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SEL DATA QUALITY MANUAL

9010-QSP03-R02-041621

STATE ENVIRONMENTAL LABORATORY

www.deq.ok.gov

www.deq.ok.gov/divisions/sels/



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TABLE OF CONTENTS

1. INTRODUCTION 7

2. DATA QUALITY 9

2.1. Quality Assurance Project Plans (QAPPs or work plans) 9

2.2. Data Quality Components 10

2.2.1. Technically Valid 11

2.2.2. Traceable 11

2.2.3. Complete 12

2.2.4. Correct 12

2.2.5. Consistent (Reliable) 13

2.2.6. Relevant 13

2.2.7. Defensible 13

3. PROJECT PLANNING AND SAMPLE HANDLING 15

3.1. Program Support Contacts: 15

3.2. Sample Collection Preparation and Planning 15

3.3. Data Delivery Planning 15

3.4. Sample Scheduling 15

3.5. Sampling Instructions 16

3.6. Project Setup (Pre-logging) 16

3.7. Sampling Requirements 16

3.7.1. Containers 16

3.7.2. Preservation 17

3.7.3. Hold Time 17

3.7.4. Volume 17

3.7.5. Sample Labels 18

3.7.6. Chain of Custody (COC) 18

3.8. Transport, Storage, and Delivery to the SEL 18

3.9. Accessioning and Acceptance of Samples 19

3.10. Cancellation of Samples 19

3.11. Laboratory Sample Custody, Storage, and Transfer 19

3.12. Sample Retention & Disposal 19

3.13. Sample Subcontracting/Outsourcing 19

4. DATA HANDLING 21

4.1. Raw Data 21

4.2. Data Reduction 21

4.3. Units of Measure 21


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4.4. Significant Figures and Rounding 22

4.4.1. Significant Figures 22

4.4.2. Rounding 24

4.4.3. Reporting Rounded Data 25

4.5. Correction of Data for Moisture 25

5. QUALITY ASSURANCE AND QUALITY CONTROL 27

5.1. Quality Assurance 27

5.2. Quality Control 27

5.3. Proficiency Testing 28

6. DATA QUALITY ELEMENTS, STATISTICS, AND CALCULATIONS 31

6.1. Statistics and Calculations 31

6.1.1. Populations and Samples 31

6.1.2. Accuracy 32

6.1.3. Precision 33

6.1.4. Mean 36

6.1.5. Deviation 37

6.1.6. Variance 38

6.1.7. Standard Deviation 39

6.1.8. % Relative Standard Deviation 41

6.1.9. Relative Percent Difference (RPD) 41

6.1.10. Confidence Intervals and Limits 42

6.1.11. Control Charts 43

6.2. Determination of Outliers 43

6.3. Measurements of Error, Bias, And Uncertainty 43

7. DETECTION AND REPORTING LIMITS 47

7.1. Sensitivity Measurements 47

7.1.1. Detection Limit (DL) 47

7.1.2. Limit of Detection (LOD) 47

7.1.3. Method Detection Limit (MDL) 47

7.1.4. Instrument Detection Limit (IDL) 48

7.1.5. Limit of Quantitation (LOQ) 48

7.1.6. Reporting Limit (RL) 48

7.2. Instrument Sensitivity Relationships 49

7.3. Project Reporting Limit Requirements 50

8. LINEARITY AND CALIBRATION 51

8.1. Initial Calibration 51

8.2. Calibration Verification 51

8.3. Calibration Acceptance and Reporting 51

8.4. Calibration Standards Requirements 51


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8.5. Record Requirements 52

8.6. Linearity 52

9. DATA VERIFICATION 53

10. DATA REPORTING 55

10.1. Report Walkthrough 55

10.2. Data Delivery Options 55

10.3. Corrected Reports 55

10.4. Specialized Deliverables 55

APPENDIX A- SAMPLE CUSTODY DOCUMENTATION 57

APPENDIX B- QUALIFIERS AND FLAGS 59

APPENDIX C- METHOD AND ANALYTE INFORMATION 61

APPENDIX D- REFERENCED WIDS, PROCEDURES, AND DOCUMENTS 81

APPENDIX E- GUIDE TO THE SELSD REPORT OF ANALYSIS 83

APPENDIX F- PPT (PROJECT PLANNING TOOL) 91

APPENDIX G- ACRONYMS 97

APPENDIX H- AFTER HOURS SAMPLE DELIVERY WID 99


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1. INTRODUCTION

In support of the SELSD Quality Assurance Plan and the associated analytical SOPs, this Data

Quality Manual (DQM) was created to document the various components, definitions,

calculations, and acceptance criteria associated with the generation of data by the State

Environmental Laboratory (SEL).

This Manual is designed for use in conjunction with the SELSD QAP. The QAP addresses

Division-wide quality policy to be implemented by both the Lab and the Laboratory

Accreditation Program (LAP) and the Data Quality Manual addresses technical and operational

policy to be implemented by the lab.

The SEL provides analytical support for DEQ environmental programs, programs for other State

agencies, Oklahoma tribes, public and private entities as identified in the Program Support

Section 1.4 of the QAP.

The SEL is composed of Radiochemistry, Environmental Microbiology, General Chemistry,

Metals, GC/MS Organics, GC Organics, Statewide Sample and Data Management (SSDM), and

the Laboratory Customer Assistance Field sections.

The SEL is prepared to handle environmental samples that include soils, sediments, biological

tissue, wastes, waste waters, ground waters, surface waters, and drinking waters. All other

sample types require notification prior to delivery. Provisions are made on a case-by-case basis.

This Manual describes the laboratory’s quality assurance activities, data quality objectives, and

general data generation policies. This Manual also provides guidance for meeting certain

analytical requirements outlined in Quality Assurance Project Plans (QAPPs or work plans)

developed and submitted to EPA Region 6 for DEQ projects that are funded by federal grant

dollars. This Manual outlines how the laboratory generates high quality, useful, and defensible

data.

This DQM supports the tests, methods, and matrixes performed by the SEL, as indicated in

Appendix C. Methods in which the SEL maintains certification or accreditation are included in

this table. Scopes of certification and accreditation are available upon request.

This Manual and the protocols described within are not meant to be all-inclusive, but rather serve

as a foundation for continually building a stronger data quality program within the Laboratory.

While the development of a data quality system is essentially a management task, each

individual shares responsibility for maintaining knowledge of the data quality program and for

implementing and following established data generation procedures.

It is mandatory that all SEL staff read, understand, and implement all aspects of this DQM and

participate in training that is provided by QS.


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2. DATA QUALITY

The mission of the State Environmental Laboratory is to generate consistent, reliable,

reproducible, and defensible laboratory data of known and documented quality to support the

decisions that promote the quality of life in Oklahoma and to meet the analytical needs of our

clients, communities and the citizens of Oklahoma. Information extracted from the data

generated within the laboratory is utilized to make decisions that affect the environment and

public health. Laboratory data can be used, for example, for risk assessment, contamination

extent, feasibility studies, or compliance monitoring. High quality data is critical in supporting

sound environmental decisions. When the quality of data is insufficient or inadequate,

subsequent decisions may adversely affect public health, with an additional time and financial

burden to the data user or decision maker.

The function of the SEL Data Quality Manual is to ensure that data generated by the laboratory

is of the highest possible quality and usability. This section serves to address the major

components of data quality and documents how the SEL generates data that is appropriate for

use. The reader is referred to subsequent chapters for additional procedures and information

regarding various data quality and quality system applications.

2.1. Quality Assurance Project Plans (QAPPs or work plans) To ensure data that is of sufficient quality and usability, efforts must be adequately

planned and prepared. A QAPP or work plan is a document that provides the framework

for generating high quality data to be used when making environmental decisions. A

QAPP or work plan establishes the outline for the planning, implementation, and

assessment of a project. It also guides the data acquisition and decision-making

activities. A QAPP or work plan describes the quality assurance procedures, quality

control specifications, and other technical activities that should be implemented to

ensure that the results of the project meet project specifications. Data Quality Objectives

(DQOs), a critical component of the QAPP or work plan, are identified and documented

to assist the generation of high quality data by defining the degree to which uncertainty

in a data set must be controlled to achieve an acceptable level of confidence for

decisions based on the data. DQOs are the qualitative and quantitative statements that

clarify study objectives, define the appropriate type of data, and specify tolerable levels

of potential decision errors that are used as the basis for establishing the quality and

quantity of data needed to support decisions. The DQOs identify the data needs for the

project and defines the criteria that the data collection design should satisfy, such as:

Sample and measurement type (e.g., matrices)

Analyte(s) of interest

Time and location of sample collection

Number and volume of samples to collect

Sample preservation and storage requirements

Type and frequency of project QC samples

Project precision and accuracy acceptance limits

Detection, reporting, or action limits required for decision making

Relevant SOPs to be followed

Sample tracking requirements and turn-around-times


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Documentation requirements

Relevant background data

Intended use of data

Decision making criteria

Requirements for QAPP or work plan development can be found in the EPA

Requirements for Quality Assurance Project Plans (QA/R-5) and additional guidance

can be found in EPA Guidance for Quality Assurance Project Plans (G-5).

The SELSD QAP and SEL DQM are designed for utilization by the DEQ environmental

Project Managers and laboratory customers as a reference tool for the development of

the analytical activities described in QAPPs or work plans for which the SEL analyzes

data. The laboratory has established acceptance criteria for accuracy and precision

based on historical laboratory capabilities or from method defined acceptance criteria.

Information regarding SEL methods, parameters, and reporting limits, are located in

Appendix C.

Project Managers and laboratory customers and contractors requesting analytical

services for environmental projects should review Appendix C to evaluate whether the

analytical services offered are appropriate to meet specific project data quality objectives

(DQOs) outlined in individual project plans or project needs. Clients requesting data for

special project applications or alternate reporting levels not addressed in Appendix C

should contact the appropriate Laboratory Group Manager or the laboratory QA Officer,

identified in Section 3.1, to determine if alternate procedures are available which might

meet the needs of the project.

To assist in the evaluation of client Data Quality Objectives, the SEL has developed a

Project Planning Tool (PPT), which documents and tracks analytical components, such

as sampling start date and duration, number of samples, parameter, matrix, requested

methods, reporting limits, special analytical requests, QC planning and reporting,

deliverables, and turnaround time. This planning tool goes beyond the basic information

collected on the chain of custody (COC) and provides detailed documentation of client

needs.

Contact [email protected] for assistance with documenting or reviewing the

analytical components of a QAPP or work plan or setting up QAPP or work plan-based

analytics.

2.2. Data Quality Components

Many QAPPs or work plans rely significantly on laboratory-generated data to provide

information needed to make decisions that address environmental problems. The data

from the lab must be of sufficient quality, quantity, and type to support and defend the

actions and decisions of the Project Managers and laboratory customers. The following

components are required for analytical laboratory data that is appropriate for use:


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2.2.1. Technically Valid

Technically valid data is data that has been derived from methods that have been

properly validated. Method validation (method standardization) is the process of

demonstrating that an analytical method is suitable for its intended use and

involves a variety of studies to evaluate method performance under defined

conditions. EPA, for example, validates methods prior to approving them as

mandated methods for Compliance Monitoring under the Safe Drinking Water

Program. Method validation ensures that the procedure is capable of identifying a

particular analyte within a given concentration range with an acceptable degree of

sensitivity, accuracy, precision, and reliability. Method validation includes

evaluations covering the full array of activities associated with a method,

including sample collection, preservation, transport, storage, and sample analysis.

SEL samples must be collected and preserved by approved or accepted sampling

methods; analysis must be performed by approved or accepted technical methods,

within the holding times required and incorporating the prescribed QC elements;

sample and QC data must be reviewed, verified, and accepted against the

appropriate acceptance criteria; and data must be reported as program, project, or

regulation requires. Data not meeting these criteria are to be qualified as such.

Laboratory data generated by the SEL is valid in that it is obtained by the

methods and procedures required, approved, or accepted relative to the end

use of the data.

2.2.2. Traceable

Data must be traceable such that the data user can follow the data through the

lifecycle of that data from collection to reporting. This includes the ability to

track access and possession of samples and data as well as changes occurring to

them. Traceability is essentially the “paper-trail” (hard copy or electronic) that

supports the data. Documented traceability ensures the ability to recreate or

reconstruct the actions and information involved in the generation of data,

including the activities relating to sample collection, preparation, support

equipment, raw data, data reduction, and data calculation. Proper traceability is

supported as a transparent process and sustains the claim that the data adheres to

the quality assurance properties of the program or project requirements.

An additional, but independent component of traceability includes the

documentation of consumables that require a stated degree of quality or purity,

such as chemicals, reagents, standards, glassware, containers, media, etc., that

were used during data generation. Traceability documentation includes vendor

supplied Certificates of Quality or Certificates of Purity that verify the lot and

purity of a chemical or consumable and Certificates of Traceability that reference

NIST-traceability of a standard or reference material.

Laboratory data generated by the SEL is traceable through the use of COCs,

bench sheets, analytical spreadsheets, instrument use logs, reagent and


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standards prep logs, digestion logs, instrument and support equipment

calibrations and verifications, and bar-coding. Additionally, the lab

maintains materials traceability where these are applicable to data quality.

2.2.3. Complete

Analytical data must be whole and complete. Information and actions relevant to

the generation of the data should not be excluded or omitted. Modifications and

deviations must be documented and approved. Any potential negative impact to

the quality of the data must be communicated to the data user. Deficiencies must

be identified, documented, and data must be qualified accordingly.

Completeness also refers to the project described “level of completeness” which

addresses the percentage of samples available for decision making from the entire

sample set. Many projects require that a percentage of the total number of

submitted samples be completed (progressing from collection to reporting with no

qualification that indicates a major negative impact to data quality) for effective

decision-making.

Laboratory data generated by the SEL is complete in that relevant actions

taken during the course of data generation are maintained with the original

batch data, including deviations, professional judgement, flags and

qualifications.

2.2.4. Correct

Data must represent the real-world construction of the actual activities performed

during data generation. The data must also accurately represent the environment

from which the samples were taken. For data to be correct, it must be

documented exactly as generated. The use of standard operating procedures,

records, forms, data narratives, corrective actions, and data qualifiers assist to

document actions relevant to data generation. These documents capture normal

actions associated with data generation, as well as occurrences that are out of

control or compliance or that require correction.

Data must be properly documented to support the claim that it is justifiably

correct. Anomalies, errors, and deviations must be identified and documented,

and data must be qualified to indicate when these situations may affect the

decision-making value of the data.

Laboratory data generated by the SEL is correct in that standard procedures

are followed during the course of data generation, that method control

samples are evaluated to ensure that methods are performing accurately, and

that questionable data quality is indicated using data flags, qualifiers, project

narratives, or customer contacts. Analysts must successfully perform

Demonstration of Capability as instructed in 9000-QSP02 to show they are

proficient with the analytical system prior to releasing data.


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2.2.5. Consistent (Reliable)

Data must be both consistent and reliable. Data must be generated through

consistent and appropriate laboratory activities and actions. These processes must

be documented and followed during data generation. Consistent actions are

derived from implementing, maintaining, and training to well-written

standardized procedures and documents. The documents are controlled to ensure

that employees have access to approved procedures that are relevant and current

and that obsolete documents are removed from use. Consistent laboratory actions

provide data that is consistent over time and across various projects and programs.

This consistency can be observed through the use of QC charts.

Laboratory data generated by the SEL is consistent in that standardized

procedures are followed during the course of data generation and that

method precision elements are evaluated to ensure that methods are

performing consistently.

2.2.6. Relevant

For data to be truly of high quality, it must meet the requirements given for its

intended use. The intended use of the data should be thoroughly described in a

QAPP or work plan or communicated by the contract, customer, or program.

Data that is relevant must be generated using required, approved, or accepted

methodologies and standards, and must adhere to the relevant requirements and

regulations for which the data is to be used. It is essential that SEL employees

have an understanding of the various programs supported by the Division to aid in

proper generation of data that is relevant for use.

Laboratory data generated by the SEL is relevant in that data objectives are

evaluated for program and project requirements and qualified where

negative effects to end use may be detected.

2.2.7. Defensible

Data must be generated in a way that maintains legal defensibility. Data must be

suitable for the stated purpose and must be supported by sufficient documentation

to verify suitability and to defend the decisions resulting from the data. Data that

is utilized as legal evidence may undergo intense scrutiny and must therefore be

generated by reliable verified methods that have been documented using clear

concise records.

Defensibility requires credible laboratory witnesses with the knowledge to present

and defend the accuracy, precision, and methods used for sampling, preservation,

receipt, handling, and analysis. A single questionable step may cast doubt on the

integrity of the data and render it useless. Data must be generated with the ability

to withstand any reasonable challenge regarding the quality, integrity, or

authenticity of the approach taken during the generation of the data or the

decisions based on the data. Data must be consistent, in agreement with the


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anticipated outcome for the procedures utilized, and free from contradictions in

the analytical documentation.

Laboratory data generated by the SEL is defensible in that:

The laboratory ensures physical integrity through the use of custody (bar

code) tracking and enhanced storage requirements

Correct, approved, and controlled documentation is utilized

The SELSD Ethics and Data Integrity Program and associated training

are implemented to ensure that employees know proper from improper

practices relative to data generation

All records related to sample analysis are maintained and stored per

program requirements as required to facilitate the recreation of data

generation.


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3. PROJECT PLANNING AND SAMPLE HANDLING

This section of the DQM addresses planning, sampling, and delivery procedures.

3.1. Program Support Contacts

When planning analytical activities, contact the Laboratory Customer Assistance

Manager, Jayme Jones at 405 702-1029 or [email protected]. He will assist in

organizing the laboratory aspect of the sampling event, such as supplying sampling

materials, confirming laboratory capacity, ensuring method availability and reporting

limits, discussing sample scheduling and delivery options, addressing QA and QC needs,

and verifying data reporting and delivery requirements.

3.2. Sample Collection Preparation and Planning

Appropriate and accurate sample collection activities and documentation are essential

for traceability and construction of data of known and defensible quality. The laboratory

may cancel or reject improperly collected or documented samples. To achieve the best

quality of data, Project Managers and laboratory customers should plan sample

collection activities with the laboratory to ensure physical integrity is established

initially upon collection and maintained throughput transportation and receipt by the

laboratory. Most of these activities are centralized around the Statewide Sample and

Data Management section (SSDM).

3.3. Data Delivery Planning

The project specific requirements for data deliverables, data package levels, specialized

QC reporting, and the data distribution timetable should be outlined in the QAPP or

work plan or discussed with the laboratory if a QAPP or work plan is not relevant to the

project.

The laboratory should be included in the planning stages of a project to provide input for

data deliverables and deliverable templates, as well as to provide adequate timelines for

developing EDDs or generating additional QC deliverables. Delivery requests, other

than routine final reports, should be communicated in writing, using the SEL Project

Planning Tool (PPT).

3.4. Sample Scheduling

Scheduling analytical work should be coordinated through the Laboratory Customer

Assistance Manager, Jayme Jones.

Method requirements (such as sample hold time) may necessitate the delivery of certain

sample types on a given day of the week for optimal analysis or to ensure readout times

can be properly planned. Advanced planning and scheduling of ongoing or large

projects allows lab staff adequate time to prepare to meet specific needs of the project or

to address issues related to lab capacity or instrument scheduling for timely analysis

during high volume periods.


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3.5. Sampling Instructions

This DQM is not designed to address in-depth field and sampling activities. Individual

environmental programs and projects should reference a QAPP or work plan outlining or

referencing their field and sample collection activities. A properly documented QAPP

or work plan identifies sample collectors, collection procedures, and sampling locations.

For PWS samples and some general analytical methods, sampling instructions are

provided with the sampling kits and collection and submittal tutorials are provided at

https://www.deq.ok.gov/state-environmental-laboratory-services/sample-collection-

assistance/. Sample collectors should use current sample collection and submittal

instructions. For some analyses, SEL staff must collect the samples. In other instances,

SEL staff can provide field sampling and technical assistance upon request.

3.6. Project Setup (Pre-logging)

The SEL prefers that projects be logged prior to collection (pre-logged) so that sampling

kits can be prepared with certain site-specific sample information pre-populated on the

field COC. Pre-logging samples into the LIMS generates a COC with matching sample

container labels specific to the sampling event. The LIMS generated label includes a

unique alpha-numeric identifier and bar code, other relevant identifiers such as sample

description or PWS sampling point, the container and preservative type, and the

requested analyses for the sample.

Pre-logging samples simplifies the paperwork for the customer, improves traceability,

and provides a more efficient way of generating appropriate forms. It also streamlines

physical sample receipt as pre-logged samples can be received more quickly than

samples received on an ad-hoc basis. This up-front process reduces the amount of time

the sample courier must remain at the SEL in the sample receiving area during

accessioning, but it also permits the analyst faster access to samples to begin analysis.

3.7. Sampling Requirements

Compliance samples are cancelled if received in an improper container, with inadequate

volume, incorrect preservation, or beyond the allowable hold time. These requirements

can be found in Appendix C.

Non-compliance samples received as outlined above may be analyzed and

flagged/qualified if there is a negative impact to the data quality. See Appendix B.

3.7.1. Containers

Improper containers may negatively affect sample results by introducing

contaminants, leaching or adsorbing chemicals, or introducing a non-sterile

environment. In some cases, an unapproved container may degrade or even form

potential analytes of interest. These events may result in significant negative

impact to data quality or render results useless.

The SEL furnishes sample collection containers for laboratory analysis. Samplers

should use the designated containers as they meet the QA requirements specific


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for the method used, parameter requested, and any regulatory requirement. These

containers may contain or be supplied with preservatives as required by the

reference method. These requirements are essential for proper analysis and

materials traceability.

3.7.2. Preservation

Some sample types require preservation to prevent or reduce chemical or

biological changes, reduce volatility, or reduce absorption affects. Improper

preservation may result in significant negative impact to data quality or render

results useless.

Approved methodologies require some sample types to undergo chemical or

thermal preservation. Sample collectors should always preserve samples

immediately following collection unless otherwise noted in the Appendix C or

per special instruction from the Laboratory.

If thermal preservation is required, immediately after collection the sample should

be packed with sufficient ice to reach and maintain the appropriate preservation

temperature. It is recommended such samples be hand delivered, mailed

overnight, or shipped via expedited service to the SSDM to ensure the sample is

received at the proper temperature.

The use of “blue ice” is highly discouraged because it generally does not maintain

the sample at the acceptable temperature.

Samples in the “cooling-down” phase are processed only if received promptly

after collection and packed with adequate ice. These samples will be assessed

individually, based on the collection time, collection location, current

temperature, and presence of ice.

3.7.3. Hold Time

Samples should be delivered to the laboratory as soon as possible after collection.

Timely delivery is extremely important as many samples are only stable for a

brief period of time following collection. Samples that exceed these holding

times may have questionable data quality and the data could potentially be unfit

for use.

3.7.4. Volume

When Customer Assistance personnel receive a request for containers, the

customer is instructed on the proper volume of sample required to obtain valid

analytical results. This is the minimum volume needed for adequate analysis and

laboratory quality control activities. If an insufficient volume is collected, the

analysis of all requested parameters and quality control samples may be

impossible. Volumes listed in Appendix C should ONLY be used as guidance

and should be confirmed with Customer Assistance personnel prior to project

onset to avoid additional collection activities.


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3.7.5. Sample Labeling

When SEL provided labels are not used, sample containers must somehow be

identified with a unique identifier in permanent ink and contain suitable

information to prevent the possibility of confusing, mixing up, or misrepresenting

the sample.

Traceability is critical for the generation of defensible data, as this step documents

that the sample analyzed was the actual sample taken. Inaccuracies in this step

could render a sample useless for litigation.

3.7.6. Chain of Custody (COC)

The COC is essential for data quality in that it supports traceability and

defensively documents sample collection, transport conditions, and transfer

activities as well as the type of container and preservative, and date and time of

collection to indicate adherence to allowed test holding times. The COC should

also contain the sampling location, sample type and the requested analysis. Each

individual having physical custody of the samples before and during receipt must

sign the COC and record the date and time of all custody transfers. Any special

remarks about the sample condition or integrity should also be recorded. Access

the online COC at https://www.deq.ok.gov/state-environmental-laboratory-

services/sample-collection-assistance/.

Record of custody transfers of samples within the SEL will be documented

electronically (section 3.11).

3.8. Transport, Storage, and Delivery to the SEL

New customers or those needing to make updates must complete a Customer Profile.

Access the online form at https://www.deq.ok.gov/state-environmental-laboratory-

services/sample-collection-assistance/ or contact SSDM.

Normal operating hours of the Statewide Sample and Data Management Section

(SSDM), sample receiving area) are from 8:00 a.m. to 4:30 p.m., Monday through

Friday. Samples may be delivered to the SEL by hand-delivery during business hours or

can be mailed or couriered to the following address:

Oklahoma State Environmental Laboratory

P.O. Box 1677

Oklahoma City, OK 73101-1677

For additional questions or special arrangements regarding sample delivery contact the

SSDM at 405-702-1000 or 1-866-412-3057 and request to speak to a SSDM

representative. To review the laboratory’s policy on after-hours sample delivery, refer to

Appendix H.


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3.9. Accessioning and Acceptance of Samples

Samples are received and maintained under access-controlled conditions until all

appropriate receipt activities are complete. Upon receipt and according to procedure

SSDM personnel:

Organize and verify the received samples against those indicated on the custody

record. Ensure sample IDs and any affixed labels match the COC.

Inspect samples and container to verify receipt conditions and integrity: Custody,

Container, Condition, Temperature/Preservation, and Volume.

Gather signatures to document physical custody transfer.

Samples not already pre-logged are logged into the LIMS and assigned a unique

sample identification label and barcode.

3.10. Cancellation of Samples

Inability of SEL staff to secure missing or incomplete required sample information in a

suitable timeframe may also result in cancellation. Customers are notified of cancelled

tests or samples, typically by telephone, and assistance is provided if

additional/replacement samples are needed.

Sample or test cancellation, flagging, and qualification are documented on the final

analytical report. See Appendix B.

3.11. Laboratory Sample Custody, Storage, and Transfer

SSDM staff place accessioned samples in the appropriate storage location with

appropriate thermal preservation, storage conditions (light or heat sensitivity), and

isolated from standards, and samples known to be highly contaminated. Access to the

sample management area is restricted to authorized personnel through key card access.

Additional areas of the SEL also have restricted access.

3.12. Sample Retention & Disposal

Sections maintain physical custody of samples until analytical activities have been

completed, results verified and reported to the customer, and hold time expired, unless

otherwise noted in procedures. The SEL assumes the responsibility for the disposal of

samples unless the customer has requested that the samples be returned. The SEL

requires notification of situations where samples need to be relinquished back to the

customer. Such transfers must be documented using a COC process. Samples are

disposed of according to procedures and in compliance with regulations.

For some projects, it may be necessary to store samples beyond the analytical hold time.

The SEL must be notified prior to sample submittal if samples need to be retained longer

than the retention policy to ensure that appropriate storage space is available. For

samples that may be used as evidence in a criminal investigation, the laboratory will

follow appropriate procedures to protect the integrity of the sample.

3.13. Sample Subcontracting/Outsourcing

During normal operations due to workload, expertise, or temporary incapacity, SEL

subcontracts analytical work to another laboratory. This work is performed under the


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following conditions: The subcontracted laboratory is competent for the required field of

testing, the customer is notified, SEL assumes responsibility to the customer for the work

performed by the subcontracted lab, SEL maintains a register of all subcontractors for

tests performed and that the work complies with all relative and regulatory standards,

SEL will provide a copy of the subcontractor’s report to the client if requested.


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4. DATA HANDLING

Environmental problems, such as those addressed in a QAPP or work plan, are assessed and

confirmed by analytical data and the resulting decisions are supported by that data. Data are a

gathering of facts and information that are obtained from experiments and surveys that are used

to make calculations, draw conclusions, or make decisions. For the environmental laboratory,

analytical data typically comes from the analysis of environmental samples. Data may be

produced at any point during planning, collection, analysis, and verification of sample-related

activities. The process of obtaining data that are sufficient for making and supporting

environmental decisions requires that data be handled appropriately to ensure there is no loss to

the quality of data. This section covers how the SEL handles analytical data. Additional details

can be found in the individual analytical SOPs.

4.1. Raw Data

Raw data is any data that has been collected but has not been processed for use. In the

environmental laboratory, raw data generally refers to the information collected on

analytical instrumentation during sample analysis, such as the signal plotted on

chromatograms and calibration plots, but also includes lab worksheets, records, original

observations, and similar information. This information may require extraction,

organization, conversion, calculation, or other actions to be presented as understandable,

useful information. This process of taking raw data and creating purposeful information

is called data reduction.

4.2. Data Reduction

Data reduction for the laboratory typically refers to the process of converting raw

instrument data into more usable final analyte concentrations. Data reduction may

incorporate statistical calculations, standard curve development for concentration

determinations, unit conversions, and other means to more efficiently demonstrate the

information.

Staff must follow data reduction requirements documented in the reference method,

analytical method SOPs, and this DQM. Method specific data reduction activities are

documented in the method SOPs or associated WIDs. Some data reduction may also be

achieved using instrumentation software and our LIMS.

4.3. Units of Measure

Analytes are typically reported in the units indicated in the reference method or as

identified by a regulatory program. Individual SOPs indicate the final reporting units for

the analyte or method.

Special projects may require different reporting units than those documented in the SOP

or DQM. In these cases, the project must be planned to ensure that reporting

accommodations can be made.

Upon reduction, data is presented and reported in standard units, typically as seen

below:


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Section Description Units

General Chemistry,

Organics, Metals

Concentration mass per volume mg/L, µg/L

Concentration mass per mass µg/g, mg/kg, µg/kg

Concentration mass per area unit µg/m3

Temperature °C, °F

Environmental

Microbiology

Colony Forming Units per unit volume CFU/1mL, CFU/100mL

Most Probable Number per unit volume MPN/100mL

Organisms as “Present” or “Absent” Present/Absent

Cells per unit volume Cells/mL

Radiochemistry

Activity per volume pCi/L

Activity per mass pCi/g

Total activity DPM

Concentration variations, program regulations, and project or client requests may necessitate

conversion between reported units. Refer to the table below for conversion information.

Concentration Conversions:

Kg g mg μg ng Kg g mg μg ng

% ppth ppm ppb ppt Kg % ppth ppm ppb ppt L

% ppth ppm ppb g % ppth ppm ppb mL

% ppth ppm mg % ppth ppm μL

% ppth µg

% ng L ≈ Kg

mL ≈ g

μL ≈ mg

4.4. Significant Figures and Rounding

To better represent the confidence of the calculated value, it is necessary to know how

many digits to retain, where to truncate, and when and how to round the value.

4.4.1. Significant Figures

The significant figures in a calculated number indicate the amount and location of

rounding required to appropriately indicate the accuracy and confidence of the

measurement. Only place values that are significant should be reported.

Example 1: Values and Digit Accuracy

For the result 3.25 ppm:

3.2 has in inherent degree of confidence and certainty

The 0.05 has a lesser degree of certainty associated

The application of the significant figure rules are relevant to all calculations

performed during the generation of data, unless a specific format is prescribed in

the approved or accepted reference method, program regulations, or customer

request, in which case the required or requested format is utilized.


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Exceptions are applied to vendor-supplied software and in-house

spreadsheets that make the application otherwise impossible.

The basic instructions for determining significance of digits for reporting data is

as follows:

1. Start with the left-most non-zero digit and determine the significant digits

using significant digit rules in the Significant Figures table below.

2. Keep “n” digits

3. For values that contain less than “n” digits, replace remaining spaces with

zeros

4. For values that contain more than “n” digits, round the value using rounding

rules and tips listed in the Rounding table in the following section.

Table: Rules and Tips for the Determination of Significant Figures (sf)

Rule or Tip Example # of

sf

All non-zero numbers ARE significant 14.65 4 sf

All zeros in between non-zero numbers ARE significant 0.40497 5 sf

Leading zeros are NOT significant. They are placeholders to represent the

magnitude or scale of a number.

0.004

1 sf

If there are no non-zero digits to the LEFT of the decimal, all zeros in between

the decimal and the preceding non-zero values RIGHT of the decimal are NOT

significant

0.00045 2 sf

Ending zeros after a decimal ARE significant IF they are accuracy markers. 15.500 5 sf

Zeros on the LEFT side of a decimal with a preceding non-zero number ARE

significant 405.5 4 sf

Zeros on the LEFT side of a decimal with a NO preceding non-zero number are

NOT significant 0.523 3 sf

All non-preceding zeros LEFT of a written decimal in a number greater than 10

ARE significant 5002.23 6 sf

If you can write the number in scientific notation and eliminate the zeros, they are NOT significant

Final zeros in a calculated value may or may not be significant, depending on reporting criteria

When multiplying or dividing, the calculated result should have as many

significant figures as the number with the smallest number of significant figures.

The QUANTITY of significant figures in each factor is important; the

POSITION is not.

In this example, 12 has the smallest number of significant figures (2); the result

would therefore also have only 2 significant figures.

12

X 14.6

X 735.3

128824.56

1.2

X105


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When adding or subtracting, the calculated result should have as many decimal

places as the number with the smallest number of significant figures. The

POSITION of significant figures in each factor is important; the QUANTITY is

not.

In this example, 12 is significant to the ones place, while the remaining numbers

are significant to the tenths place. The final result is significant to the ones

position.

12

+ 14.6

+ 735.3

761.9

762

You cannot round to “n” significant digits, a digit is either significant, or it is not. Rounding is all-

together a different process and is used to reduce any digits in the value that are not significant.

Once you determine which digits are significant, you can employ a rounding rule.

4.4.2. Rounding

Once the significant figures are determined for a type of analysis, rounding rules

should be applied to eliminate any unneeded digits. Employees should employ the

mathematical rules for rounding to any calculated values.

Rounding is performed to obtain a value that is easier to work with than the

original number or to eliminate unneeded digits. Once the number of significant

digits (or decimal place reporting requirements) has been determined, rounding

may be needed.

Rounding numbers leads to unavoidable rounding error. During a sequence of

calculations, the rounding error may potentially accumulate making the results

meaningless.

Employ the rounding rules and tips listed in the Rounding Rules Table below to

obtain data that is of the appropriate number of significant figures.

Table: Rounding Rules

Rules, Tips and Examples Value Result

If the digit to be dropped is LESS than 5, drop the digit and leave the

preceding digit as is

15.222 15.22

If the digit to be dropped is GREATER than 5, drop the digit and

INCREASE the preceding digit by 1

15.226 15.23

While performing addition or subtraction operations, round to smallest

number of places (i.e., the least precise number).

11.1 is the least precise number, to the tenths place, so the resulting value is

only precise to the tenths place.

11.1

+ 11.12

+ 11.13

33.35

33.4

When rounding during multiplication or division, carry all digits through

then round the product/quotient to the same number of significant figures

as the multiplier/divisor/dividend with the fewest significant figures

In the example, 9.7 has only two significant figures, therefore the product is

rounded to two significant figures.

0.0174

x 9.7

/ 7.75

0.021778…

0.022

If a number has “n” significant figures, its root can be relied on for “n” digits, but its power can rarely be

relied on for “n” digits


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For data values below the reporting limit, results are not rounded, and the sample

data is reported as less than the given method reporting limit.

For methods that report sample results as a “total” of the individual analytes, the

individual analyte results are first rounded according to the rounding rules, then

the individual results are totaled and reported.

4.4.3. Reporting Rounded Data

Sample results for compliance samples is reported as stated in the regulatory

requirements or with the same number of significant figures as documented in the

reference method or as designated by the MCL value.

In general, reporting rules are as follows:

Sample data is not reported with more than three significant figures

Sample data is not reported with more decimal places than the LOQ

Sample data is not rounded and reported if less than the LOQ

QC data is reported to one decimal place

4.5. Correction of Data for Moisture

A measurement of percent solids is determined on soil, sediment, and non-aqueous solid

waste samples unless otherwise specified by the requestor. The % solids value is used

during data reduction for calculating final analytical concentrations on a dry weight

basis. These values are reported with the sample data when appropriate.

Corrections for moisture require the application of the dry weight factor and raise the

method reporting limit accordingly.

% Solids = 100weightwetsample

weightdrysample


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5. QUALITY ASSURANCE AND QUALITY CONTROL

The Quality System (QS) consists of two primary components: Quality Assurance and Quality

Control.

5.1. Quality Assurance

Quality assurance (QA) includes the activities the laboratory implements to provide

confidence to customers that data has the appropriate quality and meets any intended or

expected requirements. QA relates to how data is generated. QA activities, which

undergo ongoing assessment and improvement, are maintained, tracked, and reported

through a variety of processes.QA activities implemented by the laboratory include:

Updates and Improvements: The laboratory implements new quality assurance

components in the ongoing process of improving the quality system. Many of these

updates require approval, verification, or tracking as a component of the QS.

Laboratory Supplies and Services: The SEL maintains the supplies and services that

are required to generate high quality defensible data for the methods for which the

SEL is certified, accredited, and/or contractually obligated. The supplies and services

meet or exceed relevant requirements and laboratory reagents and standards must be

of the required or approved quality and traceability. Certificates of Traceability or

quality are retained and available for review to authorized personnel upon request.

Laboratory Instrumentation and Equipment: The SEL maintains an inventory of the

instruments and equipment needed for high quality data generation. Lists of major

instruments and support equipment are located in the Lab Capacity Log 9010-QSL01.

Analyst Training: The SEL provides analysts with the training needed to complete

their analytical work. Prior to reporting generated data, the SEL demonstrates the

ability of the analyst, instrumentation, support equipment, and supplies to perform the

relevant method within specified limits and performance criteria.

Laboratory Software, Programs, and Databases: Laboratory software is purchased to

aid in the generation, analysis, verification, and reporting of laboratory data.

Laboratory software requires verification to ensure that it is working properly and that

errors do not occur during the generation of data. Electronic data has proper software

support and archival procedures so that data may be accessed for assessments and

electronic data review.

5.2. Quality Control

Quality control (QC) includes the activities the laboratory implements to assess how

well the data meets the requirements applied to the generation of that data. Method QC

samples are implemented to verify that the analytical system is in control. These samples

are used to calculate accuracy and precision associated with the laboratory measurement

system and are used to aid in the detection of contamination and other method or

instrument issues. The environmental programs and associated analytical reference

methods typically specify the minimum QC requirements, frequency and limits for

method analysis. Where these are not specified, the section manager specifies them.

Method QC sample requirements are documented in the method SOPs and may include

various types of blanks, calibration verifications, accuracy samples (e.g. LFB, LCS, and

QCS), instrument performance checks, (i.e. tuning), and surrogate recovery samples.


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All QC required by a reference method must, at minimum, be performed. Some

analytical methods are performed so infrequently that accuracy and precision relate only

to the work performed in conjunction with that particular sample set or batch.

Numerous types of laboratory and project QC exist to allow different aspects of the data

to be assessed. In general, method QC is conducted to:

Determine method or instrument sensitivity

Method detection limit study (MDL)

Instrument detection limit study (IDL)

Analysis of reporting limit verification sample

Determine analyst capability

Demonstration of capability (IDC, DOC)

Proficiency test samples (PT)

Verify instrument performance

Analysis of calibration verification sample (ICV, ICC, CCC, CCV)

Analysis of interference check sample (IEC, IPC)

Analysis of internal standard (IS)

Verify of Minimum Reporting Limit

Preparation and analysis of a reagent blank sample spiked with a known

amount of target analyte (LOQ, LLOQ, MRL, PQL)

Determine contamination

Analysis of various types of blanks (RB, MB, LRB)

Determine accuracy/recovery (method performance)

Analysis of a known reference standard (SRM, LCS)

Preparation and analysis of a reagent blank sample spiked with a known

amount of target analyte (LCS, LFB)

Determine precision (sampling and/or analysis)

Analysis of method accuracy QC samples in duplicate (DUP)

Analysis of field samples in duplicate (DUP)

Analysis of spiked or diluted samples in duplicate (MS/MSD, LFM/LFMD)

Determine sample and matrix-related issues

Analysis of spiked field samples (MS, LFS)

5.3. Proficiency Testing

As an external assessment of laboratory performance, the SEL participates in double

blind proficiency testing (PT or PE) studies specific to environmental programs the SEL

supports. This participation demonstrates the laboratory’s ability to produce acceptable

analytical results. Double blind studies involve sample analyses of “unknown” samples

developed and distributed by private or public sector providers. Each study is conducted

a least once annually for overall improvement and monitoring of laboratory performance

as well as to maintain EPA certification or TNI or NRSB accreditations.


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Current SEL studies:

PROFICIENCY PROGRAM PARTICIPATION

Laboratory Section

WS

/WS

M 1

, 2,

4

CR

YP

TO

3

WP

/WP

M 1

, 2

HW

/SO

IL 2

, 4

US

T 2

US

GS

-SR

S 5

RA

DO

N

7

MR

AD

-AIR

4

MR

AD

-SO

IL 4

LE

GIO

NE

LL

A 2

DW

CY

AN

OT

OX

INS

6

RE

C.

WA

TE

R

CY

AN

OT

OX

INS

6

General Chemistry X X X X

Metals X X X X

Environmental

Microbiology X X X X X X

Radiochemistry X X X X

Gas Chromatography X X X X

Gas Chromatography/

Mass Spectrometry X X X

Statewide Sample and

Data Management X X X X

1- Phenova

2- NSI Solutions

3- WSLH

4- ERA

5- USGS

6- Eurofins Abraxis

7- Bowser-Morner

The providers, except for the USGS SRS, Cyanotoxin, Legionella, and Radon in Air

programs, are regulated by TNI endorsed oversight bodies (PTOBs), or Proficiency Test

Provider Accrediting Bodies (PTAB). The oversight groups ensure that providers

manufacture their proficiency testing materials and conduct their studies in adherence

with the 1998 USEPA “National Standards for Water Proficiency Testing Studies,

Criteria Document” or the Proficiency Testing Program portion of the TNI Standard,

Volume 1, Module 1.


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6. DATA QUALITY ELEMENTS, STATISTICS, AND CALCULATIONS

Quality Control (QC) elements are implemented to determine if a method is in control. These QC

elements are designed to detect, reduce, correct, and prevent deviations and deficiencies during

the generation of analytical data.

A primary component of the QC process is to ensure that sufficient and appropriate quality

control elements are implemented, conducted, and assessed to verify data as accurate and

appropriate for the intended use prior to release. Method and instrument QC samples are

analyzed in conjunction with routine “field” samples to assess the accuracy and precision

associated with the analytical batch or run. The accuracy and precision measurements are

compared to acceptance criteria to determine the associated quality and to demonstrate that the

analytical activities are in control.

This chapter discusses some of the QC and statistical terms and calculations commonly

encountered during the generation of environmental data. The individual method SOPs address

the specific procedures required to implement and assess the following QC aspects:

Confirmation and verification frequencies

Sterility controls

Replicate/duplicate analyses

QC sample source and requirements

Positive and negative controls

QC acceptance ranges

Corrective actions

Contingency actions

Matrix spiking

6.1. Statistics and Calculations

6.1.1. Populations and Samples

In the context of probability measurements, statistical analysis is performed on a

set of measurements to determine or define some parameter of the data related to

those measurements. The measurements may be taken on an entire population

(the sampling environment), or on a representative subset (a “sample” of the

original population) of the sampling environment. In the world of environmental

projects, it is typically impossible to analyze the entire sampling environment in

question (we cannot test ALL of the potentially hazardous material at an

abandoned refinery nor can we confirm compliance to DW standards on ALL

water before we drink it). In the laboratory setting, a representative subset (an

environmental sample) of the entire population is tested instead.

When an environmental problem needs to be addressed, decision makers

determine the best sampling design to characterize the sampling environment.

They consider what samples to take, how many to take, where to take them, etc.

to obtain the most representative collection of data from which to make decisions.

This is essential in acquiring data that supports the decision-making process.


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The Refinery Figure below represents an old refinery site. Analytical data is used

to determine if the site poses a risk to public health. The area inside of the bold

red line is the area that defines the project site borders. This entire area represents

the statistical population. It is neither feasible nor logical to analyze the entire

population (the environmental site, i.e. everything within the red border);

therefore, only a “sample” of the full population is measured. Project Managers

and laboratory customers determine the best and most representative locations to

obtain measurements. These measurements are a “sample” of the entire

population (not to be confused with an actual sample of environmental media to

be taken to the lab for testing-although in this case, an environmental sample is

taken to provide information that represents the statistical sample of the

population).

Refinery Figure:

Ideally, the sample of a population is exactly representative of the original

population; however, due to various types of errors, this is unlikely. When

analysis occurs on a single sample of a larger population, uncertainty is

introduced. This uncertainty should be accounted for by using precision-related

measurements.

6.1.2. Accuracy

Accuracy is one of the primary indicators of laboratory data quality. Accuracy is

an expression of the systematic error (bias) inherent in a measurement system.

Accuracy describes the “correctness” of a measurement by evaluating the degree

of agreement between the measurement and that of an accepted (known or

expected) value. Accuracy is typically measured through the analysis of reference

standards that have been certified to a specific, or known, concentration or value.

When the measured value is close to the known value, the accuracy is considered

“high”. When the accuracy is far from the known value, it is considered “low”.

Accuracy is well represented using the “bulls-eye” graphic. The first image

demonstrates seven arrows that have fallen in the center of the target (the

Oklahoma Refinery Site


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expected value). This archer was very accurate in hitting the bullseye. In the

second image, the archer has failed to hit the bullseye. This archer had a lower

degree of accuracy than the first archer did.

Accuracy Figure:

High Accuracy Low Accuracy

The SEL assesses accuracy, in general, by calculating “percent recovery” from

various types of quality control samples. A known concentration of whole volume

or spiked analyte is processed, and the results are compared to the known value.

These recoveries must fall within historically determined or method defined

limits.

Data are either reanalyzed or qualified when accuracy values fall outside of the

lab or method defined limits.

The accuracy of a sample or standard can be measured using the following

Percent Recovery equations:

% Recovery =

%100

ionconcentratspiked

sampleoriginalresultsamplespiked

The calculation above is used when the measurement value contains a

contribution from the sample, such as in the case of matrix spikes, matrix spike

duplicates, and surrogate recoveries.

When there is no sample contribution, such as in the case of LCS and calibration

verifications, the equation below is used:

% Recovery = %100valueknown

valuemeasured

Accuracy acceptance criteria and corrective actions for accuracy failures are

addressed in the individual method SOPs.

6.1.3. Precision

Precision is a measure of the reproducibility and repeatability of data. Precision is

the degree to which a set of measurements of the same parameter obtained under

similar conditions conform to themselves, i.e., the agreement between two or


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more results. It measures the variability, or random error, during sampling,

sample handling, preparation, or analysis and is an expression of the measurement

of uncertainty in the calculated mean value of a series of replicate measurements.

Precision is independent and unrelated to accuracy. High precision values result

in reduced uncertainty with the data (and vice versa). The SEL assesses analytical

precision through the measurement of sample duplicates, QC sample replicates,

and matrix-spike duplicates. These measurements may be dependent or

independent of matrix effects. Data is qualified when precision values fall outside

of the lab or method defined limits.

Precision measurements can be calculated from either laboratory samples or

project samples. Sample types that can yield precision measurements include:

1. Laboratory specific precision samples (assessed by laboratory staff):

a. Sample duplicates – Two independent and separate analyses of

the same sample. These samples measure precision of the

analytical method.

b. Laboratory matrix/matrix spike duplicates – A sample that is

fortified with a known concentration of the analyte of interest.

These samples measure the degree of precision relative to the

analytical method and the matrix of the samples.

c. Lab instrument/QC replicate - A blank sample that is fortified

with a known concentration of the analyte of interest or a repeated

measurement of a sample that has been prepared for counting.

These samples measure instrument drift and verify calibration.

2. Project specific precision samples (assessed by Project Managers and

laboratory customers):

a. Field duplicate samples (split sample) - A single sample taken in

the field, thoroughly homogenized, divided into two separate

containers, and analyzed as two independent samples. Field

duplicates measure the precision of the overall measurement

process, to include collection and analysis, and therefore typically

maintain a lesser degree of precision when compared to laboratory

analytical duplicates. Split samples may also be sent to two

different laboratories to assess the reproducibility of the overall

measurement process. Thorough sample homogenization is

CRITICAL to obtaining precision measurements that accurately

represent the remaining sampling and analytical activities, as

improper homogenizing greatly affects the precision between the

measurements.

b. Field replicate samples (co-located/collocated) – Samples that

are collected from the same site, at or near the same location, at

approximately the same time. These samples measure sampling

precision, matrix variations, and variations in environmental

concentration. \


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Precision is also well demonstrated using a bulls-eye example. The first image

demonstrates seven arrows that have all fallen close together, i.e., they hit

“precisely” the same area on the target. This archer was very precise. In the

second image, the seven arrows are scattered around the target, and none are

concentrated to a specific area. This archer was less precise.

Precision Figure:

High Precision Low Precision

The figure below demonstrates both accuracy and precision in relation to each

other. The first image illustrates arrows that are concentrated around the bullseye

(high accuracy) and close together (high precision). The second image shows

arrows that are on the bullseye (high accuracy) but not close together (low

precision). The third image demonstrates arrows that are far from the bullseye

(low accuracy) but close together (high precision). The last image shows arrows

that are far from the bullseye (low accuracy) and having fallen far from each other

(low precision).

A/P Figure:

High Accuracy/High Precision High Accuracy/Low Precision

Low Accuracy/High Precision Low Accuracy/Low Precision


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Analyzing known standards for short or long-term application allows the

laboratory to compare current performance to past performance and to compare

internal performance to that of other laboratories.

Precision as repeatability is the expression of random error associated with

measurements obtained under the same operating conditions over a short span of

time and ideally using the same analyst, reagents, standards, instruments, and

equipment; such as that determined with project QC and analytical batch QC.

Precision as reproducibility is the expression of random error associated with

measurements obtained over longer periods, and includes different analysts,

instruments, equipment, and standards. Reproducibility may also include

measurements between different laboratories, such as PT studies and

standardization of methods.

Precision acceptance criteria and corrective actions for precision failures are

addressed in the individual method SOPs.

There are several different statistical calculations related to precision.

Calculations associated with precision are covered, along with examples, on the

following pages.

6.1.4. Mean

The mean, X , of a group of measurements is the average value of those

measurements (i.e., the measure of the center of the distribution of the data). The

mean is calculated by summing all the individual results then dividing the sum by

the total number of results included in the sum.

The following equation can be used to determine the mean of a set of data:

𝑋 =∑ 𝑋𝑖

𝑁𝑖=1

𝑁

𝑋 = Sample mean of the measurements

𝑋𝑖 = Value of each individual measurement

N = Number of measurements


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EXAMPLE 1 (mean):

To demonstrate X , suppose you are looking at the long-term analysis of a

series of LCS data. You have the following measurements (in mg/L):

1. 10.5 6. 9.6 2. 10.3 7. 10.4 3. 10.7 8. 10.2 4. 9.9 9. 10.3 5. 10.1 10. 10.1

To determine the mean:

Add all 10 values together:

10.5+10.3+10.7+9.9+10.1+9.6+10.4+10.2+10.3+10.1= 102.1

Divide the sum (102.1) of the individual measurements by the total number

of values (10):

𝑋 ̅ = ∑ 𝑋𝑖

𝑁𝑖=1

𝑁 =

102.1

10 = 𝟏𝟎. 𝟐𝟏

10.21 mg/L is the mean (average) value of the LCS data.

The mean of a series of data is often used to calculate other precision

measurements.

6.1.5. Deviation

The deviation, id, of a measurement is the difference between an individual

measurement and the mean of a group of measurements.

𝑑𝑖 = 𝑋𝑖 − 𝑋

𝑑𝑖 = Deviation of the individual measurements

𝑋𝑖 = Value of each individual measurement



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EXAMPLE 2 (deviation):

To demonstrate di, continue with the LCS mean data from Example 1. The

deviation is simply the difference between each data point and the mean.

The mean from Example 1 was 10.21, so we would calculate the difference

between each individual point (#1-10) and the mean (10.21).

𝑑𝑖 = 𝑥𝑖 – 𝑋 ̅ = 10.5 − 10.21

# PPM Mean di Units 1 10.5 - 10.21 = 0.29 mg/L 2 10.3 - 10.21 = 0.09 mg/L 3 10.7 - 10.21 = 0.49 mg/L 4 9.9 - 10.21 = -0.31 mg/L 5 10.1 - 10.21 = -0.11 mg/L 6 9.6 - 10.21 = -0.61 mg/L 7 10.4 - 10.21 = 0.19 mg/L 8 10.2 - 10.21 = -0.01 mg/L 9 10.3 - 10.21 = 0.09 mg/L 10 10.1 - 10.21 = -0.11 mg/L

So, when determining deviation on a set of 10 data points, we have 10

individual measurements for deviation.

This value, although not typically reported, is also utilized in other statistical

calculations involving precision measurements.

6.1.6. Variance

Variance, s2, is a measured value of the spread of a data set. It is the average of

the squared deviations (di2) from the mean.

Variance = 𝑠2 = ∑ (𝑋𝑖−𝑋)

2𝑛𝑖=1

𝑁−1

(𝑋𝑖 − 𝑋) = 𝑑𝑖 = Deviation of the individual measurements

𝑋𝑖 =Value of each individual measurement

𝑋 =Sample mean of the measurements

N =Number of measurements


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EXAMPLE 3 (variance):

To demonstrate variance, continue with the LCS deviation data from the

previous examples. To determine variance, square the deviations (from

Example 2), sum them together, and then divide by the degrees of freedom

(10-1 = 9).

1

)(1

2

2

N

XX

sVariance

N

i

i

Square the deviations and calculate the sum:

# di X2 S2

1 (0.29) 2 = 0.084 2 (0.09) 2 = 0.008 3 (0.49) 2 = 0.240 4 (-0.31) 2 = 0.096 5 (-0.11) 2 = 0.012 6 (-0.61) 2 = 0.372 7 (0.19) 2 = 0.036 8 (-0.01) 2 = 0.000 9 (0.09) 2 = 0.008 10 (-0.11) 2 = 0.012 0.869 mg2/L2

Divide the sum of the squared deviations by the degrees of freedom:

Variance, s2 = 0.869

9

The variance of the data set is 0.0965

Because variance is a squared value, it is a positive number. Utilizing squared

values makes large deviations stand out; however, large values are sometimes

cumbersome. Taking the square root of the variance makes the value more

usable, as well as placing the number back in the same units as the original data.

6.1.7. Standard Deviation

Standard deviation, s or SD, the square root of the variance, is a calculation

frequently seen as a measure of analytical precision. Standard deviation is a

statistical measurement indicating how precise the average is and how well the

individual measurements compare to each other. Standard deviation demonstrates

the random error present in a measurement system by measuring the amount of

variation from the average of the results.

Standard deviation may be calculated using the following equations:


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s =√∑ (𝑋1−𝑋)2𝑁

𝑡−1

(𝑁−1) = SD = √

(𝑋1−𝑋)2

+ (𝑋2−𝑋)2

+ (𝑋3−𝑋)2

(𝑁−1)

(OR) s = √𝑉𝑎𝑟𝑖𝑎𝑛𝑐𝑒

s = (SD) = Standard deviation 𝑋𝑖 = Value of each individual measurement

N = Number of measurements 𝑋 = Sample mean of the measurements EXAMPLE 4 (standard deviation):

To demonstrate s, continue with the variance data from the previous

examples. We take the square root of the variance calculated in example 3.

s = √variance

s = √0.0965 = 𝟎. 𝟑𝟏𝟎𝟕𝟑 𝒎𝒈/𝑳

We can also calculate s using the variance equation. We need to square the

deviations, then sum the resultant values, then divide by the degrees of

freedom.

Square the deviations:

X deviation variance 1 0.292 = 0.084 2 0.092 = 0.008 3 0.492 = 0.240 4 -0.312 = 0.096 5 -0.112 = 0.012 6 -0.612 = 0.372 7 0.192 = 0.036 8 -0.012 = 0.000 9 0.092 = 0.008 10 -0.112 = 0.012

Sum the squared deviations (variance):

0.084 + 0.008 + 0.240 +0.096 + 0.012 + 0.372 + 0.036 + 0.000 + 0.008 +

0.012 = 0.8690

Divide the sum of the squared deviations by the degrees of freedom:

0.8690

(10 − 1) = 0.0965

Take the square root of 0.0965: √0.0965 = 0.31073

The standard deviation of the data set is 0.31073 mg/L (or the square root of

the variance value)


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6.1.8. % Relative Standard Deviation

To report the standard deviation, RSD (%RSD, Coefficient of Variation, CV,

%CV), in relative terms (without units, as a percentage), the %RSD calculation is

used. %RSD calculations are useful for comparing the degree of uncertainty

between measurements of varying absolute magnitude, typically when there are at

least three measurements for comparison.

The calculation is as follows:

%𝑅𝑆𝐷 = 𝑠

𝑋 × 100

%RSD =% Relative Standard Deviation

S =Standard deviation

𝑋 =Sample mean of the measurements

EXAMPLE 5 (%RSD):

To demonstrate %RSD, continue with the standard deviation data from the

previous examples. We use the standard deviation (0.31073) calculated in

Example 4 and the mean (10.21) calculated in Example 1.

%𝑅𝑆𝐷 = (𝑠

�̅�) × 100% = (

0.31073

10.21) × 100% = 3.04%

The %RSD for the data is 3.04%

6.1.9. Relative Percent Difference (RPD)

Relative percent difference is used to compare the precision between two

measurements, such as sample duplicates that are expected to behave similarly.

𝑅𝑃𝐷 = (𝑋1 − 𝑋2)

𝑋 × 100

RPD

= Relative Percent Difference


𝑋1 = Value of measurement

𝑋2 = Value of comparison measurement


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EXAMPLE 6 (RPD):

To calculate RPD, we continue with the data from the above examples.

Suppose we want to assess the first and last LCS in a run to evaluate

instrumental drift.

#1 measurement: 10.5

#10 measurement: 10.1

𝑅𝑃𝐷 = (10.5 − 10.1)

((10.5 + 10.1)/2)× 100% =

0.4

10.3 × 100% = 3.88%

The RPD between the two data points is = 3.88% (which indicates a low drift)

6.1.10. Confidence Intervals and Limits

The confidence interval is the range around the mean in which a data value is

likely to occur. The standard deviation value can be used to determine confidence

intervals for the evaluation of replicate data.

Confidence limits are the upper and lower numbers designating a range of values

(the confidence interval) in which the true value should reside at a stated

confidence level. Confidence limits are typically set at 95%, but may also include

levels for 90% or 99%, depending on the application or desired confidence.

Confidence limits, determined using a normal distribution under the empirical

rule, contain approximately 68% of the measured replicates at 1s (standard

deviation), about 95% at 2s, and about 99.7 at 3s, as seen in Normal Distribution

figure below.

Normal Distribution Figure:

Normal distribution curve that illustrates standard deviations

Dark blue is one standard deviation from the mean. For the normal distribution, this accounts for 68.27% of

the set; while two standard deviations from the mean (medium and dark blue) account for 95.45%; and three

standard deviations (light, medium, and dark blue) account for 99.73%.

http://upload.wikimedia.org/wikipedia/commons/8/8c/Standard_deviation_diagram.svg


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A laboratory application of confidence levels would be the calculation of control

limits and warning limits on a control chart.

6.1.11. Control Charts

Control charts are useful to monitor data for analytical performance, method

stability, and trends. Charts are typically developed using a minimum of 20

consecutive data points that are plotted along with a central line, often the mean

value for the percent recovery, percent difference, percent relative standard

deviation, or other type of normally distributed data.

The standard deviation, s, of the data points are calculated and used to determine

confidence intervals for the data. Upper and lower warning limits are calculated

at two standard deviation (2s) to define the limit in which approximately 95% of

the data should fall. Upper and lower control limits are calculated at three

standard deviation (3s) to define the limits in which approximately 99% of the

data should fall. These limits define the region in which a data point must lie for

the analytical system to be considered in control.

Data points close to the reference line represent data with less variation in the

inherent error, and points scattered closer to the limits represent data with larger

error variations. Data beyond the control limits indicate data that is out of control

and should be addressed. The figure below illustrates a control chart with upper

and lower warning and control limits.

Control Chart Example:

6.2. Determination of Outliers

A data point should not be discarded as an outlier without proper explanation or valid

justification. This applies to all data points collected (e.g. LCS, MDL/LOD, linear

curves, DOCs, duplicates, etc.). Justifiable reasons for removing outliers would include

a known and documented laboratory error or the use of an appropriate statistical outlier

test.

6.3. Measurements of Error, Bias, And Uncertainty

Most analytical results have some inherent degree of loss and error associated with the

measurements. Uncertainty results from the natural variations associated with analytical

systems relative to fluctuations in measuring devices, equipment, instruments, standards,

8.5

9

9.5

10

10.5

11

11.5

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30

LCS

Mean

UCL

UWL

LWL

LCL


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chemicals, and reagents; limits associated with the technical aspects of a method or

process; characteristics of the sample matrix or individual analytes; and human error in

collection, preserving, transporting, analyzing, or evaluating data.

This uncertainty, though normal, should be accounted for, evaluated, or addressed when

the project, program, or customer requires. The cumulative impact of these errors is

important in that they could potentially bias data, creating a situation where the sample

concentration is no longer representative of the actual environmental concentration.

Estimating the potential impact of errors increases the usability and reliability of the

data. For environmental projects, the tolerance levels, if relevant, for this error should

be defined in the QAPP or work plan, along with the consequences associated with

making decisions based on biased data.

Uncertainty is measured as an accumulation of the random and systemic errors that

could be introduced and is often called “total uncertainty”. Total uncertainty is the sum

of all uncertainty caused by measurement errors, personal interpretations, and natural

variability.

Analytical uncertainty is a component of measurement uncertainty that includes the

laboratory activities that are performed as part of analysis.1 Analytical uncertainty is

influenced by numerous everyday activities encountered in the laboratory. Activities

that may potentially introduce error include:

Sampling and subsampling:

o Collection

o Homogenization

o Preservation

o Transport

o Aliquoting (subsampling)

o Weather conditions

Storage conditions

Properties and condition of samples being tested

Equipment being used for collection, preservation, and analysis

Prep and test method being used

Reference standards and materials

Chemicals, reagents, standards, preservatives, waters

Environmental conditions:

o Temperature

o Humidity

o Power fluctuations

Calibration:

o Instrument drift

o Variations

o Standards quality

1 TNI


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Operator (sample collector or analyst skill and experience level)

Physical characteristics of the matrix and the individual analytes in the

matrix

Data processing

During analytical activities, an estimate of the analytical uncertainty can be determined

from routine Quality Control (QC) samples. Duplicate analyses indicate uncertainty

through precision measurements; calibration checks, spiked samples, and reference

materials indicate uncertainty through accuracy measurements; and proficiency testing

allows for inter-laboratory comparisons.

Reference materials, such as those traceable through NIST have an applied level of

accuracy assigned through the reference. Tracking QC sample data in a control chart

with a defined confidence interval can provide an indicator of the fluctuations of errors

over time.


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7. DETECTION AND REPORTING LIMITS

Historically, the SEL has maintained the term “MDL (Method Detection Limit)”. The term

MDL and LOD are interchangeable for the scope of this document. The Region 6 Minimum

Quantitation Level (MQL) Guidance Report defines the MDL and the LOD using similar

descriptors. The laboratory incorporates the term “Limit of Detection (LOD) when referring to

the laboratory generated detection limits, with exception to EPA Region 6 certified DW

compliance samples, which will retain the term MDL for the context of certification.

Numerous terms are associated with sensitivity of environmental analytical systems. The term

“detection limit” is a general collective term that may reference several types of sensitivity

limits, and in general, refers to the minimum concentration that can be distinguished as actual

analyte signal over instrument noise. Some technologies, such as meter systems, will have MDLs

that are based on the readout or display limitations of the instrument. For some technologies,

spiking solutions are not available, or MDLs cannot be determined.

7.1. Sensitivity Measurements

7.1.1. Detection Limit (DL):

DL is the lowest concentration of an analyte that can be detected.

A measure of the capability of an analytical method to distinguish samples that do

not contain a specific analyte from samples that contain low concentrations of the

analyte; the lowest concentration or amount of the target analyte that can be

determined to be different from zero by a single measurement at a stated level of

probability. DLs are analyte and matrix-specific and may be laboratory-

dependent.

7.1.2. Limit of Detection (LOD):

LOD is the minimum concentration that can be measured and reported with 99%

confidence that the value is larger than zero.

Some programs define the LOD as the minimum concentration of a substance

being analyzed with a 99 % probability of being identified. The minimum

concentration of an analyte that, in a given matrix and with a specific method, has

a 99% probability of being identified, qualitatively or quantitatively measured,

and reported to be greater than zero. In some programs, the LOD is equivalent to

(or referred as) the MDL (Method Detection Limit).

7.1.3. Method Detection Limit (MDL):

MDL is defined in 40CFR Part 136 Appendix B, through the “Definition and

Procedure for the Determination of the Method Detection Limit, Revision 2”, as

the minimum concentration of a substance that can be reported with 99%

confidence that the measured concentration is distinguishable from method blank

results. The MDL is determined through the analysis of a series of low-level

spiked samples and calculated using the standard deviations of the results. In


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some programs, the MDL is equivalent to (or referred as) the Limit of Detection

(LOD).

A DL must be reestablished or verified when there is a change in instrumentation,

technology, or method that may affect the sensitivity of the method.

7.1.4. Instrument Detection Limit (IDL):

IDL is associated specifically with an instrument and defined as the lowest

concentration that can be detected by an instrument. It is determined as three

times the standard deviation of the mean of the noise.

7.1.5. Limit of Quantitation (LOQ):

The LOQ is defined as the lowest concentration that can reliably be detected with

a defined level of precision and accuracy during “normal” operating conditions.

LOQ is typically derived as a multiple of the calculated MDL.

The LOQ is the minimum concentration of an analyte or category of analytes in a

specific matrix that can be identified and quantified above the method detection

limit and within specified limits of precision and bias during routine analytical

operating conditions. Also called the Practical Quantitation Limit (PQL).

7.1.6. Reporting Limit (RL):

The RL is the lowest concentration verified by the laboratory with an acceptable

degree of precision and accuracy. RL is the minimum value in which the lab

reports data without qualification. The RL may also be defined as the lowest

concentration or amount of the target analyte required to be reported from a data

collection project.

Reporting limits are greater than detection limits and are usually not associated

with a probability level. This value must be equal to or greater than the LOQ.

Some programs require certain RL to be verified and maintained prior to reporting

data.

These low-end reporting limits are established using calculations that consider the

normal daily fluctuations in instrument sensitivity as well as other laboratory

variables and are typically equivalent to the lowest calibration standard used and

accepted during the development of the calibration curve.

SEL reporting limits are set at levels greater than the established laboratory

detection limit to provide data of known accuracy. Every attempt is made to set

the reporting limit at a level less than or equivalent to federally mandated

detection limits to meet necessary program requirements. However, this is not

always achievable.

Routine analyte LOQs are provided in Appendix C. These limits are often

adjusted based on sample dilution, non-standard initial and final masses or


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volumes and % solids. Contact the relevant laboratory Section Manager or the

QAO for additional information regarding reporting limits for specific QAPP,

work plan, or client DQOs. For additional information relating to EPA Region 6

MQLs, contact the QAO. Reporting limit can also be referred to as the Minimum

Reporting Limit (MRL).

7.2. Instrument Sensitivity Relationships:

Analytical sensitivity is the ability of a test method or instrument to differentiate between

measurement responses representing different levels (e.g., concentrations) of a variable of

interest.2 Analytical sensitivity is affected by the preparation and analytical method

utilized; instrumentation and equipment used; analyst capability and experience;

standard, reagent and chemical quality; analyte of interest; sample matrix; contamination;

background noise; and measurement variability.

The Sensitivity figure below shows the relationship between the various terms and levels

of reporting limits.

Sensitivity Figure:

ZERO

ANALYTICAL SIGNAL

Section #1: This is the area between the zero (no analyte present) and the

LOD (analyte detectable) region. In this section, the signal of analyte is

often so weak that the instrument cannot differentiate actual analyte signal

from instrument noise, even though a small amount of analyte may be

present.

Section #2: The detection limit is the minimum concentration of a

substance that can be measured and reported with a 99% confidence that

the analyte concentration is greater than zero. This means that, with 99%

confidence, it can be stated that analyte is present, however, this leaves a

1% chance that identified analyte is not present, resulting in a false

positive. There is also a 50% probability of a false negative at the LOD. 2 TNI

Highest Calibration Standard

Upper Reporting Limit

Maximum Quantitation Limit

Lowest Calibration Standard

Lower Reporting Limit

(RL, PQL, LOQ, MRL)

Reportable Values

Detection Limit

(LOD, IDL, MDL)

1 2 4 3

NOISE /

BACKGROUND


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This means that an instrument can “see” the analyte but cannot determine

the amount of analyte with reliable accuracy or precision. Data reported

in this region can only be estimated.

Section #3: This is the area that the instrument can detect an analyte with

an acceptable degree of accuracy and precision.

Section #4: This is the area above the highest calibration standard or

verified linear range of the instrument. The instrument can “see” the

analyte but cannot determine the amount of analyte with reliable accuracy

or precision.

7.3. Project Reporting Limit Requirements

Data must be generated with sufficient sensitivity to meet the needs of the environmental

project. The required sensitivity for the data should be established and documented in

the QAPP, work plan, or environmental program. Project Managers and laboratory

customers should verify that the expected analytical sensitivity limit (detection level) is

obtainable for the method, analyte, and matrix of interest by the laboratory.

Project Managers and laboratory customers may meet with the laboratory group

managers or the QAO during QAPP or work plan development to verify terminology

and procedures associated with detection and reporting limits. This assists in the

prevention of errors and miscommunication during sample analysis and reporting and

ensures that the agreed upon LOQs outlined in the PPT meet the intended use for the

data. For additional information refer back to Section 3.

MDL studies are routinely demonstrated by the SEL for the establishment and

verification of reliable analyte detection, quantitation, and reporting limits. The MDL

study procedure is applicable to a wide range of analytes, matrix types, instruments, and

technologies. An acceptable MDL study is required for all suitable methods and

analyses prior to reporting data and to validate the LOQ, thereby establishing a

relationship between the two.

It is essential for Project Managers and laboratory customers and data users to

understand that DLs are developed in a clean matrix free of the interferences often found

in real-world samples. It may be impossible to obtain a DL for environmental samples

that is equivalent to the lab generated LOD. In addition, standard reporting limits may

be modified to meet project DQOs, however, the LOD is a measurement-based,

calculated value and cannot be “lowered”.


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8. LINEARITY AND CALIBRATION

8.1 Initial Calibration Analytical instrumentation and supporting equipment may require calibration or

verification to ensure proper working order and accurate and precise data. Ongoing

instrument verification is supported through instrument calibration and vendor service

and maintenance contracts

Instrument calibration consists of analyzing a known standard or series of standards of a

target parameter (e.g. concentration, volume, weight, temperature) and comparing the

measured value to a known value. Calibration requirements are typically prescribed in the

reference method, applicable program, or instrument manufacturers’ guidelines. The

method SOP includes details for calibration type, concentration range, number of

standards used, calibration and verification frequency, calibration standard information,

and acceptance criteria.

For methods that do not require a full instrument calibration on each day of use, the

calibration curve is verified through the use of a calibration verification check sample, at

minimum of once per analytical batch or as required by the method or program.

Calibration are performed with reference standards that are of the same general

characteristics as the associated samples (geometry, homogeneity, density

8.2 Calibration Verification

Some technologies have very stable calibrations and do not require full daily calibration

curves. Some technologies have daily calibrations in which the calibration curve may

lose stability throughout an analytical batch. In both of these situations, this stability is

verified using a calibration verification control sample (ICV, ICC, CCV, CCC).

The method SOPs include procedures for calibration verification, to include the

procedure, calculations, associated statistics, concentrations, frequency, calculations,

acceptance criteria and actions for unacceptable verifications.

8.3 Calibration Acceptance and Reporting

Sample results are quantified with an acceptable degree of confidence between the lower

concentration limit (lower reporting level and/or lowest calibration standard), and the

upper concentration limit (upper concentration limit or highest calibration standard) that

define the calibration range. Special requirements apply to data with values beyond

(above or below) the verified calibration range.

8.4 Calibration Standards Requirements

Initial calibrations are verified with a second source standard or that of a separate lot, and

the standard is traceable to a national standard, when commercially available.

To ensure proper instrument calibration or calibration verification, standards and

materials of the appropriate or required quality and traceability to NIST or other national

standards are purchased. Expired standards are not used for calibrations or verifications.


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8.5 Record Requirements

Sufficient raw data records are retained to permit the reconstruction of the instrument

calibration and calibration verification. Continuing calibration verification records

explicitly link the verification data to the initial calibration data.

8.6 Linearity

Linearity can be determined by measuring analyte at several concentrations and creating

a plot of signal against concentration. The resulting plot is then inspected for areas where

a linear relationship exists. This linear relationship can be utilized to extrapolate

unknown concentrations of analyte in a sample.

The general linearity range of a method is typically determined during method validation

or standardization. This linearity may vary based on laboratory specific conditions and is

verified by the laboratory at the frequency required by the reference method.

The procedures for the calibration and verification of support equipment can be found in

QS DC 9015-QSP and the referenced WIDs.


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9. DATA VERIFICATION

After data reduction activities have been completed, data verification is initiated. Data

verification is conducted during field and laboratory data collection and reporting activities to

evaluate the completeness, correctness, and conformance/compliance of a specific set of data

against predetermined method, procedural, or contractual requirements that are defined in

regulatory standards, project plans, or client requests.

Analytical data assessment includes review and verification of the quality assurance (QA) and

quality control (QC) components of the data. These QA/QC elements may be required by the

method, program, project, or client. This evaluation verifies the degree of reliability and

defensibility of the data by verifying the quality associated with the analytical system and by

quantifying any errors associated with the measurements. Sufficient records are maintained to re-

create the sample preparation and analytical processes to facilitate this verification.

Review of data does not change the quality of data generated. Due to the nature of an analytical

measurement system, data of questionable quality or certainty are occasionally generated. To

retain usability of the data, this information must be communicated to the data user. This can be

achieved through the use of data flags, qualifiers, or data narratives.

An analytical data assessment is independent and exclusive of an environmental project data

assessment. Data assessments may occur at the following levels:

1. Analysts Review (Self-Verification) - Data verification begins with the analyst of record

performing the sample preparation and analysis.

2. Peer Review (Secondary Review) - Peer review is defined as a level of review performed

by someone other than the analyst of record. Peer review is typically performed by a

trained analyst but may also be performed by any level of management or QS. Typically,

the initials of the person who does peer review appear next to the test results on the final

report.

3. Project Review, Authorization, and Closure- Project review consists of a review of the

overall information for a project, including sample collection, receiving, and other tests

involved in the sampling event. This review checks for accuracy of results using method

verification criteria in addition to project validation criteria. This level of review checks

for overall accuracy and completeness of information in data. Typically, the signature of

the person who does project review is the one that appears on the final report.

4. QS Data Verifications- Periodically, the QS will perform method-based data verifications

on raw data, data handling, or data reporting activities. These assessments are to provide

additional monitoring of the quality system or in support of special project verification

and validation.

Due to the nature and variability of field and analytical measurements, the usability of the data

may be impacted by a variety of environmental, instrumental, and/or human factors. Where

necessary, this consequence is accounted for through the use of data flags and qualifiers.


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10. DATA REPORTING

10.1 Report Walkthrough

SEL analytical results are reported on a standard report template that meets EPA

requirements for data reporting. See Appendix E for an example final report and tutorial

on how to interpret the report. Also, see Appendix B for a full list of qualifiers and flags

that may appear on the report.

10.2 Data Delivery Options

Delivery preferences are collected through Customer Profile forms (see section 3.8) with

details entered into the unique customer’s LIMS account. Delivery options include the

following: email, fax, postal mail, or online only. If no preference is made the default

delivery option will be postal mail.

PWS compliance data is automatically exported for the customer directly into the OK

PWS Compliance database at http://sdwis.deq.state.ok.us/DWW/.

10.3 Corrected Reports

Amendments to authorized and released LabWare final data reports require a corrected

final report with a new unique report identification. The corrected report shall be

identified as a corrected final report and include a reference to the original report ID.

After the corrected report is reissued to the client, the original report shall be maintained

and archived.

10.4 Specialized Deliverables

Preliminary Reports

EDD

Summary QC Table

Full QC Table

Raw Data

These deliverables are determined based on the selections made by the customer during

the project planning process. If no specialized deliverables are requested, then a final

report will be distributed.

Preliminary data reports are available upon request or when circumstances require sample

results to be provided prior to LIMS project authorization. The sample results and/or QC

samples may not have been fully reviewed or verified and the values reported on these

reports are not considered final. These reports will not have an authorization signature

and will show “Preliminary” next to the results. Preliminary data can also be provided via

email upon request.

Data validation is typically performed as a third-party assessment, independent of the

utilized laboratory. The SEL does not typically perform project validation activities,

although with special agreement, SELSD management may assist customers with

interpreting their data against program requirements or regulatory compliance limits.

A blank PPT form, which includes definitions of each specialized deliverable, is located

in Appendix F.


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APPENDIX A- SAMPLE CUSTODY DOCUMENTATION

Document defensibility and traceability is becoming more and more critical regarding

environmental Projects and Programs. Federally funded environmental programs and

evidentiary samples often require appropriate document traceability to ensure data defensibility

regarding decisions based on analytical data.

COC forms are generated from the LIMS. Some projects may be pre-logged so that the COC is

received with event specific information pre-filled. To obtain an actual sample COC or to

inquire about pre-logging, contact the Statewide Sample and Data Management Section.

To view a video on how to properly fill out a COC go to:

https://www.youtube.com/watch?v=o0DS7eLAvAw.

This sample COC is provided for reference:

https://www.youtube.com/watch?v=o0DS7eLAvAw


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APPENDIX B- QUALIFIERS AND FLAGS

At times field and analytical activities may run into situations or problems that could impact data

quality and results. The potential impact must be communicated to the data user. In these

instances, data qualifiers and flags are added to the final analytical data report in an effort to best

describe the quality or limitations of the sample data and assist the data user in determining the

usability of the data for their needs. The list provided below explains a variety of qualifiers and

flags that could appear on the final report. SDWIS is for drinking water compliance sample use

in the DWW/SDWIS database. WQX is for ambient water monitoring use in the WQX database.

General are qualifiers/flags that can be used when needed for all other customer types where

SDWIS or WQX flags are not appropriate or required. Note that since there are no requirements

for private customers, SDWIS qualifiers/flags are used for these customers, where appropriate,

as they meet method requirements. If you see a qualifier/flag that is not on this list or you need

additional explanation, please contact [email protected] for further information.

SDWIS WQX GENERAL CODE DESCRIPTION

X X BR (BR) Broken in Transit or Shipping

X CAN (CAN) Cancelled- No results reported.

X CF (CF) Corrected Final Report. Replaces

previous report.

X X CL (CL) Chlorine Present. Sample Rejected.

X CON (CON) Value Confirmed.

X CRYPTO Ongoing Precision and Recovery: --%

Cryptosporidium Oocysts and --% Giardia

Cysts

Method Blank Count: - Cryptosporidium

Oocysts and - Giardia Cysts

X X EH (EH) Exceeds Holding Time Upon Sample

Receipt

X ESTIMATED_VALUE (J) The value is an estimate.

X X FIS (FIS) Internal standard outside of range.

X X FZ (FZ) Frozen Sample

X X H (H) Analysis Method Hold Time Exceeded

X HEADSPACE_CONTAINER (HS) Sample has excessive head space. Not

suitable for volatiles analysis.

X HMSD (HMSD) Matrix spike duplicate acceptance

criteria not met- high

X HMSR (HMSR) High matrix spike recovery.

X HTH (HTH) Hard to Homogenize.

X X IF (IF) Instrument failure. Sample cancelled.

X X IP (IP) Invalid Sampling Protocol. Sample

rejected.

X ISP (ISP) Improper Sample Preservation.

Sample rejected.

X ISV (ISV) Insufficient Sample Volume. Sample

rejected.

X X J (J) The value is an estimate due to holding

time exceeded.

X X LA (LA) Lab Accident. Sample cannot be analyzed.

X LAC (LAC) No result reported. Lab accident.


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X LMSD (LMSD) Matrix spike duplicate acceptance

criteria not met- low

X LMSR (LMSR) Low matrix spike recovery.

X LOW_VOLUME Low Volume. Sample volume of less than

100mL could negatively impact the validity

of the analysis and cause the results to be

biased low.

X MATRIX_INTERFERENCE (MI) Components of the sample other than

the analyte may have affected the accuracy

or precision of the associated value of the

analyte in this sample analysis.

X MI (MI) Matrix Interference

X MTRX (MTRX) Possible matrix interference,

estimated value.

X PRESERVATION_FAILURE The sample was analyzed outside the

method required hold time of ___ days for

an unpreserved sample. Results may be

biased.

X QUALITY_CTRL_FAILURE (QCF) Quality Control Failure.

X RADON_CANISTER EPA recommends taking action to reduce

the levels of Radon in your home if the

results of one long-term test, or the average

of two short-term tests, show Radon levels

of 4pCi/L or higher. You may also want to

consider taking action if the level is below 4

pCi/L.

X X RC-R (RC) Requestor Cancelled Result/Analyte

X X RC-S (RC) Requestor Cancelled Sample

X X RC-T (RC) Requestor Cancelled Test

X SURROGATE_LOW Surrogate recoveries indicate results may be

biased low.

X TOTAL_COLIFORM_MPN The sample result of <1.0MPN/100mL

indicated that Total Coliform/E. Coli

bacteria were Absent. This sample result

meets the minimum requirements regarding

the Total Coliform standard for safe

drinking water. The state of Oklahoma does

not regulate private water wells.

X TOTAL_COLIFORM_SDW This sample result meets the minimum

requirements regarding the Total Coliform

standard for safe drinking water. The state

of Oklahoma does not regulate private water

wells.

X UCM The presence of unresolved complex

mixture (UCM) was detected. UCM has

been used extensively for decades to

describe a gas chromatographic

characteristic indicative of the presence of

fossil fuel hydrocarbons.

X X VO-S (VO) Insufficient Volume


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APPENDIX C- METHOD AND ANALYTE INFORMATION

This appendix contains general analytical information related the services the SEL is capable of

providing. This information is grouped by analytical section and includes individual analytes,

references methods, holding times, container and preservation requirements, and quantitation

and/or reporting limits by method. If you have further questions about any of the information

listed in this appendix, please contact the SEL at [email protected].

For reference, here is a key to clarify matrices and reporting limits as well as expanded TNI

definitions of these matrices.

AIR = Air and Emissions: Whole gas or vapor samples including those contained in

flexible or rigid wall containers and the extracted concentrated analytes of interest from a

gas or vapor that are collected with a sorbant tube, impinger solution, filter, or other

device.

AQU = Aqueous: Any aqueous sampled excluded from the definition of Drinking Water

or Saline/Estuarine. Includes surface water, ground water effluents, and TCLP or other

extracts.

BIO = Biological Tissue: Any sample of a biological origin such as fish tissue, shellfish,

or plant material. Such samples shall be grouped according to origin.

CW = Chemical Waste: A product or by-product of an industrial process that results in a

matrix not previously defined.

DW = Drinking Water: Any aqueous sample that has been designated a potable or

potential potable water source.

LIQ = Non-Aqueous Liquid: Any organic liquid with <15% settleable solids.

SAL = Saline/Estuarine: Any aqueous sample from an ocean or estuary, or other

saltwater source such as the Great Salt Lake.

SOL = Solids: Includes soils, sediments, sludges, and other matrices with >15%

settleable solids.

# = Contact the SEL for method specific reporting limits.


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GCMS PARAMETER MATRIX CONTAINER & PRESERVATIVE

REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

Trihalomethanes (THM) DW 40 ml amber glass maleic and ascorbic

acid EPA 524.3 14 days 1 µg/L

Total THM DW 40 ml amber glass maleic and ascorbic


Volatile Organics (VOC) DW 40 ml amber glass maleic and ascorbic

acid EPA 524.3 14 days 0.5 µg/L

Total THM DW 40 ml amber glass maleic and ascorbic


Volatile Organics (VOC

Liquid)

AQU, CW, DW,

LIQ, SAL

Clear Glass Vial 40 Milliliter Unpreserved

for Purge and Trap Analysis - No

headspace

EPA 8260C/5030C 7 days 10 µg/L

1,4-Dioxane AQU, CW, DW,

LIQ, SAL


for Purge and Trap Analysis - No

headspace

EPA 8260C/5030C 7 days 100 µg/L

Volatile Organics (VOC Solid) CW, SOL Clear Glass Vial 40 Milliliter Unpreserved

for Purge and Trap Analysis EPA 8260C/5035A 14 Days 10 µg/kg

1,4-Dioxane CW, SOL Clear Glass Vial 40 Milliliter Unpreserved


Volatile Organics (VOC

Waste)

AQU, CW, DW,

LIQ, SAL, SOL



m- and p-Xylene AQU, CW, DW,

LIQ, SAL, SOL



1,4-Dioxane AQU, CW, DW,

LIQ, SAL, SOL



Semivolatile Organics (SVOC

Liquid)

AQU, DW, CW,

LIQ, SAL

Amber Glass Bottle 1 Liter Preserved with

Sodium Thiosulfate EPA 8270D 7 days 10 µg/L


Solid) CW, SOL Clear Glass Jar 8 Ounce Unpreserved EPA 8270D 14 days 333 µg/kg


Waste)

AQU, DW, CW,

LIQ, SAL, SOL Clear Glass Jar 8 Ounce Unpreserved EPA 8270D 14 days 10 mg/kg

Percent Moisture BIO, CW, SOL Clear Glass Jar 4 Ounce Unpreserved CLP Inorganic

Superfund Method 14 days 0 PERCENT


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GENERAL CHEMISTRY PARAMETER MATRIX CONTAINER & PRESERVATIVE

REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

Color, True AQU, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 110.2 2 days 1 CU

Color, Apparent AQU, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 110.2 2 days 1 CU

Hardness, Total AQU, CW, DW Clear Plastic Bottle 8 Ounce Preserved

with Nitric Acid EPA 130.1 180 days 10 mg/L

pH AQU, CW, DW,

SAL Clear Plastic Bottle 4 Ounce Unpreserved EPA 150.1 15 mins 2 STD UNIT

Solids, Volatile Suspended AQU, CW, DW Clear Plastic Bottle 16 Ounce Unpreserved EPA 160.4 28 days 10 mg/L

Oil and Grease AQU, CW Clear Glass Jar 1 liter Preserved with

Hydrochloric Acid EPA 1664B 28 days 5 mg/L

Hexavalent Chromium AQU, CW, DW Clear Plastic Bottle with Hexavalent

Chromium Preservative, 4oz/125mL EPA 218.6 28 days 0.1 µg/L

Fluoride AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 28 days 0.2 mg/L

Sulfate AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 28 days 0.5 mg/L

Orthophosphate AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 48 hours 0.05 mg/L

Nitrite AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 48 hours 0.1 mg/L

Nitrate AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 48 hours 0.2 mg/L

Chloride AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 28 days 3 mg/L

Bromide AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 300.0 28 days 0.1 mg/L

Chlorite AQU, CW, DW Amber Glass Bottle 8 Ounce Preserved

with EDA EPA 300.1 14 days 20 µg/L

Chlorate AQU, CW, DW Amber Glass Bottle 8 Ounce Preserved


Bromide AQU, CW, DW Amber Glass Bottle 8 Ounce Preserved


Bromate AQU, CW, DW Amber Glass Bottle 8 Ounce Preserved


Chloride AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 325.2 28 days 10 mg/L

Chloride SOL Clear Glass Jar 4 Ounce Unpreserved EPA 325.2M 28 days 10 mg/kg

Cyanide, Total AQU, CW, DW Clear Plastic Bottle 500 mL Preserved

with Sodium Hydroxide EPA 335.4 14 days 0.01 mg/L

Cyanide, Total SOL Clear Glass Jar 4 Ounce Unpreserved EPA 335.4M 14 days 0.25 mg/kg

Nitrogen, Ammonia AQU, CW, DW Clear Plastic Bottle 4 Ounce Preserved

with Sulfuric Acid EPA 350.1 28 days 0.1 mg/L


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PARAMETER MATRIX CONTAINER & PRESERVATIVE REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

Nitrogen, Ammonia SOL Clear Glass Jar 4 Ounce Unpreserved EPA 350.1M 28 days 0.1 mg/kg

Nitrogen, Total Kjeldahl

(TKN) AQU, CW, DW

Clear Plastic Bottle 4 Ounce Preserved


Nitrogen, Total Kjeldahl

(TKN) SOL Clear Glass Jar 4 Ounce Unpreserved EPA 351.2M 28 days 0.1 mg/kg

Nitrogen, Nitrite AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 353.2 2 days 0.1 mg/L

Nitrogen, Nitrite SOL Clear Glass Jar 4 Ounce Unpreserved EPA 353.2M 28 days 0.1 mg/kg

Nitrogen, Nitrate AQU, CW, DW Clear Plastic Bottle 8 Ounce Unpreserved EPA 353.2 2 days 0.1 mg/L

Nitrogen, Nitrate SOL Clear Glass Jar 4 Ounce Unpreserved EPA 353.2M 2 days 0.1 mg/kg

Nitrogen, Nitrate/Nitrite AQU, CW, DW Clear Plastic Bottle 4 Ounce Preserved


Nitrogen, Nitrate/Nitrite SOL Clear Glass Jar 4 Ounce Unpreserved EPA 353.2M 28 days 0.1 mg/kg

Orthophosphate AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 365.1 2 days 0.005 mg/L

Orthophosphate, Dissolved AQU, CW, DW Flipmate for Dissolved Samples EPA 365.1 2 days 0.005 mg/L

Phosphorus, Total SOL Clear Glass Jar 4 Ounce Unpreserved EPA 365.3M 28 days 0.01 mg/kg

Phosphorus, Total AQU, CW, DW Clear Plastic Bottle 8 Ounce Preserved


Sulfate AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved EPA 375.4 28 days 10 mg/L

Sulfate SOL Clear Glass Jar 4 Ounce Unpreserved EPA 375.4M 28 days 10 mg/kg

pH SOL Clear Glass Jar 4 Ounce Unpreserved EPA 9045D 15 mins 2 STD UNIT

Benthic Pheophytin AQU, BIO Clear Glass Tube 12 Milliliter

Unpreserved

OWRB Benthic

Chlorophyll 30 days 0.5 mg/m3

Benthic Chlorophyll AQU, BIO Clear Glass Tube 12 Milliliter

Unpreserved

OWRB Benthic

Chlorophyll 30 days 0.5 mg/m3

Pheophytin-a AQU, BIO Clear Glass Tube 12 Milliliter

Unpreserved SM 10200H 1 day 0.5 mg/m3

Chlorophyll A and Pheophytin AQU, BIO Clear Glass Tube 12 Milliliter

Unpreserved SM 10200H 1 day 0.5 mg/m3

Periphyton AQU, BIO Clear Glass Tube 12 Milliliter

Unpreserved SM10300C 30 days 0.5 mg/m3

Alkalinity AQU, DW Clear Plastic Bottle 8 Ounce Unpreserved 2320B 14 days 20 mg/L

Acid Neutralizing Capacity AQU, DW Clear Plastic Bottle 4 Ounce Unpreserved WRS12A.4 7 days 20 µEq/L

Conductivity AQU, CW, DW,

SAL Clear Plastic Bottle 4 Ounce Unpreserved SM 2510B 28 days 2 µƱ/cm

Solids, Total (TS) AQU, CW, DW Clear Plastic Bottle 16 Ounce Unpreserved SM 2540B 7 days 10 mg/L


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METHOD

HOLDING

TIME LOQ UNITS

Solids, Total Dissolved (TDS) AQU, CW, DW Clear Plastic Bottle 16 Ounce Unpreserved SM 2540C 7 days 10 mg/L

Solids, Total Suspended (TSS) AQU, CW, DW Clear Plastic Bottle 16 Ounce Unpreserved SM 2540D 7 days 5 mg/L

Solids, Settleable AQU, CW, DW Clear Plastic Bottle 1 Liter Unpreserved SM 2540F 2 days 0.1 mL/L

Chlorine, Total AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved SM 4500ClG 15 mins 0.1 mg/L

Chlorine, Free AQU, CW, DW Clear Plastic Bottle 4 Ounce Unpreserved SM 4500ClG 15 mins 0.1 mg/L

Oxygen, Dissolved AQU, CW Clear Plastic Bottle 1 Liter Unpreserved SM 4500OG 15 mins N/A mg/L

Demand, Carbonaceous Bio

Oxygen (CBOD5) AQU, CW Clear Plastic Bottle 1 Liter Unpreserved SM 5210B 2 days 2 mg/L

Demand, Biochemical Oxygen

(BOD5) AQU, CW Clear Plastic Bottle 1 Liter Unpreserved SM 5210B 2 days 2 mg/L

Demand, Ultimate

Carbonaceous Bio Oxygen

(CBOD20)

AQU, CW Clear Plastic Bottle 1 Liter Unpreserved SM 5210C 2 days 2 mg/L

Demand, Ultimate

Biochemical Oxygen (BOD20) AQU, CW Clear Plastic Bottle 1 Liter Unpreserved SM 5210C 2 days 2 mg/L

Chemical Oxygen Demand

(COD) AQU, CW


with Sulfuric Acid SM 5220C 28 days 5 mg/L

Chemical Oxygen Demand

(COD) SOL Clear Glass Jar 4 Ounce Unpreserved SM 5220CM 28 days 5 mg/kg

Carbon, Dissolved Organic

(DOC) AQU, CW, DW

Amber Glass Bottle 16 Ounce Preserved

with Sulfuric Acid SM 5310C 28 days 0.5 mg/L

Carbon, Total Organic (TOC) AQU, CW, DW Amber Glass Bottle 16 Ounce Preserved

with Sulfuric Acid SM 5310C 28 days 0.5 mg/L

METALS PARAMETER MATRIX CONTAINER & PRESERVATIVE

REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

Aluminum, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with

Nitric Acid EPA 6010D 180 days # mg/L

Aluminum, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Aluminum, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with

Nitric Acid EPA 6020B 180 days 1 mg/L

Aluminum, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 5 mg/kg

Aluminum, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved

with Nitric Acid EPA 200.7 180 days 100 µg/L


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METHOD

HOLDING

TIME LOQ UNITS

Aluminum, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Antimony, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Antimony, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Antimony, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with

Nitric Acid EPA 6020B 180 days 0.02 mg/L

Antimony, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/L

Antimony, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Antimony, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Arsenic, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Arsenic, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Arsenic, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Arsenic, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Arsenic, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Arsenic, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Barium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Barium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Barium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Barium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Barium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Barium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Beryllium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Beryllium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg


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METHOD

HOLDING

TIME LOQ UNITS

Beryllium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Beryllium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Beryllium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Beryllium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Boron, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Boron, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Boron, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Cadmium Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Cadmium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Cadmium, Total BIO Clear Glass Jar 4 Ounce Unpreserved EPA6020B 180 days 0.02 mg/kg

Cadmium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Cadmium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Cadmium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Cadmium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Calcium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Calcium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Calcium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved

with Nitric Acid EPA 200.7 180 days 0.5 mg/L

Chromium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Chromium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Chromium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Chromium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg


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METHOD

HOLDING

TIME LOQ UNITS

Chromium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Chromium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Cobalt, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Cobalt, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Cobalt, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Cobalt, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Cobalt, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Cobalt, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Copper, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Copper, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Copper, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Copper, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Copper, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Copper, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Iron, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Iron, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Iron, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Lead, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Lead, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Lead, Total BIO Clear Glass Jar 4 Ounce Unpreserved EPA6020B 180 days 0.02 mg/kg

Lead, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with



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METHOD

HOLDING

TIME LOQ UNITS

Lead, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Lead, Total or Disssolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Lead, Total or Disssolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Lithium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Magnesium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Magnesium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Magnesium, Total or

Dissolved AQU, DW



Manganese, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Manganese, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Manganese, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Manganese, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Manganese, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Manganese, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Mercury, Total AQU, DW Clear Plastic Bottle 4 Ounce Preserved

with Nitric Acid EPA 245.1 28 days 0.05 ng/L

Mercury, Total AQU, DW Amber Glass Bottle 1 Liter Preserved with

Hydrochloric Acid EPA 245.7 28 days 10 µg/L

Mercury, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Mercury, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 0.25 mg/kg

Mercury, Total BIO Clear Plastic Tube 50 Milliliter

Unpreserved EPA 7473 28 days 0.05 mg/kg

Mercury, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved

with Nitric Acid EPA 200.8 180 days 0.05 µg/L

Molybdenum, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with



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METHOD

HOLDING

TIME LOQ UNITS

Molybdenum, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Molybdenum, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Molybdenum, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Molybdenum, Total or

Dissolved AQU, DW



Molybdenum, Total or

Dissolved AQU, DW



Nickel, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with

Nitric Acid EPA 6010D 180 days # µg/L

Nickel, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Nickel, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Nickel, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Nickel, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Nickel, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Potassium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Potassium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Potassium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Selenium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Selenium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Selenium, Total BIO, CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Selenium, Total AQU Clear Plastic Bottle 1 Liter Preserved with


Selenium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Selenium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Silicon as Silica, Total AQU, DW Clear Plastic Bottle 16 Ounce Preserved



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METHOD

HOLDING

TIME LOQ UNITS

Silicon as Silica, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Silicon, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Silicon, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Silver, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Silver, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Silver, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Silver, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Silver, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Silver, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Sodium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Sodium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Sodium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Strontium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Strontium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Strontium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Strontium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Thallium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Thallium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Thallium, Total AQU Clear Plastic Bottle 1 Liter Preserved with


Thallium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Thallium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg


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METHOD

HOLDING

TIME LOQ UNITS

Thallium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Thallium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Tin, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Tin, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Tin, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Titanium, Total AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Titanium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Titanium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Turbidity AQU, CW, DW,

SAL Clear Plastic Bottle 8 Ounce Unpreserved SM 2130B 2 days 0.2 NTU

Uranium, Total AQU Clear Plastic Bottle 1 Liter Preserved with


Uranium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Uranium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Uranium, Total or Dissolved AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Vanadium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Vanadium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Vanadium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with


Vanadium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6020B 180 days 1 mg/kg

Vanadium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Vanadium, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Yttrium, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with



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METHOD

HOLDING

TIME LOQ UNITS

Yttrium, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved EPA 6010D 180 days # mg/kg

Zinc, Total BIO Clear Glass Jar 4 Ounce Unpreserved EPA6020B 180 days 0.5 mg/kg or

µg/kg

Zinc, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved 6010D 180 days 0.1 mg/kg

Zinc, Total CW, SOL Clear Glass Jar 4 Ounce Unpreserved 6020B 180 days 0.05 mg/kg

Zinc, Total AQU, CW, SOL Clear Plastic Bottle 1 Liter Preserved with


Zinc, Total AQU, CW Clear Plastic Bottle 1 Liter Preserved with

Nitric Acid EPA 6020B 180 days 0.1 ug/L

Zinc, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Zinc, Total or Dissolved AQU, DW Clear Plastic Bottle 16 Ounce Preserved


Percent Solids BIO, CW, SOL Clear Glass Jar 4 Ounce Unpreserved CLP Inorganic

Superfund Method

14 days 30 PERCENT

MICROBIOLOGY PARAMETER MATRIX CONTAINER & PRESERVATIVE

REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

Anatoxin-a AQU, DW Amber glass bottle with Anatoxin

preservative

Abraxis ELISA

520060 3 days 0.15 µg/L

Cylindrospermopsin AQU, DW Amber Glass Bottle 4 Ounce Unpreserved Abraxis ELISA

522011 3 days 0.05 µg/L

Microcystins/Nodularins AQU, DW Amber Glass Bottle 4 Ounce Unpreserved Abraxis ELISA

520011 3 days 0.15 µg/L

Saxitoxin AQU, DW Amber Glass Bottle 2 Ounce Preserved

with Saxitoxin

Abraxis ELISA

52255B 3 days 0.02 µg/L

Enterococci AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate ASTM D6503-99 6 hours 1 MPN/100mL

Enterococci AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate ASTM D6503-99 6 hours N/A present/absent

Fecal Coliforms AQU Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM9222D 6 hours 1 CFU/mL

Giardia AQU Clear Plastic Cubitainer 2.5 Gallon

Unpreserved EPA 1623.1 4 days 0.1 CYSTS/L


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METHOD

HOLDING

TIME LOQ UNITS

Cryptosporidium AQU Clear Plastic Cubitainer 2.5 Gallon

Unpreserved EPA 1623.1 4 days 0.1 OOCYST/L

Giardia (Matrix Spike) AQU Clear Plastic Cubitainer 2.5 Gallon

Unpreserved EPA 1623.1 4 days 1 PERCENT

Cryptosporidium (Matrix

Spike) AQU

Clear Plastic Cubitainer 2.5 Gallon

Unpreserved EPA 1623.1 4 days 1 PERCENT

Fecal Coliforms LIQ, SOL Clear Plastic Bottle 16 Ounce Unpreserved EPA 1681 8 hours 1 MPN/g

Salmonella LIQ, SOL Clear Plastic Bottle 16 Ounce Unpreserved EPA 1682 6 hours 1 MPN/g

Iron-Related Bacteria AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate HACH IRBBART 30 hours N/A present/absent

Sulfate-Reducing Bacteria AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate HACH SRBBART 30 hours N/A present/absent

Legionella pneumophila AQU, DW Clear Plastic Bottle 120 Milliliter Legiolert L.

pneumophila 30 hours 10 MPN/100mL

Potentially Toxic

Cyanobacteria (Identification

Only)

AQU Clear Plastic Bottle 1 Liter Preserved with

Lugol Iodine SM 10900C 3 days 80

detect/non-

detect

Woronichinia sp. AQU Clear Plastic Bottle 1 Liter Preserved with

Lugol Iodine SM 10200F 3 days 80 cells/mL

Sphaerospermopsis sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Snowella sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Radiocystis sp./Snowella sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Radiocystis sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Pseudanabaena sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Planktothrix sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Microcystis sp./Woronichinia

sp. AQU

Clear Plastic Bottle 1 Liter Preserved with


Microcystis sp. AQU Clear Plastic Bottle 1 Liter Preserved with



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METHOD

HOLDING

TIME LOQ UNITS

Limnothrix sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Dolichospermum sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Cylindrospermopsis sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Cuspidothrix sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Chrysosporum sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Arthrospira sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Aphanizomenon sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Anabaenopsis sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Anabaena sp. AQU Clear Plastic Bottle 1 Liter Preserved with


Suspected Prymnesium

parvum AQU


Lugol Iodine and Acetic Acid SM 10900 3 days N/A

detect/non-

detect

Golden Algae AQU Clear Plastic Bottle 1 Liter Preserved with

Lugol Iodine and Acetic Acid SM 10900 QUANT 3 days 2000 cells/mL

Microtox (Acute Aquatic

Toxicity) AQU, DW


Sodium Thiosulfate SM 8050B 2 days N/A

toxic/non-

toxic

Pseudomonas aeruginosa AQU, DW Clear Plastic Bottle 1 Liter Preserved with

Sodium Thiosulfate SM 9213E 1 day 1 CFU/100mL

Heterotrophic Bacteria AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9215B 6 hours 1 CFU/mL

Heterotrophic Bacteria AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9215E 6 hours 2 MPN/mL

Total Coliforms AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9222B 1 day 1 CFU/100mL

Fecal Coliforms AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9222D 6 hours 1 CFU/100mL


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METHOD

HOLDING

TIME LOQ UNITS

Total Coliform AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9223B 30 hours 1 MPN/100mL

E. coli AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9223B 30 hours 1 MPN/100mL

Total Coliform AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9223B 30 hours N/A present/absent

E. coli AQU, DW Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate SM 9223B 30 hours N/A present/absent

Shigella sp. AQU, DW Clear Plastic Bottle 1 Liter Unpreserved SM 9260E 3 days 1 CFU/100mL

Shigella sonnei AQU, DW Clear Plastic Bottle 1 Liter Unpreserved SM 9260E 3 days 1 CFU/100mL

Aeromonas sp. AQU, DW Clear Plastic Bottle 1 Liter Preserved with

Sodium Thiosulfate SM 9260L 8 hours 1 CFU/100mL

Aeromonas salmonicida ssp.

salmonicida AQU, DW



Aeromonas hydrophila gr 2 AQU, DW Clear Plastic Bottle 1 Liter Preserved with


Aeromonas hydrophila gr 1 AQU, DW Clear Plastic Bottle 1 Liter Preserved with


Enterococci sp. AQU Clear Plastic Bottle 120 Milliliter

Preserved with Sodium Thiosulfate EPA 1609.1 6 hours 38 CCE

GC PARAMETER MATRIX CONTAINER & PRESERVATIVE

REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

EDB, DBCP, and 123TCP AQU, DW, SAL Clear Glass Vial 40 Milliliter Preserved

with Sodium Thiosulfate EPA 504.1 14 days 0.02 µg/L

Nitrogen Phosphorus

Pesticides AQU, DW, SAL


Sodium Thiosulfate EPA 507 14 days 1 µg/L

Chlorinated Pesticides AQU, DW, SAL Amber Glass Bottle 1 Liter Preserved with

Sodium Thiosulfate EPA 508 7 days 0.05 µg/L

Toxaphene &

Technical Chlordane AQU, DW, SAL



Chlorinated Acid Herbicides AQU, DW, SAL Amber Glass Bottle 8 Ounce Preserved

with Sodium Thiosulfate EPA 515.3 14 days 4 µg/L

Pentachlorophenol AQU, DW, SAL Amber Glass Bottle 8 Ounce Preserved

with Sodium Thiosulfate EPA 515.3 14 days 1 µg/L


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METHOD

HOLDING

TIME LOQ UNITS

Carbamate Pesticides AQU, DW, SAL

Amber Glass vial 60 Milliliters Preserved

with Potassium Dihydrogen

Citrate/Sodium Thiosulfate

EPA 531.2 28 days 2 µg/L

Glyphosate AQU, DW, SAL Amber Glass vial 60 Milliliters Preserved

with Sodium Thiosulfate EPA 547 14 days 5 µg/L

Haloacetic Acids (HAA) AQU, DW, SAL Amber Glass Bottle 8 Ounce Preserved

with Ammonium Chloride EPA 552.3 14 days 1 µg/L

Monochloroacetic acid AQU, DW, SAL Amber Glass Bottle 8 Ounce Preserved


Total Haloacetic Acids AQU, DW, SAL Amber Glass Bottle 8 Ounce Preserved


Chlorinated Pesticides and

Polychlorinated Biphenyls AQU, DW, SAL



PCBs, Aroclors,

Toxaphene &

Technical Chlordane

AQU, DW, SAL Amber Glass Bottle 1 Liter Preserved with


Nitrogen Phosphorus

Pesticides AQU, DW, SAL


Sodium Thiosulfate EPA 614 7 days 1 µg/L

Gasoline Range Organic

Constituents (OKLA-GRO)

AQU, DW, LIQ,

SAL

Clear Glass Vial 40 Milliliter Preserved

with Hydrochloric Acid for Purge-and-

Trap Analysis

EPA 8015C/8020A 14 days 20 µg/L

Gasoline Range Organics

Constituents (OKLA-GRO) CW, SOL


for Purge-and-Trap Analysis EPA 8015C/8020A 14 days 20 µg/kg

Gasoline Range Organic

Constituents (OKLA-GRO) CW, LIQ, SOL


for Purge-and-Trap Analysis EPA 8015C/8020A 14 days 20 µg/kg

Chlorinated Pesticides CW, SOL Clear Glass Jar 8 Ounce Unpreserved EPA 8081B 14 Days 10 µg/kg

Toxaphene &

Technical Chlordane CW, SOL Clear Glass Jar 8 Ounce Unpreserved EPA 8081B 14 Days 50 µg/kg

Polychlorinated Biphenyls

(PCB) CW, SOL Clear Glass Jar 8 Ounce Unpreserved EPA 8082A None 10 µg/kg

Organochlorine Pesticides in

Fish Tissue BIO

Fish Composite in Clear Glass Jar 8 Ounce

Unpreserved FDA PAM303E4C1 None

See

Below µg/kg

Trifluralin BIO Fish Composite in Clear Glass Jar 8 Ounce

Unpreserved FDA PAM303E4C1 None 2 µg/kg


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METHOD

HOLDING

TIME LOQ UNITS

Hexachlorobenzene

alpha, beta-BHC

gamma, delta-BHC

BIO Fish Composite in Clear Glass Jar 8 Ounce


trans, cis-Nonachlor

alpha, gamma-Chlordane BIO



Heptachlor Epoxide

Heptachlor

Endrin, Aldrin



Endrin ketone

Endrin aldehyde

Dieldrin



trans, cis-Permethrin

Total Chlordane

Propachlor, Methoxychlor

Hexachlorocyclopentadiene

Fipronil, Etridiazole

Dacthal, Chlorneb

Chloropyrifos

Chlorothalonil

Chlorobenzilate



Total DDT, p,p'-DDT

p,p'-DDE, p,p'-DDD

Endosulfan sulfate

Endosulfan I and II



PCBs, Aroclors,

Toxaphene BIO



Total Petroleum Hydrocarbons AQU, CW, DW,

LIQ, SAL, SOL

Clear Glass Vial 40 Milliliter Preserved

with Hydrochloric Acid TNRCC 1005M 14 days 1 mg/L

Total Petroleum Hydrocarbons CW, SOL Clear Glass Vial 40 Milliliter Unpreserved TNRCC 1005M 14 days 10 mg/kg

Total Petroleum Hydrocarbons AQU, CW, DW,

LIQ, SAL, SOL Clear Glass Vial 40 Milliliter Unpreserved TNRCC 1005M 14 days 10 mg/kg

Flashpoint AQU, CW, DW,

LIQ, SAL Clear Glass Vial 40 Milliliter Unpreserved EPA 1020B None N/A °F

di(2-ethylhexyl) phthalate DW

Contract Laboratory Bottle: (3) Amber

Glass Bottles preserved with Sodium

sulfite & HCl.

EPA 525.2 14 days 0.6 µg/L


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METHOD

HOLDING

TIME LOQ UNITS

di(2-ethylhexyl) adipate DW



sulfite & HCl.

EPA 525.2 14 days 0.6 µg/L

Benzo(a)Pyrene DW



sulfite & HCl.

EPA 525.2 14 days 0.02 µg/L

Endothall DW

Contract Laboratory Bottle: 1 Liter Amber

Glass Bottle preserved with Sodium

Thiosulfate

EPA 548.1 14 days 9 µg/L

Diquat DW

Contract Laboratory Bottle: 1 Liter Amber

Plastic preserved with Sodium Thiosulfate

and Sulfuric Acid

EPA 549.2 7 days 0.4 µg/L

Percent Moisture BIO, CW, SOL Clear Glass Jar 4 Ounce Unpreserved CLP Inorganic

Superfund Method 14 days 0 PERCENT

RADIOCHEMISTRY PARAMETER MATRIX CONTAINER & PRESERVATIVE

REFERENCE

METHOD

HOLDING

TIME LOQ UNITS

Gross Beta AIR Ziploc Bag EPA 600/R-11/122 180 days 4 DPM/SWIPE

Gross Alpha AIR Ziploc Bag EPA 600/R-11/122 180 days 3 DPM/SWIPE

Radon 222 AIR Stainless Steel Radon Canister EPA 520-5-87005 14 days 0.5 pCi/L

Gamma Emitters AQU, DW Clear Plastic Bottle 1 Liter Preserved with

Nitric Acid EPA 901.1 180 days 50 pCi/L

Radium 228 AQU, DW Clear Plastic Bottle 1 Gallon Preserved

with Nitric Acid GaTech 6 months 1 pCi/L

Radium 226 AQU, DW Clear Plastic Bottle 1 Gallon Preserved

with Nitric Acid GaTech 6 months 1 pCi/L

Gamma Emitters AQU, CW, LIQ,

SAL, SOL Clear Glass Jar 4 Ounce Unpreserved HASL 300 180 days # pCi/L

Gross Beta AQU, DW Clear Plastic Bottle 16 Ounce Preserved

with Nitric Acid SM 7110B 180 days 4 pCi/L

Gross Alpha AQU, DW Clear Plastic Bottle 16 Ounce Preserved

with Nitric Acid SM 7110B 180 days 3 pCi/L

Uranium, Total AQU, DW Clear Plastic Bottle 1 Gallon Preserved

with Nitric Acid SM 7500U-C 180 days 1 pCi/L


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APPENDIX D- REFERENCED WIDS, PROCEDURES, AND DOCUMENTS

The following documents are part of the SELSD Quality System and are referenced within the

text of this DQM. These documents are available upon request.

DQM

Section

Tracking

Number Name Category

1 9010-QSP01 SELSD Quality Assurance Plan Quality System

2.1 9900-QSF06 Project Planning Tool (PPT) Special Projects

2.2.4 9000-QSP02 Demonstration of Capability Competency

5.1 9010-QSL01 Lab Capacity Log Quality System

8 9015-QSP01 Support Equipment Calibration Quality System


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APPENDIX E- GUIDE TO THE SELSD REPORT OF ANALYSIS


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HEADER (page 1 on the example)– Key Points:

SELSD is certified by EPA to perform drinking water analysis (OK00013) and by New

Hampshire Environmental Laboratory Accreditation Program (NHELAP #2338) for

cryptosporidium and giardia testing by EPA method 1623.1.

Need to contact us for any reason? Local and toll-free phone and email options are listed for your

convenience.

Want to provide feedback? Customer surveys are located on the SELSD webpage or follow the

link provided.

The CUSTOMER appears in bold in the upper left margin. Below CUSTOMER is the location

where the customer has elected to have the final report sent and may not represent the location

where the sample was physically collected. The customer may elect to receive their report of

analysis via email or fax in which case that information will appear in place of an address.

PROJECT SUMMARY (page 1 on the example)- Key Points:

A Project by SELSD definition is a sampling event and may contain one or a series of samples

derived from one or more sampling locations.

Every SELSD customer is assigned a unique ID to differentiate between customers with the same

or similar surnames. In this caseDOE-001 is the customer ID.

The Project is a combination of the customer ID followed by a number that represents the

number of total projects submitted by that customer. Project DOE-001_0002 is the second project

submitted by this customer. If you need or want technical assistance with your samples or test

results, please refer to the specific project when contacting SELSD.

Program and Subprogram are primarily sample categories that help SELSD sort and prioritize its

workload and ensure all program specific data quality and reporting requirements are met.

The signature after the Project Summary section represents the scientist who closed the project

and authorized the data to be reported to the customer.

PROJECT SAMPLE SUMMARY (page 1 on the example)- Key Points:

In this section you will see a full listing of all the samples in the project.

The Sample Number is an alpha numeric unique identifier for each sample container received by

SELSD. This number begins with its Program affiliation followed by the unique number. When

contacting SELSD for sample assistance, please provide this number as a point of reference to

improve service.

Station ID, Customer Sample ID, and QA Code will be discussed in the Sample Information

section that follows.

PROJECT NARRATIVE (page 1 on the example)- Key Points:

In this section you will find any specific information about your project that may be pertinent to

the collection or analysis of the samples contained in the project. If no project notes are added,

this section will not display on your final report.

FOOTER (pages 1-5 on the example)- Key Points:

On the left side of the footer you will find the report number. This is the number that is

referenced on corrected reports.

The Report Date on the right side of the footer is the date that the report was printed.


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SAMPLE INFORMATION (pages 2-5 on the example)- Key Points:

This section contains all information relative to the collection of the sample. In addition to the

unique sample number, you will see the source of the sample, sampling point/Station ID (where

the sample was physically collected), who it was collected by and when. For customers who

have their own sample numbers, this number will appear to the right of the SELSD sample

number.

Also, in this section of the report you will see the date and time when each sample was received

by the laboratory and the temperature of the sample when it was received. This is critically

important information as many tests run by the lab have very specific thermal preservation and

holding time requirements.

QA Code applies to field QC activities and may not appear on your report depending on the

context under which the sample was submitted, and to which program it is affiliated.

TEST RESULTS (pages 2-5 on the example)- Key Points:

This section is organized by sample and then followed directly by data pertaining to each test

method run on the sample. If there was more than one sample in the project, each sample will

start on its own page and have its own Sample Information and Test Results sections.

On the first line in the left margin of each Test Results block you will see the Analysis Method

used for the testing next to a common name for the Analysis.

Component Name is highly variable and represents the name of the parameter, analyte, agent,

isotope, organism, or compound tested on that sample.

Once the lab completes your analysis, you will receive a single numerical result or a set of results

for each test method. In most cases this is a numerical value. However, in some cases as you can

see on page 2, the result may be listed as “Present” or “Absent” in response to the presence or

absence of a target organism or bacteria.

Most results are reported in a variety of units based on several factors that include technology

used and the sensitivity of the test method, reference ranges, and reporting level requirements.

For each SELSD test, method Limits of Quantitation (LOQ), aka reporting levels, have been

established through vigorous QC procedures. Any result that is preceded with a “<” means that

the measured result on your sample is “less than” the established LOQ or reporting limit for that

component.

Sometimes, as you can see on page 4, preliminary reports are issued at the customer’s request or

to expedite reporting of the test results. In such cases, the sample results have not gone through

full data review and authorization and are thus referred to as “preliminary”. If there are no such

preliminary designations on you test results, they should be considered final and subject to

known and documented quality.

In certain instances, it may be necessary to flag or qualify a sample or test result. As you can see

on page 5, a “J” qualifier has been applied to the test result for 1,2-Dichloroethane. Data

qualifiers and flags are added to the report of analysis to best describe the quality or limitations of

the sample data and assist the data user in determining the usability of the data for their needs. A

full list of SELSD flags and qualifiers is provided in Appendix B.

On the report of analysis, the Reviewer represents the initials of the scientist who authorized the

test result or results.

If you ever have questions about any report or data provided by the SELSD, please feel

free to contact us at the phone numbers or email provided in the header.


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APPENDIX F- PPT (PROJECT PLANNING TOOL)

The PPT below is provided to project managers by the Laboratory Customer Assistance Manager

(see Section 3.1 for contact information) when requested. It is completed and submitted

electronically then verified by the Laboratory Customer Assistance Manager prior to a project

being pre-logged and container pick-up scheduled.

STATE ENVIRONMENTAL LABORATORY PROJECT PLANNING DETAILS FORM

This form is used to document follow up and confirmation of information provided in the Project

Planning Initiation Form. This form will also allow additional information and details to be

documented that are not captured in the initiation form. These additional details typically pertain

to how the SELS will process the samples internally.

Project Name-Description (Provided on Initiation Form) Click or tap here to enter text.

Project Manager or Back-Up contacted for the completion of this form. Contact via phone or

meeting to discuss. Click or tap here to enter text.

Date of Follow-Up Contact Click or tap here to enter text.

Name of SELS Staff Completing Form Click or tap here to enter text.

1. Review Project Planning Tool Initiation Form

Review the information provided on the initiation form to ensure details and understanding

are correct for project scope and requirements. ☐ Click or tap here to enter text.

2. Lab Location and Business Hours, After Hours

☐ If DEQ staff is the project manager, does the project manager know the after-hours policy

and procedure? If not, we will provide a copy of the current procedure.

Choose an item.

-OR-

☐ If non-DEQ staff, does the project manager know the laboratory location and business

hours for sample supplies pick up and sample delivery? After hours not available for non-

DEQ staff unless approved by management.

3. Analytics

Discuss requested analytics. Compliance and non-compliance data, federal and state

regulations, QAPPs may determine appropriate or acceptable methods. Record the analytes,

methods and matrices requested in the table below- Table 3.1.

For test lists, use current reference tools for analyte and method listings.

Ex. RCRA 7, RCRA 8, Priority Pollutants, Routine Chemistry, Routine Metals, Oil and Gas


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Table 3.1 Analytics Requested

Analyte or Test List Method(s) Matrix

Click or tap here to enter

text.

Click or tap here to enter text. Choose an item.


text.



text.



text.



text.



text.


Analytics Requested Notes:

Click or tap here to enter text.

4. Reporting Limits If the project manager needs to verify reporting limits (i.e. low-level permits) meet

requirements for this project, please indicate below. Reporting limits for analytes, methods

and matrices identified in the request table will be provided to the project manager before

approvals are completed.

Current reporting limits requested? Choose an item. Reporting Limits Sent to Project Manager by Click or tap here to enter text. On Click or tap

to enter a date.

5. Sample Matrix

If solid or sediment- moisture corrections are applied to these results by default unless

otherwise indicated. If moisture correction is not needed, results will be reported as wet

weight.

Is the matrix or material to be analyzed identified or described on the initiation form? Click

or tap here to enter text.

Provide additional details below if needed, especially for abnormal matrices.

Notes: Click or tap here to enter text.

6. Field Quality Control

If field QC is requested, please list field site IDs or descriptors.

Ex. Site 1 Field Duplicate; Site 2 Field Blank

Field Duplicates



Field Blanks




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Trip Blanks



7. Analysis Quality Control

Is there a specific site or sites requested for laboratory analysis quality control?

PM can designate which sample will be duplicated or spiked if needed. If not designated,

normal laboratory quality controls and frequencies will be used.


8. Reporting

Definitions of deliverables are below. Check next to each one requested for this project.

Final reports are always provided.

☐ Final Reports Only

☐ Preliminary Data or Lab Reports may be provided for any level of reporting but must

be indicated.

☐ EDD is electronic data deliverable in the form of an excel spreadsheet of sample, test

and results information.

☐ Summary QC Table is a pass/fail table for each analyte along with the requirements

listed.

☐ Full QC Table lists all result values, calculation results and requirements listed for

each analyte. Includes batch quality control and field quality control evaluations (if

known).

☐ Raw Data is all raw and traceable data associated with the full laboratory lifecycle of

the analysis of samples for this project. Includes raw instrument data, equipment logs,

reagent and solutions logs, quality control charts for each analytical method, certificates

for standards, etc. This type of packet requires a significant amount of work and time to

compile.

9. Additional Details for QAPP Projects If project has a QAPP- did the PM send a copy of the QAPP to SELS for review?

Choose an item. SELS staff has reviewed the QAPP and understands the Quality Control requirements.

Staff Initials Click or tap here to enter text. Date Click or tap to enter a date.

10. Billing

If invoicing is indicated as billing method on initiation form, ask the following:

Is a purchase order in place to pay for this project? Choose an item.

If yes, PO # Click or tap here to enter text.

Is there a maximum amount for lab services? $Click or tap here to enter text.

Does the PM need a cost estimate per sample for the analytes requested? ☐Yes ☐ No

Cost Estimate Per Sample $Click or tap here to enter text.

Invoice Recipient Name (if other than project manager listed): Click or tap here to enter

text.


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Lab Use Only

The following sections are for lab use only to document items related to lab activities. These are

not a part of the customer interview to complete the above portion.

Lab Capacity

Provide initial details from initiation form and details above to appropriate section

managers for capacity assessment. Sample load, frequency, staffing, hold times, supplies and

instrument availability should all be considered. Assessment options are accept, delay, reject.

Manager(s) Contacted, Date(s), Assessment: Click or tap here to enter text.

Sample Logging Information

The data intent and use determine the correct program and subprogram.

Program Includes

☐ SDWA Compliance, Non-Compliance

☐ PDES Stormwater, Wastewater

☐ Private (Research, Education, Contract, etc.)

☐ Contractual (Other Agency or Tribal)

☐ Lab Priority Investigation, Criminal/Enforcement, Complaints

☐ ODEQ RCRA, Superfund, Solid Waste

Subprogram Click or tap here to enter text.

Does Project Manager have a LabWare account in the correct Address Book? If no, use a

customer profile form to record account information before logging the project.

Account: Click or tap here to enter text.

Project ID: Click or tap here to enter text.

Project Description: Click or tap here to enter text.

Login Date: Click or tap to enter a date.

Login By: Click or tap here to enter text.

Sample Logging- Log According to Information Provided Above or in the QAPP

Number of Sampling Sites Click or tap here to enter text.

Field QC Samples Click or tap here to enter text.

Sample Point Group- Address(es) or EPA Site ID- Project Manager can send for prelogging if

known Click or tap here to enter text.

Sample Point- Site IDs or locations- Project Manager can send for prelogging if known. Click or

tap here to enter text.

Notifications

Notify the project manager when the sampling materials- containers, preservatives, Chain of

Custody, sample labels, etc. are assembled and ready for pick up.

Date of Notification for Sampling Supply Pick Up: Click or tap to enter a date.

Initials: Click or tap here to enter text.

Additional Project Notes

Previous projects? Click or tap here to enter text.


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History or background? Click or tap here to enter text.

Report analyte values between MDL and RL? Click or tap here to enter text.

Sampling Instructions Needed? Click or tap here to enter text.

Preservative requirements, shipping/transport requirements, hold times known? Click or tap here

to enter text.


Approvals

1. Project Manager/Customer

Name Title Click or tap

to enter a

date.

2. SELS Project Planning Management

Name Environmental Program Manager Click or tap to

enter a date.

Name Environmental Program Manager Click or tap to

enter a date.

3. Quality Systems

Name SELS Quality Assurance Officer or

Designee

Click or tap to

enter a date.


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APPENDIX G- ACRONYMS

Acronym Term

AQ Aqueous

CCC Continuing Calibration Check

CCV Continuing Calibration Verification

COC Chain of Custody

CV Calibration Verification

DL Detection Limit

DMR Discharge Monitoring Report

DOC Demonstration of Competency

DQM Data Quality Manual

DQO Data Quality Objectives

DW Drinking Water

DWW Drinking Water Watch

GC Gas Chromatography

GC/MS Gas Chromatography/Mass Spectroscopy

ICC Initial Calibration Check

ICV Initial Calibration Verification

IDC Initial Demonstration of Competency

IDL Instrument Detection Limit

IEC Inter-element Correction Check Sample

IPC Instrument Performance Check

IS Internal Standard

LAP Laboratory Accreditation Program

LCS Lab Control Sample

LFB Lab Fortified Blank

LFM/LFMD Lab Fortified Matrix/Lab Fortified Matrix Duplicate

LFS Lab Fortified Sample

LIMS Laboratory Information Management System

LLOQ Lower Limit of Quantitation

LOD Limit of Detection

LOQ Limit of Quantitation

LRB Lab Reagent Blank

MB Method Blank

MCL Maximum Contamination Level

MDL Method Detection Limit

MQL Minimum Quantitation Level

MRL Minimum Reporting Limit

MS/MSD Matrix Spike/Matrix Spike Duplicate


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NIST National Institute of Standards and Testing

NRSB National Radiation Safety Board

PDES Pollution Discharge Elimination

PPT Project Planning Tool

PQL Practical Quantitation Limit

PT Proficiency Test

PTAB Proficiency Test Provider Accreditation Body

PTOB Proficiency Test Provider Oversite Body

PWS Public Water System

QA Quality Assurance

QAO Quality Assurance Officer

QAP Quality Assurance Plan

QAPP Quality Assurance Project Plan

QC Quality Control

QCS Quality Control Sample

QS Quality System

RB Reagent Blank

RPD Relative Percent Difference

RSD Relative Standard Deviation

SDWA Safe Drinking Water Act

SDWIS Safe Drinking Water Information System

SEL State Environmental Laboratory

SELSD State Environmental Laboratory Services Division

SOP Standard Operating Procedure

SRM Standard Reference Method

SRS Standard Reference Sample

SSDM Statewide Sample and Data Management

TNI The NELAC Institute

USGS United States Geological Survey

WID Work Instruction Document

WQX Water Quality Exchange


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APPENDIX H- AFTER HOURS SAMPLE DELIVERY WID

When samples are delivered by customers after business hours (8:00AM-4:30PM) and then

received by SSDM the next business day, there is a lack of DOCUMENTED traceability for the

time between after hour delivery and next day receipt. In a litigious situation, this gap could

bring into question the integrity of the sample and may prevent the sample from being used as

evidence.

SAMPLE CUSTODY RULES

1. Per SW-846, EPA Drinking Water Program and Standard Methods 21st ED, a sample is

considered to be in a person’s custody if:

i. In a person’s physical custody/possession.

ii. In view of the person after being in their possession.

iii. Locked/secured by that person to prevent tampering after being in their

possession.

iv. Placed in a designated or identified secured area to prevent tampering after being

in their possession.

2. Samples are not officially in SSDM custody until the SSDM staff signs for sample receipt

the following day.

3. Samples will not be accessioned if they are not documented on the sign in sheet

4. If samples are not documented on the sign in sheet the owner of the samples will be

contacted. Samples will be accessioned when the owner verifies sample drop off in

person and corrects the sign in sheet.

SSDM SECURITY

SSDM will provide a secure, restricted area for samples by following the listed protocol:

1. SSDM entrance doors are secured and monitored by building security.

2. Sample refrigerators are locked and secured.

3. Security cameras are monitoring both SSDM entrance doors by building security.

4. Secure “After Hours” sample locker.

AFTER HOUR SAMPLE DOCUMENTATION (COC) PROCEDURE

Employees who are bringing in samples after business hours will follow the protocol outlined

below:

1. Deliver samples to the designated after-hours delivery location.

2. Refresh the coolers with ice to maintain temperature until the next business day.

3. Document ALL required information in the “After Hours Sample Sign In Sheet”. The

“After Hours Sample Sign In Sheet “is located on the front of the ice machine.

i. Date Delivered

ii. Time Delivered

iii. Number of Ice Chests

iv. Delivered By

v. Condition of Samples: e.g. on ice

vi. Contact Person: Must provide name of employee (sampler or manager) who can

be contacted next business morning in case of troubleshooting

vii. Contact Person Extension or Cell Phone Number

viii. Comments: e.g. Sample Location, Project name


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4. Complete sample COC(s) and place them in the designated folder, on the ice machine,

labeled “Sample Chains.”

5. Complete and apply custody seal(s) to each of the sample coolers, across the seam of the

lid and cooler.

i. Security tags are located on the side of the ice machine.

6. Place each of the sample cooler(s) in one of the designated lockers. Then secure the door

by hinging closed the bottom and top hasps. Finally attaching the provided keyed lock to

the door in a locked position.

7. Samples will be retrieved and accessioned by SSDM staff at the beginning of the next

business day. Account for this time lag with regards to analytical holding times.

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