCLP
(40CFR 261.24
Table 1) and pH
(40CFR 261.22)
RCRA LAND BAN LIMITS
40CFR 268.48 Table UTS
ALTERNATIVE
RCRA LAND BAN
LIMITS FOR SOIL
40 CFR 268.49
WATER
QUALITY
STANDARDS*
Wastewater
(<1% TSS & <1% TOC
by weight CFR268.2)
Non-wastewater
Antimony
6 ng/L
1.9 mg/L
1.15 mg/L TCLP
11.5 mg/L TCLP
*See publication at
www.epa.gov/ost/pc/r
evcom.pdf
Arsenic
10 ng/L * as of 1/23/06
5.0 mg/L
1.4 mg/L
5.0 mg/L TCLP
50.0 mg/L TCLP
Barium
2000 ng/L
100.0 mg/L
1.2 mg/L
21 mg/L TCLP
210 mg/L TCLP
Beryllium
4 ng/L
0.82 mg/L
1.22 mg/L TCLP
12.2 mg/L TCLP
Cadmium
5 ng/L
1.0 mg/L
0.69 mg/L
0.11 mg/L TCLP
1.1 mg/L TCLP
Chromium (total)
100 ng/L
5.0 mg/L
2.77 mg/L
0.60 mg/L TCLP
6.0 mg/L TCLP
Copper
1300 ng/L * See 40CFR 141.80
Cyanides (Total)
200 ng/L, as free cyanide
1.2 mg/L
590 mg'kg (by 9010 or
9012)
5900 mg/kg (by 9010 or
9012, inferred)
Cyanides (Amenable)
NA
0.86 mg/L
30 mg/kg (by 9010 or
9012)
300 mg/kg (by 9010 or
9012, inferred)
Fluoride
2.0 mg/L (Secondary)
35 mg/L
NA
NA
Lead
15 ng/L* See 40CFR 141.80
5.0 mg/L
0.69 mg/L
0.75 mg/L TCLP
7.5 mg/L TCLP
Mercury (non-wastewater
/retort)
NA
NA
0.20 mg/L TCLP
2.0 mg/L TCLP
Mercury
2 ng/L (inorganic)
9.2 mg/L
0.15 mg/L
0.025 mg/L TCLP
0.25 mg/L TCLP
Nickel
3.98 mg/L
11 mg/L TCLP
110 mg/L TCLP
Nitrate, as N
10 mg/L
Nitrite, as N
1 mg/L
Nitrate + Nitrite
PH
<2 and> 12.5
Selenium
50 (ig/L
1.0 mg/L
0.82 mg/L
5.7 mg/L TCLP
57 mg/L TCLP
Silver
5.0 mg/L
0.43 mg/L
0.14 mg/L TCLP
1.4 mg/L TCLP
Sulfide
14 mg/L
NA
NA
Thallium
2 ng/L
1.4 mg/L
0.20 mg/L TCLP
2.0 mg/L TCLP
Turbidity
1NTU
Vanadium
4.3 mg/L
1.6 mg/L TCLP
16 mg/L TCLP
Zinc
2.61 mg/L
4.3 mg/L TCLP
43 mg/L TCLP
Page 76 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
START
Ask project manager for waste code; analyze
accordingly for regulated hazardous
constituents based on wastewater limits @
40CFR268.40 '¦*
Is sample a
listed waste
or treatment
Is sample a
RCRA
wastewater
(<1% TSS &
<1% TOC)?
Ask project manager for waste code; analyze
accordingly for regulated hazardous constituents
based on non-wastewater limits @ 40CFR268.40.
NOTE: Some limits require TCLP extraction.
Analyze original sample for regulated
hazardous constituents requested by project
managers using wastewater UTS limits @
40CFR 268.48."1 Note lower DLs required.
Is sample a
characteristic D001
- D003 (ignitable,
corrosive, reactive
waste)?
Analyze original sample for
regulated hazardous constituents
requested by project manager.
Is sample a
RCRA
wastewater?
(<1 % TSS &
<1% TOC)?
For regulated hazardous constituents, analyze
using non-wastewater UTS limits @ 40CFR
268.48. ,'3>4' May require TCLP extraction.
Perform TCLP
extraction per
Method 1311 and
analyze extract for
regulated
hazardous
constituents
Can original
sample
theoretically fail
TCLP limits?
Did any
regulated
hazardous
constituents fail
Tap?
Were total
analyte MQLs
less than 40CFR
268.48 1
If necessary, re-
analyze original
sample to get
MQLs below
wastewater limits.
Is original
sample a RCRA
wastewater (<1%
TSS & <1%
TOC)?
Report TCLP results as "cannot
fail" TCLP limits for hazardous
constituents.
Compare TCLP or original
results to non-wastewater limits
® 40CFR 268.481
Figure 6-1 Decision Tree for Analysis of Land Disposal Restrictions
Page 77 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Footnotes for Figure 6-1
1 See SESD LAN Directory K:\ASB\Current Documents\Miscellaneous Documents for LDR tables contained in 40CFR268.40 and .48.
2 At 40CFR 268.48 the D009 Wastewater concentration limit requires TCLP extraction for mercury.
3 A TCLP extraction is required for carbon disulfide, cyclohexanone, methanol, and metals because non-wastewater UTS limits for these analytes are expressed
as TCLP extract concentrations.
4Non-wastewater cyanide for LDR is performed by special request only. Because the non-wastewater cyanide LDR limits @ 268.48 are expressed in units of
mg/kg, do not perform a TCLP extraction for cyanide but instead analyze the original sample for cyanide.
Page 78 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-2
ASB LOQAM Chapter 6 Table 6-2
Capability for Potable Wal
ers-Inorganics
SDWA Analyte
SDWA
SDWA
ASB
ASB Routine
ASB MRL
MCL
Method used
SDWA
Method
for routine
(mg/L)
by ASB
MRL
(mg/L)
low level
request
(mg/L)
Aluminum (secondary)
0.05 - 0.2
Antimony
0.006
200.8
0.0005
200.8
0.0005
Arsenic
0.010
200.8
0.0005
200.8
0.0005
Barium
2
200.7 or 200.8
0.005
200.7 or 200.8
0.005
Beryllium
0.004
200.7 or 200.8
0.003
200.7 or 200.8
0.003
Cadmium
0.005
200.7 or 200.8
0.005
200.7 or 200.8
0.005
Copper (secondary)
1.0
200.7 or 200.8
0.01
200.7 or 200.8
0.01
Chloride (secondary)
250
300.0
300.0
Chromium (total)
0.1
200.7 or 200.8
0.005
200.7 or 200.8
0.005
Lead
0.0153
200.8
0.0005
200.8
0.0005
Iron (secondary)
0.3
Manganese (secondary)
0.05
Mercury (inorganic)
0.002
200.8 or 245.1
0.0004
200.8 or 245.1
0.0001
Selenium
0.05
200.8
0.001
200.8
0.001
Silver (secondary)
0.1
Thallium
0.002
200.8
0.0005
200.8
0.0005
Zinc (secondary)
5
Sulfate (secondary)
250
Asbestos
7MF/L>10u
NA2
NA2
NA2
NA2
Bromate
0.010
NA2
NA2
NA2
NA2
Chlorite
1.0
NA2
NA2
NA2
NA2
Residual Disinfectant
detectable
NA2
NA2
NA2
NA2
Fluoride (secondary)
2.0
300.0
0.05
300.0
0.05
Nitrate, as N
10
353.2
0.05
300.0 or 353.2
0.05
Nitrite, as N
1
353.2
0.05
300.0 or 353.2
0.05
Total dissolved solids
500
(secondary)
pH
6.5-8.54
NA1
NA1
9040C
1.04
Actual MRL may be higher due to variability of analytical instrument conditions or sample interferences.
1 Not available using SDWA Methods. Please contact Section Chief for more information.
2 Not available from ASB. Please contact Section Chief for options.
3 This is an action level, not the MCL. See 40CFR 141.80(c). The units of the reported numbers are in pH standard
units. NA- Not Available-ASB does not perform this analysis.
4 The units of the reported numbers are in pH standard units.
NA- Not Available-ASB does not perform this analysis.
Page 79 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-3
ASB LOQAM Chapter 6 Table 6-3
Capability for
Potable Waters - Organics
SD WA Analyte
SDWA
SDWA
ASB SDWA
ASB Routine
ASB MRL
MCL
Method
MRL
Low-Level
for routine
(mg/L)
(special
request)
(mg/L)
Method
low-level
request
(mg/L)
Benzene
0.005
524.4
0.0005
8260C
0.0005
Carbon Tetrachloride
0.005
524.4
0.0005
8260C
0.0005
Chlorobenzene
0.1
524.4
0.0005
8260C
0.0005
1,2-Dichlorobenzene
0.6
524.4
0.0005
8260C
0.0005
1,4-Dichlorobenzene
0.075
524.4
0.0005
8260C
0.0005
1,2-Dichloroethane
0.005
524.4
0.0005
8260C
0.0005
cis-1,2-Dichloroethylene
0.07
524.4
0.0005
8260C
0.0005
trans-1,2-Dichloroethylene
0.1
524.4
0.0005
8260C
0.0005
Methylene chloride
0.005
524.4
0.0005
8260C
0.0005
1,2-Dichloropropane
0.005
524.4
0.0005
8260C
0.0005
Ethylbenzene
0.7
524.4
0.0005
8260C
0.0005
Styrene
0.1
524.4
0.0005
8260C
0.0005
T etrachloroethylene
0.005
524.4
0.0005
8260C
0.0005
1,1,1 -Trichloroethane
0.2
524.4
0.0005
8260C
0.0005
Trichloroethylene
0.005
524.4
0.0005
8260C
0.0005
Toluene
1
524.4
0.0005
8260C
0.0005
1,2,4-Trichlorobenzene
0.07
524.4
0.0005
8260C
0.0005
1,1 -Dichloroethylene
0.007
524.4
0.0005
8260C
0.0005
1,1,2-Trichloroethane
0.005
524.4
0.0005
8260C
0.0005
Vinyl Chloride
0.002
524.4
0.0005
8260C
0.0005
Xylenes (Total)
10
524.4
0.005
8260C
0.0015
Trihalomethanes (Total)
0.08
524.4
0.007
8260C
0.002
2,3,7,8-TCDD (dioxin)
3x10"*
NA2
NA2
NA2
NA2
2,4-D
0.07
NA1
NA1
8321B
0.000025
Benzo[a]pyrene
0.0002
525.2
0.0002
8270D SIM3
0.0001
Carbofuran
0.04
NA2
NA2
NA2
NA2
Chlordane
0.002
NA1
NA1
808 IB3
0.0015
Dalapon
0.2
NA1
NA1
8321B
0.0000125
bis(2-ethylhexyl)adipate
0.4
525.2
0.001
NA
NA
bis(2-ethylhexyl)phthalate
0.006
525.2
0.001
8270D
0.006
Dibromochloropropane (DBCP)
0.0002
NA1
NA1
8011/8260C3
0.00005
Dinoseb
0.007
NA1
NA1
8321B
0.0000125
Diquat
0.02
NA2
NA2
NA2
NA2
Endothall
0.1
NA2
NA2
NA2
NA2
Endrin
0.002
525.2
0.002
8081B
0.00005
Page 80 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-3
Capability for Potable Waters - Organics
SD WA Analyte
SDWA
MCL
(mg/L)
SDWA
Method
(special
request)
ASB SDWA
MRL
(mg/L)
ASB Routine
Low-Level
Method
ASB MRL
for routine
low-level
request
(mg/L)
Ethylene dibromide (EDB)
0.00005
NA1
NA1
8260C3
0.00005
Glyphosate
0.7
NA2
NA2
NA2
NA2
Heptachlor
0.0004
525.2
0.0004
8081B
0.00005
Heptachlor Epoxide
0.0002
525.2
0.0002
8081B
0.00005
Hexachlorobenzene
0.001
525.2
0.001
8270D
0.001
Hexachlorocyclopentadiene
0.05
NA1
NA1
8270D
0.05
Lindane (gamma-BHC)
0.0002
525.2
0.0002
8081B
0.00005
Methoxychlor
0.04
525.2
0.015
8081B
0.0002
Oxamyl (Vydate)
0.2
NA2
NA2
NA2
NA2
PCBs (as Decachlorobiphenyl)
0.0005
NA2
NA2
8082-Aroclors
0.0005
Pentachlorophenol
0.001
NA1
NA1
8270D
0.0001
Picloram
0.5
NA1
NA1
8321B
0.0000125
Simazine
0.004
NA2
NA2
NA2
NA2
2,4,5-TP (Silvex)
0.05
NA1
NA1
8321B
0.0000125
Toxaphene
0.003
NA1
NA1
8081B
0.002
HAA5
0.060
NA2
NA2
NA2
NA2
Actual MRL may be higher due to variability of analytical instrument conditions or sample interferences.
1 Not available from ASB using SDWA Method. Please contact Organic Chemistry Section Chief for more
information.
2 Not available from ASB. Please contact Organic Chemistry Section Chief for options.
3 Analysis available upon request with sufficient lead-time.
NA - Not Available-ASB does not perform this analysis.
Page 81 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-4
ASB LOQAM Chapter 6 Table 6-4
Metals Analyte List
Minimum Reporting Limits by Matrices
ANALYTE
ASB Routine
Analytical
Method4
Water
fig/L
(ppb) 3
Soil/Sed
mg/kg
(ppm)1'3
Waste
mg/kg
(ppm)1
Tissue
mg/kg
(ppm)2'3
Antimony
EPA 200.8
0.5
0.05
0.05
0.01
Arsenic
EPA 200.8
0.5
0.05
0.05
0.01
Aluminum
EPA 6010C
100
10
10
2
Barium
EPA 6010C
5.0
0.5
0.5
0.1
Beryllium
EPA 6010C
3.0
0.3
0.3
0.06
Cadmium
EPA 200.8
0.25
0.025
0.025
0.00025
Calcium
EPA 6010C
250
25
25
5
Cobalt
EPA 6010C
5.0
0.5
0.5
0.1
Chromium
EPA 6010C
5.0
0.5
0.5
0.1
Chrom., Hexavalent
SM3500CRB
(20th ed)
10
5.0
5.0*
NA
Chrom., Hexavalent,
Dissolved
EPA 218.6
1.0, 0.025*
NA
NA
NA
Copper
EPA 6010C
10
1.0
1.0
0.2
Iron
EPA 6010C
100
10
10
2.0
Lead
EPA 200.8
0.5
0.05
0.05
0.01
Magnesium
EPA 6010C
250
25
25
5
Manganese
EPA 6010C
5.0
0.5
0.5
1.0
Mercury
EPA 200.8
or 245.1/74735
0.40
0.05
0.05
0.05
Hg, Ultra-trace
EPA 163 IE
0.5 ng/L
0.05 (xg/kg
NA
0.05 ng/kg
Molybdenum
EPA 6010C
10
1.0
1.0
0.2
Nickel
EPA 6010C
10
1.0
1.0
0.2
Potassium
EPA 6010C
1000
100
100
20
Selenium
EPA 200.8
1.0
0.10
0.10
0.02
Sodium
EPA 6010C
1000
100
100
20
Strontium
EPA 6010C
5.0
0.5
0.5
0.1
Silver
EPA 6010C
5.0
0.5
0.5
0.1
Tin
EPA 6010C
15
1.5
1.5
NA*
Page 82 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-4
Metals Analyte List
Minimum Reporting Limits by Matrices
ANALYTE
ASB Routine
Analytical
Method4
Water
fig/L
(PPb) 3
Soil/Sed
mg/kg
(ppm)1'3
Waste
mg/kg
(ppm)1
Tissue
mg/kg
(ppm)2-3
Titanium
EPA 6010C
5.0
0.5
0.5
0.1
Thallium
EPA 200.8
0.5
0.05
0.05
0.01
Vanadium
EPA 6010C
5.0
0.5
0.5
0.1
Yttrium
EPA 6010C
3.0
0.3
0.3
0.06
Zinc
EPA 6010C
10
1.0
1.0
0.2
Boron **
EPA 6010C
50
5.0
5.0
1.0
Silicon **
Uranium **
SESD routinely performs TCLP extractions and analyses. MRLs may increase due to variability of
interferences that make sample dilutions necessary. Sample sizes required for achieving the routine
quantitation limits are listed below.
1 Reporting limits are based on 1.0 g of sample (dry-weight basis, % moisture will increase MRLs).
2 Reporting limits are based on 5.0 g of sample.
3 Units as specified unless otherwise noted.
4 Routine methods may be changed at the time of analysis due to sample-specific characteristics. The
actual analytical method used will be listed on the final report.
5 Mercury methods - Water: 245.1/200.8; Soil, Waste, and Tissue: 7473
NA-Not Available-ASB does not perform this analysis.
*This level or matrix is a special request and will need to be discussed with Section Chief on a case
by case basis. Consult laboratory for more information.
**These parameters are not usually requested or part of our routine scans. However, if the need arises,
please contact ASB personnel.
Page 83 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-5
ASB LOQAM Chapter 6 Table 6-5
Nutrients and Classicals Analyte List
Minimum Reporting Limits by Matrices
ANALYTE
Analytical Method 5
Water
mg/L
(ppm)1
Soil/Sed
mg/kg
(ppm)
Waste
mg/kg
(ppm)
Tissue
mg/kg
(ppm)
Acidity
SM 2310
10
NA
NA
NA
Alkalinity
SM 2320B
1.0
NA
NA
NA
Ammonia
EPA 350.1
0.05
2.52
2.52
NA
BOD/C-BOD
SM 5210B
2.0
NA
NA
NA
Bromide
EPA 300.0
0.1
1.0
NA
NA
Chloride
EPA 300.0
0.1
1.0
NA
NA
Cyanide
SM 335.4
0.015
0.75
0.75
NA
Fluoride
EPA 300.0
0.05
0.5
NA
NA
Hardness, Calc
SM 2340B
1.654
NA
NA
NA
Nitrate
EPA 300.0/EPA 353.2
0.05
0.5
0.5
NA
Nitrite
EPA 300.0/EPA 353.2
0.05
0.5
0.5
NA
Nitrate+Nitrite
EPA 353.2
0.05
0.5
0.5
NA
pH
EPA 9040/EPA 9045
1.0 pH units
1.0 pH units
1.0 pH units
1.0 pH units
Phosphorus, Total
EPA 365.1
0.01
1.254
1.254
NA
Phosphorus, Ortho
EPA 365.1
0.01
1.254
1.254
NA
Total Dissolved Solids
USGS1-1750-85
40
NA
NA
NA
Total Solids
SM 2540B-1997
40
NA
NA
NA
Total Suspended Solids
USGS 1-3765-85
4.0
NA
NA
NA
Volatile Solids
SM 2540 E
4.0/407
NA
NA
NA
Sulfate
EPA 300.0
0.1
1.0
NA
NA
Total Kjeldahl Nitrogen (TKN)
EPA 351.2
0.05
6.254
6.254
NA
Total Organic Carbon (TOC)
SM5310/ASB 107C
1.0
12,000
NA
NA
MRLs may increase due to variability of interferences that make dilutions of sample necessary. Sample sizes
required for achieving the routine quantitation limits are listed below.
1 Units as specified unless otherwise noted.
2 Calculated using 1.0 g of sample (dry-weight basis, % moisture will increase MRLs).
3 Calculated using 5.0 g of sample (dry-weight basis, % moisture will increase MRLs).
4 Calculated using 0.2 g of sample (dry-weight basis, % moisture will increase MRLs).
5 Routine methods may be changed at the time of analysis due to sample specific characteristics. The actual analytical
method used will be listed on the final report.
6 Analysis available upon request with sufficient lead-time.
7 MRL for volatile solids for the TSS method is 4.0 mg/L; if it is derived from the TDS method, then the MRL is 40 mg/L.
NA- Not Available-ASB does not perform this analysis.
Page 84 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-6
ASB LOQAM Chapter 6 Table 6-6
Volatile Organics (VOAs) Target Analyte List
M
[inimum Reporting Limits (MRLs) b;
y Matrices
Water1
(ig/L
(PPb)
Soil/Sed2
Hg/kg (ppb)
Waste3
mg/kg (ppm)
Air4'8
ppbv (fig/m3)
ANALYTE
Analytical
Method
Routine
Level
Routine Level
(Encore®/Tared
Vial)
Routine Level
Routine Level
EPA TO-156
Acetone
EPA 8260C
4.0-10
10-20
1.6-4.0
0.22
Acrylonitrile
EPA 8260C
NA
NA
NA
0.0184
Benzene
EPA 8260C
0.50
0.05
EPA 8260C
SIM
1.0
0.20
0.044
Benzyl Chloride
EPA 8260C
NA
NA
NA
0.22
EPA 8260C
0.50
0.050
Bromobenzene
EPA 8260C
SIM
1.0
0.20
NA
EPA 8260C
0.50
0.015
Bromochloromethane
EPA 8260C
SIM
1.0
0.20
NA
EPA 8260C
0.50
0.015
Bromodichloro methane
EPA 8260C
SIM
1.0
0.20
0.0101
EPA 8260C
1.0^.0
0.10
Bromoform
EPA 8260C
SIM
2.0-10
0.40-1.6
0.011
Bromomethane
EPA 8260C
2.0-5.0
2.0
0.80-2.0
0.0220
1,3-Butadiene
EPA 8260C
NA
NA
NA
0.0440
EPA 8260C
0.50
0.05
n-Butylbenzene
EPA 8260C
SIM
1.0
0.20
NA
EPA 8260C
0.50
0.05
sec-Butylbenzene
EPA 8260C
1.0
0.20
NA
SIM
EPA 8260C
0.50
0.05
tert-Butylbenzene
EPA 8260C
1.0-2.0
0.20
NA
SIM
EPA 8260C
0.50
0.05
Carbon Tetrachloride
EPA 8260C
SIM
1.0
0.20
0.0220
Carbon Disulfide
EPA 8260C
2.0
2.0
0.80
0.22
EPA 8260C
0.50
Chlorobenzene
EPA 8260C
SIM
0.05
1.0
0.20
0.022
Page 85 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Ch
Volatile Organics (VO
Minimum Reporting L
apter 6 Table 6-
As) Target Ana
imits (MRLs) b;
-6
lyte List
y Matrices
Water1
fig/L
(PPb)
Soil/Sed2
fig/kg (ppb)
Waste3
mg/kg (ppm)
Air4'8
ppbv (fig/m3)
ANALYTE
Analytical
Method
Routine
Level
Routine Level
(Encore®/Tared
Vial)
Routine Level
Routine Level
EPA TO-156
Chloroethane
EPA 8260C
EPA 8260C
SIM
2.0-5.0
0.05
2.0
0.80-2.0
0.022
Chloroform
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
Chloromethane
EPA 8260C
0.50
1.0
0.20
0.044
3-Chloroprene
(2-Chloro- 1,3-butadiene)
EPA 8260C
NA
NA
NA
0.044
o-Chlorotoluene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
p-Chlorotoluene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
Cyclohexane
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.20
Dibromochloromethane
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.20
l,2-Dibromo-3-
chloropropane7 (DBCP)
EPA 8260C
EPA 8260C
SIM
1.0-10
0.10
2.0-10
0.40-4.0
NA
1,2-Dibromoethane (EDB)7
EPA 8260C
EPA 8260C
SIM
1.0
0.025
1.0
0.20
0.022
Dibromomethane
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
1,2-Dichlorobenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.020
1,3-Dichlorobenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.022
1,4-Dichlorobenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.020
Page 86 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-6
Volatile Organics (VOAs) Target Analyte List
Minimum Reporting L
imits (MRLs) b;
y Matrices
Water1
fig/L
(PPb)
Soil/Sed2
fig/kg (ppb)
Waste3
mg/kg (ppm)
Air4'8
ppbv (fig/m3)
ANALYTE
Analytical
Method
Routine
Level
Routine Level
(Encore®/Tared
Vial)
Routine Level
Routine Level
EPA TO-156
Dichlorodifluoromethane
(R12)
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
1,1 -Dichloroethene7
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
cis-1,2-Dichloroethene
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
trans-1,2-Dichloroethene7
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.020
1,1 -Dichloroethane7
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
1,2-Dichloroethane7
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
1,2-Dichloropropane
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
1,3 -Dichloropropane
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
NA
2,2-Dichloropropane
EPA 8260C
EPA 8260C
SIM
0.50
0.050
1.0
0.20
NA
1,1 -Dichloropropene
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
NA
cis-1,3 -Dichloropropene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.020
Dichlorotetrafluoroethane
(R114)
EPA TO-15
NA
NA
NA
0.022
trans- 1,3-Dichloropropene
EPA 8260C
EPA 8260C
SIM
0.50
0.050
1.0
0.20
0.020
1,4-Dioxane
EPA TO-15
NA
NA
NA
0.24
Ethyl acetate
EPA TO-15
NA
NA
NA
0.022
Ethyl benzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.022
Page 87 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-6
Volatile Organics (VOAs) Target Analyte List
Minimum Reporting L
imits (MRLs) tr
y Matrices
Water1
fig/L
(PPb)
Soil/Sed2
fig/kg (ppb)
Waste3
mg/kg (ppm)
Air4'8
ppbv (fig/m3)
ANALYTE
Analytical
Method
Routine
Level
Routine Level
(Encore®/Tared
Vial)
Routine Level
Routine Level
EPA TO-156
4-Ethyltoluene
(l-Ethyl-4-methyl benzene)
EPA TO-15
NA
NA
NA
0.042
Heptane
EPA TO-15
NA
NA
NA
0.040
Hexachlorobutadiene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.022
Hexane
EPA TO-15
NA
NA
NA
0.044
Isooctane
(2,2,4- Trimethylpentane)
EPA TO-15
NA
NA
NA
0.020
Isopropanol
EPA TO-15
NA
NA
NA
0.22
Isopropylbenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
p-I sopropyltoluene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0-2.0
0.20
NA
Methyl acetate
EPA 8260C
0.50
2.0
0.40
NA
Methyl cyclohexane
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
Methylene chloride
(Dichloromethane)
EPA 8260C
EPA 8260C
SIM
0.50
0.050
10
0.20
0.20
Methyl butyl ketone
EPA 8260C
EPA 8260C
SIM
1.0
0.10
5.0-10
0.40
0.22
Methyl ethyl ketone
EPA 8260C
4.0-10
5.0-10
1.6-4.0
0.20
Methyl isobutyl ketone
EPA 8260C
EPA 8260C
SIM
1.0
0.10
5.0-10
0.40
0.22
Methyl-t-butyl ether
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
Naphthalene5
EPA 8260C
EPA 8260C
SIM
0.50-5.0
0.05
1.0-10
0.20-2.0
0.20
n-Propylbenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
Page 88 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-6
Volatile Organics (VOAs) Target Analyte List
Minimum Reporting L
imits (MRLs) b;
y Matrices
Water1
fig/L
(PPb)
Soil/Sed2
fig/kg (ppb)
Waste3
mg/kg (ppm)
Air4'8
ppbv (fig/m3)
ANALYTE
Analytical
Method
Routine
Level
Routine Level
(Encore®/Tared
Vial)
Routine Level
Routine Level
EPA TO-156
Styrene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.020
1,1,1,2-T etrachloroethane7
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
1,1,2,2-T etrachloroethane7
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.020
T etrachloroethene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.022
Tetrahydrofiiran
EPA TO-15
NA
NA
NA
0.20
Toluene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.044
1,2,3-Trichlorobenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
NA
1,2,4-Trichlorobenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.044
1,1,1 -T richloroethane7
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.022
1,1,2-Trichloroethane
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
Trichloroethene
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
Trichlorofluoromethane
(RH)
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
1,2,3-Trichloropropane
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0-2.0
0.20
NA
Trichlorotrifluoroethane
(R113)
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
1,2,4-T rimethylbenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.020
Page 89 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Ch
Volatile Organics (VO
Minimum Reporting L
apter 6 Table 6-
As) Target Ana
imits (MRLs) tr
-6
lyte List
y Matrices
Water1
fig/L
(PPb)
Soil/Sed2
Hg/kg (PPb)
Waste3
mg/kg (ppm)
Air4-8
PPbv (p.g/m3)
ANALYTE
Analytical
Method
Routine
Level
Routine Level
(Encore®/Tared
Vial)
Routine Level
Routine Level
EPA TO-156
1,3 >5 -T rimethylbenzene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.022
Vinyl acetate
EPA TO-15
NA
NA
NA
0.22
Vinyl bromide
(Bromoethene)
EPA TO-15
NA
NA
NA
0.022
Vinyl chloride7
EPA 8260C
EPA 8260C
SIM
0.50
0.015
1.0
0.20
0.022
o-Xylene
EPA 8260C
EPA 8260C
SIM
0.50
0.05
1.0
0.20
0.02
(m- and/or p-) Xylene
EPA 8260C
EPA 8260C
SIM
1.0
0.10
2.0
0.40
0.04
Acrolein
EPA
8260C
10-20
NA5
4.05
0.0485
Acrylonitrile
EPA
8260C
10-20
NA5
4.05
0.0185
Methyl Methacrylate
EPA
8260C
0.50
NA5
0.25
NA5
2-Chloroethyl vinyl ether
EPA
8260C
1.0-4.0
NA5
0.45
NA5
2,3-Benzofuran
EPA
8260C
0.50
NA5
0.25
NA5
1,2,3-Trimethylbenzene
EPA
8260C
0.50
NA5
0.25
NA5
MRLs may increase due to variability of interferences necessitating sample dilutions.
1 Water - 5 mL from septum-sealed vial.
2 Routine Level Soil - 5 g in water (reported on dry-weight basis).
3 Waste -1 g dissolved in 5-mL methanol and 62.5 uL of resulting extract purged.
4 Air - 250 cc from 6-L passivated canister - nominal values. MRLs in (ie/m3 units depend on molecular weight and
vary depending on the analyte and the standard lot.
s Not routinely reported but available upon request.
6 MRLs don't account for the ~2x pressurization dilution of canisters after arrival at the lab.
7 SIM MRLs available for waters upon special request.
8 NATTS SIM MRLs are 10X lower than routine MRLs.
NA - Not Available- ASB does not perform this analysis.
Page 90 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-7
ASB LOQAM Chapter 6 T.
Semivolatile Organics Target A
Minimum Reporting Limits b;
able 6-7
jialyte List
Y Matrices
Water1
fig/L
(PPb)
Soil/Sed2
(PPb)
Waste3
mg/kg
(ppm)
Tissue4
mg/kg
(ppm)
ANALYTE
Analytical
Method
Routine
Level
Routine
Level
Routine
Level
Routine
Level
1 -Methylnaphthalene
EPA 8270D
2.0
66
20
0.066
1,1-Biphenyl
EPA 8270D
2.0
66
20
0.066
1,4-Dioxane
EPA 8270D
2.0
66
NA
NA
1,2,4-Trichlorobenzene
EPA 8270D
10
330
100
0.33
2-Nitrophenol
EPA 8270D
10
330
100
0.33
2-Methyl-4,6-dinitrophenol
EPA 8270D
10
330
100
0.33
2,4-Dimethylphenol
EPA 8270D
10
330
100
0.33
2,4-D initrotoluene
EPA 8270D
10
330
100
0.33
2,4-Dinitrophenol
EPA 8270D
20
660
200
0.66
2-Methylphenol
EPA 8270D
10
330
100
0.33
2-Nitroaniline
EPA 8270D
10
330
100
0.33
2-Chlorophenol
EPA 8270D
10
330
100
0.33
2-Methylnaphthalene
EPA 8270D
2.0
66
20
0.066
2,3,4,6-T etrachlorophenol
EPA 8270D
10
330
100
0.33
2,4,5-Trichlorophenol
EPA 8270D
10
330
100
0.33
2-Chloronaphthalene
EPA 8270D
10
330
100
0.33
2,6-Dinitrotoluene
EPA 8270D
10
330
100
0.33
2,4-Dichlorophenol
EPA 8270D
10
330
100
0.33
2,4,6-Trichlorophenol
EPA 8270D
10
330
100
0.33
3,3 '-Dichlorobenzidine
EPA 8270D
10
330
100
0.33
(3- and/or 4-) Methylphenol
EPA 8270D
10
330
100
0.33
3-Nitroaniline
EPA 8270D
10
330
100
0.33
4-Chlorophenyl phenyl ether
EPA 8270D
10
330
100
0.33
4-Chloroaniline
EPA 8270D
10
330
100
0.33
4-Nitroaniline
EPA 8270D
10
330
100
0.33
4-Nitrophenol
EPA 8270D
10
330
100
0.33
Page 91 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-7
Semivolatile Organics Target Analyte List
Minimum Reporting Limits by Matrices
Water1
fig/L
(PPb)
Soil/Sed2
fig/kg
(PPb)
Waste3
mg/kg
(ppm)
Tissue4
mg/kg
(ppm)
ANALYTE
Analytical
Method
Routine
Level
Routine
Level
Routine
Level
Routine
Level
4-Chloro-3-methylphenol
EPA 8270D
10
330
100
0.33
4-Bromophenyl phenyl ether
EPA 8270D
10
330
100
0.33
Acenaphthene
EPA 8270D
2.0
66
20
0.066
Acenaphthylene
EPA 8270D
2.0
66
20
0.066
Acetophenone
EPA 8270D
10
330
100
0.33
Anthracene
EPA 8270D
2.0
66
20
0.066
Atrazine
EPA 8270D
10
330
100
0.33
Benzo [a] anthracene
EPA 8270D
2.0
66
20
0.066
Benzo[a]pyrene
EPA 8270D
2.0
66
20
0.066
Benzo [b] fluoranthene
EPA 8270D
2.0
66
20
0.066
B enzo [k] fluoranthene
EPA 8270D
2.0
66
20
0.066
Benzo[g,h,i]perylene
EPA 8270D
2.0
66
20
0.066
Benzaldehyde
EPA 8270D
10
330
100
0.33
Benzyl butyl phthalate
EPA 8270D
10
330
100
0.33
Bis(2-ethylhexyl) phthalate
EPA 8270D
10
330
100
0.33
Bis(2-chloroethyl) ether
EPA 8270D
10
330
100
0.33
B is(chloroethoxy)methane
EPA 8270D
10
330
100
0.33
Bis(chloroisopropyl) ether
EPA 8270D
10
330
100
0.33
Caprolactam
EPA 8270D
10
330
100
0.33
Carbazole
EPA 8270D
2.0
66
20
0.066
Chrysene
EPA 8270D
2.0
66
20
0.066
Di-n-butyl phthalate
EPA 8270D
10
330
100
0.33
Di-n-octyl phthalate
EPA 8270D
10
330
100
0.33
Dibenz(a,h)anthracene
EPA 8270D
2.0
66
20
0.066
Dibenzofiiran
EPA 8270D
2.0
66
20
0.066
Diethyl phthalate
EPA 8270D
10
330
100
0.33
Page 92 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-7
Semivolatile Organics Target Analyte List
Minimum Reporting Limits by Matrices
Water1
(ig/L
(PPb)
Soil/Sed2
fig/kg
(PPb)
Waste3
mg/kg
(ppm)
Tissue4
mg/kg
(ppm)
ANALYTE
Analytical
Method
Routine
Level
Routine
Level
Routine
Level
Routine
Level
Dimethyl phthalate
EPA 8270D
10
330
100
0.33
Fluoranthene
EPA 8270D
2.0
66
20
0.066
Fluorene
EPA 8270D
2.0
66
20
0.066
Hexachlorobenzene (HCB)
EPA 8270D
10
330
100
0.33
Hexachlorobutadiene
EPA 8270D
10
330
100
0.33
Hexachlorocyclopentadiene (HCCP)
EPA 8270D
10
330
100
0.33
Hexachloroethane
EPA 8270D
10
330
100
0.33
Indeno[l ,2,3-cd]pyrene
EPA 8270D
2.0
66
20
0.066
Isophorone
EPA 8270D
10
330
100
0.33
N-Nitrosodiphenylamine
EPA 8270D
10
330
100
0.33
Naphthalene
EPA 8270D
2.0
66
20
0.066
Nitrobenzene
EPA 8270D
10
330
100
0.33
Nitroso-di-n-propylamine
EPA 8270D
10
330
100
0.33
Pentachlorophenol
EPA 8270D
10
330
100
0.33
Phenanthrene
EPA 8270D
2.0
66
20
0.066
Phenol
EPA 8270D
10
330
100
0.33
Pyrene
EPA 8270D
2.0
66
20
0.066
MRLs may increase due to possible interferences necessitating sample dilutions and moisture content of soil
samples.
1 Water - 1000 mL; final extract volume 1 mL.
2 Soil - 30 g extracted (reported as dry-weight); final extract volume 1 mL.
3 Waste -1 g extracted (reported as wet-weight); final extract volume 10 mL.
4 Fish or biological tissue - Same as soil.
s SA = Special Analysis requiring additional QC currently not in place. Contact OCS Section Chief. Tentative MRL.
NA-Not Applicable -ASB does not perform analysis for this compound.
Page 93 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-8
ASB LOQAM C
Semivolatile Organic*
Minimum Reportin
hapter 6 Table 6-8
Full Scan - Low Level
g Limits by Matrices
Water1
fig/L
(PPb)
Soil/Sed2
fig/kg
(PPb)
Waste
mg/kg
(PPm)
Tissue
mg/kg
(PPm)
ANALYTE
Analytical
Method
Low
Level
Low
Level
Low
Level
Low
Level
1 -Methylnaphthalene
EPA 8270D
0.1
3.33
NA
NA
2-Methylnaphthalene
EPA 8270D
0.1
3.33
NA
NA
Acenaphthene
EPA 8270D
0.1
3.33
NA
NA
Acenaphthylene
EPA 8270D
0.1
3.33
NA
NA
Anthracene
EPA 8270D
0.1
3.33
NA
NA
B enzo [a] anthracene
EPA 8270D
0.1
3.33
NA
NA
Benzo[a]pyrene
EPA 8270D
0.1
3.33
NA
NA
Benzo[b]fluoranthene
EPA 8270D
0.1
3.33
NA
NA
B enzo [k] fluoranthene
EPA 8270D
0.1
3.33
NA
NA
Benzo[g,h,i]perylene
EPA 8270D
0.1
3.33
NA
NA
Carbazole
EPA 8270D
0.1
3.33
NA
NA
Chrysene
EPA 8270D
0.1
3.33
NA
NA
Dibenz(a,h)anthracene
EPA 8270D
0.1
3.33
NA
NA
Fluoranthene
EPA 8270D
0.1
3.33
NA
NA
Fluorene
EPA 8270D
0.1
3.33
NA
NA
Indeno[ 1,2,3-cd]pyrene
EPA 8270D
0.1
3.33
NA
NA
Naphthalene
EPA 8270D
0.1
3.33
NA
NA
Pentachlorophenol
EPA 8270D
1.03
33.3
NA
NA
Phenanthrene
EPA 8270D
0.1
3.33
NA
NA
Pyrene
EPA 8270D
0.1
3.33
NA
NA
MRLs may increase due to interferences necessitating smaller extraction amounts, dilutions and moisture
content of soil samples. The above analytes can also be analyzed by full scan GC/MS at the stated MRLs.
1 Water - 1000 ml; final extract 1 mL1 Water - 1000 mL; final extract volume 1 mL.
2 Soil - 30 g extracted (reported as dry-weight); final extract 1 mL
3 0.2 ug/L can be reported if specifically requested.
NA- Not available- ASB does not perform this analysis.
Page 94 of 100
-------
ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-9
ASB LOC
Routine Pestii
Minimum Repori
(AM Chapter 6 Table 6-9
cide/PCB Target Analyte List
ing Limits (MRLs)* by Matrices
Water1
fig/L (ppb)
Soil/Sed2
fig/kg (ppb)
Waste3
mg/kg (ppm)
Tissue4
mg/kg (ppm)
ANALYTE
Analytical
Method(s)
Routine
Level
Routine
Level
Routine
Level
Routine
Level
Aldrin
EPA 8081B
0.04
1.3
SA5-0.50
0.020
Heptachlor
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Heptachlor epoxide
EPA 8081B
0.04
1.3
SA5-0.50
0.020
a-BHC
EPA 808IB
0.04
1.3
SA5-0.50
0.020
P-BHC
EPA 808IB
0.04
1.3
SA5-0.50
0.020
y-BHC
EPA 808IB
0.04
1.3
SA5-0.50
0.020
8-BHC
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Endosulfan I
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Dieldrin
EPA 808IB
0.04
1.3
SA5-0.50
0.020
p,p'-DDT
EPA 808IB
0.04
1.3
SA5-0.50
0.020
p,p'-DDE
EPA 808IB
0.04
1.3
SA5-0.50
0.020
p,p'-DDD
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Endrin
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Endosulfan II
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Endosulfan sulfate
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Endrin aldehyde
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Endrin ketone
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Methoxychlor
EPA 808IB
0.04
1.3
SA5-1.0
0.050
¦y-Chlordane
EPA 808IB
0.04
1.3
SA5-0.50
0.020
a-Chlordane
EPA 808IB
0.04
1.3
SA5-0.50
0.020
Aroclor 1221
EPA 8082A
1.0
33
SA5-5.0
0.20
Aroclor 1232
EPA 8082A
1.0
33
SA5-2.5
0.10
Aroclor 1242
EPA 8082A
1.0
33
SA5-2.5
0.10
Aroclor 1016
EPA 8082A
1.0
33
SA5-2.5
0.10
Aroclor 1248
EPA 8082A
1.0
33
SA5-2.5
0.10
Aroclor 1254
EPA 8082A
1.0
33
SA5-2.5
0.10
Aroclor 1260
EPA 8082A
1.0
33
SA5-2.5
0.10
Page 95 of 100
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ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOC
Routine Pestii
Minimum Repori
(AM Chapter 6 Table 6-9
cide/PCB Target Analyte List
ing Limits (MRLs)* by Matrices
Water1
fig/L (ppb)
Soil/Sed2
fig/kg (ppb)
Waste3
mg/kg (ppm)
Tissue4
mg/kg (ppm)
ANALYTE
Analytical
Method(s)
Routine
Level
Routine
Level
Routine
Level
Routine
Level
Aroclor 1262
EPA 8082A
1.0
33
SA5-2.5
0.10
Aroclor 1268
EPA 8082A
1.0
33
SA5-2.5
0.10
Toxaphene
EPA 808 IB
5.0
170
SA5-20
SAM.O
MRLs may increase due to possible interferences necessitating sample dilutions and moisture content of
soil samples.
1 Water - 1000 mL extracted; 8081/8082A, final extract volume 10 mL.
2 Soil - 30 g extracted (reported as dry-weight); 8081/8082A, final extract volume 10 mL.
3 Waste -1 g extracted (reported as wet-weight); final extract volume 10 mL.
4 Fish or biological tissue - 10 g extracted (reported as wet-weight); final extract volume 10 mL.
s SA = Special Analysis requiring additional QC currently not in place. Contact OCS Chief. Tentative MRL.
*Pesticide/PCB water and soil MRLs set by ASB at CLP reporting levels.
Page 96 of 100
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ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-10
ASB LOQAM Chapter 6 Table 6-10
Pesticide/PCB Analvte l ist Performed hv SPECIAL RFOIJFST ONI.Y
Minimum Reporting Limits (MRLs) by Matrices
Water1
(ig/L (ppb)
Soil/Sed2
fig/kg (PPb)
Waste3
mg/kg (ppm)
Tissue4
mg/kg (ppm)
ANALYTE
Analytical
Method(s)
Routine
Level
Routine
Level
Routine
Level
Routine
Level
Technical Chlordane6
EPA 8081B
SA5-1.5
SA5-50
SA5-1.5
SA5-0.050
P-Chlordene
Modified 8270
SA5-0.50
SA5-20
SA5-0.50
SA5-0.020
Chlordene
Modified 8270
SA5-0.50
SA5-20
SA5-0.50
SA5-0.020
a-Chlordene
Modified 8270
SA5-0.50
SA5-20
SA5-0.50
SA5-0.020
trans-Nonachlor
Modified 8270
S A5-0.50
SA5-20
S A5-0.50
SA5-0.020
cis-Nonachlor
Modified 8270
S A5-0.50
SA5-20
S A5-0.50
SA5-0.020
Dicofol
Modified 8270
0.080
5.0
NA
NA
4,4'-Dichlorobenzophenone
Modified 8270
0.080
5.0
NA
NA
Chlorobenzilate
Modified 8270
SA5-0.020
SA5-0.67
NA
NA
2,4'-DDT
Modified 8270
SA5-0.040
SA5-1.3
NA
SA5-0.0013
2,4'-DDE
Modified 8270
SA5-0.020
SA5-0.67
NA
SA5-0.0067
2,4'-DDD
Modified 8270
SA5-0.040
SA5-1.3
NA
SA5-0.0013
PCB (as Congeners) - Green List
EPA 8082A
0.020
1.0
SA5-0.20
SA5-0.0010
Diazinon
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Methyl Parathion
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Trithion (Carbophenothion)
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Malathion
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Guthion
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Dichlorvos (DDVP)
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Vernolate
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Dimethoate
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Dursban (Chlorpyrifos)
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Phorate
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Ronnel
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Atrazine
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Alachlor
EPA 8270D
SA5-1.0
SA5-33
SA5-12.5
SA5-0.25
Stirofos
EPA 8270D
SA5-1.0
SA5-33
SA5-2.5
SA5-0.050
Page 97 of 100
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ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
ASB LOQAM Chapter 6 Table 6-10
Pesticide/PCB Analyte List Performed by SPECIAL REQUEST ONLY
Minimum Reporting Limits (MRLs) by Matrices
Water1
Hg/L (ppb)
Soil/Sed2
Hg/kg (ppb)
Waste3
mg/kg (ppm)
Tissue4
mg/kg (ppm)
ANALYTE
Analytical
Method(s)
Routine
Level
Routine
Level
Routine
Level
Routine
Level
Toxaphene (as congeners except
Parlar 62)
EPA 8276
0.0010
0.033
SA5-0.005
0.0001
Toxaphene Parlar 62
EPA 8276
0.0050
0.17
SAs-0.0250
0.0005
MRLs may increase due to interferences necessitating smaller extraction amounts and dilutions. Percent moisture
content of soil samples also affects MRLs.
1 Water - 1000 mL extracted: 8081A/8082, final extract volume 10 mL; 8276, final extract volume 1 mL;
- 35 mL extracted: 8011, final extract volume 2 mL.
1 Soil - 30 g extracted (reported on dry-weight basis); 8081A/8082, final extract volume 10 mL.
3 Waste -1 g extracted (reported on wet-weight basis); final extract volume 10 mL.
14 Fish or biological tissue -10 g extracted (reported on wet-weight basis); final extract volume 10 mL. Toxaphene
congeners: 10 g extracted (reported on wet-weight basis); final extract volume 1.0 mL.
5 SA = Special Analysis requiring additional QC currently not in place. Contact OCS Section Chief. Tentative MRL.
6 For TCLP samples, Chlordane must be specifically requested if it is an analyte of interest.
7 See Appendix 3 VOA MRLs - 8260 SIM method
NA - Not Available- ASB does not perform this analysis.
Page 98 of 100
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ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-11
ASB LOQAM Chapter 6 Table 6-11
Herbicides Target Analyte List
Minimum Reporting Limits (MRLs) by
Matrices
Water1
M'g/L (ppb)
Soil/Sed
fig/kg (ppb)
Waste
mg/kg
(ppm)
Tissue
mg/kg
(ppm)
ANALYTE
Analytical
Method
Routine
Level
Routine
Level
Routine
Level
Routine
Level
2,4,5-T
EPA 832IB
1.0
NA
NA
NA
2,4-D
EPA 832IB
1.0
NA
NA
NA
2,4-DB
EPA 832IB
2.0
NA
NA
NA
Silvex (2,4,5-TP)
EPA 832 IB
1.0
NA
NA
NA
Dalapon
EPA 832 IB
2.0
NA
NA
NA
Dicamba
EPA 832IB
1.0
NA
NA
NA
Dichlorprop
EPA 832IB
1.0
NA
NA
NA
Dinoseb
EPA 832IB
4.0
NA
NA
NA
MCPA
EPA 832IB
5.0
NA
NA
NA
MCPP
EPA 832IB
5.0
NA
NA
NA
MRLs may increase due to interferences necessitating smaller sample amounts and dilutions.
NA - Not Available-ASB does not perform this analysis.
Page 99 of 100
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ASB LOQAM
Chapter 6
Effective Date: April 24, 2018
Table 6-12
ASB LOQAM Chapter 6 Table 6-12
Per - and Polyfluoroalkyl Substances (PFAS) Target Analyte List
Minimum Reporting Limits (MRLs) by Matrices
Water
fig/L
(PPb)
Soil/Sed
fig/kg
(PPb)
Waste
fig/kg
(PPb)
Tissue
mg/kg
(ppm)
ANALYTE
Analytical
Method
Routine
Level
Routine
Level
Routine
Level
Routine
Level
Perfluorotetradecanoic acid (PFTeDA)
ASBPROC-800
0.080
NA
0.047
NA
Perfluorotridecanoic acid (PFTrDA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorododecanoic acid (PFDoA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluoroundecanoic acid (PFUDA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorodecanoic acid (PFDA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorononanoic acid (PFNA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorooctanoic acid (PFOA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluoroheptanoic acid (PFHpA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorohexanoic acid (PFHxA)
ASBPROC-800
0.040
NA
0.047
NA
Perfluoropentanoic acid (PFPeA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorobutyric acid (PFBA)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorodecanesulfonate (PFDS)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorononanesulfonate (PFNS)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorooctanesulfonate (PFOS)
ASBPROC-800
0.040
NA
0.040
NA
Perfluoroheptanesulfonate (PFHpS)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorohexanesulfonate (PFHxS)
ASBPROC-800
0.040
NA
0.040
NA
Perfluoropentanesulfonate (PFPeS)
ASBPROC-800
0.040
NA
0.040
NA
Perfluorobutanesulfonate (PFBS)
ASBPROC-800
0.040
NA
0.040
NA
Perf luorooctanesulfonamide (FO S A)
ASBPROC-800
0.040
NA
0.040
NA
Fluorotelomer sulfonate 8:2 (8:2 FTS)
ASBPROC-800
0.040
NA
0.040
NA
Fluorotelomer sulfonate 6:2 (6:2 FTS)
ASBPROC-800
0.040
NA
0.040
NA
Fluorotelomer sulfonate 4:2 (4:2 FTS)
ASBPROC-800
0.040
NA
0.040
NA
N -ethyl-N -((heptadecafluorooctyl)sulfonyl)glycine
(N-EtFOSAA)
ASBPROC-800
0.040
NA
0.040
NA
N-(Heptadecafluorooctylsulfonyl)-N-methylglycine
(N-MeFOSAA)
ASBPROC-800
0.040
NA
0.056
NA
Hexafluoropropylene oxide-dimer acid (HFPO-DA)
ASBPROC-800
0.040
NA
0.040
NA
MRLs may increase due to interferences necessitating smaller sample amounts and dilutions.
NA -Not Available- ASB does not perform this analysis.
Page 100 of 100
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