QUALITY MANUAL

for

State of Florida
Department of Environmental Protection
Bureau of Laboratories
FDOH Certification Number E31780

January 2012

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Quality Manual for

State of Florida
Department of Environmental Protection
Central Laboratory

FDOH Certification #E31780

Central Laboratory
Laboratory Annex
2600 Blair Stone Road
Tallahassee, FL 32399-2400
(850) 245-8085

Prepared and Maintained by

FDEP Bureau of Laboratories
Laboratory Support Section

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Table of Contents
QA Plan Elements

Contents

Description

Page #

Title Page

Table of contents

Acronyms

Introduction, Scope and Applicability

12

1.1 Introduction
1.2 Scope
1.3 Applicability

12
12
12

2.0

References

12

3.0

Terms and Definitions

12

4.0

Management Requirements

13

4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9
4.10
4.11
4.12
4.13
4.14
4.15
4.16

13
15
25
26
27
28
28
29
29
29
30
31
31
36
37
37

1.0

5.0

Organization
Management System
Document Control
Review of Requests, Tenders and Contracts
Subcontracting of Environmental Tests
Purchasing Services and Supplies
Services to the Client
Complaints
Control Of Non-conforming Environmental Test Work
Improvement
Corrective Action
Preventive Action
Control of Records
Internal Audits
Management Reviews
Date Integrity Investigations

Technical Requirements
5.1 General
5.2 Personnel

38
38
38

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Contents

Appendix A

Appendix B

Appendix C

Description

Page #

5.3 Accommodation and Environmental Conditions

5.4 Environmental Test Methods and Method Validation
5.5 Calibration Requirements
5.6 Measurement Traceability
5.7 Collection of Samples
5.8 Handling Samples and Test Items
5.9 Quality Assurance for Environmental Testing
5.10 Reporting Results

39
40
43
45
45
46
52
58

Roles and Responsibilities for the Chemical Agent Laboratory

61

1.1
1.2
1.3
1.4
1.5
1.6

Laboratory director
Laboratory Manager
Chemical Agent Hygiene Officer
Agent Manager
Chemical Agent Operators
Inventory Witness

61
61
62
63
63
64

Chemistry Essential Quality Controls

65

1.0
2.0
3.0
4.0
5.0
6.0
7.0

65
65
65
65
65
67
68

Introduction
Scope
Terms and Definitions
Method Selection
Method Validation
Demonstration of Capability
Technical Requirements

References

73

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FIGURES
Figure Number

Description

Page Number

4.1

Chemistry Organization Chart

19

4.2

Biology Section Organizational Chart

21

4.3

Laboratory Support Section Organization Chart

23

4.4

DEP Contract Task Assignment Form

27

4.5

Sampling Kit Packing List

33

4.6

Chain of Custody Record

33

4.7

Laboratory Custody Log

33

4.8

Biology Bench Sheets and Logs

34

4.9

Chemistry Preparation Logs

34

4.10

Laboratory Audit Checklists

37

5.1

Sample Backlog Report

51

TABLES
Table Number

Description

Page Number
30

4.1

Corrective Actions in Biology

31

4.2

Preventive Maintenance Biology

31

4.3

Waste Disposal Procedures

34

5.1

Chemistry QA Targets for MDL/PQL, Precision and Accuracy

40

5.2

Biology QA Targets for MDL/PQL, Precision and Accuracy

40

5.3

Biology Instrument Calibration

43

5.4

Standard Sources, Preparation, Storage and Traceability

45

5.5

Reagent Storage

45

5.6

Sampling Equipment in Biology

46

5.7

Chemistry Method Modifications

40

5.8

Biology Method Modifications

40

5.9

Sample Containers, Preservation Techniques and Hold Times

51

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ACRONYMS
ADaPT
AM
AMU
BETX
BFB
BOD
BNA
CA
CAHO
CAO
CAS Number
CBOD
CCC
CCCS
CCV
CFR
CHO
CHP
CI
CLP
cm
COD
COR
CV
CVAAS
CVAFS
DF
DFTPP
DOT
DSHP
ECBC
ECD
EI
EICP
EPA
ERLN
FAC
FDEP

Automated Data Processing Tool

Agent Manager
Atomic Mass Unit
Benzene, Ethyl benzene, Toluene and Xylenes
Bromofluorobenzene used for mass spectral tuning
Biochemical Oxygen Demand
Base/Neutral, Acid Extractables
Chemical Agent
Chemical Agent Hygiene Officer
Chemical Agent Operator
Chemical Abstract Services Number
Carbonaceous Biochemical Oxygen Demand
Continuing Calibration Compounds
Continuing Calibration Check Standard
Continuing Calibration Verification
Code of Federal Regulations
Chemical Hygiene Officer
Chemical Hygiene Plan
Chemical Ionization
Contract Laboratory Program
centimeter
Chemical Oxygen Demand
Contract Officer's Representative
Coefficient of Variation
Cold Vapor Atomic Absorption Spectrometry
Cold Vapor Atomic Fluorescence Spectrometry
Dilution Factor
Decafluorotriphenyl Phosphine
Department of Transportation
Dilute Solution Hygiene Plan
U.S. Army Edgewood Chemical and Biological Center and Engineering Center
Electron Capture Detector
Electron Ionization
Extracted Ion Current Profile (plot of ion abundance vs. time)
Federal Environmental Protection Agency
Environmental Response Laboratory Network
Florida Administrative Code
Florida Department of Environmental Protection

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FDOH
GC
GC/AFD
GC/MS
GLP
HPLC
Hz
I.D.
ICAL
ICCS
ID
IR
IS
ISE
IUPAC
L
LC
LCS
LFB
LIMS
LM
LOD
LOQ
m
MDL
MS
MSD
MW
NELAP
NIOSH
NIST
NPD
NPDES
NTU
C
P&T
PDF
PE
PM 2.5

Florida Department of Health

Gas Chromatograph
Gas Chromatograph/Atomic Fluorescence Detection
Gas Chromatograph/Mass Spectrometry
Good Laboratory Practice
High Pressure Liquid Chromatography
Hertz
Internal Diameter
Initial Calibration
Initial Calibration Check Standard
Identification
Infrared
Internal Standard
Ion Selective Electrode
International Union of Pure and Applied Chemistry
Liter
Liquid Chromatography
Laboratory Control Sample
Laboratory Fortified Blank
Laboratory Information Management System
Laboratory Manager
Limit of Detection
Limit of Quantitation
Meter
Method Detection Limit
Mass Spectrometry
Matrix Spike Duplicate or Mass Selective Device
Molecular Weight
National Environmental Laboratory Accreditation Program
National Institute of Occupational Safety and Health
National Institute for Standards and Technology
Nitrogen Phosphorus Detector
National Pollution Discharge Elimination System
Nephelometric Turbidity Units
Degrees Celsius
Purge and Trap
Portable Document Format
Performance Evaluation
Particulate Matter 2.5 Microns

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ppb
PPE
ppm
ppt
PQL
PT
PTFE
QA/QC
QAP
QATs
QCCS
QM
RCRA
RF
RL
RPD
RRF
RRT
RSD
RT
S/N
SARA
SD
SIM
SOP
SPCC
TCLP
TIC
TNI
UDA
VOA
VOC
ZHE

Parts per billion

Personnel Protective Equipment
Parts per million
Parts per trillion
Practical Quantitation Limit
Proficiency Testing
Polytetrafluoroethylene
Quality Assurance/Quality Control
Quality Assurance Plan
Quality Assurance Targets
Quality Control Check Standard
Quality Manual
Resource Conservation and Recovery Act
Radio Frequency; Response Factor
Reporting Limit
Relative Percent Difference
Relative Response Factor
Relative Retention Time
Relative Standard Difference
Retention Time
Signal-to-Noise Ratio
Superfund Amendments and Reauthorization Act
Standard Deviation
Selective Ion Monitoring
Standard Operating Procedure
System Performance Check Compounds
Toxicity Characteristic Leaching Procedure
Total Ion Current; Tentatively Identified Compound
The NELAC Institute
Ultra Dilute Agent
Volatile Organic Analysis
Volatile Organic Compound
Zero Headspace Extraction

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1.0

INTRODUCTION, SCOPE AND APPLICABILITY

1.1

INTRODUCTION

The FDEP Bureau of Laboratories mission is to aid in the protection of Floridas environment
by providing legally defensible and scientifically credible analytical and technical support to
the Department. Information generated by the Bureau of Laboratories is fundamental to
the Department in carrying out its mission to preserve, protect, conserve, and restore the
air, water, and natural resources of the state. The Bureau of Laboratories management is
committed to generating data of the highest quality necessary for fulfilling the mission of the
laboratory.
1.2
SCOPE
The FDEP Central Laboratory is a full service environmental laboratory which provides
chemical and biological analytical support to the following:
a. departmental programs
b. district operations
c. water management districts
d. environmental operations of other state agencies and commissions
e. local, state, and federal law enforcement agencies
The laboratory also provides chemical and biological analytical consulting services to the
above listed programs.
1.3

APPLICABILITY

This document serves as the Quality Manual (QM) for the Chemistry and Biology sections of
the Bureau of Laboratories.

2.0

REFERENCES

See Appendix C

3.0

TERMS AND DEFINITIONS

The relevant definitions from The NELAC Institute Standard, Volume 1, Module 2, Section 3.0
are the preferred references. See the TNI Standard. Definitions related to this document
that are used differently or do not exist in the above references are defined in the text.

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4.0

MANAGEMENT REQUIREMENTS

4.1

ORGANIZATION

4.1.1 The Bureau of Laboratories is part of the Division of Environmental Assessment and
Restoration of the Florida Department of Environmental Protection. The Central Laboratory
is located at 2600 Blair Stone Road, Laboratory Annex, Tallahassee, FL 32399-2400. The
telephone number is (850) 245-8085. The Florida Department of Health (FDOH) Certification
Number is E31780.
4.1.2 This Quality Manual (QM) in conjunction with the Standard Operating Procedures
(SOPs) provides guidance for the laboratory operations and serves as the document that
defines the criteria necessary to meet the standards of TNI. This QM details the activities
and evaluation criteria necessary to ensure that analytical data meet the requirements of
TNI. This QM also documents procedures intended to ensure that all data are of high and
known quality in order to meet the scientific objectives of the Department.
4.1.3 Unless otherwise agreed upon with the customer in order to meet the objectives of a
given project, the management system described in this document is applicable to all
chemistry and biology tests performed by the facility described in 4.1.1.
4.1.4 The responsibilities of key personnel are outlined in Section 4.1.5 of the QM. These
responsibilities are performed by the key personnel identified or duly delegated
representatives.
4.1.5 The FDEP Central Laboratory:
(a) Conducts an annual management review according to Bureau Standard Operating
Procedure SOP LB-010, Quality System Management Review, to ensure the maintenance
of data integrity, quality and efficiency.
(b) Requires that all laboratory employees are responsible and conduct themselves in a
manner that does not impact the competence and operational integrity of the laboratory
as outlined in SOP LB-012, Code of Ethics.
(c) Is subject to Chapter 119 of Florida Statutes; therefore all records and documents
generated by the FDEP Central Laboratory, except those associated with active criminal
investigations, are public records and may be subject to disclosure according to the
guidelines and exceptions published in said Chapter. The Laboratory cannot guarantee
the confidentiality of reports transmitted electronically or by facsimile.
(d) Has a data integrity training program (See section 5.2.7).
(e) Has a defined organizational structure including quality management, support
services and technical operations, see Figure 4.1 (Chemistry Organization Chart), Figure
4.2 (Biology Organization Chart) and Figure 4.3 (LAB Support Organization Chart).

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(f) Maintains job descriptions for all employees. See Figures 4.1, 4.2 and 4.3 for the
responsibilities of key personnel.
(g) Annually reviews and updates (if necessary) all SOPs. The protocol for updating and
reviewing SOPs is described in SOP LB-001, Protocol for Preparing Standard Operating
Procedures, and in SOP LB-010, Quality System Management Review. Any updates to
SOPs must have the approval of the supervisor responsible for the procedure contained
in said SOP and must conform to the policies of the laboratory. It is the responsibility of
laboratory supervisors to ensure proper documentation demonstrating that their
employees have read, understood and are using the latest versions of SOPs and that this
is documented in the LIMS training module. The latest official versions of SOPs are only
located on the FDEP Intranet site and are accessible to all analysts and technicians
throughout the laboratory. Laboratory analysts are required to successfully analyze
initial and on-going demonstrations of capability according to Appendix B, section 6.0.
(h) Has technical management as identified in section 4.1.7.2.
(i) Has a full time designated Quality Assurance Officer. See section 4.1.7.1 for a
description of responsibilities.
(j) Has alternate supervisors who, in the absence of key management personnel, are
assigned to assume their responsibilities. In the absence of the Laboratory Director the
Environmental Administrators will assume his duties.
(k) Has ethics training described in section 5.2.7 emphasizing the importance of the
activities of each employee and the ramifications of them not performing their
responsibilities according to laboratory procedures and policies.
4.1.6 A Quality System Management Review takes place annually to ensure that
management holds regular staff meetings to discuss quality issues, workload and staffing
issues and other items of importance to the laboratory. Necessary changes to the quality
system as a consequence of performance on proficiency samples, round robins, split samples
or audits are discussed for incorporation and implementation. See SOP LB-010, Quality
System Management Review, for further information.
4.1.7 Additional requirements
4.1.7.1 The Quality Assurance Officer or his designee:
(a) serves as the primary contact for oversight and review of quality control data
(b) conducts all Quality Assurance responsibilities independent of other laboratory
operations
(c) conducts oversight of QA data without outside influence
(d) has experience in QA/QC procedures and the laboratory Quality System
(e) has experience with the analytical methods

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(f) conducts annual internal audits

(g) monitors QA/QC activities of the laboratory and notifies management of
deficiencies
(h) monitors and ensures corrective actions are effective
4.1.7.2 The technical managers in the Chemistry and Biology sections exercise day-to-day
supervision over their staff and are responsible for the operations of their respective
groups and laboratories. The Bureau Chief and Laboratory Directors are responsible for
the FDEP Central Laboratory.
4.2 MANAGEMENT SYSTEM
4.2.1 Description
The Central Laboratory is part of the Bureau of Laboratories in the Division of Environmental
Assessment and Restoration. The laboratory is comprised of Chemistry and Biology
laboratories and a Laboratory Support Section. Each section is managed by a Program
Administrator who reports directly to the Bureau Chief.
CHEMISTRY
The Chemistry Section is divided into two subsections: organic analysis and inorganic
analysis. The Section is headed by a Program Administrator, who is responsible for both the
technical and administrative direction of the Section. The Program Administrator and the
Quality Assurance Officer are committed to the QA program described in this plan. See
Figure 4.1 for the organizational structure.
The analytical subsections are headed by Environmental Administrators who are responsible
for ensuring their staff are cognizant of the objectives and requirements of the QM and SOPs
and that data submitted to the QA Officer or Section Administrator meet these requirements.
Each Environmental Administrator is supported by supervisors (either Environmental
Managers or Chemist Administrators) responsible for all bench analysts and technicians in
their group. The inorganics subsection is divided into three work groups; nutrients, general
chemistry and metals. The organics subsection consists of the volatiles, semi-volatile and
pesticide work groups.
BIOLOGY
The Biology Section is divided into three subsections: bench biology, applied biology and
taxonomy. The Section is headed by a Program Administrator, who is responsible for both
the technical and administrative direction of the Section. The Program Administrator and
the Quality Assurance Officer are committed to the QA program described in this plan. See
Figure 4.2 for the organizational structure.
The biology subsections are headed by Environmental Managers who are responsible for
ensuring their staff are cognizant of the objectives and requirements of the QM and SOPs and

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that data submitted to the QA Officer or Section Administrator meet these requirements.
The Environmental Manager over the Bench Biology subsection is supported by two
Environmental Supervisors, each of which is responsible for supervising the bench analysts
and technicians in one of two work groups; toxicology/chlorophyll/sediment and
microbiology/BOD. The Environmental Manager over the taxonomy subsection supervises
the analysts and technicians within the taxonomic preparation, algal ID, and invertebrate ID
work groups. The Environmental Manager over the Applied Biology subsection supervises all
of the staff within that subsection.
Organization and Management of Ultra-Dilute Chemical Agent Facility
The Florida Department of Environmental Protection has been selected to participate in a
national network of laboratories known as the Environmental Response Laboratory Network
(ERLN). This network is one of several laboratory networks established through Presidential
directives to ensure that critical services are available to support response and recovery
operations following an emergency of national significance or terrorist attack. The
Environmental Response Laboratory Network will be administered by the U.S. Environmental
Protection Agency with support from the U.S. Department of Homeland Security.
The roles and responsibilities of the management and staff involved with work performed
for the ERLN are provided in Appendix A.
Laboratory Support Section
The Laboratory Support Section (LSS) is composed of three groups; data support, laboratory
quality assurance and sample support. Each of these groups is supervised by an
Environmental Administrator or Environmental Manager that reports directly to the Program
Administrator. See Figure 4.3 for the organizational structure.
4.2.2 Quality Policy Statement
The FDEP Bureau of Laboratories mission is to aid in the protection of Floridas environment
by providing legally defensible and scientifically credible analytical and technical support to
the Department. The Bureaus management is committed to generating data of the highest
quality necessary for fulfilling the mission of the laboratory.
4.2.3 Management Commitment
The Bureau of Laboratories management is committed to generating data of the highest
quality necessary for fulfilling the mission of the laboratory and satisfying customer
expectations.

Bureau of Laboratories
G. William Coppenger, Ph.D.: Bureau Chief
Directs all administrative and technical activities of the Bureau of Laboratories.

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Chemistry Laboratory
Timothy W. Fitzpatrick, M.S.: Chemistry Program Administrator
The Program Administrator directs activities of the Chemistry Section and serves as Chief
Chemist for the Department. Certifies analytical reports for release to clients. Serves as the
Laboratory Director for the ERLN Ultra-Dilute Chemical Agent Laboratory.
Liang-Tsair Lin, Ph.D.: Environmental Administrator
Supervises the organic chemistry subsection of the laboratory. Responsible for results
generated from analyses of water, soil/sediment, tissue and waste samples submitted for
pesticide, volatile and semi-volatile organic analyses. Ensures compliance with quality
control and laboratory quality assurance objectives. Certifies analytical reports for release
to clients. Serves as the Assistant Laboratory Director for the ERLN Ultra-Dilute Chemical
Agent laboratory.
Colin Wright, Ph.D.: Environmental Administrator
Supervises the inorganic chemistry subsection of the laboratory. Responsible for results
generated from analyses of water, soil, tissue and waste samples submitted for inorganic
analyses including metals, nutrient, general chemistry and major anion content and other
related analyses. Ensures compliance with quality control objectives and laboratory quality
assurance in the inorganic subsection. Certifies analytical reports for release to clients.
Dr. rer. nat. Bettina Steinbock, Environmental Manager
Supervises the nutrients and general chemistry work groups. Responsible for results
generated from analyses of water, soil, tissue and waste samples submitted for inorganic
tests including nutrient, general chemistry and major anion content and other related
analyses. Ensures compliance with quality control objectives and laboratory quality
assurance in the nutrients and general chemistry group.
Sathavaram Reddy, Ph.D.: Chemist Administrator
Supervises the HPLC, semi-volatile and organic sample preparation work groups, and
analyzes samples for the presence of semi-volatile organic pollutants and pesticides.
Analyses are performed using HPLC and GC techniques. Responsible for: developing daily
work plan for routine analytical work to ensure that sample holding time requirements and
turn-around commitments are met; resolving analytical and instrumental problems;
maintaining protocols to meet QA/QC objectives of the laboratory; supervising analysts and
technicians in their duties; ensuring subordinates are following proper laboratory safety and
waste management procedures; and implementing new or modified analytical procedures
and instruments.
Michael Thompson, B.A.: Environmental Manager
Supervises the metals analysis work group. Responsible for results generated from metals
analyses of water, soil, tissue and waste samples submitted to the laboratory. Ensures

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compliance with quality control objectives and laboratory quality assurances in the metals
group.
Marek Topolski, Ph.D.: Chemist Administrator
Supervises the GC pesticide work group, which includes the sample preparation and analysis
of target pesticides and PCBs. Analyses are performed using GC/ECD and GC/NPD
techniques. Responsible for: results generated from pesticides and PCB analyses of water,
soil, tissue and waste samples. Resolves analytical and instrumental problems, ensures
compliance with QA/QC laboratory protocols and develops and implements new or modified
analytical procedures.
Kerry Tate, Ph.D.: Environmental Manager
Supervises the volatile organics (VOC), methyl mercury and the PM 2.5 work groups.
Analyses are performed using GC/MS, GC/AFD and gravimetric techniques, respectively.
Responsible for analytical work generated from the analysis of environmental samples
submitted to the laboratory for measurement of volatile organic pollutants, methyl mercury
and atmospheric particles. Ensures compliance with quality control objectives, laboratory
quality assurances, laboratory safety and waste management procedures in the VOC and
PM2.5 work groups. Certifies analytical reports for release to clients. Serves as the
Laboratory Manager, Agent Manager, and Co-Chemical Agent Hygiene Officer for the ERLN
Ultra-Dilute Chemical Agent Laboratory.
Chambray Dowdell, B.S.: Chemist Administrator
Supervises the general chemistry and major ion analysis work group. Responsible for results
generated from general chemistry and major ion analyses of water, soil, tissue and waste
samples submitted to the laboratory. Ensures compliance with quality control objectives
and laboratory quality assurances in the general chemistry and major ions work group.
Christelle Roper, Ph.D.: Chemist Administrator
Supervises the nutrients work group. Responsible for results generated from nutrient
analyses of water, soil, tissue and waste samples submitted to the laboratory. Ensures
compliance with quality control objectives and laboratory quality assurances in the nutrients
work group.
Nhon Vo: Engineering Specialist IV
Plans, designs and coordinates building renovations and construction for the FDEP Bureau of
Laboratories. Coordinates and maintains the building mechanical and electrical systems
overseeing upgrades and repair. Serves as the Property Inventory Officer, the Division
Health and Safety Officer, the Hazardous Waste Coordinator, the Radiation Safety Officer
and the Co-Chemical Agent Hygiene Officer for the ERLN Ultra-Dilute Chemical Agent
Laboratory.
Figure 4.1 shows an organizational chart of the management staff of the chemistry
laboratory.

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Figure 4.1
Chemistry Section Organizational Chart
G. William
Coppenger
Chief
Bureau of
laboratories
Timothy Fitzpatrick
Program
Administrator

Nhon Vo Engineering
Specialist IV

Liang Lin

Colin Wright

Environmental
Administrator

Environmental
Administrator

Organics

Inorganics

Kerry Tate

Marek Topolski

Environmental
Manager

Chemist
Administrator

VOC/LC/BNA

GC Pesticides

S.M. Reddy Chemist

Administrator
LC/BNA

Michael Thompson
Environmental
Manager

Bettina Steinbock

Metals

Nutrients/General
Chemistry

Environmental
Manager

Chambray Dowdell
Chemist
Administrator
General Chemistry

Christelle Roper
Chemist
Administrator
Nutrients

Biology Laboratory
David D. Whiting, M.A.: Biology Program Administrator
The Program Administrator directs the activities of the Biology Section and acts as the
Departments lead in issues relating to harmful algal blooms (HABs), oil spills and aquatic
toxicity. Responsible for overseeing all issues related to personnel, budget, infrastructure,
workload, and analytical services within the Biology Section. Coordinates document review

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and technical services for other agency programs. Directly manages the supervisors for all of
the groups in the Biology Section. Represents the Biology Section in meetings with clients
and management.
Elizabeth Miller, B.S.: Environmental Manager
Manager of the Bench Biology Workgroup. Assists with issues related to personnel, budget,
infrastructure, workload, and analytical services. Responsible for overseeing administrative,
technical, and analytical issues for the Bench Biology Workgroup. Represents the Biology
Section in meetings with clients and management. Certifies analytical reports for release to
clients.
Loretta Wolfe, M.S.: Environmental Manager
Manager of the Applied Biology Workgroup. Assists with issues related to personnel,
budget, infrastructure, workload, and analytical services. Responsible for overseeing
administrative, technical and analytical issues for the Applied Biology Workgroup. Reviews
documents submitted to the Department for technical merit. Represents the Biology
Section in meetings with clients and management. Certifies analytical reports for release to
clients.
Cheryl Swanson, M.S.: Environmental Manager
Manager of the Taxonomy Workgroup. Assists with issues related to personnel, budget,
infrastructure, workload, and analytical services. Responsible for overseeing administrative,
technical and analytical issues for the Taxonomy Workgroup. Assists with field sampling.
Reviews documents submitted to the Department for technical merit. Represents Biology
Section in meetings with clients and management. Certifies analytical reports for release to
clients.
J. Marshall Faircloth, B.S.: Environmental Supervisor II
Production coordinator for the Bioassay, Algal Growth Potential, Chlorophyll, and Sediment
tests. Responsible for coordinating staff in the scheduling, preparation, and analysis of
samples for the group, including associated quality control and data reporting. Performs onsite performance audit inspections of laboratories performing NPDES compliance monitoring
tests. Serves as the liaison to the FDEP Ground Water Protection section in the evaluation of
pesticides. Reviews documents submitted to the Department for technical merit.
Daisys Tamayo, B.S.: Environmental Supervisor II
Production coordinator for the Microbiology and BOD portion of the Bench Biology
Workgroup. Responsible for coordinating staff in the scheduling, preparation and analysis of
samples for the group, including associated quality control and data reporting. Assists with
field sampling.
Figure 4.2 shows an organizational chart of the management staff of the biology laboratory.

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Figure 4.2
Biology Section Organizational Chart
G. William Coppenger
Bureau Chief

Dave Whiting
Program Administrator

Elizabeth Miller

Lori Wolfe

Cheryl Swanson

Environmental
Manager

Environmental
Manager

Environmental
Manager

Bench Biology

Applied Biology

Taxonomy

Marshall Faircloth
Env. Supervisor II
Toxicology/Algal Growth
Potential/Chlorophyll/Sediment
Analysis
Daisys Tamayo
Env. Supervisor II
Microbiology/BOD

Laboratory Support Section

Kathleen Lurding, M.Sc., Program Administrator
Directs the Bureaus laboratory support section. Supervises professional, technical and
clerical staff as required. Oversees the design, construction, testing and implementation of
data acquisition and management applications. Oversees user training. Consults with
Bureau staff on hardware and software purchases. Provides technical assistance to FDEP
staff and external stakeholders on issues of data management and assessment.

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John Watts, B.Sc., Environmental Manager

Organizes and assists with prioritization of workload activities to support the analysis and
interpretation of scientific data used to support FDEP and external programs. Plans,
coordinates, and directs staff and/or contractors in the development or acquisition of
computer software for use by the Bureau of Laboratories. Acts as the Web Administrator for
the Bureau of Laboratories, overseeing the maintenance of information available to the
Department and the public sector and the development of web-based tools for retrieving or
storing information. Oversees computer software and hardware purchases, according to
procedures outlined in the Governors One Florida initiative. Supervises staff that performs
the following functions:
provides hardware and software technical support for the Bureau, including
administration of servers and backup of data from analytical instruments and personal
computers;
supports the electronic acquisition, quality assessment, storage, and archive of
chemical and biological analytical data according to approved QA/QC protocols;
manages the computer hardware and software inventories for the Bureau.
Kate Brackett, B.A.: Environmental Administrator
Serves as the Project Manager for the Bureau of Laboratories. Is the customer contact point
in scheduling sample analyses and in responding to customer inquiries. Manages overflow
laboratory and external contracts. Supervises operation of the laboratory receiving work
group. Certifies analytical reports for release to clients.
T. M. Chandrasekhar, Ph.D.: Quality Assurance Officer/Chemist Administrator
Serves as the laboratorys Quality Assurance Officer. Initiates and oversees all internal
QA/QC audits. Manages the laboratorys blind proficiency testing program and maintenance
of the laboratorys SOPs. Evaluates quality control results, corrective actions and establishes
policy for laboratory quality management. Reviews, certifies and signs analytical reports.
Figure 4.3 on the next page shows an organizational chart of the management staff of the
laboratory support section.

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Figure 4.3
Laboratory Support Section Organizational Chart
G. William Coppenger
Chief
Bureau of laboratories

Kathleen Lurding
Program Administrator

John Watts
Environmental Manager
Data Support
Kate Brackett
Environmental
Administrator
Lab Support

T. M. Chandrasekhar
Chemist Administrator
Quality Assurance Officer

4.2.4 Meeting Customer Requirements

Samples must be scheduled with the laboratory prior to acceptance of the samples by the
laboratory. The decision to formally accept samples is based on the clients expectations for
analytical methods, turnaround times, laboratory capacity, sensitivity and confidentiality (for
criminal events). All scheduled work is reviewed by Chemistry and Biology Section managers
or the Project Manager prior to approval for receipt by the laboratory. Samples are
accepted for analysis by logging them into the LIMS and assigning tests.
See SOP LB-018, Standard Operating Procedure for Using the LIMS Scheduler. The LIMS
software system for scheduling samples assesses the capacity and previously scheduled
workload of the laboratory and warns the user whenever laboratory capacity for any work
group may be exceeded. The laboratory may elect to accept samples in excess of stated
capacity if there is a reasonable expectation that the work can be completed within holding
times.

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See SOP LB-028, Standard Operating Procedure for Tracking Priority Projects, for details on
how priority projects are handled and clients are kept informed of progress.
The customer is notified of any non-conformances that may affect the integrity of the data.
The samples are analyzed unless the customer requests otherwise or the nature of the nonconformance makes analysis impractical. Data from compromised samples are flagged with
the appropriate qualifier(s) or comments and a non-conformance report is issued with the
report. The Laboratory non-conformance system procedures are described in SOP LB-002,
Non-Conformance Reporting System.
Significant deviations from standard policies or practices of the laboratory are reported to
the client and documented with the analytical reports. Any samples that are prepared or
analyzed beyond accepted holding times have a statement automatically stamped with the
data alerting the client to the fact that tests were conducted after the sample had expired.
Similarly, the failure of any quality control checks is commented with the data, directing the
client to the Quality Control Report for details of failures. Data qualifiers are used to alert
clients of quality control problems and holding time exceedances.
Accepted samples that were improperly preserved are documented in the LIMS and
analytical reports as sample level comments and/or in a LIMS non-conformance report. All
other significant observations that do not conform to accepted practices or policies are
documented and reported along with analytical results. Those documents may be as letters,
interoffice memoranda or appendices to analytical reports. Sample integrity such as
improper temperature and pH preservation, insufficient volume, leaking or broken bottles,
etc., are entered into a non-conformance report in the LIMS as well as documented on a login check form with the log-in technicians initials.
4.2.5 Technical and Supporting Procedures
The laboratory SOPs are divided into three groups, those for the chemistry laboratory, the
biology laboratory, and the Bureau. The only location at which current revisions of all SOPs
(PDF files) should be accessed is at http://www.dep.state.fl.us/labs/library/lab_sops.htm
Printed copies are not considered by the laboratory to be official SOPs. For the purpose of
reviewing and revising SOPs annually, copies of current revisions (Word) can be saved to the
reviewers computer from \\Tlhlab3\sops. The versions stored on TLHlab3 are locked and
maintained for archival purposes only. The format of the SOPs is detailed in SOP LB-001,
Protocol for Preparing Standard Operating Procedures (SOPs).
4.2.6 The responsibilities of all supervisors within the Bureau of Laboratories can be found
in the appropriate job descriptions detailed in section 4.2.3. Personnel authorized to certify
reports are stipulated in these job descriptions.
4.2.7 All laboratory personnel are required to annually review and update (if necessary) all
SOPs that pertain to the work they perform within the laboratory (SOP LB-010). See section
4.1.5 (g) for further information on notifying personnel of system changes.
4.2.8 Additional Management System Requirements

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4.2.8.1 See section 5.2.7 for a description of the Laboratory Data Integrity System.
4.2.8.2 The Quality Assurance Officer is responsible for keeping the Laboratory QM up
to date. The QM is reviewed and revised at least annually and posted to the Bureau of
Laboratories web site at: http://www.floridadep.org/labs/library/progplan.htm.
Revisions are approved through the laboratory supervisors and forwarded to the
Quality Assurance Officer for incorporation into the QM. The posted version is the
latest official version of the QM.
4.2.8.3 This QM along with the laboratory SOPs detail the FDEP Bureau of
Laboratories Quality System for the laboratory. This document contains all of the
mandatory information required by Section 4.2.8.3 of the TNI standards Volume 1,
Management and Technical Requirements for Laboratories Performing Environmental
Analysis, Module 2: Quality System Requirements.
4.2.8.4 This QM contains or references all of the topics in Section 4.2.8.4 of the TNI
standards Volume 1, Management and Technical Requirements for Laboratories
Performing Environmental Analysis, Module 2: Quality System Requirements.
4.2.8.5 SOPs addressing all activities of the laboratory including all test methods and
supporting activities may be found at:
http://www.floridadep.org/labs/library/lab_sops.htm. All of the required topics in
4.2.8.5 (f) of the TNI standards are in or referenced in the test method SOPs.
4.3 DOCUMENT CONTROL
4.3.1 FDEP SOP LB-001, Protocol for Preparing Standard Operating procedures (SOPs),
describes how SOPs are created, revised, and approved. This SOP details where the current
SOPs are maintained and archived. The electronic system for maintaining the SOPs has the
capability of creating reports to track revision and effective dates.
Record archiving procedures are found in SOP LB-013, Standard Operating Procedure for
Archiving/Retrieving Documents and Using the Document Control System. Archived records
include raw laboratory data, laboratory notebooks, final reports, administrative files,
personnel records, purchase requisitions and purchase orders. The electronic document
control system allows entering new archive records, identifying archives and locations and a
check out system.
The QM is updated at a minimum on an annual basis. The official version of the QM is
available for viewing by all employees at
http://www.floridadep.org/labs/library/progplan.htm. All revisions of the QM are archived
and easily accessible on a network drive at TLHlab3/SOPs/QA Manual.
4.3.2 Document Approval and Issue
4.3.2.1 The procedure by which an SOP is implemented or revised is as follows:

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The technician, chemist/biologist, and/or analytical group supervisor involved in

carrying-out the procedure prepares a draft SOP detailing methodology.

The draft SOP is reviewed by the Environmental Manager (EM) or Environmental

Administrator (EA) in charge and submitted to the QA Officer as a final SOP.

The QA Officer (or delegate) posts the final SOP to the Bureau of Laboratories
Internet site in portable document format (PDF). The name of the person
authorizing the SOP (supervisor submitting the final version), the effective date
and the revision date are recorded using the SOP Update Utility module of the
Laboratory Information Management System. The SOP expiration date will be set
one year from the date the version was revised.

To revise an existing SOP the revised SOP is submitted to the EM in charge of the
pertinent work group. The EM reviews the SOP and submits it to the QA Officer,
indicating whether the change is a minor or major revision. Minor revisions are
those which do not involve modifications to the method, while major revisions
indicate the method has been altered. A change in procedure that produces
results that are incomparable with those reported before the method was
modified would also justify a major revision. All SOPs must contain an Appendix of
Significant Changes made during the revision period. The Appendix must include
the date of any significant edits and should indicate the pertinent SOP sections
that have been edited. The final SOP is submitted to the QA Officer (or delegate)
as a Word document with track changes turned on to indicate the content altered
during the revision.

Note: In cases where a specific SOP version has been certified and subsequently
undergoes a major revision, additional steps are required. The supervisor submitting
the revision must also submit a method validation package and the appropriate
paperwork for requesting NELAP certification of the new SOP version. Supervisors
are responsible for ensuring that analysts are trained on new or revised SOPs and
that former printed versions of SOPs are replaced with new versions. The only
official versions of SOPs are those that reside on the laboratorys internet (or
intranet) site for SOPs. Printed copies are not considered by the laboratory to be
official SOPs.
4.3.2.2 Revisions to the QM are submitted by the technician, chemist, biologist, and/or
analytical group supervisor involved in carrying-out the procedure. The proposed
revisions are reviewed by the Environmental Manager/Environmental Administrator and,
if acceptable, forwarded to the QA Officer. The QA Officer evaluates the changes for
compliance with laboratory policies and procedures and quality assurance issues and then
is responsible for posting the revised manual.
4.4 REVIEW OF REQUESTS, TENDERS AND CONTRACTS
4.4.1 Contract/order review is an integral part of the FDEP Bureau of Laboratories. All
contracts/orders are reviewed and accepted only if the requirements are clear and

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understood, and the laboratory has the capability and capacity to meet full customer
expectations. The criteria used to review and accept projects are described in SOP LB-033,
Procedure for Receiving and Accepting Laboratory Projects. Upon receiving a request from a
client the FDEP Project Manager obtains specific project information. The information
includes but is not limited to the following:

The project description (and purpose if needed)

The analyses requested

The sample matrices

The number/frequency of the samples

Completion expectations

The FDEP Project Manager disseminates the information to the Laboratory Administrators
for evaluation. If the FDEP Laboratory is able to accept the work then the FDEP Project
Manager provides the following information in writing (or by e-mail) to the client:

A list of the analytical methods the FDEP Lab will use.

Information on whether the FDEP Lab has FDOH certification for the methods

The detection limits and quantitation limits for the methods

The costs of the analyses (if applicable)

Additional information upon request, such as non-NELAP proficiency studies and

quality assurance/control information

Once the client and the Lab mutually agree upon the project then the FDEP Project Manager
obtains the account information.
4.4.2 Records of reviews, including any significant changes, are maintained.
4.4.3 Communications are maintained with the client from request/quote through
commencement of work. This includes informing the client of any deviation from the
contract or agreement.
4.5 SUBCONTRACTING OF ENVIRONMENTAL TESTS
Samples that need to be sent out to an overflow contract laboratory will show transfer to an
overflow lab in the LIMS custody record. There is a task assignment number (e.g. SA034)
documented on a task assignment form, Figure 4.4. The task assignment form includes the
FDEP Project Managers signature authorizing the work, a list of sample ID's and requested
analyses with turnaround time, the date/time the samples were sent out, cost information
and the identity of the custodian responsible. Samples, along with copies of the field
information and the task assignment form, are delivered to the contract lab. The delivery
person and the recipient at the contract lab must sign the task assignment form indicating
the transfer date and time. The task assignment form becomes part of the custody record.

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See SOP LB-008, Standard Operating Procedure for Outsourcing Analyses through a Contract
Laboratory, for further details.
4.6 PURCHASING SERVICES AND SUPPLIES
4.6.1 A list of state approved suppliers for the purchase of supplies and services is
maintained by the Florida Department of Management Services (DMS) at
http://dms.myflorida.com/business_operations/state_purchasing/vendor_information

The laboratory maintains an inventory list of chemicals and supplies commonly used for
analyses performed in the laboratory. See SOP LB-030, Standard Operating Procedure for
Purchasing and Receiving Laboratory Chemicals and Supplies. This SOP includes procedures
ensuring the necessary quality of the purchase, checking that the proper quality was
received and how the supplies are stored if needed to maintain the quality.
4.6.2 Purchased services, supplies and consumable materials are not used until an
inspection is performed to ensure compliance with purchasing specifications.
4.6.3 The quality of items being ordered is specified prior to the purchase. This applies to
the specifications of durable goods such as laboratory instrumentation and software.
Similarly, the lab orders consumables such as chemical reagents of known quality (purity)
from reputable vendors. The quality of the chemical is usually specified by grades that
conform to industry standards prior to their purchase. Examples include the American
Chemical Society (ACS) Reagent Grade chemicals, Trace Metal Grade acids, HPLC Grade
organic solvents, UHP Grade gases etc.
4.6.4 If a chemical or consumable ordered by the lab is found to be lacking in the minimum
quality required for its intended use, then the lab will pursue the purchase of the desired
item from an alternative supplier that meets the required specifications and is listed in the
Florida DMS database of state approved vendors. The list is maintained at:
http://dms.myflorida.com/business_operations/state_purchasing/vendor_information

4.7 SERVICES TO THE CLIENT

4.7.1 The FDEP Bureau of Laboratories does its utmost to meet its clients needs, including:

Affording customers access to the laboratory to witness testing when requested.

Preparing, packaging and dispatching test items and reports as required by our
customers for verification purposes.

Advising, guiding and communicating with our customers on technical matters,

providing opinions and interpretations for testing performed or to be performed.

Communicating to our customers any major deviations in testing being performed.

See SOP LB-002, Non-conformance Reporting System.

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Communicating to customers any delays that may result in the customers not
receiving their test results in a timely manner.

Notifying customers of any event that casts doubt onto the validity of results
supplied to them.

4.7.2 The laboratory solicits customer feedback from its customers using a comprehensive
written survey once a year. Feedback from our clients by other channels such as phone and
email is encouraged throughout the year to improve our operations. Feedback from lab
customers are maintained by the QA officer.
4.8 COMPLAINTS
The Bureau of Laboratories is committed to resolving complaints and implementing
suggestions for improvement. All informal complaints, suggestions or requests for
information are directed to the appropriate supervisor for resolution. If immediate
resolution cannot be attained, the matter is submitted to the section administrator who may
investigate and direct the resolution. Formal written complaints are logged with the section
and, after investigation and resolution, are responded to in writing. Copies of responses are
organized and filed by the Quality Assurance officer for reference.
4.9 CONTROL OF NON-CONFORMING ENVIRONMENTAL TEST WORK
(See SOP LB-002, Non-conformance Reporting System).
4.9.1 Significant deviations from the laboratories policies and procedures, as outlined in
the Quality Manual and SOPs, are not approved without appropriate documentation.
Significant deviations from standard policies or practices of the laboratory are reported to
the client and documented with the analytical reports. Any samples that are prepared or
analyzed beyond accepted holding times have a statement automatically stamped with the
data alerting the client to the fact that tests were conducted after the samples had expired.
Similarly, the failure of any quality control checks is commented with the data, directing the
client to the Quality Control Report for details of the failures.
4.9.2 Where non-conformances are indicative of systematic errors, the corrective action
procedures described in section 4.11 are instituted.
4.10 IMPROVEMENT
The Bureau of laboratories is committed to continually improving the quality management
system by:

Multi-tier and electronic data review process (see SOP LB-025, Event Level
Authorization Checklist and SOP LB-026, Job Level Authorization Checklist)

Internal and external audits

Systematically evaluating quality data and updating allowable acceptance criteria

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Participating in round robins and laboratory intercomparisons

Performing quality system management reviews (see SOP LB-010, Quality System
Management Review)

4.11 CORRECTIVE ACTION

4.11.1 General
Corrective actions for the chemistry section are described in the method SOPs. A list of
method SOPs sorted by subsection or category can be found at
http://www.dep.state.fl.us/labs/library/lab_sops.htm.
Corrective actions and notification protocols for the biology section are listed in Table 4.1.
Corrective actions are initiated based on either internal QC checks, data validation by a
reviewing authority or performance audits. Outside sources such as performance evaluation
studies, split samples as well as recommendations by the FDEP QA Officer may initiate
corrective actions. See FDEP SOP LB-002, Non-Conformance Reporting System, for additional
information on initiating corrective actions.
4.11.2 Cause Analysis
All non-conformances are evaluated to determine the root cause. Many factors are taken
into consideration in this evaluation and the cause may not be directly attributable to
laboratory operations. Non-conformance causes, where identified, are documented in nonconformance reports and stored within the Laboratory Information Management System
(LIMS). Where necessary, re-training and/or changes to SOPs are implemented to address
controllable errors.
4.11.3 Selection and Implementation of Corrective Actions
The details of identifying corrective actions and remedies taken are detailed in SOP LB-002.
The likely causes of a given problem are first identified and then corrective actions put into
place to alleviate the problem. The extent of the corrective actions required is evaluated
against the seriousness of the non-conformance. All corrective actions are administered
within a reasonable time frame.
4.11.4 Monitoring
All corrective actions are documented and monitored to ensure compliance with the
laboratorys policy and procedures. The laboratory QA officer maintains a list of corrective
actions undertaken by lab personnel.
4.11.5 Additional Audits
The efficacy of any corrective actions is evaluated during routine internal and performance
audits. Additional audits are scheduled to address non-conformances that will not allow the
laboratory to meet their established operating protocols.

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4.11.6 All actions taken under this section are documented.

4.12 PREVENTIVE ACTION
4.12.1 Preventive action is a proactive process, used to identify process and quality system
improvement opportunities (see for example, SOP LB-010, Quality System Management
Review). Routine lab and field procedures are listed in Table 4.2, Preventive Maintenance
Biology, and in the individual operational SOPs
(http://www.floridadep.org/labs/library/lab_sops.htm). They list the types of analytical
equipment utilized to perform routine analyses and the frequency of preventive
maintenance tasks performed to ensure data quality.
4.12.2 All maintenance or repair to equipment is documented in a laboratory notebook.
Documentation includes a description of the problem(s), work performed, date and analyst's
initials. See section 5.5.6 for details. The management system is also be evaluated to
institute process revisions to create a continuous improvement process. See Section 4.1.6
for an explanation of the Management Review system.
4.13 CONTROL OF RECORDS
4.13.1 General
4.13.1.1 For a description of laboratory records, see SOP LB-006, Standard Operating
Procedure for Records Maintenance and Storage. Records associated with QA activities
including external and internal audits, certification records, and PT studies are filed in a
dedicated quality assurance filing cabinet.
4.13.1.2 All records are legible, easily accessible and stored in a manner that will
minimize loss, damage or deterioration. The Department continues to maintain client
access to electronic and paper records for a period of not less than 5 years after the
completion of the laboratory project (see SOP LB-006 and SOP LB-013 for details).
4.13.1.3 See section 4.1.5 (c) concerning access to laboratory records and documents.
4.13.1.4 Electronic records are copied (incremental backups) onto backup tapes each
business night. Full backups are conducted during weekends and the files archived to
DVD as needed.
The laboratory maintains a document control system for tracking the archive process for
paper records and laboratory logbooks. The document control system is an electronic
database that resides on the laboratorys server and is available through the Department
Intranet. Paper records are boxed, labeled and submitted to the State Records Center for
storage. The State Records Center assigns the boxes a tracking number that is entered into
the document control system, along with a description of the box contents, the date range
of records in the box, the archival date and the name of the submitter. When records are
needed for retrieval, the document control system database is searched for the pertinent
box identification number and that number is submitted to the State Records Center for
retrieval.

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The Office of Technology and Information Services (OTIS) maintains the Oracle database
where LIMS records are stored. A complete backup of the oracle tables is exported to a
password-protected server administered by OTIS. This backup file is copied onto backup
tape each business night. Copies of pertinent raw and processed data may be maintained in
electronic and paper format. Additionally, the laboratory maintains paper copies of all final
analytical reports and client custody records. These paper records are maintained in the
laboratory and archived offsite as needed in the State Records Center. All paper records are
maintained in a temperature and humidity controlled environment and are protected by fire
suppression equipment.
4.13.2 Technical Records
4.13.2.1 Most of the data generated by the laboratory during the analytical testing
process is in the form of electronic records. Those data consist of raw data files
generated by analytical instrumentation, chromatography acquisition software, etc. as
well as processed and final database records residing in the Laboratory Information
Management System (LIMS).
All raw data files, including processed chromatography data and formatted, processed
instrument files are stored on servers maintained by OTIS. Those files are organized by
file type and date of generation and are copied onto backup tapes each business night.
The files are archived to optical compact disk (DVD) as needed. Software and hardware
systems will be maintained to ensure that raw data are available for a period of not less
than five (5) years after completion of the laboratory project. Records maintained shall
allow the re-creation of the calibration and test procedures and personnel responsible for
the different aspects of the test procedure. See Bureau of Laboratories SOP LB-006,
Standard Operating Procedure for Records Maintenance and Storage, for complete
details.
14.13.2.2 The nature and intent of all documentation are clearly established and all
records are captured at the time of generation.
14.13.2.3 Entry errors on paper records are not obliterated or erased. Corrections are
made by marking a line through the error so that it is legible. The marked error is initialed
and dated and a reason for the correction is annotated when the cause is not obvious or
due to simple transcription errors. Access to electronic records is restricted and where
possible an electronic audit trail is maintained for write access only.
4.13.3 Additional Records
a) Documentation of Sample History
Sample Custody
The custody of a sample is defined as one of the following:

It is in the sampler's or transferee's actual possession;

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It is in the sampler's or transferee's view, after being in his/her physical possession;

It was in the sampler's or transferee's physical possession and then he/she

secured it or placed in a designated secure area to prevent tampering.
Routine Custody
For most projects the FDEP Laboratory provides sampling containers to field
personnel. The sample chain of custody begins prior to shipping empty containers
to the field personnel. Prior to shipping, the lot numbers of containers are
documented on the Sampling Kit Packing List, e.g., Figure 4.5, and in the LIMS. The
Packing List is signed by the lab technician and shipped with the containers.
Samples are collected by field personnel utilizing procedures identified within their
field QA Plans. If sample bottles are provided by the Central Laboratory, custody
begins at the point of sample kit preparation. After collection, the samples are
shipped to the Central Laboratory by common carrier or are hand-delivered by the
field staff. See SOP LB-015, Standard Operating Procedure for the Packing and
Shipping of Sampling Kits, and SOP HG-015, Preparation of Sampling Kits for the
Preparation of Trace Level Mercury Water Samples.
Legal chain of Custody
For legal chain of custody samples, a chain of custody form is used in addition to, or
instead of, a sample submittal form although the submittal form can also provide
legal chain of custody information. See examples of the chain of custody record in
Figure 4.6. For any given sampling event, custody Records are kept with the other
field paperwork in the event folder at all times until the analysis is complete. A
copy is sent with the final report to the customer while the original is kept in the
section file with the report. At the customers request, a copy of the internal
custody records (from the LIMS and laboratory log books) can also be sent. See SOP
LB-023, Standard Operating Procedure for Documenting Evidentiary Chain of
Custody within the DEP Laboratory, for complete details.

Sample Custody Policy

See section 5.8 under Handling Samples and Test Items and SOP LB-016, Laboratory
Support Section Receiving Room: Standard Operating Procedure for the Receipt and
Log-in of Samples by the DEP Central Laboratory
Once a sample is logged in, a custody log is automatically created for that sample in
the LIMS. This log tracks the sample's movement throughout the lab, from sample
receipt to sample disposal. See an example of the laboratory custody log in Figure
4.7. When a sample is removed from the sample storage area, the custody is
transferred from the storage area to the user. This transaction is recorded in the
custody log by date, time and user. Each LIMS user is issued a unique ID card with a
bar code with their User ID. Bar code scanners are located throughout the
laboratory. When users wish to check out or transfer samples, they scan their ID

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card, which transfers their unique user ID to the custody record. As each sample has
a bar code label, the user can easily check out samples by using the bar code scanner.
In the event the network or LIMS is down, the user can also manually record their
user ID and use a logbook for recording sample custody.
When users are finished with samples, they must return them to their designated
storage locations for check-in and secure storage. After samples have been analyzed
and final analysis reports are issued to the customer, samples are either disposed of
properly (see Table 4.3, Laboratory Waste Disposal Procedures), returned to the
client, or (in the case of legal samples) stored until the client approves disposal or
transfer of the samples. For routine sample disposal the technician scans the samples
in the LIMS. The sample custody record notes the date, time and identity of the
person disposing of the sample. While records of sample login, sample checkin/check-out, sample transfers between analysts and sample disposal are recorded
electronically in the LIMS custody log, movements of other samples (extracts,
digestates, etc.) are documented in various digestion, extraction and analysis
logbooks. All logbook records are dated and initialed by the person(s) who carries
out the task. Any errors in the documents are struck through with a single line and
marked with the person's initials. See examples of biology logbooks in Figure 4.8 and
chemistry logbooks in Figure 4.9 .
Inter-laboratory Custody
See section 4.5 for a description of custody for samples sent to a sub-contract
laboratory.
Laboratory Information Management System (See SOP LB-009, Standard Operating
Procedure for Validation of LIMS Software Development or Modifications that Affect
the Calculation/Assessment of Analytical Results)
The laboratory uses a custom Oracle based LIMS using client-server technology. The
main server is maintained by the Office of Technology and Information Services. The
database applications and client hardware are maintained by the Laboratory Support
Section.
To gain access to the LIMS, users must provide valid network and LIMS usernames
and passwords. They are then presented with a menu containing only those
functions required to perform their job duties, based on the security access level
assigned to their unique username. For example, only the Program Administrator,
Environmental Administrators, Environmental Managers and Chemist Administrators
can change any part of an authorized job or change the sample information and its
data. Any changes made are documented by the person's name and dated
automatically in the LIMS records. When all the jobs within a LIMS event are
authorized for release, the event analysis report is reviewed and certified in LIMS
(see SOP LB-025, Event Level Authorization Checklist). The review process is
described in section 5.10.2.

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The LIMS software is modified on a continuing basis by the Bureau's Support Section.
Revisions of the code are documented with each application. Requests for code
changes, additional functionality or interface enhancements are logged in to a webbased Help Desk application. They are prioritized according to the potential for
interference with data integrity or workload efficiency. Resolutions to each help desk
case are documented and stored in the Help Desk data tables. See SOP LB-009,
Standard Operating Procedure for Validation of LIMS Software Development or
Modifications that Affect the Calculation/Assessment of Analytical Results.
b) Laboratory records are maintained to ensure their availability for a minimum of five
years after completion of the laboratory project.
c) Records are made available to the accreditation body.
d) FDEP SOP LB-006, Standard Operating procedures for Records Maintenance and
Storage, clarifies that software and hardware systems are maintained to ensure that raw
data are available for a period of not less than five (5) years after completion of the
laboratory project.
e) Procedures for accessing archived records are in SOP LB-013, Standard Operating
Procedure for Archiving/Retrieving Documents and Using the Document Control System.
f) Copies of pertinent raw and processed data are maintained in electronic and/or paper
format. Additionally, the laboratory maintains paper copies of all final analytical reports
and client custody records. Records retained include:

A test method description and reference Sample ID

Instrument identification and a reference to operating conditions

A reference to the method SOP describing calculations on the raw data,

verification of reported results and QC assessment

Method performance and quality control expectations

Software security, documentation and assessment

Analysts signatures, initials or electronic identification

Documentation to support all aspects of sample handling to include preparation,

cleanup, incubation periods, weights, and instrument readouts

Test results and record of responsible parties for laboratory records

Documentation supporting reagent and standard history

Calibration and calibration acceptance criteria

Proficiency Test Results

Record of demonstration of capability for all analysts

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g) All hand written records are recorded in permanent ink and any errors in the
documents are struck through with a single line and marked with the persons initials. If
the reason for the correction is not obvious an explanatory comment is provided.
h) In the event that the Bureau of Laboratories ceases operation, all records will be
turned over to the Departments Chief Information Officer and all clients will be notified.
The Department continues to maintain client access to electronic and paper records for
a period of at least five (5) years after the completion of the laboratory project.
4.14 INTERNAL AUDITS
Internal system audits of the laboratory systems are conducted as described below. In
addition, internal performance audits are initiated to help resolve problems and confirm the
efficacy of the testing system. System audits of overflow laboratories are conducted
following the pattern of the internal system audits.
4.14.1 The laboratory Quality Assurance Officer conducts internal system audits on select
laboratory systems. These internal audit procedures follow these general guidelines:

Selected systems are audited annually.

The QA Officer conducts the audits.

The audit consists of the random selection of a previously reported sample project,
tracking of these samples through the system, evaluation of sample results, and a
follow-up laboratory audit.

System components to be audited include, but are not limited to:

(i) All documentation associated with sample and data handling, including
linkage mechanisms employed between all records for tracking
documentation for any sample datum.
(ii) Use of established, approved procedures as outlined in this QM
(iii) Proper execution of established procedures.
(iv) Sample and data handling activities including:
[a] All sample log-in, trafficking, and log-out
[b] Sample preparations
[c] Method calibrations
[d] Sample analyses
[e] Data reduction, validation and reporting
[f] Preventive maintenance and repair procedures
[g] Standard and reagent preparations and storage
[h] Sample and waste disposal

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[i] Container and labware decontamination

[j] QC management practices and assessment of analytical precision,
accuracy and sensitivity.
4.14.2 See examples of typical audit checklists, Figure 4.10. A report is completed identifying
deficiencies and corrective actions to be taken.
4.14.3 Deficiency lists and associated corrective action orders are formally promulgated to
responsible staff. Corrective actions are taken in a timely manner and all customers are
notified in writing if the laboratory results were impacted.
4.14.4 Subsequent checks are made to verify the implementation and effectiveness of the
corrective actions. Details are provided in section 4.11.
4.14.5 Additional items:

The laboratory notifies clients immediately upon the identification of the need for
corrective actions that affected the generated data.

Management ensures that effective corrective actions have been instituted within
the agreed upon time frame.

Internal audits as described in this section are conducted annually.

4.15 MANAGEMENT REVIEWS

4.15.1 Management reviews are conducted according to FDEP SOP LB-010 , Quality System
Management Review. The Quality Assurance Officer prepares a report summarizing the
completion of items 4.14.1 through 4.14.5 including the completion date and responsible
personnel for each of the activities. This report includes a summary of corrective or
preventive actions, assessments by external bodies, the results of inter-laboratory
comparisons or proficiency tests, QC activities, staffing issues or any relevant client feedback
or complaints.
4.15.2 Performance reports are generated monthly, semi-annually and annually to track
workload performance, efficiency and spending. The reports are maintained by the
laboratory and disseminated to laboratory supervisors.
4.15.3 The Quality Assurance Officer prepares a Quality System Management Review report
on an annual basis.
4.16 DATA INTEGRITY INVESTIGATIONS
See Section 5.2.7 for a description of the data integrity program. All investigations are
conducted in a confidential manner. Investigations are documented and affected clients are
notified.

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5.0

TECHNICAL REQUIREMENTS

5.1 GENERAL
5.1.1 The laboratory recognizes that many factors affect the correctness and reliability of
the tests that the laboratory performs, including:

human factors
accommodation and environmental conditions
test methods and validation
equipment
measurement traceability
sampling
handling of test items

5.1.2 The laboratory takes into account these factors in developing test procedures,
personnel training and equipment selections.
5.2 PERSONNEL
5.2.1 All laboratory personnel are required to maintain SOPs that pertain to the work they
perform within the laboratory and laboratory analysts must perform initial and continuing
demonstrations of proficiency according to Section 4.1.5 (g).
Qualifications for personnel performing specific tasks are based on education, experience
and training procedures. All personnel must meet established minimum requirements to
perform their assigned tasks of performing tests, evaluating results, and certifying results.
Personnel do not perform tests unsupervised without passing minimum training
requirements. Position descriptions (PDs) are maintained for each position and contain the
minimum qualifications required for employment (see Section 5.2.4).
Managers responsible for interpreting results are knowledgeable of the test procedures, the
intent of their use and typical interferences, requirements for their use and the significance
of deviations from accepted protocols.
5.2.2 Personnel training is conducted according to DEP SOP LB-011, Laboratory Training
System and Records Management. All analysts and technicians engaged in analytical work
are required to complete training in the methodological requirements for assigned analyses
on an annual basis.
5.2.3 All tests performed by the FDEP Bureau of Laboratories are conducted by personnel
employed by the Florida Department of Environmental Protection. Procedures for
subcontracting environmental tests are provided in Section 4.5.
5.2.4 Job descriptions are maintained for each position within the Bureau of Laboratories.
Summaries of the responsibilities of the laboratory supervisors/managers may be found in
Section 4.1.5(f) of this manual.

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The job/position descriptions include, where appropriate:

Planning and performing tests.

Evaluation of test results.
Reporting opinions and interpretations.
Method modification and development and validation of new methods.
Qualifications and training programs.
Expertise and experience required.
Managerial duties.

5.2.5 FDEP management ensures the competency of all who operate equipment, perform
tests, evaluate results and sign test reports. Adequate supervision is provided for staff
undergoing training. Personnel performing specific tasks are qualified on the basis of
education, training, experience and/or demonstrated skills, as required. See position
descriptions, personnel files, SOP LB-011, Laboratory Training System and Records
Management, and the management descriptions in Section 4.1.5 (f).
5.2.6 Additional Personnel Requirements
Technical Manager Qualifications
Technical managers at the FDEP laboratory meet all the requirements of the State of
Florida Department of Management Services broadband classifications and NELAC
standards for education and experience.
5.2.7 Data Integrity Training
All employees of the FDEP Central Laboratory are held to high professional ethical standards
in the performance of their duties. All employees are required to read, understand and sign
an Ethics Statement attesting to their commitment to honesty and integrity in performance
of their duties. In addition, all employees are required to attend an annual ethics training
class. Improper, unethical or illegal actions will be dealt with according to the published
Administrative Directives of the Florida Department of Environmental Protection found at:
http://www.dep.state.fl.us/admin/depdirs/pdf/202.pdf.
a) See SOP LB-012, Code of Ethics, for additional information.
b) The annual training includes protocols for reporting ethics issues, providing examples
of ethical violations and reviewing the consequences of unethical behavior and resources
where additional information can be referenced. The training is updated each year to
address current issues. All attendees of the training course are required to sign an
attendance sheet verifying that they participated in the course.
5.3 ACCOMMODATION AND ENVIRONMENTAL CONDITIONS
5.3.1 Environmental controls in the laboratory are appropriate for the tests being
performed. Environmental conditions that can affect test results are listed in the relevant

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SOPs. For each area that requires a controlled environment, the conditions are
documented. Environmental factors such as light, temperature, ventilation and space are
considered to allow tests to be performed safely and effectively.
5.3.2 Environmental conditions are maintained to meet test procedure requirements and
are controlled so as not to invalidate test results or increase measurement uncertainty. If it
is determined that test results are being adversely impacted by the test conditions, the tests
are terminated, corrective actions instituted and clients are notified of any impacted data.
5.3.3 The physical location of activities will be such that potential contamination will be
minimized.
5.3.4 Access to all laboratories is restricted to authorized personnel and approved visitors.
Visitors are supervised at all times.
5.3.5 All laboratory areas are maintained in a clean and orderly manner.
5.4 ENVIRONMENTAL TEST METHODS AND METHOD VALIDATION
5.4.1 Table 5.1 contains a listing of all chemistry analytes, preparative and analytical methods,
matrices, accuracy and precision targets derived from LCSs or method requirements, and
MDL's/PQL's. Modifications to methods in Table 5.1 are summarized in Table 5.7 and in the
method SOPs. Details concerning the procedures used for validating methods and
determining MDLs/PQLs are described in SOP LB-007, Procedure and Policy for
Demonstration of Capability for Method, Instrument, and Lab Staff.
Table 5.2 contains the listing of all biology parameters and their associated matrices,
methods and QA targets. Modifications to methods in Table 5.2 are summarized in Table 5.8
and in the method SOPs.
MDLs are set such that the risk of reporting a false positive is less than 1%. MDLs are
determined using the method specified in the Federal Register, 40 CFR Part 136 Appendix B,
using LCSs prepared near the estimated detection limit as surrogates to estimate
methodological noise for censored methods (e.g., chromatographic methods which censor
analytical noise) or, for uncensored methods, using actual method blanks to directly
measure methodological noise. Where the possibility exists for significant systematic bias
from sample preparation and handling or from the analytical determinative step (typically
inorganic analyses), bias is taken into account when calculating detection limits. Published
MDLs may be set higher than experimentally determined MDLs to (1) avoid observed
positive interferences from matrix effects or common reagent contaminants or (2) for
reporting convenience (i.e., to group common compounds with similar but slightly different
experimentally determined MDLs). MDLs are determined in a suitable analyte-free matrix
when possible. For certain analytes and matrices, no suitable, analyte-free matrix may be
available. In those cases, MDLs are determined in the absence of any matrix, but in the
presence of all preparatory reagents carried through the full preparatory and determinative
steps. LOD verification procedures may be found in SOP LB-031, Limit of Detection
Verification.

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Practical Quantitation Limits (PQLs) are set at 3 to 5 times the reported MDL unless
otherwise noted. Because PQL level checks are required, the practicality of the preparation
of standards using commercial analytical mixes may dictate to some extent the reported
PQL. Generally the PQL is not set at less than 3 times the MDL. However, in some instances,
systematic bias (e.g., analyte background in reagents, etc.) necessitates that the reported
MDL be elevated to levels that are readily quantifiable. In those instances, the PQL may be
set at a level less than 3 times the reported MDL.
Except where specified in individual methods, the QA targets for all inorganic analyses are
within the range of 80 - 120 % for accuracy and < 20 RPD for precision, unless laboratorygenerated data indicate that tighter control limits can be routinely maintained. This
convention was adopted due to the fact that targets set according to historical data are
usually less stringent. The organic QA targets are likewise statutory in nature. Warning and
control limits for organic analyses are initially set for groups of compounds based on
preliminary method validation data. When additional data is available, the QA targets may
be reconsidered. All QA targets are routinely re-evaluated at least annually (and updated, if
necessary) against laboratory generated data to insure targets continue to reflect realistic,
methodologically achievable goals.
The sources for these methods may be found in:
EPA

Methods for Chemical Analysis of Water and Wastes; USEPA Office of

Research and Development, Cincinnati, OH, 3/83; EPA 600/4-79-020.

Methods for the Determination of Metals in Environmental Samples,

USEPA Office of Research and Development, Washington DC, 6/91,
EPA/600/4-91/010.

Test Methods for Evaluating Solid Wastes, Physical/Chemical Methods,

SW-846; USEPA Office of Solid Waste and Emergency Response, Washington,
D.C.

Method for the Determination of Organic Compounds in Drinking Water,

Supplement I, EPA 500/4-90/020, July 1990.

Code of Federal Regulations, Title 40, Part 136; U.S. Government Printing
Office, Washington, D.C., July 1993.

Methods for the Determination of Nonconventional Pesticides in Municipal

and Industrial Wastewater; USEPA Office of Water, Washington, D.C., 8/93.

EPA Quality Assurance Guidance Document 2.12: Monitoring PM2.5 in

Ambient Air Using Designated Reference or Class I Equivalent Methods.
Volume II, Part II, U.S. Environmental Protection Agency, November
1998.

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APHA-AWWA-WPCF

Standard Methods for the Examination of Water and Wastewater, 19th

Edition, 1995 (designated as SM in Table 5.1).

Standard Methods for the Examination of Water and Wastewater, online

Edition (designated as SM in Table 5.1 and Table 5.2).

Standard Operating Procedures, Laboratory Services, Florida Department

of Health and Rehabilitative Services (designated HRS SOP).

HRS

FDEP

Method for Determination of Petroleum Range Organics Rev. 1,

11/1/1995, Florida Department of Environmental Protection (designated
FL-PRO).

Massachusetts DEP

Method for Determination of Extractable Petroleum Hydrocarbons,

01/1998, Massachusetts Department of Environmental Protection
(designated MA DEP EPH).

SOPs address all applicable aspects of the testing procedures including sample handling,
transport, storage, preparation, calibration, test procedures, statistical techniques for
evaluating data and measurement uncertainty.
5.4.2 Selection of Methods
The laboratory employs published analytical methods or methods that have been recognized
to meet the needs of the client and are appropriate for the tests being conducted. Guidance
will be provided by the laboratory when there is a question about the test method to be
used. The laboratory will notify the client when an inappropriate method is requested.
5.4.3 When a new test method must be developed, validation procedures as developed
under the QA Rule, 62-160, FAC, of the Department of Environmental Protection will be
followed before it is put into use.
5.4.4 See TNI Standard Volume 1, Modules 4, 5 and 7 for the use of non-standard methods
in Chemistry, Microbiology and Toxicology respectively.
5.4.5 See TNI Standard Volume 1, Modules 4, 5 and 7 for the validation of new methods in
Chemistry, Microbiology and Toxicology respectively.
5.4.6 For quantitative laboratory measurements, statistical quality control measures are
used within the Bureau of Laboratories to estimate the uncertainty associated with

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analytical methods. See SOP LB-003, Estimation of Measurement Uncertainty, for a

complete discussion.
5.4.7 Control of Data
5.4.7.1 Calculations and data transfers are evaluated by a multi-level system detailed in
SOP LB-025, Event Level Authorization Checklist and SOP LB-026, Job Level Authorization
Checklist.
5.4.7.2 Tracking changes to the Laboratory Information Management System (LIMS) and
software used for data calculations and assessments are detailed in FDEP SOP LB-009,
Standard Operating Procedure for Validation of LIMS Software Development or
Modifications that Affect the Calculation/Assessment of Analytical Results , and SOP LB006, Standard Operating Procedure for Records Maintenance and Storage. Permissions
are established for all electronic records to restrict unauthorized access.
5.5 CALIBRATION REQUIREMENTS
5.5.1 All necessary equipment to perform the tests and associated calibrations for the
methods in Table 5.1 are under the control of the FDEP Bureau of Laboratories, and
described in the labs SOPs.
Instrumentation utilized by the biology laboratory for the determination of test parameters
in Table 5.2 is described in the labs Biology SOPs. Calibration requirements for laboratory
and field instruments in Biology are listed in Table 5.3.
5.5.2 The laboratory ensures that all equipment and associated software used by the
laboratory meet the accuracy requirements and specifications of the test methods before
being placed in service.
5.5.3 Supervisors ensure that all personnel have received adequate training on the use of
laboratory equipment and that manufacturers instruction manuals are easily accessible.
5.5.4 All equipment and instruments including software, where applicable, are uniquely
identified.
5.5.5 Records are maintained for all equipment and associated software including:

Identity of the piece of equipment and associated software

Unique identifier
Checks that equipment meet specifications
Location of the equipment
Manufacturers instructions
Calibration records
Maintenance logs

5.5.6 All maintenance or repair to equipment is documented in laboratory notebooks.

Documentation includes a description of the problem(s), work performed, date and

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analyst's initials. Sample analyses plans for instrument failure or maintenance are handled
in this order: use backup instrument, delay the analysis if holding time can be met, postpone
the sampling event or send samples to the overflow laboratory.
5.5.7 Any equipment found to be unserviceable is tagged with an Out of Service tag if
it is shared by multiple work groups or will be out of service for an extended period. If the
unserviceable equipment is used only by a single work unit and the condition is deemed
temporary (a service call has been made and/or the equipment is awaiting repairs by
qualified technicians), then the supervisor may elect to notify staff directly rather than to tag
the equipment.
5.5.8 All support equipment requiring calibration is labeled or otherwise documented to
indicate that calibration has been performed and when it is due.
5.5.9 The calibration of all instruments will be verified following instrument maintenance.
5.5.10 See the calibration procedures in the associated test SOPs that detail the type of
checks and the frequency to verify continued calibration.
5.5.11 Any allowable correction factors, e.g. thermometer calibrations, which require the
readout to be adjusted, will be clearly labeled and positioned for easy access by the analyst.
5.5.12 Procedures to gain access and the tracking of changes to the LIMS are addressed in
section 4.13.3 (a) under the Laboratory Information Management System. Only authorized
personnel are allowed access to the laboratory to avoid tampering with the instrumentation.
5.5.13 Additional Requirements and Clarifications
5.5.13.1 Support Equipment

All support equipment is maintained in proper working order.

Maintenance or repair to equipment is documented in a laboratory notebook.
Documentation includes a description of the problem(s), work performed, date
and analyst's initials.
Calibration procedures for support equipment are found in SOP CM-011,
Gravimetric Analysis: Analytical Weight and Balance Calibration, and the test
SOPs.
Calibration checks are conducted against nationally recognized standards.
Calibrations or verifications are checked against the required specifications for
the use of the equipment. If the calibration or verification results are not within
the required specifications equipment is removed from service until appropriate
repairs can be conducted.
Correction factors to be applied associated with the results of any thermometers
are clearly labeled and positioned for easy access by the analysts
Auto-Pipets are calibrated at least quarterly according to SOP NU-039, Calibration
of Auto-Pipettes

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5.6 MEASUREMENT TRACEABILITY

5.6.1 This section of the ISO standard is not applicable to environmental measurements.
5.6.2 This section of the ISO standard is not applicable to environmental measurements.
5.6.3 Reference Standards and Reference Materials
5.6.3.1 Reference Standards
Standard sources, preparation frequency, storage and traceability are detailed in the
method SOPs and Table 5.4.
5.6.3.2 Where possible, Reference Materials are traceable to NIST or EPA.
5.6.3.3 Intermediate checks
Continuing calibration checks are conducted according to the technical SOPs,
http://www.dep.state.fl.us/labs/library/lab_sops.htm.
5.6.3.4 Standards are stored as specified in Table 5.4 and the method SOPs.
5.6.4 Additional Requirements and Clarifications
5.6.4.1 The laboratory is a participant in TNIs Performance Evaluation Study, the RCRA
Laboratory Evaluation Program, and the USGS Standard Reference Sample Project. The
QA Officer manages the performance testing program.
5.6.4.2 All purchased reagents and solvents are dated upon receipt. Reagents and
solvents that are commonly used by multiple groups within the lab are tracked using a
computerized inventory program. Table 5.5 lists the location and storage of reagents
used by the chemistry and biology laboratories. Commonly used solvents, chemicals and
laboratory consumables such as gloves, pipette tips, sampling containers etc. are
maintained in the central lab inventory. When the stock for any item in the inventory
dips below a pre-determined threshold, the program alerts purchasing staff who
maintain the inventory to order additional supplies. The preparations of laboratory
standards from primary stock standards, neat standards or reagents are documented in
laboratory notebooks or the Standard Preparation Tracker module of the LIMS.
Additional documentation can be found in the relevant test SOPs and (for example) the
following SOPs: SOP HG-012, Mercury Group Standards Preparation Procedures, SOP LC039, HPLC Standard Preparation, SOP NU-041, Reagent Preparation Procedures for
general chemistry and nutrients, SOP NU-042, Standard Preparation Procedures for
general chemistry and nutrients and SOP SV-009, BNA Standard Preparation.
5.7 COLLECTION OF SAMPLES
The FDEP Chemistry Laboratory does not provide field sampling services. The laboratory
does provide sample containers (sampling kits) to its customers on request. However, the

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FDEP Biology Laboratory provides field sampling services. Table 5.6 lists the sampling
capabilities and associated sampling equipment of the Biology Laboratory.
5.7.1 The Biology Section follows the protocols described in the Departments Statewide
SOP for Field Activities. All FDEP Field SOPs referenced in this document are available on the
Departments Internet site,
http://www.dep.state.fl.us/water/sas/sop/sops.htm. They include:
FS 1000
FS 2000
FS 2100
FS 2200
FS 2300
FS 2400
FS 3000
FS 4000
FS 5000
FS 6000
FS 7000
FS 8100
FS 8200

General Sampling Procedures

General Aqueous Sampling
Surface Water Sampling
Groundwater Sampling
Drinking Water Sampling
Wastewater Sampling
Soil Sampling
Sediment Sampling
Waste Sampling
General Biological Tissue Sampling
General Biological Community Sampling
Contaminated Surface Sampling
Clean Sampling for Ultra-Trace Metals in Surface Waters

Sampling details such as the choice of container materials, sample volumes, preservation
techniques, and holding times for analytes are described in DEP SOP FS 1000, General
Sampling.
5.7.2 Deviations from documented sampling procedure are documented in the field as
comments on the submittal form which is part of the chain of custody for the samples.
Figure 4.6 shows examples of the submittal form used during the collection of chemical and
biological samples. Depending on the nature of the deviation, the deviation is recorded as a
non-conformance and a non-conformance report is included with the sample report. The
sample data will be suitably qualified by the laboratory to accurately reflect the nature of
the deviation.
5.7.3 Documentation procedures for recording relevant data during sampling are
described in field SOP FD 1000, Documentation Procedures. This SOP, along with other field
SOPs is located at http://www.dep.state.fl.us/labs/bars/sas/qa/sops.htm.
5.7.4 All submittal forms include the date and time of sample collection. Deviations from
documented sampling procedure are documented at collection as described in section 5.7.2.
5.8 HANDLING SAMPLES AND TEST ITEMS
5.8.1 See Section 4.13.3 (a), SOP LB-016, Laboratory Support Section Receiving Room:
Standard Operating Procedure for the Receipt and Log-in of Samples by the DEP Central

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Laboratory. All calibration standards, whether purchased or prepared are tracked in the
LIMS Standard Preparation Tracker. Calibration standards are disposed upon expiration
while samples, except samples involved with criminal events, are disposed two weeks after
reporting data. Details are described in SOP LB-023, Standard Operating Procedure for
Documenting Evidentiary Chain of Custody within the DEP Laboratory.
5.8.2 See Section 4.13.3 (a) and SOP LB-023, Standard Operating Procedure for
Documenting Evidentiary Chain of Custody within the DEP Laboratory and SOP LB-016,
Laboratory Support Section Receiving Room: Standard Operating Procedure for the Receipt
and Log-in of Samples by the DEP Central Laboratory, for identifying samples upon receipt
and movement through the laboratory.
5.8.3 See Section 4.2.4 for procedures associated with any non-conformances that may
affect the integrity of the data. See SOP LB-016, Laboratory Support Section Receiving Room:
Standard Operating Procedure for the Receipt and Log-in of Samples by the DEP Central
Laboratory, Section 3, for sample receiving and documentation of non-conformances
associated with sample receipt.
5.8.4 Sample location can be tracked from most workstations in the laboratory and can be
changed if the sample is relocated. Samples are stored in a number of different areas,
separate from all standards and reagents:
(a) air conditioned room: metal samples and others not requiring refrigeration.
(b) walk-in refrigerator 5: organic samples (e.g. BNA, pesticides)
(c) walk-in refrigerator 4: nutrients
(d) double wide refrigerator 6: nutrients
(e) incoming sample refrigerator: temporary storage for temperature sensitive biology
samples awaiting login
(g) double door refrigerator 1: soils/sediments
(h) triple door refrigerator 7: nutrients and VOCs
(i) triple door refrigerator 8: soils/sediments
(j) walk-in bio-freezer: biological tissue and other samples requiring freezing
(k) walk-in bio-refrigerator: biology samples that require refrigeration
(l) flammables storage refrigerator 9
(m) mercury clean lab
(n) Biology
(o) three double-door refrigerators, ERLN01, ERLN02 and ERLN03 for emergency
sampling events
5.8.5 Additional Requirements Documentation

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For both chemistry and biology, samples of a similar nature submitted together from one
collector are aggregated into a single event. Event identification numbers are unique and
have the format Customer Name -YYYY-MM-DD-xx where YYYY-MM-DD is the date the event
is created and xx is an accession number that is reset to -01 each day and incremented as
events are logged in. Within each event, samples are grouped by analyses into jobs. All final
review and reporting of data to submitters is event specific.
Additionally, each sample is assigned a unique sample identification number of the format
LLL-YYYY-MM-DD-xx-yy where LLL-YYYY-MM-DD-xx is the job identification number and yy is
an accession number between -01 and -99. LLL represents the lab location (TLH is for
Tallahassee). YYYY-MM-DD represents the day the samples are logged into the LIMS. The
LIMS also maintains an additional internal accession number (with bar code) for each
sample. At log-in, a bar coded label corresponding to the samples unique laboratory
identification number is printed and placed on each sample bottle.
All log-in information is cross-checked by a second log-in technician, after which, event login
is authorized in the LIMS. The event folder is placed in a central location to await the final
report.
Biology
The sample station, replicate number (if any), date, and analysis type form a unique
identification for each sample. Each sample container is labeled with this information plus
preservation type (if any) using waterproof markers. Field and laboratory sheets use the
same nomenclature. Time of sampling is marked on the submittal form to document
sequence of sampling. Laboratory bench sheets are filled out using pens with waterproof
black ink. Data submittal forms are filled out using pens with waterproof black ink if
conditions allow, or dark, soft-lead pencils if conditions are wet.
Algal Growth Potential/Limiting Nutrient Bioassays, Physical-chemical parameters,
Phytoplankton, Toxicity Bioassays
Sample containers are identified with the site name, station number, replicate, date
sampled, and time collected. The sample submittal form (Figure 4.6) is completed, including
time of sampling as well as any physical-chemical parameters. Habitat assessments (FDEP
SOP forms FD 9000-04 through FD 9000-06) and Physical-Chemical Characterization Field
Data Sheet (FDEP SOP form FD 9000-03) may be completed.
Chlorophyll-a, Microbiology, BOD, Grain-size analyses
Refer to SOP BB030, Sample Custody, Preparation Labels, and Worksheet Instructions for
Bench Biology Samples.
Benthic macroinvertebrates
Sample containers are identified with the site name, station number, replicate, and date
collected. This information is written directly on the Whirlpak bags used for holding HesterDendy samplers. Physical-chemical parameters, associated site information, and substrate
sampling information (for Stream Condition Index samples) are recorded on the Physical-

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Chemical Characterization Field Data Sheet (FDEP SOP form FD 9000-03) and Habitat
Assessment data sheets (FDEP SOP forms FD 9000-04 and FD 9000-05).
Periphyton
Sample containers are identified with the site name, station number, and date collected.
Physical-chemical parameters, associated site information, and substrate sampling
information are recorded on the Physical-Chemical Characterization Field Data Sheet (FDEP
SOP form FD 9000-03) and Habitat Assessment data sheets (FDEP SOP forms FD 9000-04 and
FD 9000-05). ). FDEP SOP form FD 9000-25, Rapid Periphyton Survey, may also be completed
and submitted with the samples.
5.8.6 Sample Acceptance Policy
Samples arriving at the FDEP Central Laboratory are evaluated at the time of receipt. The
samples must meet certain requirements in order to be processed in the laboratory. If some
of the requirements are not met, the customer is notified of the discrepancy by the receiving
staff and a Non-conformance Report (NCR) is created. For Biological samples, receiving
room staff contact Biology Section staff with notification of the types of samples received
and that they need to be picked up.
The Receiving staff member inspects the samples for damage and sustained holding
conditions and, if anything is improper, notes it on the Log-in Checklist. For short hold
biology samples, the samples are picked up by biology staff and checked out using the LIMS
system to establish custody. See SOP BB-030 for details. Samples must meet the following
requirements or they will be subject to rejection:

The labels and writing on the containers must be waterproof so that the containers
can be correctly identified upon receipt at the lab.
There must be a unique identifier on each container (field ID/test ID combination).
The information on the submittal form must coincide with that on the containers.
Examples of the submittal form supplied by the Central Laboratory are given in Figure
4.6. The minimum information required includes:
a) a unique sample location/field ID combination
b) the date and time of sample collection
c) the collectors name
d) a LIMs Request ID (contains customer/project information)
e) a sample matrix
f) the analyses requested

The containers must be preserved appropriately.

The samples must be collected in the appropriate type of container.
There must be sufficient volume for analysis.
The samples must be delivered to the lab with sufficient time remaining for the
laboratory to meet analytical holding times.

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If the information provided is insufficient to correctly process the samples an effort is made
to reach the collector by phone. If the information cannot be obtained in a timely manner,
the samples are subject to rejection.
5.8.7 Sample Receipt Protocols
5.8.7.1 At the time of receipt, log-in technicians check the temperature of the coolers.
The log-in technicians verify the submittal form information against the sample bottles;
any discrepancies are resolved. The pH of preserved samples is checked by technicians
prior to sample login. The sample is checked for sufficient volume. Sample integrity such
as improper temperature and pH preservation, insufficient volume, leaking or broken
bottles etc., are entered into a non-conformance report in the LIMS as well as
documented on a Log-in Check form with the log-in technicians initials. The VOC vials
are checked for the presence of bubbles by analysts in the VOC laboratory. Trace level
mercury and methylmercury water samples have special handling and custody
procedures. Details of these procedures are described in SOP LB-016 and SOP HG-001.
Hazardous samples received as part of the Environmental Response Laboratory Network
(ERLN) must be handled according to procedures described in the SOP ERLN-001 and SOP
LB-029, Standard Operating Procedure for Handling Perceived Threat Materials.
5.8.7.2 See section 4.2.4 for procedures associated with non-conformances that may
affect data quality.
5.8.7.3 The samples are logged into the LIMS with all the information listed above from
the submittal form plus the following:

STORET station number or NPDES number (if available)

field parameter values (if available)
work module number (if available)
mode of sample delivery (e.g. common carrier, Federal Express, etc.) and delivery
date
field comments (if available)
lab comments (if available)
sample storage location in the laboratory
name of the log-in person is stored in LIMS automatically, with the time and date
of sample log-in.
bottle lot number (manufacturers lot number on bottle)

Samples are assigned to analysts or technicians by generation of assignment worksheets

or backlog reports as appropriate. As the samples move through the laboratory, they
and the individual analyses assume the following status designations automatically or
when manually flagged by authorized personnel:

W- awaiting preparation (i.e., digestion or extraction) = appears

automatically at log-in for samples with analyses that require sample preparation

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V- available for analysis = appears automatically at log-in for samples that do not
require sample preparation or appears when the completion of sample
preparation is flagged by the technician
C- analysis and data entry complete = changes from 'V' automatically when data
are entered into the LIMS
A- results authorized for release = changes from 'C' when data are authorized
X- canceled

Sample holding times relating to sample preparation or analysis are entered

automatically at sample login. The deadline is calculated and updated each day by the
computer and printed out on the worksheet or backlog report. Supervisors have the
responsibility to ensure that all analyses under their supervision are prepared and
analyzed within the holding times. Table 5.9 describes the list of acceptable sample
containers, preservation techniques and holding times for samples received by the
laboratory. Chemists, biologists and technicians who schedule their work priority from
backlog reports have the responsibility to complete their individual work within the
holding time. An example of a backlog report is given in Figure 5.1.
5.8.7.4 Copies of the submittal form and any field sheets are scanned into a computer
and the file is named using the event ID. The originals of the submittal form, log-in check
forms and other related documents are filed together in an event folder labeled with the
event name.
5.8.7.5 Sample custody procedures are described in section 4.13.3. Figure 4.6 shows
examples of submittal forms used as transmittal forms for routine sample custody and
documentation of custody. The information on the submittal form must coincide with
that on the sample containers and include elements listed in section 5.8.6.
5.8.8 Legal chain of custody procedures are described in section 4.13.3.
5.8.9 Additional Requirements Sample storage and disposal
Samples, sample fractions, extracts and digestates are stored according to the storage
instructions in the preservation tables FS 1000-4 through FS 1000-11 from DEP SOP FS 1000,
General Sampling Procedures (http://www.dep.state.fl.us/water/sas/sop/sops.htm). The
manner of storage prevents cross contamination and isolates the samples from standards,
reagents and food.
Completed samples with jobs authorized (checked from computer) are disposed of. Samples
flagged as hazardous in the LIMS are disposed of according to Table 4.3. Nonhazardous
aqueous samples are poured down the sink drain while flushing with tap water. Nonhazardous solid samples are disposed of in the garbage. Disposal of all samples is
documented on the LIMS chain of custody record with the technician's name and date.

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5.9 QUALITY ASSURANCE FOR ENVIRONMENTAL TESTING

5.9.1 The laboratory has an established quality control program for monitoring the
performance of test methods conducted under this manual. The types of quality control
(QC) checks and the frequency at which they are performed are listed in the method or test
SOPs. A batch of samples consists of 20 or fewer samples that are prepared and/or analyzed
in a single run. Saline matrices are batched separately where the test is impacted by high
conductivity samples.
The QC objectives are considered when selecting methods and in evaluating the capability of
the laboratory to handle sample loads that meet the QC objectives.
a) Calibration standards are checked against certified reference materials or other
independently prepared standards where available.
b) The laboratory is a participant in performance testing studies. See section 5.6.4.1.
c) Replicate analyses are used to evaluate precision. Precision is expressed by the relative
percent difference (RPD) to compare duplicate samples/spikes A and B and is based on the
formula:

Precision may be determined from duplicate authentic samples, from duplicate LCSs or from
matrix spike duplicates. Where RPDs are calculated based on matrix spike duplicates, A and
B represent the raw results of the spiked sample (spike plus the background).
d) The accuracy of the test method is assessed in terms of percent recovery for LCSs
(fortified blanks) and matrix spikes to evaluate matrix impact.
Percent Recoveries for an LCS is calculated as:

or for Matrix Spikes as

where:
SC = Concentration in the spiked sample
UC = Concentration in the unspiked sample (in the case of results below the MDL for
the unspiked sample zero is used as the concentration)
EV = Expected value

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5.9.2 Quality assurance targets (QATs) for each QC check are defined in terms of relative
precision (P) or accuracy (A). Analyte concentrations associated with each QC check are
defined as high, mid, or low, depending on what range of the calibration curve the check
concentration falls.
A statistical program, written in Borland Delphi and integrated with the LIMS, handles the
calculations of mean and standard deviation and also calculates warning and control limits
for QC elements. QC data are uploaded from electronic QC analysis tools to the LIMS for
storage. The statistical program looks at historical data and at a specified frequency, recalculates accuracy and precision acceptance limits for a specific sample matrix, instrument
type and QC element. Warning and control limits are calculated when at least seven or
more data points are available.
They may be updated when:
(a) a minimum of at least 7 new data points are available;
(b) significant changes are made to the instrument or analytical method;
(c) they have not been updated in the last twelve months.
The user selects at least 7 new, or the most recently generated data points (accuracy,
precision or MDL values). The program calculates warning limits for these elements based
on approximately two standard deviations from the mean and control limits based on
approximately three standard deviations from the mean. In general, the laboratory utilizes
method or laboratory defined warning and control limits for reporting data (i.e., statutory
control limits). Those statutory limits may be modified utilizing statistical information
collected over time. The precision and recovery data are used for the diagnosis of analytical
problems. For laboratory parameters, calculated statistical control limits are used as criteria
to accept or reject data only if they are more stringent than the criteria listed in Table 5.1.
The formulae used for the calculation of standard deviation, mean, upper and lower control
and warning limits are shown below. (Reference chapter 6 of "Handbook for Analytical
Quality Control in Water and Wastewater Laboratories" - EPA 600/4-79-019, March 1979).
(a) Standard deviations are calculated based on the formula:

Where Sp = standard deviation of the population

n = total number of points in the population
Pi = the value for each point
(b) The mean is calculated as the average of all points:

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(c) For recovery, the upper and lower control limits are based on a 99% confidence level.

UCL = P + t0.99Sp
LCL = P t0.99Sp
(d) The upper and lower warning limits for recovery are based on a 95% confidence level.

UCL = P + t0.95Sp
LCL = P t0.95Sp
where t0.99 and t0.95 are Students t factors for 99% and 95% confidence, respectively.
Because levels of statistical confidence vary with sample size, a fixed level of statistical
confidence is employed that approximates 2 and 3 standard deviations. Those control limits
are based on requirements specified in various EPA methods and in EPAs Handbook for
Analytical Quality Control in Water and Wastewater Laboratories. The statistical program
utilizes a Students t table, setting warning limits at 95% confidence and control limits at 99%
confidence. Those Students t factors correspond approximately to 2 and 3 standard
deviations for 7 collected datum points (~1.9 Sp and ~3.1 Sp, respectively). The advantage of
using Students t factors is that control limits are based on known confidence limits
regardless of the number of datum points in the population.
5.9.3 Essential Quality Control Procedures
(a) Standard Quality Controls
Standard quality controls include the following essential controls:
i) Positive and negative controls (LCSs, and method blanks)
ii) Controls to evaluate the variability, repeatability of the test (replicates/duplicates)
iii) Test method accuracy (calibrations, continuing calibrations, certified reference
materials, PT studies and matrix spikes)
iv) Measures to evaluate test method capability

Detection Limit Studies

Determination of Quantitation Limits
Range of applicability

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Method Detection Limits (MDL and Practical Quantitation Limits (PQL))

The Method Detection Limit (MDL) and Practical Quantitation Limit (PQL) are defined
and used for the same objectives in all analyses. However, because of differences in
the nature of various analyses, the calculation procedures vary; nevertheless, the
underlying principles and concepts are applied uniformly. Described below are the
most representative procedures used in this laboratory. (See Appendix C for specific
references.) Details of calculations for each analytical method may be found in the
laboratory's SOPs.

The MDL is defined as the minimum concentration of an analyte that can be

measured by the method with 99% confidence of its presence in the sample
matrix. For measurements that always produce a measurable analytical signal in
method blanks (e.g., inorganic parameters) that are near or above the signal
produced at an estimated detection limit, MDLs may be determined from
samples of reagent water containing all preparation reagents and carried through
the preparation procedure. The MDL is established at a level that excludes 99%
of the analytical noise, consistent with the intent of 40 CFR part 136 Appendix B.
The applicable Students T value (corresponding to the appropriate degrees of
freedom; = 0.01) is multiplied by the measured standard deviation of the
population of method blank results. That factor is added to the average method
blank value. If the average blank result is less than zero, either zero is used as the
average or, if analytical interferences are suspected in playing a role in the
measurements, the absolute value of the average method blank value may be
used as the average. The latter option has the potential of elevating the MDL to
accommodate unknown interferences and should be used with discretion. This
protocol, generally consistent with the intent and practice of 40 CFR part 136
Appendix B, avoids reporting method detection limits that are unrealistically low
and below or within the population of method blank results.
For measurements that do not produce an analytical signal in method blanks
(e.g., organic parameters and some inorganic parameters) MDLs are established
by analyzing 7 to 20 replicate reagent spikes fortified at 1 to 5 times the
estimated MDL, per 40 CFR part 136 Appendix B. The MDL is set to the students
T value (corresponding to the appropriate degrees of freedom; = 0.01) times
the resulting standard deviation of the measured concentrations of the
replicates.
Note: Tables 5.1 and 5.2 are updated annually so the MDLs used by the
laboratory may sometimes vary with those listed in both tables.

The PQL is the lowest level of concentration that can be reliably achieved within
specified limit of precision and accuracy during routine laboratory operating
conditions. This laboratory sets the PQLs at 3 to 5 times the MDL depending on
the method of analysis and the analyte, unless otherwise specified.

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A System Performance Check is defined as the procedure in which a standard

consisting of one or more analytes is introduced into the analytical system to
verify its performance (responses, peak shapes, retention times or spectra) meets
the minimum acceptable criteria. See SOP LB-031, Limit of Detection Verification.
Additional details about the labs procedures for evaluating test method
capability can be found in SOP LB-007, Procedure and Policy for Method and
Instrument Validation.

v) Data Reduction
A LIMS module performs sample and QC calculations (e.g., accuracy, precision and %
RSD). This module called the QC Manager is also used to upload sample and QC results
into the LIMS data tables. Sample and QC result calculations are reduced as follows:

Results from analyzed sample extracts or digestates are processed by the

analytical instruments PC-based data systems or by the laboratory
Chromatography software, based on the method protocols in Table 5.1 and Table
5.2. These raw sample results are electronically downloaded from the analytical
instrument to the QC Manager. For those instruments not interfaced to a PC,
results from the instruments are manually entered into the QC Manager.

Sample results and QC results are linked together by batch numbers which are
generated by the QC Manager, so sample prep and analysis batches are always
identified with their associated QC. The analyst enters pertinent sample
prep/analysis data (amount sample digested or extracted, final digestate or
extract volume, dilution factors, spiking level/solution used, etc.) and then signals
the QC Manager to begin calculations. Examples of typical water and sediment
calculations performed follow:
For water samples: C (g/L) = D (g/mL) Vf (mL) / Vi (L)
For soil/sediment samples: C (g/kg) = D (g/mL) Vf (mL) / [Ms (kg) k]
where:
C = Concentration of analyte in sample
D = Concentration in extract or digestate
Vf = Volume of extract or digestate
Vi = Initial volume digested or extracted in L.
Ms = Mass of sample digested or extracted
k = Dry weight correction factor

The resulting sample and associated QC results are reviewed by the analyst, and if
deemed acceptable, are then uploaded to the LIMS. Current acceptance criteria
(warning and control limits) for each QC element are stored within the QC

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Manager. If QC results are outside of the current control limits, data are flagged
as unacceptable, and the associated sample batch may then be re-submitted for
re-digestion/re-extraction and/or re-analysis. Additional information may be
found in the individual test SOPs.
vi) All chemical reagents and standards are procured from reputable vendors with the
proper specifications (grade, purity) to ensure performance within the appropriate
laboratory and test method specifications. Table 5.5 summarizes reagent storage.
vii) Selectivity is evaluated by employing method requirements and practices established
by the laboratory detailed in the test SOPs to confirm responses to the analyte. Checks
used include dual column confirmation, inter-element interference checks, retention
time windows, mass spectral tuning, method blanks. viii) All test conditions are
monitored and documented where required by the method to ensure constant,
consistent and documentable conditions.
(b) The laboratory utilizes method or laboratory defined warning and control limits for
reporting data. Those limits may be modified utilizing statistical information collected over
time. The precision and recovery data are used for the diagnosis of analytical problems. For
laboratory parameters, calculated statistical control limits are used as criteria to accept or
reject data only if they are more stringent than the criteria. QA targets and their use are
provided in Tables 5.1 and 5.2. QC data are deemed acceptable if the following condition is
met:
Lower Control Limit (LCL) QC Result Upper Control Limit (UCL)
Each analyst and/or technician is responsible for determining that the results of each
analytical measurement have all associated QC measurements and that the acceptance
criteria are evaluated and documented according to protocol. The analyst and/or technician
is responsible for checking calculations, completing sample preparation, calibration, analysis
and instrument logs, and completing all internal custody documentation. All written records
and logs must be made using indelible ink and must include the analysts signature or initials.
Any corrections to written records must be made using a single strikeout of the original
entry. The corrected entry must be dated and initialed by the individual making the
correction. No correction fluid or obliterations may be made to the written records.
Each supervisor is responsible for reviewing this work for completion and correctness prior
to authorizing the individual results for release.
The data verification procedures consist of all the QC validations and calculations checks
discussed above. In addition, soundness of all data is evaluated by the nature of the
sample, the inter-relationship among the parameters and the historical values if available,
etc. Any discrepancy or inconsistency will initiate a recheck of data or reanalysis of the
sample(s).
(c) The laboratory has developed in-house methods/SOPs that are not cited in rules or
regulations such as the Clean Water Act or SW-846. The methodology used to develop and

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validate these methods is identical to that used to validate regulatory methods. The quality
control procedures described in sections 5.9.3 (a) and 5.9.3 (b) apply to in-house
methods/SOPs as well.
5.10 REPORTING RESULTS
5.10.1 Test results are reported accurately, clearly, unambiguously and objectively and
contain all method required information, reporting requirements of the TNI standards and
requirements of the State of Florida QA Rule, Chapter 62-160, FAC.
5.10.2 Test reports contain all of the information required in 5.10.2 of the TNI standard.
Each supervisor or workgroup designee is responsible for authorizing the individual analysis
results and samples for release. When all the samples within a job are authorized, the
managers or supervisors are responsible for reviewing and authorizing the job for release.
After all the jobs in an event are authorized, the LIMS automatically generates a list of
reports that are ready to be reviewed and certified. The Program Administrator (or his/her
designee) reviews the report in LIMS and evaluates the data using a quality assessment tool,
Automated Data Processing Tool (ADaPT). See SOP LB-025, Event Level Authorization
Checklist, for complete details.
Once the review is completed, the report is certified in LIMS. After certification of noncriminal case reports, one copy of the event analysis report is printed with an electronic
signature and retained, with the original submittal form, in the laboratory. A pdf file of the
signed report is automatically created and, along with a pdf of the sample submittal form,
and any associated paperwork (e.g. reports received from a subcontract laboratory), and an
ADaPT data file, transferred to an ftp directory accessible to the client. All final sample
results with associated QC data are archived together in the LIMS committed database and
can be retrieved in the future if necessary.
For criminal case reports the generated printout does not have an electronic signature. The
reviewing manager must sign and date two hard copies. One copy is retained by the FDEP
Bureau of Laboratories and the second copy is mailed to the client.
If any analyses or preparations exceed holding time before completion, the results are
automatically qualified. See SOP LB-027, Standard Operating Procedure for Reporting
Qualified Data, for the laboratory data qualification policies and application of Table 1 of the
FDEP QA Rule, Chapter 62-160, FAC. Results associated with quality control data that are
outside the acceptance criteria are qualified with a J.
An appropriate comment is used to qualify results whenever:
1) batch or sample specific quality control results for an analyte cannot be
realistically assessed (e.g., due to excessive analyte levels in a matrix spike);
2) quality control data indicate the uncertainty associated with the measurement(s)
is outside acceptable limits;

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3) sample matrix presents an unusual challenge to a method or instrument. The

decision to qualify a result on these factors is at the discretion of the authorizing
supervisor and must comply with FDEP SOP LB-027, Standard Operating Procedure
for Reporting Qualified Data.
The report includes the page number and total number of pages.
5.10.3 Test Reports
5.10.3.1 Content in addition to the requirements of 5.10.2
a) Any deviations from the test method or any conditions affecting the reported
results are described in the final report.
b) Any non-conformances to the procedures in this manual or to the test method are
identified in a report comment or a non-conformance report. See FDEP SOP LB-002,
Non-conformance Reporting System.
c) A quality control report including results for method blanks, laboratory control
samples (accuracy and precision), matrix spikes (accuracy and precision), surrogates
(accuracy) and calibration verification samples (accuracy).
d) See SOP LB-003, Estimation of Measurement Uncertainty, for reporting of
measurement uncertainty. All reports indicate that uncertainty associated with the
analytical results can be estimated from the reported quality assurance results and
from published test performance acceptance criteria.
e) See section 5.10.5 below for opinions and interpretations.
f) Additional information required by specific methods and clients will either be
provided in the report as deemed necessary or communicated directly to the client.
5.10.3.2 An electronic copy of the report, along with copies of the submittal form is
provided to the customer or submitting agency. Sampling records and comments are
limited to the submittal forms provided by the sampling party or agency to the
laboratory.
5.10.4 Calibration Certificates as addressed in ISO 17025 are not applicable to
environmental testing.
5.10.5 Laboratory test data will be qualified according to FDEP SOP LB-027, Standard
Operating Procedure for Reporting Qualified Data. Upon request, laboratory supervisors can
assist clients in interpreting data reported by the lab. Such consultation will be conducted
and documented where appropriate directly with the client.
5.10.6 Analyses performed by a subcontract laboratory are clearly identified on the test
report. See section 4.5 for additional information.
5.10.7 Electronic Transmission of Results

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Although the laboratory may transmit data in various electronic formats to clients
upon request, the laboratory considers that only the report with a signature represents
the official analysis report.
5.10.8 Report contents are uniform and designed to clearly and unambiguously present the
required test information to the client.
5.10.9 Amendments to Test Reports
Required amendments to test reports will consist of a recreation of the entire report. The
amended report is identified as such and the original report is referenced.
5.10.10 Exceptions
All reports are created following the same procedures. Abbreviated reports are not created
for any sample analyzed by the laboratory.
5.10.11 Additional Requirements
a) A preparation and analysis log is included with each test indicating the prep and
analysis date of each sample. If the activity (preparation or sampling) has a holding time
of 72 hours or less the time of the activity is included.
b) Unless otherwise noted, analytical values for soil and sediment samples are reported
on a dry weight basis, and analytical values for waste and tissue samples are reported on
a wet weight value. This information is provided in the remarks section of the analytical
report.
c) All test components that are not accredited are identified on the test report.
d) Numeric results outside of the calibration range, where possible, are diluted and reanalyzed. In situations where this is not possible the reported results will be qualified
according to established laboratory data qualification protocols. See FDEP SOP LB-027,
Standard Operating Procedure for Reporting Qualified Data.

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APPENDIX A
ROLES AND RESPONSIBILITIES FOR THE CHEMICAL AGENT LABORATORY
The implementation of safety, security, and chemical hygiene procedures is the
responsibility of all facility staff. The following subsections describe specific safety and
chemical hygiene responsibilities for the Florida Department of Environmental Protection
Bureau of Laboratories Chemical Agent Laboratory. It is the responsibility of all laboratory
staff and their managers to know and follow the provisions of this plan. Responsibilities are
listed by title.
1.1

Laboratory Director

The Laboratory Director is responsible for ensuring that this administrative practice is
followed by all users of ultra-dilute chemical warfare agent (CWA) solutions and that
resources and support are provided for the implementation of this plan and the
requirements outlined therein. The following tasks are the responsibility of the Laboratory
Director:

Responsible for the health and safety of personnel.

Responsible to ensure all recognized hazards are promptly addressed.

Interact with laboratory management and personnel to ensure that DSHP procedures are
understood and followed and assistance or resources are provided as needed.

Serve as a back up to the Agent Manager (AM) by holding a back-up key (primary lock and
key entry system) to the UDA standard storage refrigerator in case of the AMs absence.

1.2

Laboratory Manager

The Laboratory Manager (LM) is responsible for the daily operation of the CWA laboratory and
daily execution of the Dilute Solution Hygiene Plan as it relates to the laboratorys activities. The
LM is responsible for the health and safety of the Chemical Agent Operators (CAOs) during all
UDA procedures. The LM also shares responsibilities for development, implementation, review,
and support of the DSHP with the Chemical Agent Hygiene Officer (CAHO). The following tasks
are the responsibility of the Laboratory Manager:

Ensure that the Ultra-Dilute Agent laboratory has required safety supplies and equipment
necessary to handle or store UDA materials safely.

Ensure that UDA personnel are familiar with the Dilute Solution Hygiene Plan (DSHP) and
routinely follow the requirements and procedures.

Ensure that safety equipment is checked and ready for use.

Request and coordinate delivery of UDA reference material from the U.S. Army
Edgewood Chemical and Biological Center and Engineering Center (ECBC) with
Contracting Officers Representative (COR) or ECBC Chemical UDA Accountability Officer.

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Document all requests, coordination, and communication concerning delivery of UltraDilute Agents in the Accountability Assessment log.

Appoint a qualified CAO to perform the dry runs with dilute agents to test Standard
Operating Procedures (SOPs) and approve staff readiness.

Routinely observe CAOs performing UDA SOPs and provide recommendations in

conjunction with the CAHO to improve UDA laboratory safety.

Determine staffing, UDA laboratory access and/or training level needs as necessary and
ensure identified training levels are met by the individual.

Conduct regular UDA inspections of housekeeping, personal protective equipment (PPE),

and emergency equipment.

Ensure that current copies of the CHP, DSHP, procedures, and other pertinent documents
are readily accessible for use in the Ultra-Dilute Agent laboratory.

Ensure that security requirements are met as specified in the Security Plan.

Perform quarterly accountability audits with the Agent Manager as a formal witness.

Serve as back-up for the Agent Manager for receipt of Standard Reference Materials
(SRMs).

Serve as a back-up Agent Manager for other functions.

1.3

Chemical Agent Hygiene Officer

The Chemical Agent Hygiene Officer (CAHO) is a UDA laboratory specific position and is an
extension of the facility Chemical Hygiene Officer (CHO). It may or may not be the actual
facility CHO. The CAHO position is held by an individual who has the knowledge and
competence to develop and implement this plan, as qualified by appropriate levels of
education, training, and experience. The CAHO also must demonstrate the ability to use
appropriate equipment and testing procedures to anticipate, identify, and evaluate health,
safety, and environmental hazards, as well as the ability to suggest means for reducing those
risks. The following tasks are the responsibility of the Chemical Agent Hygiene Officer:

Development, implementation, review, and technical support of the DSHP in

conjunction with the Laboratory Manager.

Provide technical, environmental, health and safety guidance to the LM in

development and implementation of programs and procedures related to the UDA
laboratories.

Advise and assist in the improvement of Ultra-Dilute Agent laboratory safety

procedures, and review and update the DSHP on an annual basis as necessary.

Responsible for the DSHP with full authority to prepare and enforce safety policies.

Investigate reports or situations of non-conformance with DSHP requirements.

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Prepare and/or approve UDA training materials for required visitor, Chemical Agent
Operator (CAO), responder and remediation training levels.

Provide and/or approve training level certifications for visitors, staff, managers, and
others as appropriate for the assigned duties and level of potential exposure.

Audit UDA laboratory functions for compliance with the DSHP, Occupational Safety
and Health (OSHA) regulations, Resource Conservation and Recovery Act (RCRA)
regulations and other requirements for laboratory procedures.

Determine the level and type of personnel protective equipment (PPE) required for
the various UDA procedures, conditions, audits, dry runs, and emergency response
for decontamination procedures.

1.4

Agent Manager

The Agent Manager (AM) is responsible for assuring the accurate accountability of the UDA
agent reference materials, from receipt and storage of the primary materials from ECBC
through usage and disposal. The following tasks are the responsibility of the Agent
Manager:

1.5

Serve as the primary contact with the UDA regulatory authorities and is the team
leader for compliance surveys, audits and inspections by EPA, ECBC or other bodies.

Assure accurate accountability of UDA agent reference materials (primary material as

received from ECBC) from receipt through disposal, and is responsible for
maintaining the security and integrity of stored and in-use primary UDA solutions at
all times.

Sign courier forms for receipt of CWA material, complete the ECBC chain of custody
form, and accompany the UDA solutions until they are secure in the laboratory.

Perform checks for each working day of accountability records and housekeeping in
the UDA laboratories. (Note: A working day is defined as any day where UDA
materials are removed from secured storage.)

Prepare monthly agent inventory reports and perform and document quarterly
accountability audits.

Serve as backup for coordinator of UDA primary solution delivery in case the
Laboratory Manager is not available.

Hold the keys (primary lock and key entry requirement) to the UDA standard storage
refrigerator.
Chemical Agent Operators

A Chemical Agent Operator (CAO) is anyone that works directly with dilute agent solutions or
unknown samples potentially containing chemical warfare agents. Chemical Agent Operators

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must be certified on the SOP under which they will be using CWA dilute solutions. The
following tasks are the responsibility of the CAO:

1.6

Perform all UDA operations using only the current and approved SOP for which
operator certification has been completed.

Conduct all operations strictly in accordance with the provisions of the DSHP, SOPs,
and all applicable regulations, manuals, and directives. Any improvements or
alternations must be formally approved by laboratory management before changes
to the original SOP operations or procedures can be implemented.

Observe receipt of UDA materials at the loading dock, transport of the material to
the UDA laboratory, and completion of the initial entry in the UDA Accountability log.

Document the preparation, transfer, and disposal of dilute agent standards of the
Chemical Agent in the LIMS Standard Preparation Module.

Ensure all chemical solutions are properly labeled and stored; this also includes good
housekeeping practices within the work area. Responsible for maintaining the
security and integrity of the UDA solutions at all times.

Responsible for tracking the current location of all CWA dilute standards they are
using. This includes documentation of transfer to other laboratories for analysis or
use.

Responsible for maintaining security for stored and in-use CWA Dilute standards at
all times. Hold the numerical combination to the key pad entry system (secondary
lock and key entry requirement) on the UDA standard storage refrigerator.

Receive chemical agent orientation and safety training, and comply with the
accountability procedures in addition to responsibilities under the primary CHP.

Responsible for informing their supervisor of any factors that may compromise the
safe operation of the UDA program.

Report any accidents, incidents, hazardous conditions, or unusual circumstances to

the immediate supervisor, LM, AM, or CAHO/CHO. Any event that could potentially
cause or resulted in exposure or injury within the designated UDA laboratory areas
must be reported.

Use Personnel Protection Equipment required by the SOPs in the prescribed manner.
Inventory Witness

A witness is required when auditing the CWA dilute solution inventories. The witness is
selected by the Agent Manager from the list of personnel with training appropriate to enter
the CWA Dilute Solution Laboratory. The witness must be independent of the dilute agent
operations being audited. The physical inventory witness verifies the status of the chemical
inventories by signing and dating the inventory logbook.

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APPENDIX B
CHEMISTRY ESSENTIAL QUALITY CONTROLS
1.0

INTRODUCTION

This section details the Quality Controls used by the FDEP Bureau of Laboratories for
chemical testing. Adherence to the Quality System detailed in the DEP Quality Manual will
ensure that all the QC checks addressed in this appendix are being followed.
2.0

SCOPE

This section lists the essential quality control procedures performed by the FDEP
Laboratories for all testing where applicable. Additional requirements detailed in the
applicable regulations, test or FDEP SOP are also followed.
3.0

TERMS AND DEFINITIONS

The relevant definitions from The NELAC Institute Standard, Volume 1, Module 2, Section 3.0
are the preferred references. See TNI Standard. Definitions related to this document that
are used differently or do not exist in the above references are defined in the text.
4.0

METHOD SELECTION

The FDEP Laboratory only uses standard methodologies (where available) acceptable to our
clients and in compliance with regulatory requirements. Supporting information may be
found in section 5.4 on environmental methods and method validation.
Test method quality controls, QC outlined in the test SOPs and other requirements are
followed for all tests where applicable. If no QC exists in a method employed by the
laboratory checks are instituted from a similar method where available.
5.0

METHOD VALIDATION

5.1

Validation of Methods
a) Methods are validated by performing LOD and LOQ determinations, evaluating
precision and bias and employing and achieving method criteria for checks such as mass
spectral tuning and retention time windows. See SOP LB-007, Procedure and Policy for
Method and Instrument Validation.
b) New methods, non-standard methods and laboratory designed methods and method
modifications are validated to confirm that the methods are fit for the intended use. The
validation procedures are conducted according to SOP LB-007 and the requirements of
the FDEP QA Rule, Chapter 62-160, FAC.

5.2

Limit of Detection and Quantitation

Procedures are documented for each quality system matrix.

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5.2.1 All sample processing and analysis steps are included in the test determination and are
documented. Test methods utilized by the laboratory will provide a LOD that meets the
objectives of the analytical project.
(a) The LOD is determined for each matrix/technology/analyte by the protocol
stipulated in the test method or appropriate regulation. In the absence of this
information it is performed as detailed in Section 5.4 and 5.9.3 of the general
requirements module.
(b) The LOD verification is conducted according to SOP LB-031.
(c) An LOD study is not be conducted if spiking solutions or QC samples are not
available.
(d) The LOD is determined in a matrix free of interferences, where available.
(e) The LOD is performed each time there is a change in how the method is performed
or when an instrumentation change impacts the sensitivity of the method.
(f) The LOD is verified annually for each matrix, technology and analyte.
5.2.2 Limit of Quantitation
The established Limit of Quantitation (LOQ) shall be the same as or above the LOD. See
sections 5.4 and 5.9.3 for the methodology used for establishing the LOQ or PQL. Since FDEP
regulations require reporting down to the LOD, annual LOQ verifications are not required.
5.3

Evaluation of Precision and Bias

(a) Precision and bias is evaluated according to Section 5.9.2 in the General Requirements
Module. Initial precision targets are established from the demonstration of capability or
method validation and limits may be updated as more data is generated.
(b) Procedures for assessing precision and accuracy for non-standard methods are described
in section 5.9.2 of the general requirements module and the QC from the SOPs associated
with the individual tests. If there are variations on how the QC is assessed due to the unique
nature of the tests they are discussed in the appropriate SOP. Precision and bias are
evaluated against test method, client or contractual targets and laboratory established
targets. Precision and bias are evaluated over varying analyte concentrations defined as
high, mid, or low, depending on what portion of the calibration curve the check
concentration falls. The assessment of precision and bias is done independently for each
quality system matrix and each analyte is assessed through the entire measurement system.
(c) The range of applicability is determined as detailed in section 5.9.3.
(d) Method validation protocols detailed in SOP LB-007, Procedure and Policy for Method
and Instrument Validation, are also used for precision and bias assessments.
5.4

Evaluation of Selectivity

All analytical method and checks identified in the associated test procedure SOPs are used to
evaluate selectivity. These checks include, but are not limited to, mass spectral tuning,

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retention time windows, second column confirmation, interference checks and method
blanks.
6.0

DEMONSTRATION OF CAPABILITY

6.1

General

Demonstrations of Capability (DOC) are documented electronically as detailed in FDEP

Bureau of Laboratories SOP LB-011. All supporting data related to the demonstration of
capability is retained and easily accessible.
6.2

Initial DOC

Initial demonstrations of capability are performed for all analytes and methods prior to use
of the method and if there are any changes in instrument type, personnel, test method or
anytime the test method has not been performed by the laboratory or analyst in a 12 month
period.
6.2.1 Records of the initial demonstration of capability include at a minimum the
requirements of section 1.6, Volume 2, Module 4 of the TNI standard.
6.2.2 Procedures for conducting the Initial Demonstration of Capability
(a) The Initial Demonstration of capability is performed as stipulated in section 1.6.2,
Volume 1, Module 4 of the TNI standard.
(b) The test is repeated for either the failed analyte(s) or all of the parameters of
interest when there is a failure of one or more of the established test acceptance
criteria.
(c) Repeated failures trigger corrective actions to remedy problems with the
measurement system.
(d) An initial demonstration of capability is performed whenever an analyte is added to
an existing accredited test method.
6.3

On-going DOC

6.3.1 On-going demonstrations of capability are conducted annually (at least once every 12
months) by laboratory analysts by successfully analyzing either:
(a) another initial DOC;
(b) a blind sample (single blind) or successful analysis of a blind performance sample;
(c) four consecutive laboratory QC or laboratory control samples (LCS);
(d) greater than 95% success rate for all LCS samples (N > 20) analyzed in a prescribed
period within the previous 12 months; for example, depending on the analysis, the
prescribed period could be a month, a quarter (3 months) or 6 months;
(e) 95% confidence limits for all LCS samples reported by an analyst during a prescribed
period within the previous 12 months that fall within the long-term statistical limits

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established for the method (and within required method performance limits, if
available);
(f) no more than one LCS failure (5 < N 20) in the previous 12 months;
(g) an authentic sample that has been analyzed by another trained analyst.
If an analyst fails to demonstrate on-going capability using the criteria listed above, then the
analyst must complete a successful initial DOC to demonstrate capability. The analyst will be
suspended from reporting data until the successful completion of the initial DOC.
6.3.2 Documentation for only one test method is maintained for similar test methods using
the same technology. EPA test method 1311 (TCLP) and 1312 (SPLP) are considered similar
methods differing only in the leaching solution. For some methods, it is not feasible or
practical to include all analytes in the blind performance samples, LCSs or authentic samples.
If an analyst is demonstrating on-going capability using one of those samples and an analyte
was not added or present in the sample, the analyte must still be reported by the analyst.
Acceptability of results for analytes not added or present in ongoing capability
demonstration samples shall be based on the supervisors judgment (either using nondetection as a criterion or, if the amount is judged to be a co-contaminant, based on
comparability of results produced by other experienced analysts).
7.0

TECHNICAL REQUIREMENTS

7.1.

Initial Calibration

7.1.1 Calibration and standardization procedures, frequencies and documentation protocols

for instrumentation are found in the technical SOPs,
http://www.dep.state.fl.us/labs/library/lab_sops.htm
It is the laboratory's policy that method calibration requirements will be followed if more
stringent than those described in this manual.
Protocol for Determining the Test Method Range of Applicability:
During the development of new test methods and during initial demonstrations of capability
(method validation studies), an evaluation will be made of the dynamic range over which the
method is applicable. That evaluation will take into consideration the type of calibration
protocol (linear, nonlinear), the change in sensitivity over the tested calibration region, the
detection limit of the method and the limit of quantitation. Once a valid range of
applicability is established, calibration standards will be used to bracket the range over
which quantitation will occur. Results reported from data that were generated outside the
determined range of applicability will be flagged as estimates (unless the sample was diluted
prior to analysis in order to bring concentrations within the established test method range of
applicability).
During the establishment of the test method range of applicability, calibration standards will
be prepared and analyzed over the estimated or published range of applicability. If a linear
calibration protocol is to be used, either a) the correlation coefficient of the calibration

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values plotted against their respective response factors must be greater or equal than 0.995,
b) the relative response factors (response factor/calibration value) over the range of
calibration must have a relative standard deviation of less than or equal to 10% or c)
conditions for linearity specified in the applied, published method must be met. If the above
conditions are not met, either the linear dynamic range must be decreased until those
conditions are met or a non-linear calibration protocol must be used. Whenever a non-linear
calibration protocol is utilized, a minimum of 5 calibration points must be defined for a
second order fit; a third order fit requires a minimum of 6 calibration points. When using
non-linear calibration procedures, loss in sensitivity ( response/ concentration) can occur
at high concentrations. To ensure that signals are not quantified in regions of poor
sensitivity, control standards must be analyzed at the highest point of the nonlinear
calibration curve during method validation and must meet the reference method acceptance
criteria for calibration. The lower limit of the test method range of applicability is normally
established at the method detection limit. The initial demonstration of capability includes
establishment of the method detection limit and lower limit of quantitation.
7.2

Continuing calibration

Acceptance criteria for continuing calibration are outlined in the laboratorys technical SOPs,
http://www.dep.state.fl.us/labs/library/lab_sops.htm. These criteria follow the requirements
described in Section 1.7.2 of the 2009 TNI Standard, Vol. 1, Mod. 4.

7.3

Quality Control

Quality control checks are detailed in the test SOPs and QC SOPs associated with the test
type. The QC types addressed are:
7.3.1 Negative Controls
a) Method blanks are analyzed with the same procedure and test conditions as the
test samples and are used to assess possible contamination during the sample
preparation and processing steps. Corrective actions associated with a contaminated
blank will include reprocessing the associated batch samples or qualifying all of the
associated prep batch samples according to the procedures given in SOP LB-027,
Standard Operating Procedure for Reporting Qualified Data.
b) Method blanks are performed at a minimum of one per prep batch and consist of a
quality system matrix that is similar to the associated samples that is known to be free
of the analytes of interest. In instances when no readily available and economical
analyte free matrix can be identified at the levels of detection required to satisfy client
objectives laboratory grade water will be used.
c) Method blanks are not applicable to certain tests.
7.3.2 Positive Controls
7.3.2.1 The LCS is taken through the entire preparation and analysis procedure and
the results are compared against established acceptance criteria. Results outside of
the acceptance criteria are re-analyzed or qualified according to SOP LB-027.

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7.3.2.2 LCSs are performed at a minimum of one per preparation batch. LCSs are not
applicable to analytes for which no spiking solutions are typically available such as
total suspended solids, total dissolved solids, color, and turbidity
7.3.2.3 The LCS is prepared by spiking a known concentration of analyte into a quality
system matrix known to be free of the analyte of interest or it may be a media
containing a verified concentration of the analyte. The analytes to be spiked are those
specified by the test method or in the absence of this information in the method:
a) The analytes selected represents the chemistries and elution patterns of the
reported components.
b) For multi-component tests the number of analytes spiked conforms to the TNI
standard and the laboratory ensures that all targeted compounds are spiked over a
two year period.
7.3.3 Sample Specific Controls
These controls document the effect of the matrix on the method performance and are not a
measure of laboratory performance. The results of these control samples are evaluated and
documented.
7.3.3.1 Matrix Spike; Matrix Spike Duplicates
a) Corrective actions for results outside of routine performance specifications include
qualifying the impacted sample. See SOP LB-027, Standard Operating Procedure for
Reporting Qualified Data.
b) The procedure for determining the spiked analytes is the same as for the LCS given
in section 7.3.2.3 above.
7.3.3.2 Matrix Duplicates
These are sample duplicates that are taken through the entire analytical process
except for in-bottle digestions (e.g. some low-level mercury analyses) where a sample
is split into matrix duplicates after digestion. These checks are only performed when
there is a good chance that the target analyte is present. The RPD of the duplicates is
calculated and compared to established acceptance criteria or method requirements..
7.3.3.3 Surrogate Spikes
Surrogates are added prior to extraction and are used for all appropriate tests. The
surrogates used represent the chemistries of the targeted compounds of the method.
Results are compared to method requirements and historical laboratory performance.
Corrective actions include qualifying the individual samples when surrogate recoveries
are outside of the established range.
7.3.4 Protocols for data reduction are in Section 5.9.3 (a) (v) of the general requirements
module and the individual test and supporting SOPs. All data reduction procedures are
documented.
7.3.5 Reagent Quality, Water Quality and Checks

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(a) Reagent grade chemicals are used for all tests where the test method does not
specify the reagent purity. Reagent purity requirements within the test method are
followed. All purchased reagents and solvents are dated upon receipt.
(b) Water sources are monitored through the use of method blanks. Corrective actions
are immediately taken when blank contamination is attributable to the water source.
(c) Titrant concentrations are verified and documented according to procedures
identified in the test method SOPs.
7.3.6 Selectivity is evaluated by following all required checks within the test method and the
FDEP test SOP.
7.4

Data Acceptance/Rejection Criteria

7.4.1 Negative Controls Each method blank is evaluated to determine the impact on the
associated sample batch. See the test method SOPs and SOP LB-027, Standard Operating
Procedure for Reporting Qualified Data for corrective actions and documentation associated
with method blank contamination.
7.4.2 Positive Controls LCSs
a) The results of the LCS is calculated according to Section 5.9 of the general
requirements module and compared against established acceptance criteria. The
result of the calculation is documented.
b) The protocol for allowable marginal exceedances follows Section 1.7.4.2 of the 2009
TNI Standard, Vol 1, Mod. 4. Further details are provided in SOP LB-027, Standard
Operating Procedure for Reporting Qualified Data.
7.4.3 Sample Specific controls
a) Matrix Spike; Matrix Spike Duplicate
Percent recovery from matrix spikes and relative percent difference from duplicate
matrix spikes are calculated as detailed in Section 5.9 of the general requirements
module. The results of these calculations are documented and compared against
established acceptance criteria.
b) Matrix Duplicates
Precision is evaluated using the calculation for RPD in Section 5.9 of the general
requirements. Results are documented and compared against established acceptance
criteria.
c) Surrogate Spikes
The recoveries of surrogates are calculated according to the formula given in Section
5.9 of the general requirements module. Results are documented and acceptance
criteria are established based on the test method or a documented internal procedure.
Results are evaluated for the effect on individual samples.

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7.5

Sample Handling

a) Samples requiring thermal preservation are monitored to meet the preservation

requirements referenced in Section 5.8.7 and in Table 5.9. Samples that are delivered to the
laboratory on the same day of sample collection and have not had adequate time to achieve
the required temperature are considered acceptable if they are received on ice. This is
documented as part of the sample receipt procedure.
b) See section 5.8.6, for the laboratory sample acceptance policy and FDEP SOP LB-016,
Laboratory Support Section Receiving Room: Standard Operating Procedure for the Receipt
and Log-in of Samples by the DEP Central Laboratory.

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APPENDIX C
REFERENCES
1.

Definition and Procedure for the Determination of the Method Detection LimitRevision 1.11, 40 CFR Part 136, Appendix B.

2.

Nomenclature, symbols, units and their usage in spectrochemical analysis II,

Spectrochim. Acta B, 33B, 242 (1978).

3.

Limit of Detection: A Closer Look at the IUPAC Definition, Analytical Chemistry 55,
712A-718 A (June 1978).

4.

Handbook for Analytical Quality Control in Water and Wastewater. EPA 600/4-79-019.
March 1979.

5.

Methods for Chemical Analysis of Water and Wastes, USEPA Office of Research and
Development, Rev. 3/83. Cincinnati, OH, 3/83; EPA 600/4-79-020.

6.

Test Methods for Evaluating Solid Wastes, Physical/Chemical Methods, SW-846; USEPA
Office of Solid Waste and emergency Response, Washington, D.C.

7.

Method for the Determination of Organic Compounds in Drinking Water, Supplement I,

EPA 600/4-90/020, July 1990.

8.

Standard Methods for the Examination of Water and Wastewater (designated SM),
American Public Health Association, Washington, DC, 1995.

9.

Standard Operating Procedures, Laboratory Services, Florida Department of Health and

Rehabilitative Services (designated HRS SOP).

10. Methods for the Determination of Nonconventional Pesticides in Municipal and

Industrial Wastewater, USEPA Office of Water, Washington, D.C., 8/93.
11. Code of Federal Regulations, Title 40, Part 136; U.S. Government Printing Office,
Washington, D.C., July 1993.