Quality Assurance Project Plan 

for the Chlorine and 

Chlorinated Hydrocarbons 

Analytical Data Review and Validation 

 Prepared for: 

U.S. Environmental Protection Agency 

Engineering and Analysis Division 

Office of Water 

1200 Pennsylvania Avenue, NW 

Washington, DC 20460 

Prepared by:

Eastern Research Group, Inc.

14555 Avion Parkway 

Suite 200 

Chantilly, VA 20151-1102 

June 2009 

EPA Contract No. 68-C2-095 

Work Assignment 5-18 

iii

TABLE OF CONTENTS 

Page 

1.0 INTRODUCTION ..................................................................................................... 1-1 

2.0 PROJECT MANAGEMENT ELEMENTS ..................................................................... 2-1 

2.1 Element A.3: Distribution List ................................................................. 2-1 

2.2 Element A.4: Project Organization ......................................................... 2-2 

2.3 Element A.5: Problem Definition/Background ....................................... 2-5 

2.3.1 Statement of Key Questions and Project Outcome ...................... 2-5 

2.3.2 Background .................................................................................. 2-6 

2.4 Element A.6: Project/Task Description .................................................. 2-8 

2.5 Element A.7: Quality Objectives and Acceptance Criteria ..................... 2-9 

2.6 Element A.8: Special Training/Certification ........................................ 2-14 

2.7 Element A.9: Project Documents and Records ...................................... 2-15 

3.0 DATA GENERATION AND ACQUISITION ................................................................. 3-1 

3.1 Element B.3: Sample Handling and Custody .......................................... 3-1 

3.2 Element B.4: Analytical Methods ............................................................ 3-2 

3.3 Element B.5: Quality Control .................................................................. 3-2 

3.4 Element B.6: Instrument/Equipment Testing, Inspection, and 

Maintenance ............................................................................................. 3-2 

3.5 Element B.7: Instrument/Equipment Calibration and Frequency ............ 3-3 

3.6 Element B.10: Project Data Management ................................................ 3-3 

4.0 ASSESSMENT AND OVERSIGHT ELEMENTS ............................................................ 4-1 

4.1 Element C.1: Assessments and Response Actions .................................. 4-1 

4.1.1 Technical Support ........................................................................ 4-1 

4.1.2 Analytical Data Review ............................................................... 4-2 

4.1.3 Corrective Action ......................................................................... 4-2 

4.2 Element C.2: Reports to Management ..................................................... 4-3 

5.0 DATA VALIDATION AND USABILITY ELEMENTS ................................................... 5-1 

5.1 Elements D.1 and D.2: Data Review, Verification, and Validation ........ 5-1 

5.2 Element D.3: Reconciliation with User Requirements ............................ 5-2 

6.0 REFERENCES ......................................................................................................... 6-1 

Attachment 1: DATA REVIEW PROCEDURES 
iv 

LIST OF TABLES 

Page 

1-1 Chemicals in the Chlorine and Chlorinated Hydrocarbon Manufacturing Segment1-3 

2-1 QAPP Distribution List ........................................................................................ 2-2 

2-2 Standard Analytical Methods and Procedures ................................................... 2-16 

3-1 Typical Database Structure .................................................................................. 3-5 
v 

LIST OF FIGURES 

Page 

2-1 ERG CCH Data Review and Validation QA Organization ................................. 2-3 
Section No. 1 

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1.0 INTRODUCTION

 ERG is providing technical support to the U.S. Environmental Protection Agency 

(EPA) to evaluate the potential revision of effluent limitations, guidelines, and standards (ELGs) 

for facilities that manufacture chlorine and chlorinated hydrocarbons (including polyvinyl 

chloride (PVC)). EPA refers to the manufacturers of chlorine and chlorinated hydrocarbons as 

the Chlorine and Chlorinated Hydrocarbon (CCH) manufacturing segments. CCH 

manufacturing involves the production of the chemicals listed in Table 1-1. 

 EPA is collecting information and data regarding the sources and characteristics 

of discharges from CCH manufacturing. EPA is conducting a sampling program to collect: 1) 

wastewater characterization data and 2) wastewater treatment technology/pollution prevention 

performance data. EPA will use these data in combination with other CCH data to evaluate 

pollution prevention and treatment of CCH wastewater. 

 As directed by Work Assignments 2-18, 3-18, and 4-18 of Contract No. 68-C02-

095, ERG prepared several Quality Assurance Project Plans (QAPPs) to address various parts of 

the CCH technical evaluation. Specifically, ERG has prepared the following QAPPs: 

 Final Quality Assurance Project Plan for the Chlorine and Chlorinated 

Hydrocarbon Sampling Program dated May 4, 2006 and approved June 

14, 2006; 

 Final Quality Assurance Project Plan for the Chlorine and Chlorinated 

Hydrocarbon Sampling Program 2007 Addendum dated July 9, 2007 and 

approved July 9, 2007; 

 Draft Quality Assurance Project Plan for the Technical Portion of the 

Chlorine and Chlorinated Hydrocarbons Manufacturing Segments 

Effluent Guidelines Questionnaire dated November 28, 2006; and 

 Draft Quality Assurance Project Plan for the Chlorine and Chlorinated 

Hydrocarbons Effluent Guidelines Regulatory Support Secondary Data 

Collection and Analysis dated February 28, 2007. 
Section No. 1 

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 EPA is currently working with CCH industry representatives to collect additional 

data to characterize discharges of chlorinated dibenzo(p)dioxin and chlorinated dibenzofuran 

congeners (dioxin and furans) from CCH facilities. Therefore, due to changes in priorities, EPA 

has not approved the Questionnaire and Secondary Data QAPPs since work on these topics has 

been postponed. 

 As directed by a Technical Directive dated January 7, 2008 under Work 

Assignment 5-18 of Contract No. 68-C02-095, ERG prepared this QAPP to address the review 

and validation of analytical data for two CCH sampling episodes (Episodes 6542 and 6543). 

This QAPP is responsive to all applicable elements specified in EPA Requirements for Quality 

Assurance Project Plans (1) and will be used by EPA and ERG. 

 Section 6.0 presents the references cited in this QAPP. Throughout this 

document, each time a reference is cited, a number corresponding to the Section 6.0 listing is 

shown in parentheses. 
Section No. 1 

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Table 1-1. Chemicals in the Chlorine and Chlorinated Hydrocarbon Manufacturing 

Segment 

International Union of Pure and Applied Chemistry 

(IUPAC) Name Common Name 

Chlorinated Paraffins 

Chlorine Chlorine 

Chlorobenzene Monochlorobenzene 

2-Chlorobutadiene Chloroprene 

1-Chlorobutane Butyl Chloride 

Chloroethane Ethyl Chloride 

1-Chlorohexane Hexyl Chloride 

Chloromethane Methyl Chloride 

Chloromethyl Benzene Benzyl Chloride 

1-Chloro-2-methylpropene Methyl Allyl Chloride 

1-Chloropropane n-Propyl Chloride 

3-Chloro-1-propene Allyl Chloride 

Chlorotoluene o,m,p-Chlorotoluene 

1,2-Dichlorobenzene o-Dichlorobenzene 

1,3-Dichlorobenzene m-Dichlorobenzene 

3,4-dichloro-1-butene 

1,4-dichloro-2-butene 

1,1-dichloro-2-chloroethylene Trichloroethylene 

1,1-Dichloroethane Ethylidene Chloride 

1,2-Dichloroethane Ethylene Dichloride 

1,1,-Dichloroethene Vinylidene Chloride 

1,2-Dichloroethene Acetylene Dichloride 

Dichloromethane Methylene Chloride 

1,1-Dichloropropane Propylidene Chloride 

1,2-Dichloropropane Propylene Dichloride 

1,3-Dichloropropane Trimethylene Dichloride 

2,2-Dichloropropane Dimethyl-dichloromethane 

1,2-Dichloropropene 1,2-Dichloropropylene 

Hexachlorobenzene (HCB) Amatin 

Hexachlorobutadiene Perchlorobutadiene 

Hexachlorocyclopentadiene Perchlorocyclopentadiene 

1,1,1,2,2,2-Hexachloroethane Hexachloroethane 

Monochloroethylene Vinyl Chloride 

1,2,3,4,5-Pentachlorobenzene Pentachlorobenzene 

Pentachloroethane Ethane pentachloride 

Polyvinyl Chloride Polyvinyl Chloride 
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Table 1-1 (Continued) 

International Union of Pure and Applied Chemistry 

(IUPAC) Name Common Name 

1,2,3,4-Tetrachlorobenzene Tetrachlorobenzene 

1,1,1,2-Tetrachloroethane Chloromethyltrichloromethane 

1,1,2,2-Tetrachloroethane Acetylene Tetrachloride 

1,1,2,2-Tetrachloroethylene Perchloroethylene 

trans-1,4-Dichloro-2-butene trans-2-Butylene Dichloride 

Trichlorobenzene Trichlorobenzene 

1,1,2-Trichloroethane Vinyl Trichloride 

Trichloromethane Chloroform 

1,2,3-Trichloropropane Allyl trichloride 

1,2,3-Trichloropropene Trichloropropene 
Section No. 2 

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2.0 PROJECT MANAGEMENT ELEMENTS

 This section addresses project management, including project history and 

objectives, roles and responsibilities, and project goals. In addition, this section presents the 

mechanisms EPA and ERG will use to ensure that all participants understand the goals and the 

approach to be used for the CCH data review and validation. EPA has identified nine elements 

to be discussed in this section. 

 A.1: Title and Approval Sheet; 

 A.2: Table of Contents; 

 A.3: Distribution List; 

 A.4: Project Organization; 

 A.5: Problem Definition/Background; 

 A.6: Project/Task Description; 

 A.7: Quality Objectives; 

 A.8: Special Training/ Certification; and 

 A.9: Project Documents and Records. 

Elements A.1 and A.2 have been provided earlier in this document. The remaining elements are 

presented below. 

2.1 Element A.3: Distribution List

 Table 2-1 presents the distribution list for this data review and validation QAPP. 

As additional ERG staff members are required to participate in the project, ERG will notify the 

EPA WAM. 
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Table 2-1. QAPP Distribution List 

Organization Role 

US EPA/OW EPA QA Coordinator 

US EPA/OW EPA Work Assignment Manager 

US EPA/OW EPA Alternate Work Assignment Manager 

US EPA/OW EPA Project Officer 

ERG ERG Program Manager 

ERG ERG Work Assignment Manager 

ERG ERG Lead for Data Review and Validation 

ERG ERG Project QA Coordinator 

ERG ERG Senior Chemists 

2.2 Element A.4: Project Organization

 Figure 2-1 shows the project organization for the CCH data review and validation. 

Under EPA Contract No. 68-C02-095, ERG is providing technical support to EPA to evaluate 

and potentially revise discharge regulations for CCH operations. Under this contract, ERG 

conducted two sampling episodes in July 2007 (Episodes 6542 and 6543) following the 

procedures outlined in the site-specific sampling plans and the Final Quality Assurance Project 

Plan for the Chlorine and Chlorinated Hydrocarbon Sampling Program (2) and Final Quality 

Assurance Project Plan for the Chlorine and Chlorinated Hydrocarbon Sampling Program 2007 

Addendum (3). This document describes ERG’s procedures for reviewing and validating the 

results of chemical analysis of samples collected in Episodes 6542 and 6543 to ensure their 

quality for use in CCH technical analyses. This document will be used in conjunction with the 

guidelines and standard operating procedures described in ERG’s Draft Data Review Procedures 

for Office of Water Effluent Guidelines Sampling Data (Data Review Plan) (Attachment 1). 
ERG Data 

Lines of Communication Review StaffReporting and Authority

ERG

Work Assignment

Manager

ERG

Data Review Lead

ERG

Program

Manager

ERG

Project QA

Coordinator

EPA

Work Assignment

Managers

EAD QA 

Coordinator

ERG Data 

Lines of Communication Review StaffReporting and Authority

ERG

Work Assignment

Manager

ERG

Data Review Lead

ERG

Program

Manager

ERG

Project QA

Coordinator

EPA

Work Assignment

Managers

EAD QA 

Coordinator

Figure 2-1. ERG CCH Data Review and Validation QA Organization 
Section No. 2 

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 A Senior Chemical Engineer, will serve as ERG’s Work Assignment Manager 

(WAM). The ERG WAM will be responsible for ensuring the project staff follows this QAPP. 

The WAM is also responsible for all management and administrative aspects of the work 

performed and for ensuring that the quality of work, schedule, and budget meet the requirements 

of the CCH effluent guidelines project. The ERG WAM will be the principal contact for the 

EPA WAM on data review tasks, issues, deliverables, and schedule. The ERG WAM will also 

keep the Project QA Coordinator and the ERG Program Manager advised of any quality 

problems that arise. 

 The ERG Project QA Coordinator is responsible for developing and executing 

ERG’s QA activities throughout the course of the data review task. Additional details on ERG’s 

project QA organization can be found in ERG's April 2007 Quality Management Plan (a 

successor to the June 2002 Quality Management Plan for Technical Support for the Strategy for 

National Clean Water Industrial Regulations) (4). ERG's QMP details the responsibilities of the 

ERG Quality Assurance (QA) coordinators and Project Management Team and describes 

procedures used to plan, implement, and assess project quality. 

 A Senior Analytical Chemist will serve as ERG’s lead for the data review and 

validation task and will oversee ERG laboratory and data review staff in conducting this work. 

Senior ERG chemists will perform the data review. 

 As additional ERG staff are required to participate in this project, ERG will notify 

the EPA WAM. The ERG WAM will ensure that any new staff members receive a copy of this 

QAPP. Additional details on ERG’s project QA organization can be found in the QMP, Section 

1.2 Project Organization and Staff Responsibilities (4). 
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2.3 Element A.5: Problem Definition/Background

 This subsection explains the primary purpose of the CCH sampling program, 

provides background information on the sampling program, and a describes the data review that 

will be performed for Episodes 6542 and 6543. 

2.3.1 Statement of Key Questions and Project Outcome 

 The sampling program included the collection of in-process wastewater sampling 

points to characterize the CCH processes and paired influent and effluent sampling points to 

evaluate CCH pollution prevention and treatment techniques. The CCH sampling program will 

evaluate end-of-pipe or in-process pollutant control technologies that may reduce dioxin 

discharges. The analytical results from the CCH sampling program will support EPA in 

answering the following key questions: 

 What pollutants are being discharged by CCH operations? 

 What are the sources of dioxin from CCH operations? 

 What are the concentrations and quantities of pollutants currently being 

discharged (i.e., “baseline” concentration)? 

 What is the performance/efficiency of pollution prevention and 

wastewater treatment technologies being used to reduce pollutants 

discharged from CCH operations? 

 The purpose of the data review and validation project is to ensure the results of 

the chemical analyses of samples collected in Episodes 6542 and 6543 are appropriate for use in 

answering the overall project key questions. For the data review, ERG will support EPA in 

answering the following questions: 

 Did the analytical laboratory document the sample receipt and receipt 

conditions properly? 
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 Did the analytical laboratory follow the sample handling and preparation 

procedures specified in the method (e.g., hold times)? 

 Did the laboratory follow method-specific QC requirements (e.g., 

instrument performance and calibration, method blanks, recovery of 

labeled compounds)? 

 Should any data qualifiers be added to the analytical database prior to 

using the results in technical analyses? 

2.3.2 Background 

 Section 304(m) of the Clean Water Act requires EPA to publish a plan every two 

years to establish a schedule for the annual review and revision of effluent guidelines required by 

Section 304(b). During the 2004 annual review, EPA selected the Organic Chemicals, Plastics, 

and Synthetic Fibers (OCPSF) Point Source Category (40 CFR Part 414) for further review 

because it ranked highest in terms of toxic, priority, and nonconventional pollutant discharges 

among all industrial point source categories. One of the pollutants driving the OCPSF pollutant 

discharges in the screening analysis was dioxin. EPA identified the manufacture of ethylene 

dichloride (EDC), vinyl chloride monomer (VCM), and polyvinyl chloride (PVC) as possible 

sources of dioxin and conducted a detailed study of these manufacturing processes in 2004. 

 In addition, because many chlor-alkali operations are collocated with vinyl 

chloride manufacturing, and because these operations discharge significant quantities of 

pollutants, EPA also selected the chlor-alkali industrial segment of the inorganic chemical 

industry for review. Wastewater from chlorine manufacturing via the chlor-alkali process is 

regulated by the Inorganic Chemicals Manufacturing Point Source Category (40 CFR Part 415). 

 During 2005, EPA identified other manufacturing processes for regulatory 

review. First, EPA is including all chlorine manufacturers in the CCH manufacturing segments 

to obtain a complete overview of the chlorine industry. Second, EPA identified several 

additional chlorinated hydrocarbons currently regulated under OCPSF that are manufactured via 

direct chlorination, oxychlorination, and dehydrochlorination. Because their manufacturing 
Section No. 2 

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processes may also discharge toxic pollutants, EPA is including manufacturing of these 

chlorinated hydrocarbons in the project scope. Chlorinated hydrocarbon manufacturing that is 

regulated under the Pesticide Chemicals Manufacturing (40 CFR Part 455) and Pharmaceutical 

Manufacturing (40 CFR Part 439) Point Source Categories are not included in the CCH 

manufacturing segments. In summary, the scope of this regulatory review project includes all 

chlorine manufacturers and manufacturers of the chlorinated hydrocarbons listed in Table 1-1. 

 Although the CCH manufacturing segments were selected for potential revision 

primarily due to high levels of dioxin discharged, EPA will also evaluate other pollutants that 

contribute significantly to the overall pollutant discharge, such as chlorine, metals, 

polychlorinated biphenyls, and other organic pollutants. 

 ERG supported EPA in planning and executing a CCH sampling program in 2006 

and 2007. The sampling program comprised five sampling episodes at four different facilities. 

ERG developed site-specific sampling plans to serve as the primary source of procedural 

information and as guides for the field sampling crew and facility personnel. 

 In 2007, EPA conducted two-day sampling episodes at two facilities that 

manufacture EDC and VCM (Episodes 6542 and 6543). At each facility, EPA collected samples 

of the influent to and the effluent from the plant’s wastewater treatment system and of several 

intermediate points within the system. The samples were collected as manual composites 

comprising six aliquots. The six aliquots were composited to create one representative sample 

for each 24-hour time period. Details for the sampling episodes are site-specific and are 

confidential business information (CBI). See Section 2.6 for information on ERG’s CBI 

handling procedures. 

 ERG will document information and data collected during all five episodes in 

sampling episode reports (SERs) and the data will be used by EPA and ERG in conducting 

additional technical analyses. The SERs are considered CBI. 
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2.4 Element A.6: Project/Task Description

 Prior to use in the SER and technical analyses, results of chemical analyses of the 

wastewater samples must be reviewed for completeness, comparability, precision, accuracy, and 

sensitivity. For the first three sampling episodes, EPA provided ERG with analytical data that 

had already undergone QC review. For the next two sampling episodes (Episodes 6542 and 

6543), ERG has outlined procedures it will use to conduct the data quality review in the Data 

Review Plan (Attachment 1). This QAPP will be used in conjunction with the Data Review Plan 

to assess the quality of the results of chemical analyses received from the laboratories for these 

two episodes. 

 ERG has received electronic data packages consisting of Microsoft® Excel 

spreadsheets containing the analytical results and documentation packages consisting of traffic 

reports and sample receipt information, laboratory analysis sheets and checklists, instrument 

data, and analyte chromatograms, where applicable. ERG will review, verify, and validate the 

chemical results and supporting documentation provided by the laboratory using method-specific 

checklists. The checklists provide the method-specific QC objectives for each parameter in the 

review (e.g., acceptable instrument signal to noise ratio, use of correct spiking concentration, 

acceptable recovery ranges). Each checklist contains the following standard sections that list the 

detailed criteria ERG will use to verify and validate the results of chemical analyses: 

 General Review of Sample Identity and Handling – ERG will use Sections 

A and B of the checklist to verify sample identity and traceability. ERG 

will confirm that all data required for the data review, verification, and 

validation are contained in the laboratory data package and will review 

information in the data package to verify that the laboratory identified and 

handled samples properly; 

 Review of General QC Requirements – ERG will use Sections C and D of 

the checklist to evaluate the common QC requirements in all methods 

which include sample preparation and extraction procedures; and 

 Detailed Review of Method-Specific Parameters – ERG will use Sections 

E through H of the checklists to perform method-specific QC validation 
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which includes reviewing the primary instrument calibrations and 

performance evaluation samples. 

 ERG will provide a completed checklist for each sample number and each analyte 

in the final analytical data review, verification, and validation package. ERG will also provide a 

data review narrative that summarizes the results documented in the checklist for each group of 

compounds shown in Table 2-2 at the end of this section. Project documentation will be 

discussed in greater detail in Section 3.6. 

2.5 Element A.7: Quality Objectives and Acceptance Criteria

 The QA objectives for the collection of the samples were documented in sitespecific sampling plans, the Sampling QAPP, and 2007 Sampling QAPP Addendum. The 

primary objective of the data review is to assess whether the results from chemical analyses from 

Episodes 6542 and 6543 are of the quality necessary for use in developing effluent guidelines for 

this industry. This QAPP, the Data Review Plan, and the method-specific checklists document 

the procedures for the quality review. ERG will review the results of chemical analyses and the 

supporting documentation provided by the laboratory to assess the completeness, comparability, 

precision, accuracy, and sensitivity of the data. 

 

Completeness 

 Completeness for Episodes 6542 and 6543 is defined in terms of the percentage of 

samples collected, analyzed, and deemed to be acceptable for use in this study. Completeness is 

assessed in three different areas and is defined as follows: 

 Sampling completeness is the number of samples collected and received in the 

laboratory relative to the number of samples planned for collection; 

 Analytical completeness is the number of valid sample measurements relative to 

the number of samples collected; and 
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 Overall completeness is the number of valid sample measurements relative to the 

number of samples planned for collection. 

 The number of samples planned for collection is documented in the site-specific 

sampling plans and any deviations are noted in the sampling episode reports. The traffic reports 

list all the samples that were sent to the laboratory for analysis. 

 This project goal is a minimum of 90% for both sampling and analytical 

completeness and a minimum of 81% for overall completeness (determined by multiplying 

sampling and analytical completeness goals). Completeness may also be evaluated in terms of 

subsets of samples (e.g., completeness for influent samples versus completeness for effluent 

samples). 

 ERG will use Sections A and B of the method-specific checklists to verify 

analytical completeness. 

Comparability 

 Comparability is a qualitative measure of the confidence with which datasets can 

be compared. This project will ensure data comparability by following approved, standard 

analytical procedures and by reporting the results in the standard units of measure required in the 

methods. ERG will use Sections C and D of the method-specific checklists to document data 

comparability. ERG will check that all data were generated with the appropriate method, the 

laboratory followed the procedures for sample handling and sample preparation/extract handling 

listed in the method, and the results were reported using the standard units required by the 

method. 
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Precision 

 Precision is a measure of the agreement among repeated measurements. To 

evaluate precision, the laboratories calculate the relative percent difference (RPD) among the 

results from one or more types of “duplicate” analyses using the following equation: 

100

S D

S D RPD 



 







 

where: 

RPD = Relative percent difference; 

S = First sample result; and 

D = Duplicate sample result. 

 Laboratories use the results of duplicate analyses to evaluate the precision of their 

operations. Laboratories often use matrix spike (MS) /matrix spike duplicate (MSD) samples to 

evaluate both precision and accuracy. 

 Table 2-2 (located at the end of this section) presents the analytical methods used 

for samples collected in these two episodes. The method-specified QC limits for duplicate 

precision will serve as the DQO for this project. If the method does not contain QC limits for the 

RPD value, the RPD should not exceed 20 percent. This is not intended to be a required 

precision, but to be a target. ERG will use Section H of the checklist to validate laboratory 

performance evaluation samples in terms of precision. 

Accuracy 

 Accuracy is a measure of the agreement between a measured value and a 

reference or “true” value. Because the “true” concentration of an analyte in a field sample is 

never known, spiked samples (e.g., a matrix spike (MS)) are used to evaluate accuracy. 

Laboratories prepare an MS sample by adding known amounts of the compounds of interest to 

the field sample. The spiked samples receive the same handling, extraction, cleanup, and 
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analysis steps as the field samples. The laboratories then perform a percent recovery (%R) 

calculation to determine their accuracy: 

100

SA

SSR -SR Percent Recovery 



 



 

where: 

SSR = Spiked sample result; 

SR = Sample result; and 

SA = Spike added. 

 The successful evaluation of accuracy depends on the choice of spiking 

concentration. To determine the appropriate spiking concentration for the MS sample, the 

laboratory must first analyze the original sample. In general, the spiking concentration must be 

at least twice the concentration of the analyte present in the original sample, and ideally, should 

be no more than ten times that concentration. 

 The QC limits for the recovery of spiked analytes for most of the analytical 

methods listed in Table 2-2 (located at the end of this section) will serve as the DQO for this 

project. These limits are based primarily on method validation studies using matrices as treated 

effluents from wastewater treatment plants. If the method does not specify percent recovery, it 

should be between 50 and 150 percent. This is not intended to be a required percent recovery, 

but to be a target. 

In addition to MS/MSD sample, the laboratory analyzes a laboratory blank, which 

consists of reagent water or “clean matrix” material that does not contain the analytes of interest 

or interfering compounds. ERG will review laboratory blank results to verify the absence of 

contamination originating at the laboratory. 

 ERG will use Section H of the checklist to validate laboratory performance 

evaluation samples to validate the accuracy of the results of chemical analyses. 
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Sensitivity 

 Sensitivity is the ability of the method or instrument to detect the target analytes 

at the level of interest (method or instrument detection limit). Sensitivity can be evaluated using 

the following: 

 Method Detection Limits - A method detection limit (MDL) is defined as 

the minimum concentration of a substance that can be measured and 

reported with 99 percent confidence that the analyte concentration is 

greater than zero. For organics and metals analytical methods, 

laboratories are required to perform MDL studies for each instrument with 

which analyses will be performed and any time a modification is made 

that will effect the MDL. Laboratories must demonstrate that they obtain 

an MDL value that is less than or equal to either of the following: (1) the 

MDL (if listed in the method) or (2) one-third the minimum level (if listed 

in the method). Appendix B of 40 CFR Part 136 describes the EPA 

procedure used for establishing MDLs. 

 

ERG was not responsible for selecting analytical laboratories or reviewing 

MDL studies. For methods that have MDL studies, ERG will review the 

laboratory-supplied MDL or reporting limit to ensure the laboratories’ 

MDL meets the method requirements. ERG will not evaluate MDLs for 

classical pollutants. 

 Aqueous Performance Standard - To assess laboratory performance and 

evaluate error sources in the laboratory, the laboratory prepares an 

aqueous performance standard (ongoing precision and recovery (OPR)) 

sample by adding known amounts of the analytes of interest to a matrix 

with known characteristics. Reagent water is usually used as the reference 

matrix. The laboratory processes the standard through all sample 

preparation and analysis steps and evaluates analyte recoveries against 

method specific limits. 

ERG was not responsible for selecting analytical laboratories or verifying 

the selected laboratories are qualified through a certification process or 

through the use of performance evaluation samples. 

 Instrument Calibration Check Standard - To ensure that the instrument 

calibration remains in control, the laboratory performs a calibration check 

standard by adding analytes of interest to a laboratory reagent blank over a 

range of concentrations as required by the method. Analyte recoveries are 

evaluated using limits specified in the applicable method. 
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ERG will verify that the laboratory performed appropriate initial 

calibration and periodic calibration checks by reviewing criteria in listed 

in Section E of the checklists. 

 Surrogates and Internal Standards for Organic Analyses - Organic analysis 

methods that have solvent extraction steps require the use of surrogate 

compounds or, in the case of isotope dilution methods, isotopically labeled 

analogue compounds to monitor extraction efficiency and extract handling 

procedures. Because these steps can greatly impact the recovery of the 

target analytes, the laboratories must monitor these steps carefully to 

ensure data quality. The applicable methods specify the surrogate and 

isotope compound recovery limits, based on method validation study 

results. 

 ERG will compare the reported recovery of the isotopically labeled compounds 

by reviewing criteria in listed in Sections F and G of the checklists. 

2.6 Element A.8: Special Training/Certification

 All information and data collected via this sampling program has been claimed 

CBI by the CCH facilities. ERG did not use site names or sample point descriptions when 

transmitting samples to the analytical laboratories. The analytical results received from the lab 

are not CBI because the results are identified only by episode number, sampling point number, 

and Sample Control Center (SCC) number. ERG data review staff will not have access to CCH 

CBI data for this task and therefore do not need to be trained in handling CBI. ERG has handled 

CBI for other portions of the CCH project under Work Assignment 5-18 of Contract 68-C2-095. 

All ERG staff that have access to CBI have been trained in CBI handling procedures as outlined 

in ERG’s CBI security plan entitled Security Plan for Handling Confidential Business 

Information Under the Clean Water Act, dated March 5, 2004 and approved by Ahmar Siddiqui, 

EPA’s Document Control Officer for this contract, on March 19, 2004 (5). 
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2.7 Element A.9: Project Documents and Records

 ERG has developed and instituted document control mechanisms for reviewing, 

revising, and distributing QAPPs. Each QAPP has a signed approval form, title page, table of 

contents, and EPA-approved document control format (see header that appears at the top of each 

page in this QAPP). 

 Table 2-1 presents the distribution list for this QAPP. During the course of the 

project, any revision to the QAPP will be circulated to everyone on the distribution list. 

 Section 5 of ERG’s QMP (4) presents standard controls for project-related data, 

documents, and records. ERG’s WAM is responsible for designating an individual to maintain 

all project files. All information collected, generated, and analyzed on the project is handled and 

stored in a centralized record, as described in the Chlorine and Chlorinated Hydrocarbons 

Project File Management Plan, dated May 16, 2005 (6). This centralized record contains all 

information collected or accessed from other sources, documents the analytical data review, and 

documents analyses of any data collected (e.g., site visit reports, sampling plans, sampling 

episode reports, laboratory data packages). The contents of the record are indexed using a 

Microsoft® Access database. 

 Management of project data is specifically described in Element B.10, Data 

Management (Section 3.6). 
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Table 2-2. Standard Analytical Methods and Procedures 

Method Number Title Method Type 

Classicals 

EPA 160.2 Total Suspended Solids (TSS) Gravimetric 

EPA 160.1 Total Dissolved Solids (TDS) Gravimetric 

EPA 300.1, Rev 2.1 Sulfate Colorimetric, Gravimetric, 

or Turbidimetric 

EPA 300.1, Rev 2.1 Chloride Colorimetric or Titrimetric 

EPA SM2320 B Alkalinity Colorimetric or Titrimetric 

EPA SM5210 B Carbonaceous Biochemical Oxygen Demand (CBOD5) 5 day; DO Depletion 

EPA SM5210 B Biochemical Oxygen Demand (BOD5) 5 day; DO Depletion 

EPA 410.4, Rev 2 Chemical Oxygen Demand (COD) Colorimetric or Titrimetric 

EPA SM5310 C Total Organic Carbon (TOC) Combustion or Oxidation 

Metals

EPA 200.7, 245.1 Total Metals – 27 Element Quantification 

Mercury 

ICP and GFAA 

Organics 

EPA 1624C Volatile Organic Compounds GC/MS 

EPA 1625C Semivolatile Organic Compounds GC/MS 

Other 

EPA 1668A Chlorinated Biphenyls Congeners by Isotope Dilution HRGC/MS 

EPA 1613B Tetra- Through Octa-Chlorinated Dioxins and Furans by 

Isotope Dilution 

HRGC/MS 

GC/MS: Gas chromatography with mass spectrometry. 

HRGC/MS: High resolution gas chromatography with mass spectrometry. 

GFAA: Graphite furnace atomic adsorption. 

ICP: Inductively coupled plasma. 

CVAA: Cold vapor atomic adsorption. 

GC/FID: Gas chromatography with flame ionization detection. 
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3.0 DATA GENERATION AND ACQUISITION

EPA’s sample collection procedures were documented in the site-specific sampling 

plans, Sampling QAPP, and 2007 Sampling QAPP Addendum. The site-specific sampling plans 

include the following: 

 EPA’s criteria for selecting the CCH facility for sampling; 

 Samples to be collected (number of samples and location); 

 Sample collection procedures (manual composites or grabs); 

 Analytes for each sampling point; 

 Analytical methods; 

 Sample handling and preservation requirements; and 

 Collection of QC samples. 

 EPA has identified 10 elements to be discussed related to data generation and 

acquisition (1). Most of these elements were covered by the Sampling QAPP and 2007 Sampling 

QAPP Addendum. This section discusses the following elements that pertain to the analytical data 

review, verification, and validation for Sampling Episodes 6542 and 6543: 

 B.3: Sample handling and custody; 

 B.4: Analytical methods; 

 B.5: Quality control; 

 B.6: Instrument/equipment testing, inspection, and maintenance; 

 B.7: Instrument/equipment calibration and frequency; and 

 B.10: Project data management. 

3.1 Element B.3: Sample Handling and Custody

 During the data review, ERG will compare documentation for sample receipt to the 

actual handling of the sample once received in the laboratory to ensure all method requirements 

were met. ERG data review checklists include items pertaining to storage requirements and 

sample hold time requirements to verify the laboratory’s sample handling procedures and 

documentation (Sections B and C). 
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3.2 Element B.4: Analytical Methods

 Table 2-2 at the end of Section 2.0 lists the analytical methods that EPA used in 

Episodes 6542 and 6543. ERG will verify that the laboratory followed all method-specified 

requirements and document the findings in the method-specific checklists. The attached Data 

Review Plan contains the method checklists. 

3.3 Element B.5: Quality Control

 EPA’s data generation quality control procedures were documented in the sitespecific sampling plans, Sampling QAPP, and 2007 Sampling QAPP Addendum. For the data 

review, verification, and validation, ERG will review the laboratory data packages to ensure that 

proper laboratory quality control procedures were followed. ERG will document the results of the 

laboratory QC review in the method-specific checklists and final data review narrative. Section 2.5 

discusses the quality objectives and acceptance criteria for the data review project. 

3.4 Element B.6: Instrument/Equipment Testing, Inspection, and Maintenance

 The laboratories selected to analyze samples must perform preventive maintenance 

on all of their analytical equipment. Equipment maintenance log books must contain records of 

equipment usage, maintenance, modifications, calibrations, and repairs. If data on supplies 

acceptance testing or equipment maintenance is provided in the laboratory documentation package, 

ERG will review the information to determine if any procedures would affect sample analysis data 

quality. 

 ERG will review the laboratory data packages to determine if the laboratories used 

the appropriate equipment, preparation material, columns (if applicable), and detectors during the 

analysis of each sample. If so supplied, ERG will review the instrument/equipment maintenance 

records to ensure the equipment was properly maintained throughout its operation including 
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verification that calibrations follow major changes in instrument configuration or maintenance 

events. 

3.5 Element B.7: Instrument/Equipment Calibration and Frequency

 The laboratories selected to analyze samples are responsible for performing all 

required instrument calibrations. Instrument calibration procedures, including frequency 

specifications and maintenance requirements, are specified in the analytical methods and in the 

laboratory contracts. Whenever changes are made to a system or a method, the laboratory must 

ensure that its equipment is operating properly by performing the appropriate QC tests. Analytical 

instruments requiring calibration must be uniquely identified to allow proper association of 

calibration records. 

 To ensure that the calibration standard is met, the laboratory must analyze test 

samples that are either certified as to purity, concentration, and authenticity, or prepared from 

materials of known purity and composition. ERG will verify that calibration measurements were 

performed and/or verified with calibrated systems at the specified frequencies by reviewing the 

criteria listed in Section E of the method-specific checklists. 

3.6 Element B.10: Project Data Management

 ERG has received electronic data packages of the results of chemical analyses for 

Episodes 6542 and 6543 from EPA. For each episode and each analyte group listed in Table 2-2 

(classicals, metals, organics, and other analytes), the data package contains a Microsoft® Excel 

spreadsheet containing the chemical analysis results and a portable document format (PDF) file 

containing the supporting laboratory documentation (e.g., traffic reports, laboratory checklists, 

instrument calibration information). ERG will use the electronic data package to conduct the 

analytical data review, verification, and validation. 
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 ERG will document the results of the analytical data review using method-specific 

checklists and a data review narrative as follows: 

 Method-specific checklists – ERG will provide a completed method-specific 

checklist for each sample number or range of sample numbers for each 

analyte; and 

 Data review narrative – ERG will provide a data review narrative for each 

analyte group) which will summarize the results of the data review, 

verification, and validation. The data review narrative will also include a 

discussion of any data qualifiers and the reason for the qualifier. The data 

qualifiers that will be used in this project are discussed in Section 5.1. 

 After reviewing the data, ERG will post the analytical results including any data 

qualifiers on the EPA mainframe computer. Table 3-1 lists the elements in the analytical database. 

ERG will check that all data provided by the laboratory in Microsoft® Excel spreadsheet format is 

transferred to the EPA mainframe computer. 
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Table 3-1. Typical Database Structure 

Field Description Field Name Source of Data

Analyte Concentration AMOUNT Laboratory, in same order as chemical name 

Analyte Name ANALYTE Laboratory 

CAS Registry Number CAS_NO Laboratory 

Calculated Detection Limit DETLIMIT Laboratory, in same order as chemical name 

Episode Number EPISODE Upper right corner of Traffic Report 

Laboratory Name LABNAME Laboratory 

Column or Extraction Type PROCEDUR Laboratory 

Reason for Qualification REASON Laboratory(a) 

Sample Number SAMPLE Traffic report 

Data Qualifier QUAL ERG 

Concentration Units UNIT Laboratory, in mg/L or as specified in method or laboratory contract 

Laboratory Method Used METHOD Laboratory 

CAS - Chemical Abstract Service. 

(a) A “greater than” sign (>) will be the qualifier (QUAL) when the corresponding reason (REASON) is “sample 

result is greater than the upper calibration range.” 
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4.0 ASSESSMENT AND OVERSIGHT ELEMENTS

 This section describes the methods ERG will use to assess the quality of the 

analytical data collected for Episodes 6542 and 6543 of the CCH sampling program. 

4.1 Element C.1: Assessments and Response Actions

 This subsection describes the technical review, audits, and corrective actions that 

will be performed on the CCH project. ERG will not conduct audits of laboratory systems and 

procedures during this project. 

4.1.1 Technical Support 

 All work conducted by ERG on Work Assignment 5-18 for the analytical data 

review will be subject to technical review. As discussed in Section 1.3.4 of the QMP (4), 

technical review is a documented critical review of work that has been performed within the 

“state of the art.” A senior chemist at ERG will complete method-specific checklists and create 

review narratives to document the analytical data review, verification, and validation. Dr. Ray 

Merrill will review the final data review narrative. If incomplete data packages are received or if 

questions develop that impact ERG’s ability to perform the data review, ERG’s senior chemist 

will forward a request to the ERG WAM and QA coordinator, who will notify the EPA WAM 

about the issue. 

 Ms. Betsy Bicknell will serve as the Project QA Coordinator for this project. To 

assess the implementation of QA/QC procedures on this project, she will: 

 Review this QAPP for completeness and applicability. 

 Audit project files to ensure project staff have developed QC procedures 

and are using these procedures. 
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 At any time or at the end of the project or work assignment, Ms. Bicknell, or her 

designee, may inspect the project QA files. 

4.1.2 Analytical Data Review 

 At the completion of each data review, the ERG Project QA Coordinator will 

review records of activities and will evaluate the following elements: 

 Overall level of organization and professionalism; 

 Compliance with all procedures outlined in this QAPP; and 

 Completeness of documentation (i.e., method-specific checklists and data 

review narratives). 

 The ERG Project QA Coordinator will discuss any deficiencies with the project 

team and identify any necessary corrective actions. If any of these deficiencies may potentially 

affect the use of the analytical data for technical analyses, the ERG Project QA Coordinator will 

immediately inform the EPA and ERG WAMs, so that any corrective actions can be taken. 

4.1.3 Corrective Action 

 ERG will review all laboratory data generated from Sampling Episodes 6542 and 

6543 for accuracy and precision, completeness, representativeness, and comparability to ensure 

that the quality objectives and criteria discussed in Section 2.5 of this QAPP have been met. 

ERG will report any deficiencies in the laboratory reports to the EPA WAM. ERG will not 

contact the laboratories or take corrective action to modify or change the data. ERG will 

document any recommended data qualifiers in the data review narrative and post the qualifiers to 

EPA’s computer mainframe as discussed in Section 5.1. 
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4.2 Element C.2: Reports to Management

 ERG will append this QAPP as required. ERG will inform the EPA WAM of the 

progress of all data review activities through the semimonthly and monthly written reports 

required under Work Assignment 5-18. 

 Any quality deficiencies detected by the ERG data review chemists or the Project 

QA Coordinator will be communicated, in writing, to the EPA WAM. The ERG WAM is 

responsible for ensuring that appropriate corrective action is taken and reported to the Project 

QA Coordinator. In addition, as required by Work Assignment 5-18, ERG will provide quality 

assurance updates to the EPA WAM on a quarterly basis. 
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5.0 DATA VALIDATION AND USABILITY ELEMENTS

 This section describes data review, verification, and validation. It also discusses 

how EPA will evaluate data to determine if it is acceptable for use in answering the questions 

posed in Section 2.3.1. 

5.1 Elements D.1 and D.2: Data Review, Verification, and Validation

 This subsection discusses the procedures used for the data review, verification, 

and validation. ERG will review sample analysis results for completeness, comparability, 

precision, accuracy, and sensitivity as outlined in Section 2.5. ERG will perform the following 

steps in conducting the data review: 

1. Obtain laboratory data package from EPA. 

2. Verify all required samples have an analytical result and were handled 

properly by the laboratory using method-specific checklist sections A 

through C. 

3. Validate chemical analysis results using method-specific checklist sections 

D through H. 

4. Complete method-specific checklists for all sample numbers. 

5. Determine if any data qualifiers are required (see discussion below). 

6. Summarize the results of the review in a data review narrative. 

7. Transfer method-specific checklists and data review narratives to the EPA 

WAM. 

 

8. Resolve EPA comments on the method-specific checklists and data review 

narratives. 

9. Upload the data to the EPA mainframe computer. 
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Data Qualifiers 

 ERG will add qualifiers to the analytical database to notify users of the data about 

particular data quality issues. Only two qualifiers will be added directly into the Data Qualifier 

field (QUAL) in the analytical database on EPA’s mainframe computer as appropriate: 

1. Result represents a maximum (add ‘>’) – Laboratory dilutions may be 

necessary when there are sample matrix interferences or when levels of an 

analyte in a sample exceed the calibration range. ERG will verify that all 

samples are within the method-specified calibration range. If not (a 

sample should have been diluted to bring a result into the calibration range 

and the laboratory data package contains no documentation explaining the 

reason), ERG will consider these data as the upper limit of the calibration 

range and will enter a ‘>’ in the QUAL field for that analyte. 

2. Result should be excluded (add ‘EXCLUDE’) – In some cases the data 

will be considered unusable due to gross QC deficiencies or failures. ERG 

will enter ‘EXCLUDE’ in the QUAL field for that analyte. Some 

instances where data may be excluded are: 

— QC is missing or grossly outside limits (e.g., 0 percent recovery); 

— Statements in the laboratory narrative that indicate there were 

matrix problems that interfere with identification or quantitation; 

— Statements in the laboratory narrative that indicate that the 

identification or quantitation of the data may be questionable; 

— High levels of target analyte contamination in the blank associated 

with the samples; and 

— Analyte was not detected in any spiked samples (MS/MSD and 

OPR). 

Any other qualification of the data will be discussed in the data review narratives and will not be 

flagged in the analytical database. 

5.2 Element D.3: Reconciliation with User Requirements

 The data collected during the CCH sampling program can be used to answer the 

questions posed in Section 2.3.1 by clearly identifying the presence (concentrations of pollutants 

above the analytical method minimum level) or nonpresence (concentrations of pollutants below 
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the analytical method detection level) of analytes in the sampled wastewater. ERG will perform 

the analytical data review to ensure that the laboratory results meet the method-specified quality 

control objectives and are suitable for use in answering the overall project key questions. For 

this data review project, ERG will provide a narrative describing the quality of the data and their 

fit for use in developing effluent guidelines for the CCH manufacturing segment. 
Section No. 6 

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6.0 REFERENCES

1. U.S. Environmental Protection Agency. EPA Requirements for Quality 

Assurance Project Plans QA/R-5. EPA/240/B-01/003. Office of Environmental 

Information. March 2001. 

2. Eastern Research Group, Inc. Final Quality Assurance Project Plan for the 

Chlorine and Chlorinated Hydrocarbon Sampling Program. May 2006. 

3. Eastern Research Group, Inc. Final Quality Assurance Project Plan for the 

Chlorine and Chlorinated Hydrocarbon Sampling Program 2007 Addendum. 

July 2007. 

4. Eastern Research Group, Inc. Quality Management Plan. April 2007. 

5. Eastern Research Group, Inc. Security Plan for Handling Confidential Business 

Information Under the Clean Water Act. Revision 1. March 5, 2004. 

6. Eastern Research Group, Inc. Chlorine and Chlorinated Hydrocarbons Project 

File Management Plan. May 2005. 
Attachment 1 

DATA REVIEW PROCEDURES 
Data Review Procedures for Office of Water 

Effluent Guidelines Sampling Data 

Prepared for:

U.S. Environmental Protection Agency

Engineering and Analysis Division 

Office of Water 

1200 Pennsylvania Avenue, NW 

Washington, D.C. 20460 

Prepared by: 

Eastern Research Group, Inc.

14555 Avion Parkway 

Suite 200 

Chantilly, VA 20151-1102 

March 2009 

EPA Contract No. 68-C-02-095 

Work Assignment 5-18
ii

TABLE OF CONTENTS 

Page 

1.0 BACKGROUND.......................................................................................................1-1 

2.0 DATA QUALITY REVIEW GOALS ...........................................................................2-1 

3.0 DATA REVIEW PLAN.............................................................................................3-1 

3.1 General Review of Sample Identity and Handling ..................................3-2 

3.2 Review of General QC Requirements......................................................3-2 

3.3 Detailed Review of Method-Specific Parameters....................................3-3 

3.3.1 Dioxins and Furans (Method 1613B) ..........................................3-4 

3.3.2 Total Suspended Solids (TSS) (Method 160.1) ...........................3-5 

3.3.3 Volatile and Semivolatile Organic Compounds (Methods 1624C 

and 1625C)...................................................................................3-7 

4.0 DATA REVIEW SUMMARIES ..................................................................................4-1 

5.0 RECOMMENDATIONS AND BUDGET.......................................................................5-1 

Appendix A: DATA REVIEW CHECKLISTS 
iii

LIST OF TABLES 

Page 

2-1 Data Package Detail Expected for Project Categories......................................... 2-3 

5-1 Number of Samples by Method for CCH Analytical Data Review..................... 5-2 
1-1

1.0 BACKGROUND

 EPA is considering possible revision of the national effluent guidelines 

regulations for the chlorine and chlorinated hydrocarbon (CCH) manufacturing segments. 

Currently, wastewater discharges from chlorinated hydrocarbon manufacturing are subject to the 

Organic Chemicals, Plastics, and Synthetic Fibers (OCPSF) Point Source Category (40 CFR Part 

414) and wastewater discharges from chlor-alkali manufacturing of chlorine are subject to the 

Inorganic Chemicals Point Source Category (40 CFR Part 425). Both of these industries have 

been identified as discharging significant quantities of toxics as represented by “toxic weighted 

pound equivalents” (TWPEs). Of particular concern is the quantity and toxicity of dioxin 

discharges in treated effluent. 

 EPA is collecting information and data regarding the sources and characteristics 

of discharges from CCH manufacturing. As part of the evaluation, EPA is conducting a 

sampling program to 1) obtain wastewater characterization data and 2) obtain wastewater 

treatment technology and pollution prevention performance data. EPA will use the analytical 

data from the sampling program in combination with other CCH data to evaluate possible 

pollution prevention and treatment options for these wastewaters. 

 In 2007, EPA conducted two, two-day sampling episodes at CCH manufacturing 

facilities (Episodes 6542 and 6543). At each facility EPA collected samples at the influent to 

and effluent from the plant’s wastewater treatment system and several intermediate points within 

the system. The samples were collected as manual composites in which six aliquots were 

collected for each sampling point approximately four hours apart. The six samples were 

composited to create one sample representative of a 24-hour time period. Samples for dioxins 

and furans, polychlorinated biphenyls (PCBs), and volatile organic hydrocarbons (VOAs) were 

composited at the analytical laboratory. 

 ERG will document information and data collected during these episodes in 

sampling episode reports (SERs), which will be used by EPA and ERG in conducting additional 

technical analyses. Prior to using the data in the SER and technical analyses, the analytical data 

received from the laboratories must undergo a quality control (QC) review to ensure the 
1-2

completeness, representativeness, and accuracy of the laboratory results. This document outlines 

procedures that can be used by ERG’s measurements group to complete the laboratory quality 

review. ERG’s measurements group, located in Research Triangle Park, North Carolina, 

performs analytical data review for various media (e.g., air, water, waste). This group has 

actively supported EPA’s measurements and data review needs since 1986. 
2-1

2.0 DATA QUALITY REVIEW GOALS

 The Quality Assurance Project Plan for the Chlorine and Chlorinated 

Hydrocarbons Sampling Program dated May 4, 2006 lists the following key questions that will 

be addressed by the CCH sampling program: 

• What pollutants are being discharged by CCH operations? 

y What are the sources of dioxin from CCH operations? 

y What are the concentrations and quantities of pollutants currently being 

discharged (i.e., “baseline” concentration)? 

y What is the performance/efficiency of pollution prevention and 

wastewater treatment technologies being used to reduce pollutants 

discharged from CCH operations? 

All data collected must be reviewed to qualify it for use in answering these questions. In 

addition, data collected may be reviewed by interested stakeholders and compared to split 

samples collected by industry during each sampling episode. 

 The end use of the laboratory data determines the extent of QC and quality 

assurance (QA) review. Implementation of a “one size fits all” approach to quality requirements 

is not appropriate. Implementation of the EPA Quality System1 is based on the principle of a 

“graded approach” since this approach allows quality systems and quality plans for different 

programs to vary according to the specific objectives and needs of the organization or project. In 

EPA’s Requirements for Quality Assurance Project Plans2

, EPA recommends that QA and QC 

activities applied to a project be sufficient for: 

y The purpose of the environmental data operation (e.g., enforcement, 

research and development, rulemaking); 

y The type of work to be done (e.g., pollutant monitoring, site 

characterization, risk characterization, bench level proof of concept 

experiments); and 

 

1

 For more information on EPA’s Quality System, see http://www.epa.gov/QUALITY/. 2

 See EPA Requirements for Quality Assurance Project Plans (March 2001), available online at 

http://www.epa.gov/QUALITY/qs-docs/r5-final.pdf. 
2-2

y The intended end use of the results (e.g., compliance determination, 

selection of remedial technology, development of environmental 

regulation). 

 EPA offices specify project categories based on the intended end use of the data 

collected.3 The following describes typical QC requirements:

y Category 1: Projects defined as a study to generate data used for 

enforcement activities, litigation, or some research projects involving 

human subjects. The Quality Assurance Project Plan (QAPP) for category 

1 projects must address all elements listed in EPA Requirements for 

Quality Assurance Project Plans.

4

y Category 2: Project defined as a study to generate data used in support of 

the development of environmental regulations or standards. The QAPP 

for category 2 must address all elements listed in EPA Requirements for 

Quality Assurance Project Plans.

5

y Category 3: An applied research project defined as a study to generate 

data to demonstrate the performance of accepted processes or technologies 

under defined conditions. These studies are often pilot- or field-scale. 

 

y Category 4: A basic research project defined as a study to generate data 

used to evaluate unproven theories, processes, or technologies. These 

studies are often bench-scale. 

QA/QC data supporting each of these categories is provided with different levels of detail. 

Based on the key questions listed in the CCH QAPP, the CCH analytical data would be classified 

as Category 2 data since EPA may use the data to develop regulations or characterize the 

performance of various treatment technologies. Table 2-1 shows the typical review steps 

included for each of the project categories. As shown in Table 2-1, Category 2 projects should 

receive a Level 3 data review. 

 

3

 See http://www.epa.gov/ORD/NRMRL/qa/guide/qadocsformsplanning.htm 4

 See EPA Requirements for Quality Assurance Project Plans (March 2001), available online at 

http://www.epa.gov/QUALITY/qs-docs/r5-final.pdf. 
2-3

Table 2-1. Data Package Detail Expected for Project Categories 

Quality Review 

Procedure 

Category 1 

Projects 

Category 2 

Projects 

Category 3 

Projects 

Category 4 

Projects 

Screening Level Data 

Review: 

Review of traffic reports, 

sample handling, and 

proper sample preparation 

9 9 9 9

Level 2 Data Review: 

Screening level review 

plus a review of sample 

QA/QC results 

9 9 9

Level 3 Data Review: 

Level 2 review plus 

review of instrument 

performance 

9 9 

Level 4 Data Review: 

Level 3 review plus 

analysis of raw data such 

as chromatograms or 

primary instrument output 

9 
3-1

3.0 DATA REVIEW PLAN

 The CCH project will use analytical data that must be of known quality for 

technical analyses. Prior to each sampling episode, EPA developed a detailed sampling plan that 

lists the number of samples collected for each sampling point and analyte, detailed sample 

collection procedures including preservation requirements, QA samples collected, and sample 

tracking and shipping procedures. Laboratories send detailed data packages to EPA which can 

include: an analytical narrative discussing exceptions or QC irregularities, a list of the samples, 

the traffic reports for the samples, and method-specific information such as initial method 

calibration, continuing quality control results, other quality control measures, sample results, and 

raw instrument data. This section outlines ERG’s plan for reviewing the packages received from 

the laboratories to ensure they are of sufficient quality for use in CCH technical analyses. 

 ERG uses standard review procedures and detailed method-specific checklists to 

review laboratory data packages. Appendix A contains the method-specific checklists. ERG 

will complete a detailed, method-specific checklist for each sample set and provide specific 

information for individual samples, as needed. For example, ERG will review all samples 

analyzed by the laboratory for a single calibration in a valid sequence that includes calibration 

and sample results. 

 Each data review consists of three major stages which are described in the 

following sections: 

y Section 3.1 describes the general procedures for verifying sample identity 

and traceability; 

y Section 3.2 describes the general QC for sample handling and preparation; 

and 

y Section 3.3 describes the method-specific QC requirements. 

ERG will review data for each sample and summarize the results. Section 4.0 of this plan 

describes the overall data review summaries that ERG will prepare. 
3-2

3.1 General Review of Sample Identity and Handling 

 Sections A and B of the detailed review forms are common to all analytical 

methods and are fundamental to the identity and traceability of the sample. These sections are 

described below: 

y SECTION A: Data Package Contents and Sample Identifiers. Each 

sampling episode data package needs to identify samples and include 

sufficient data for the data review to ensure the quality of the results can 

be determined. Items for this part of the check list include laboratory 

name, EPA project name, sampling episode number, sample identification 

number (SCC number), ERG data reviewer signature, and date. The data 

reviewer will perform an initial check to confirm that all the data required 

for the review is in the data package. Section A-2 provides a table of 

contents for the review checklist and notes which requirements are 

applicable for each of the review categories discussed in Section 2.0. 

y SECTION B: Traffic reports. Traffic reports are the link between the 

field sampling information and the laboratory analysis. Traffic report 

forms are generated with every set of samples sent to a laboratory for 

analysis. The traffic report is the source of the data identifiers necessary 

to track the origin of the samples. Items for the check list include assuring 

completeness of the sample receipt records, receipt date, sample 

identification numbers, sample receipt temperature, and condition. 

3.2 Review of General QC Requirements

 Sections C and D of the review forms evaluate the common QC requirements in 

the methods. All methods include specifications for sample hold time and preparation/extraction 

of samples. 

y SECTION C: Sample Handling Information. Sample shipments 

received by a laboratory are checked for proper container use, preservation 

and hold time. The initial hold time check ensures samples were not held 

in the field past their expiration date making the analysis results invalid. 

Hold time prior to extraction is determined from the day of collection to 

the day samples are processed by extraction. ERG will determine if 

sample results are invalid due to improper preservation or excessive hold 

time prior to extraction. 

y SECTION D: Sample Preparation and Extract Handling Information. 

ERG ensures that samples were stored at the appropriate temperature as 
3-3

specified by the method. ERG also checks the validity of the analysis hold 

time. The analysis hold time is measured from the time of 

preparation/extraction of the samples by the laboratory to the time of 

sample analysis. 

3.3 Detailed Review of Method-Specific Parameters 

 Sections E through I are reserved for the detailed review of method-specific 

parameters. Method-specific QC involves reviewing the primary instrument calibration and 

performance measures. At a minimum, these reviews typically include verification of equipment 

calibration, blank preparation, spiking procedures, and assessment of field QA samples from the 

sampling episode. Classical parameters, such as total suspended solids (TSS), are measured 

following simple calibration, blank, and spike procedures, and typically require only the 

minimum review components. Reviews for higher level instrumental techniques, such as toxic 

metals or specific organic compound methods, typically involve evaluation of the response and 

recovery of unique and/or labeled analytes as a key indicator of method performance. Several 

methods also require laboratories to provide data on initial precision and accuracy to demonstrate 

their ability to perform the requested analysis on a sample in a “clean” matrix. 

 For example, in Method 1613B, the isotopic dilution method for dioxins and 

furans, isotopically labeled carbon compounds are spiked into all samples. The recovery of the 

labeled compounds must meet initial precision and recovery (IPR) method specifications. ERG 

will also review ongoing precision and recovery (OPR) QC data from the data package to 

determine if the laboratory performance met method requirements during the sample analysis 

period. If OPR results do not meet method requirements, the data review for this sample series 

will indicate data quality for sample analysis could be compromised. 

 The following list presents the analytical methods used for CCH Sampling 

Episodes 6542 and 6543: 

y Classical Parameters 

— Total Suspended Solids (TSS) EPA Method 160.2 (Gravimetric) 

— Total Dissolved Solids (TDS) EPA Method 160.1 (Gravimetric) 

— Sulfate 300.0 EPA Method Rev 2.1 (Colorimetric, Gravimetric, or 

Turbidimetric) 
3-4

— Chloride EPA Method 300.0 Rev 2.1 (Colorimetric or Titrimetric) 

— Alkalinity SM2320B (Colorimetric or Titrimetric) 

— Biochemical Oxygen Demand (BOD) SM5210B (5 day; DO 

Depletion) 

— Chemical Oxygen Demand (COD) EPA Method 410.4, Rev 2 or 

HACH 8000 (Colorimetric or Titrimetric) 

— Total Organic Carbon (TOC) SM5310B or SM5310C 

(Combustion or Oxidation) 

y Total Metals Methods 

— Total Metals – 27 Element Quantitation EPA Method 200.7 (ICP 

and GFAA) 

— Mercury Method 245.1 

y Major Organics Group Methods and Data Review 

— Volatile Organic Compounds (VOC) EPA Method 1624C (isotope 

dilution GC/MS) 

— Semivolatile Organic Compounds EPA Method 1625C (isotope 

dilution GC/MS) 

y Specific Organic Class Methods and Data Review 

— Chlorinated Biphenyls Congeners (PCBs) EPA Method 1668A 

(isotope dilution HRGC/MS) 

— Tetra- Through Octa-Chlorinated Dioxins and Furans (D/F) EPA 

Method 1613B (isotope dilution HRGC/MS) 

The following subsections summarize the method-specific QC requirements for some of the high 

priority analytes for the CCH sampling program. These methods include analysis of dioxins and 

furans (Method 1613B), total suspended solids (Method 160.1), and major organic group 

methods (1624C and 1625C). Appendix A contains the checklists for all methods. 

3.3.1 Dioxins and Furans (Method 1613B) 

 This section summarizes the method-specific QC requirements for Method 

1613B. Details are provided in Sections E through I of the attached detailed checklist (see 

Appendix A). Completion of Sections E through H correspond to a Level 3 data review and 

completion of Section I is included in a Level 4 data review (see Table 2-1). The analysis of 

dioxin and furan congeners includes the following QC procedures: 

y Instrument performance (Section E-1) and calibration (Section E-2): 

Laboratories must provide documentation of the instrument performance 
3-5

and calibration. Data reviewers must verify that the instrument used for 

the analysis has a sufficient resolution, measures the correct ion 

abundance ratios and retention times for labeled and unlabeled compounds 

in the calibration standard, that calibration standards were prepared 

correctly, and that the recovery of labeled compounds falls within the 

method-specified parameters. 

y Method Blanks (Section E-3): Laboratories must provide information 

about the preparation of method blanks analyzed with the sample set. 

Reviewers must verify that the laboratories used the correct procedures to 

prepare the blanks and spike the clean matrix samples with the correct 

concentrations of surrogates. In addition, 1600 series methods require 

analysis of OPR samples spiked with labeled and unlabeled compounds. 

y Recovery of Labeled Compounds (Section F) and Instrument Recovery of 

Internal Standards (Section G): The amount of labeled compounds 

recovered from spiked samples must be within the method-specified limit. 

y Performance Evaluation (QA) Samples (Section H): If QA samples (e.g., 

field duplicates or equipment field blanks) are submitted with the sample 

set, and the QAPP specifies requirements for QA sample results, then 

ERG will determine if results of QA samples meet the QAPP 

specifications. 

y Detailed Raw Data Review – Compound Identification (Section I): 

Reviewers will verify that the relative retention times, signal-to-noise 

ratios, ion abundance ratios, and valley heights are within the methodspecified parameters for identifying a compound. This review is 

performed to identify interferences, errors in specific congener 

identification, and unusual treatment of the data. 

3.3.2 Total Suspended Solids (TSS) (Method 160.1) 

 TSS is a measure of the retained material on a standard glass fiber filter after 

filtration of a well-mixed sample. The determination is a gravimetric measurement of the 

residue dried to a constant weight at 103 to 105°C. This method is applicable to drinking, 

surface, and saline waters as well as domestic and industrial wastes over a range of 4 to 

20,000 mg/L. Samples high in filterable residues may be subject to positive interference. 

 The internal quality control procedures for TSS by EPA Method 160.1 include: 

y Verification of Equipment, Calibration, and Lab Environment: 
3-6

— Is the drying oven temperature recorded and between 103 to 

105°C? Is the oven temperature recorded and correct for the 

method? 

— Is a desiccator with active color indicator recorded ? 

— Is the balance make and model recorded and capable of weighing 

to 0.1 mg? Does the report indicate the analytical balance been 

serviced and calibrated within the last year? Is the balance 

checked with “S” class weights? 

— Are suitable filter holders and filtering apparatus referenced and in 

use? 

y Verification of Preparation Procedures: 

— Is there a record of filters dried at 103 to 105°C for 1 hour before 

use? 

— Is the filter drying done until a constant weight is achieved? 

— Are filters stored in a desiccator, after preparation until needed? 

y Verification of Analytical Procedure and Record Keeping: 

— Are the filters weighed immediately before use? 

— Is the filter placed wrinkle side up in the filtering apparatus? 

— Is the sample brought to room temperature before analysis? 

— Are non representative particles (e.g., leaves and sticks) excluded 

from the sample? 

— How soon are samples analyzed after collection? 

— Do sample volume or filter size selected to yield between 10 and 

200 mg of total residue? 

— Are temperature and humidity recorded for the weighing facility? 

— Is the start weight recorded on a bench sheet? 

— Is the sample volume recorded on the bench sheet? 

— Is the final weight of the crucible and dry sample recorded on the 

bench sheet? 

— Are the oven times written on the bench sheets? 

— Are calculations shown on the bench sheets? 

— Are the analyst’s initials recorded? 

— Are the sample date and the analysis date recorded? 

— Does the analytical balance check agree within 0.5 mg of known 

weight? 

y Verification of Performance Evaluation Samples: 

— Are the method blanks (MBs) less than one tenth the sample 

results? 

— Are the relative percent difference of duplicate sample (DUP) less 

than 20% for samples >5X the method detection limit? 

— Have one set per of mineral reference samples been analyzed per 

batch of samples? Are the results within ±15% from expected 

concentration? 
3-7

3.3.3 Volatile and Semivolatile Organic Compounds (Methods 1624C and 1625C) 

 Methods 1624C and 1625C are used to determine the volatile and semivolatile 

toxic organic pollutants associated with the Clean Water Act (as amended 1987); the Resource 

Conservation and Recovery Act (as amended in 1986); the Comprehensive Environmental 

Response, Compensation, and Liability Act (as amended in 1986); and other compounds 

amenable to either: 

y Purge and trap gas chromatography/mass spectrometry (GCMS) for 

Method 1624C; or 

y Extraction and analysis by capillary column gas chromatography-mass 

spectrometry (GCMS) for Method 1625C. 

The chemical compounds may be determined in waters, soils, and municipal sludges by the 

methods. The detection limits of the methods are usually dependent on the level of interferences 

rather than instrumental limitations. 

 Each laboratory that uses Methods 1624C and 1625C is required to operate a 

formal QA program. The minimum requirements of this program consist of an initial 

demonstration of laboratory capability, analysis of samples spiked with labeled compounds to 

evaluate and document data quality, and analysis of standards and blanks as tests of continued 

performance.5

 Low resolution mass spectrometric analysis of organic compounds involves the 

addition of surrogate compounds that must be measured with acceptable recovery for analyses to 

be validated. Laboratory performance is compared to established performance criteria to 

determine if the results of analyses meet the performance characteristics of the method. 

 

 Detailed quality control and quality assurance requirements are listed in Section 8 

of Methods 1624C and 1625C. The checklists for Methods 1624C and 1625C include: 

 

5

 If the method is to be applied routinely to samples containing high solids with very little moisture (e.g., soils, filter 

cake, compost), the high solids reference matrix is substituted for the reagent water in all performance tests, and the 

high solids method is used for these tests. The CCH samples are not expected to have high levels of solids. 
3-8

y Verification of initial precision and accuracy, including verification that 

recoveries of compounds in standards fall within the method-specified 

ranges; 

y Verification of spiked compound recoveries; 

y Verification that records maintained by the lab are adequate to define that 

quality of the data; 

y Verification of method blanks including method blank preparation and 

results of analysis; 

y Verification of equipment calibration; and 

y Analysis of field QA samples. 
4-1

4.0 DATA REVIEW SUMMARIES

 The level of detail for the data quality review should be based on a graded 

approach that varies according to the intended end use of the data. The end use of the data is 

described in Section 2.0 of this report and is defined during the planning and preparation of the 

QAPP. The amount and sophistication of data review should depend on the data available and 

the Category of the project (Table 2-1). If the data qualifiers fail at any stage of the data review, 

the reviewer may recommend not proceeding with the next stage of data review. The levels of 

data review are summarized below. As stated in Section 2.0 and shown in Table 2-1, CCH is a 

Category 2 project and Levels 1 through 3 are required. ERG will start with the Level 1 review 

and work through to Level 3. 

y Level 1 – Perform Screening Review of Sample Receipt and 

Condition. This level of review is applicable for data that are intended for 

screening purposes (e.g., determining the presence or absence of a target 

or surrogate). 

y Level 2 – Evaluate Sample Receipt and Condition Plus Basic QA/QC 

Review. This level of review is applicable to data that are used to 

characterize process performance and is used to determine if the data 

adequately represent the process. Basic QC at Level 2 includes findings 

about sample condition on receipt, storage, stabilization, preparation and 

QC spiking requirements. 

y Level 3 – Evaluate Instrument Performance and ongoing QC . This 

level of review is applicable for data that are intended for use in regulatory 

development or compliance certification. Level 3 review includes review 

of the data for compliance with all sections of the method-specific 

checklist except raw data review. 

y Level 4 – Evaluate Raw Data. This level of review is applicable for data 

used in enforcement and litigation activities or for research projects 

involving human subjects. Since CCH is a Category 2 project, this stage 

of review is not recommended and not described in this section. Level 4 

review includes review of the data for compliance with all sections of the 

method specific checklist. 

 ERG’s data review reports will include a narrative summary and findings of all 

areas where the QC does not meet the QAPP or method requirements. No data will be discarded, 

rather each data review narrative will include a sufficient summary for data users to decide if the 
4-2

data can be used for its design purpose(s). At all levels of data review, the resulting report will 

summarize the findings and identify what quality criteria have not been met. 

 ERG will provide a narrative discussion describing potential limitations in the 

data quality. The narrative discussion will include all of the components of a Level 3 data 

review. If the data fail to meet requirements at any level of review, ERG may recommend that 

EPA not proceed to the next level of data review and limit use of the data since the quality can 

not be established. However, ERG expects all data in the CCH program will undergo a Level 3 

data review. Data review findings that results in noncompliance with method requirements (i.e., 

a check list “No” is indicated) will be supported by comments regarding use of the data and the 

appropriate flag that should be entered into the corresponding data base. 
5-1 

5.0 RECOMMENDATIONS 

 ERG recommends the following steps for the CCH analytical data review: 

y Perform Level 1 and Level 2 data reviews for all samples from Episodes 

6542 and 6543. 

y The number of samples for the Level 3 review will be specified by EPA. 

Level 3 data review is not necessary for 100 percent of the samples 

because laboratories follow the same protocols during sample analysis, 

and as a result, typically will make the same QC mistakes or omissions for 

all samples. However, if data will be used in court hearings for legal 

decisions, EPA may decide that a more thorough review is necessary and 

request that the Level 3 review include up to 100 percent of the samples. 

y ERG does not recommend a review of the instrumental data or hand 

interpretation of the mass spectra since the procedures for analysis are 

documented and QA/QC for the procedures are well established (Level 4 

review). 

Table 5-1 lists the number of samples for the data quality review for the two episodes. 
5-2 

Table 5-1. Number of Samples by Method for CCH Analytical Data Review 

Method and Parameters 

Number of 

Samples for 

Episode 6542 

Number of 

Samples for 

Episode 6543 

Classical Parameters 

Method 160.1 - Total Dissolved Solids (TDS) 13 + 1QC 15 + 1QC 

Method 160.2 - Total Suspended Solids (TSS) 13 + 1QC 15 + 1QC 

EPA Method 300.0 Rev 2.1 – Sulfate and Chloride 13 + 1QC 15 + 1QC 

SM 2320B - Alkalinity 13 + 1QC 15 + 1QC 

EPA Method 410.1, Rev2 – Chemical Oxygen Demand (COD) 13 + 1QC 11 + 1QC 

SM 5310B/C – Total Organic Carbon (TOC) 13 + 1QC 11 + 1QC 

SM 5210B – Biochemical Oxygen Demand (BOD5) 13 + 1QC 9 + 1QC 

Total Metals 

EPA Methods 200.7, 200.8, and 200.9 – Total Metals 13 + 1QC 11 + 1QC 

EPA Method 245.1 - Mercury 13 + 1QC 11 + 1QC 

Major Organics Group Methods 

EPA Method 1624C – Volatile Organic Compounds (VOCs) 9 9 

EPA Method 1625C – Semivolatile Organic Compounds 7 7 

Specific Organic Class Methods 

EPA Method 1668A – Chlorinated Biphenyl Congeners (PCBs) 5 5 

EPA Method 1613B – Dioxin and Furan Congeners 14 18 
Appendix A 

DETAILED DATA REVIEW CHECKLISTS
Laboratory Name:______________ CCH Episode #.:___________ Method 160.1 – Page 1 of 3 

OW Effluent Guidelines Data Review Checklist 

Total Dissolved Solids (TDS) Method 160.1 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

 Record reviewer comments in the Reviewer Comment section. 

 Record detailed information in the “Comments and Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. Overall Method Total Dissolved Solids Data Package Checklist 

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 1 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

1 

Results Summary for Each Sample and Blank 1, 2, 3 

Initial Calibration Data 1,2 

Copies of Sample Preparation Work Sheets 1,2,3 

Copies of Analysis Run Logs 1,2 

1. COMPLIANCE SCREENING (ERG Sections A through D)-- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through E)-- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through E)-- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks. 
Laboratory Name:______________ CCH Episode #.:___________ Method 160.1 – Page 2 of 3 

Criterion Met

EPA METHOD for Total Dissolved Solids Reviewer Comment Y N 

SECTION B. Sample Receipt, Traffic Report

1. Sample Receipt Record: Signatures Complete? 

2. Receipt Date: Entered by Analysis Laboratory? 

3. Receipt Temperature: Storage temperature <4°C but not 

frozen. Correct receipt temperature indicated? 

4. Condition (Breakage?/Leakage?) 

SECTION C. Sample Handling Information

1. Sample container: Was the correct sample container used?

[Method specifies glass or plastic] 

2. Maximum holding time: Were the samples held for 7 days 

or less? 

SECTION D. Sample Preparations/Filtration and Drying Information

1. Were the samples stored at 6°C but not less then 0°C? 

2. Was the drying oven operated at 180°C? (7.2) 

3. Was desiccant type noted in report? If so, was a desiccator 

with active color indicator used? Was desiccant active? 

 

4. Were suitable filter holders and filtering apparatus in use? 

(7.1) 

 

5. Were the filters prewashed three times with 20 mL of 

distilled water? (7.1) 

6. Were evaporating dishes dried at 180 or 550°C for 1 hour 

before use? (7.2) 550°C is required when volatile residue is 

also to be determined. (TSA information may not be part of 

data pkg.) 

 

7. Were the evaporating dishes stored in a desiccator, after 

drying until needed? (TSA information may not be part of 

data pkg.) 

 

8. Was the sample well mixed prior to filtration? 

9. Was the filter rinsed three times with 10 mL portions of 

distilled water? (TSA information may not be part of data 

pkg.) 

 

10. Was the sample brought to room temperature before 

analysis? (TSA information may not be part of data pkg.) 

 

11. Was the desicator drying cycle repeated until a constant 

weight is achieved or weight loss is less than 4% of the 

previous weight or less than 0.5 mg between successive 

weighing? 

 

12. Was a sample volume selected to yield between 1.0 and 200 

mg of total non-filterable residue? 

 Sample Volume Effluent: 

 Influent: 

 
Laboratory Name:______________ CCH Episode #.:___________ Method 160.1 – Page 3 of 3 

Criterion Met

EPA METHOD for Total Dissolved Solids Reviewer Comment Y N 

SECTION E. Instrument Parameter Review

SECTION E-1. Analysis QC Information – 

1. Were the analyst’s initials recorded with the data? 

2. Was an example calculation shown in the narrative or 

supporting data sheets? Calculation performed correctly? 

mg TDS/L = (weight of dried residue - weight of evaporating dish (g)) x 1000

 L of sample used 

 

3. Was the temperature and humidity of the laboratory or 

weighing room recorded? 

 

4. Was the tare weight of the drying dish reported? 

5. Was the sample volume recorded in the proper units? 

6. Was the final weight of the drying dish dry sample 

recorded? 

 

7. Were the oven-drying times reported? 

Was the evaporated residue dried for at least one hour at 180 

±2°C for at least 1 hour? 

 

8. Was there a record that the analytical balance was zeroed 

and leveled prior to each weighing? 

 

9. Was desiccant kept inside the balance to maintain humidity 

control in the balance? 

10. Was the oven temperature checked for proper setting and 

stability and the temperature recorded? 

11. Was the oven thermometer immersed in a sand bath or other 

suitable thermal mass? 

12. Did the desiccator have a good seal? (vacuum or grease) 

SECTION E-2. QC Information – Instrument Calibration

13. Was the balance checked with “S” class weights? 

(100 mg, 1g, and 100g) 

14. Has the analytical balance been serviced and calibrated 

within the last year? Date: _______________ 

SECTION E-3. QC Information – Method Blanks, Duplicates, Reference Samples

15. Was a blank water (method blank) value reported? 

(One per batch or Sample Delivery Group, 1 per 20 samples 

minimum) Is the blank water value >0.5 mg. 

 

16. Was a duplicate sample reported? (One per batch or Sample 

Delivery Group (1 per 20 Samples minimum) RPD <20% 

for samples > 5X required DL, ± required DL for samples 

<5X DL 

 

17. Was a reference sample result reported? (One mineral 

reference sample per batch or delivery group, 1 per 20 

samples minimum) (criteria ± 15% from expected value) 

 
Laboratory Name:______________ CCH Episode #.:___________ Method 160.2 – Page 1 of 4 

OW Effluent Guidelines Data Review Checklist 

Total Suspended Solids (TSS) Method 160.2 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

 Record reviewer comments in the Reviewer Comment section. 

 Record detailed information in the “Comments and Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. Overall Method Total Suspended Solid Data Package Checklist 

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 1 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

1 

Results Summary for Each Sample and Blank 1, 2, 3 

Initial Calibration Data 1,2 

Copies of Sample Preparation Work Sheets 1,2,3 

Copies of Analysis Run Logs 1,2 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through E) -- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through E) -- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks. 
Laboratory Name:______________ CCH Episode #.:___________ Method 160.2 – Page 2 of 4 

Criterion 

Met 

EPA METHOD for Total Suspended Solids Reviewer Comment Y N 

SECTION B. Sample Receipt, Traffic Report

1. Sample Receipt Record: Signatures Complete? 

2. Receipt Date: Entered by Analysis Laboratory? 

3. Receipt Temperature: Storage temperature <4°C but not 

frozen. Correct receipt temperature indicated? 

4. Condition: Breakage?/Leakage? 

SECTION C. Sample Handling Information

1. Sample container: Was the correct sample container used?

[Method specifies glass or plastic] 

2. Maximum holding time: Were the samples held for 7 days 

or less? 

SECTION D. Sample Preparations/Filtration and Drying Information

1. Were the samples stored at 6°C but not less then 0°C? 

2. Was the drying oven operated at 103 to 105°C? (2-54) 

3. Was a desiccator with active color indicator used? (2-54) 

 Was desiccant noted in report? 

 

4. Were suitable filter holders and filtering apparatus in use? 

(2-55) 

5. Were the filters prewashed three times with 20 mL of 

distilled water? (7.1) 

6. Were the filters/Gooch filters dried at 103 to 105°C for 1 

hour before use? (7.1) 

 

7. Were filters/Gooch filters stored in a desiccator, after drying 

until needed? (6.2) 

 

8. Was the filter placed wrinkle side up in the filtering 

apparatus? (7.1) (TSA information may not be part of data 

pkg.) 

 

9. Were the filters seated with a small volume of distilled water 

to create a seal before filtering sample to avoid sample loss? 

(7.1) (TSA information may not be part of data pkg.) 

 

10. Was the sample brought to room temperature before 

analysis? (Standard Methods 2-54) 

 

11. Were non representative particles (e.g. leaves and sticks) 

excluded from the sample? (2-56) 

12. Were samples analyzed as soon as possible after collection? 

(2-53). Method specifies 7 days. Were the sampling date and 

the analysis date recorded? (Were the analysis times 

recorded?) 

 

13. Was the sample well mixed prior to filtration? (7.4) 
Laboratory Name:______________ CCH Episode #.:___________ Method 160.2 – Page 3 of 4 

Criterion 

Met 

EPA METHOD for Total Suspended Solids Reviewer Comment Y N 

14. Was a sample volume or filter size selected to yield between 

1.0 and 200 mg of total non-filterable residue? (7.2) 

 Sample Volume Effluent: 

 Influent: 

 

15. If the filtration time exceeds 5 to 10 minutes, was the 

filtration volume adjusted using the recommended method? 

(7.2) 

 

16. Were filters (if Gooch not used) transferred to an aluminum 

or stainless steel planchet? (Standards Method requirement) 

17. Were the graduated cylinders and filters/Gooch filters 

washed (after sampling) with three successive 10 ml 

volumes of distilled water? (7.5) 

 

18. Were the filters/Gooch filters dried at least 1 hour and 

cooled in the desiccators before final weighing? (7.6) 

SECTION E. Instrument Parameter Review

SECTION E-1. Analysis QC Information – 

1. Were the analyst’s initials recorded with the data? 

2. Was an example calculation shown in the narrative or 

supporting data sheets? Calculation performed correctly? 

mg TSS/L = (weight of filter with residue (g) - weight of filter tare(g)) x 1000

 L of sample used 

 

3. Was the temperature and humidity of the laboratory or 

weighing room recorded? 

 

4. Was the tare weight of the crucible or filter reported? 

5. Was the sample volume recorded? 

6. Was the final weight of the crucible and dry sample recorded 

on the bench sheet? 

 

7. Was the desicator drying cycle repeated until a constant 

weight is achieved or weight loss is less than 4% of the 

previous weight or less than 0.5 mg between successive 

weighing? 

 

8. Were the oven-drying times reported? 

(Method requires 103 to 105 °C) 

 

9. Was there a record that the analytical balance was zeroed 

and leveled prior to each weighing? 

10. Was desiccant kept inside the balance to maintain humidity 

control in the balance? 

11. Was the oven temperature checked for proper setting and 

stability and the temperature recorded? 

12. Was the oven thermometer immersed in a sand bath? (TSA 

information may not be part of data pkg.) 

13. Did the desiccator have a good seal? (vacuum or grease) 

(TSA information may not be part of data pkg.) 
Laboratory Name:______________ CCH Episode #.:___________ Method 160.2 – Page 4 of 4 

Criterion 

Met 

EPA METHOD for Total Suspended Solids Reviewer Comment Y N 

SECTION E-2. QC Information – Instrument Calibration

14. Was the balance checked with “S” class weights? 

(100 mg, 1g, and 100g) 

15. Has the analytical balance been serviced and calibrated 

within the last year? Date: _______________ 

SECTION E-3. QC Information – Method Blanks

16. Was a blank water value reported? 

Was the blank water value >0.5 mg 

 
CCH Study Data Review Checklist 

Chloride and Sulfate EPA Method 300 

(Ion Chromatography-Not for Disinfection Byproducts) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank 1, 2, 3 

Laboratory Fortified Blank Spike Results 1, 2, 3 

Laboratory Fortified Matrix (LFM) (Matrix 

Spike/Duplicate Matrix Spike Recovery Summaries 

1, 2, 3 

Field or Laboratory Duplicate Results 1,2,3 

Instrument Performance Check (Resolution) 2, 3 

Initial Calibration Data 2, 3 

Continuing Calibration Data 2, 3 

Windows Defining Mixture/Column Resolution 

Check 

3 

Selected Chromatograms for Each Sample, Blank, and 

Standard 

3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F)-- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G-2)-- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.

Laboratory Name:________________ CCH Episode #.:_____________ Method 300 – Page 1 of 3 
Criterion met

EPA METHOD 300 REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Receipt Temperature: Storage in the dark at a temperature 

≤6 C. (40 CFR 136 Table II) 

Correct receipt and storage conditions indicated? 

4. Sample Condition: Sample bottle breakage? Sample 

leakage? 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Polyethylene, fluoropolymer, or glass. 

Correct sample container used? 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Sample holding time prior to analysis: 28 days maximum 

recommended for Method A compounds. (300/8.3) Correct 

hold time indicated? 

2. Sample holding time prior to analysis: Immediate analysis 

is recommended for Method B compounds. (300/8.3) Were 

Method B compounds analyzed immediately?

3. Storage conditions: Extract stored between 0 and 4 C. 

Correct storage conditions indicated? 

SECTION E-1. QC INFORMATION – Instrument Performance 

1. Initial Demonstration of Performance, Quality Control 

Sample (QCS): Before sample analysis and on a quarterly 

basis QCS sample must be analyzed. Was recovery of QCS 

targets within ± 15% of the stated values? (300/9.2.2)

SECTION E-2. QC INFORMATION – Instrument Calibration 

2. Initial Calibration (ICAL): Was an initial calibration curve 

with at least three points performed for each analyte? 

(300/10.2.2) 

3. Continuing Calibration Verification (CCV): was the CCV 

calibration standard analyzed prior to analyzing samples, 

blanks? (300/10.5) 

SECTION E-3. QC INFORMATION – Method Blanks 

4. Laboratory Reagent Batch Blanks: Was a blank sample 

analyzed after with each analysis batch? (300/9.3.1) 

Were any of the target compounds or interfering compounds 

found in the blank at > Method Detection Limit (MDL)? 

If so, was analysis stopped and contamination eliminated? 

5. Laboratory Fortified Blank (LFB): Was an LFB analyzed 

with every sample batch or one for every 20 samples (if more 

than 20 samples were analyzed)? (300/10.8)

6. LFB Recovery: Was accuracy as percent recovery within 

the required control limits? (300/9.3.2, 9.4.1.3, 9.3.2.2)

Were ongoing LFB results within control limits (x ± 3S)? 

(300/9.3.2.3) 

7. Laboratory Fortified Sample Matrix (LFM) (MS/MSD): 

Were 10% of field samples per batch fortified at ≥ 5x the 

lowest calibration standard? 

Were LFM recoveries within the 75 to 125 % limit? 

(300/9.4.1.1)

8. Field or Laboratory Duplicates: Were a minimum of 10% 

of the field samples or at least one sample per analysis batch 

Laboratory Name:________________ CCH Episode #.:_____________ Method 300 – Page 2 of 3 
Laboratory Name:________________ CCH Episode #.:_____________ Method 300 – Page 3 of 3 

Criterion met

EPA METHOD 300 REQUIREMENT Reviewer Comment Y N 

analyzed in duplicate? (300/9.4.3)

Do the duplicate analysis meet acceptance criteria (MRL to 

10x MRL then %Diff limited to ±20%, 10% for 10xMRL or 

higher)? (300/9.4.3.2) 

SECTION F. INSTRUMENT PERFORMANCE CHECKS 

1. Continuing Calibration Verification (CCV): Was a CCV 

calibration standard analyzed after every 20 samples and 

whenever the anion eluent was changed? Did the retention 

time and response for each analyte agree withing 10% of the 

original calibration?(300/9.4) 

2. Continuing Calibration Verification Control Limits: Did 

the continuing calibration results meet the method 

requirements? (MRL to 10xMRL 75 – 125% recovery, 

10xMRL and above 85 – 115% recovery) (300/10.5)

3. Interference Check: Did target analyte peaks show 

distortion, shoulders or interference that would interfere with 

accurate calculation of target quantity?

SECTION G-2. DETAILED RAW DATA REVIEW – Sample Results

1. Sample Results: Were the sample results less than five 

times the Method Blank results?

2. Sample Results: Were the sample results at least greater 

than ten times the Method Blank results?

3. Minimum Levels: Were the minimum levels reported by 

the lab comparable to those specified in the method?

4. Duplicate Samples: Were duplicate samples collected? 

Were the RPDs less than 20%?

5. Calculation Check: Was sufficient data provided to 

recalculate a sample result? Does the hand calculated value 

agree with the reported value?
Laboratory Name:________________ CCH Episode #.:_____________ Method 2320B – Page 1 of 3 

CCH Study Data Review Checklist 

Alkalinity EPA Method 2320B 

(Titrimetric) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank 1, 2, 3 

Laboratory Fortified Blank Spike Results 1, 2, 3 

Laboratory Fortified Matrix (LFM) (Matrix 

Spike/Duplicate Matrix Spike Recovery Summaries 

1, 2, 3 

Field or Laboratory Duplicate Results 1,2,3 

Instrument Performance Check (Resolution) 2, 3 

Initial Calibration Data 2, 3 

Continuing Calibration Data 2, 3 

Windows Defining Mixture/Column Resolution 

Check 

3 

Selected Chromatograms for Each Sample, Blank, and 

Standard 

3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F)-- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G)-- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.
Laboratory Name:________________ CCH Episode #.:_____________ Method 2320B – Page 2 of 3 

Criterion met

EPA METHOD 2320B REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Receipt Temperature: Storage at a temperature between 0 

and 6 C. (40 CFR 136 Table II) 

Correct receipt and storage conditions indicated? 

 

4. Sample Condition: Sample bottle breakage? Sample 

leakage? 

 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Polyethylene, fluoropolymer, or glass. 

Correct sample container used? 

 

SECTION D. SAMPLE HANDLING INFORMATION 

1. Sample holding time prior to analysis: Analysis within 14 

days maximum. How soon after collection were samples 

analyzed? (40 CFR 136 Table II)

 

2. Temperature: Was the temperature documented during 

tritation? Was the temperature at 25 ± 2 oC (room 

temperature)?

 

3. Sample alteration: Was the sample filtered, diluted, 

concentrated, or altered in any way during the titration?

 

SECTION E-1. INSTRUMENT PERFORMANCE CHECKS 

1. Reagents: If reagents were prepared by the laboratory, was a 

titration curve constructed for the standardization of the 

reagents?

 

2. Titration Equipment: Was a pH meter, color indicators, or 

an electrically operated titrator used for titration?

 

3. Initial Calibration: Was an initial calibration curve with at 

least three points performed for the pH meter? 

 

4. Buffer Solutions: Were the buffer solutions used for the pH 

meter calibration certified solutions? 

 

5. Calibration Verification: Was the calibration checked with 

a buffer solution routinely while analyzing samples?

 

6. Sluggish response: If the pH meter exhibited a sluggish 

response, was the electrode allowed to reach equilibrium, or 

cleaned between samples (ex. oily samples can leave 

residue)?

 

SECTION E-2. QC INFORMATION – Method Blanks 

7. Indicator Blank: If using color indicators, was an indicator 

blank prepared for each batch of samples? 

 

8. Blank Interference Check: Was any turbidity or interfering 

color in the indicator blank documented?

 
Laboratory Name:________________ CCH Episode #.:_____________ Method 2320B – Page 3 of 3 

SECTION G. DETAILED RAW DATA REVIEW 

1. Low-alkalinity: Alkalinity less then 20 mg CaCO3/L must 

be determined by the low-alkalinity method. Was any 

alkalinity determined to be < 20 mg CaCO3/L. If so, was it 

determined by the low-alkalinity method?

 

2. Alkalinity Calculations: Were the alkalinity and total 

alkalinity calculated according to Method SM 2320B 

Sections 5a and 5b?

 

3. Classifications: Was the phenolphthalein alkalinity not zero 

but less than total alkalinity? Then the alkalinity can be 

classified as carbonate alkalinity.

 

4. Classifications: Was the phenolphthalein alkalinity more 

than half total alkalinity? Then the alkalinity can be 

classified as hydroxide alkalinity.

 

5. Classifications: Was the phenolphthalein alkalinity less 

than half total alkalinity? Then the alkalinity can be 

classified as bicarbonate alkalinity.

 

6. Nomographic Calculations: Were the alkalinity 

relationships calculated nomographically (optional)? If so, 

were the relationships calculated according to Method SM 

2320B Section 5c?

 

7. Phenolphthalein Alkalinity Calculation: Was the 

phenolphthalein alkalinity calculated nomographically 

(optional)? If so, was it calculated according to Method SM 

2320B Section 5c?

 

8. Duplicate Samples: Were duplicate samples collected? 

Were the RPDs less than 20%?

 

9. Calculation Check: Was sufficient data provided to 

recalculate a sample result? Does the hand calculated value 

agree with the reported value?

 
Laboratory Name:________________ CCH Episode #.:__________ SM 5210B Page 1 of 3 

CCH Study Data Review Checklist 

STANDARD METHOD 5210B BOD 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank 1, 2, 3 

Field or Laboratory Duplicate Results 1,2,3 

Initial Calibration Data 2, 3 

Calibration Check Data 2, 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F) -- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through F) -- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.

Criterion 

met

STANDARD METHOD 5210 B Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Receipt Temperature: Storage in the dark at a temperature 

≤6 C. 

Correct receipt and storage conditions indicated? (40 CFR 

 
Laboratory Name:________________ CCH Episode #.:__________ SM 5210B Page 2 of 3 

Criterion 

met

STANDARD METHOD 5210 B Reviewer Comment Y N 

136 Table II) 

4. Sample Condition: Sample bottle breakage? Sample 

leakage? 

 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Polyethylene, fluoropolymer, or glass. 

Correct sample container used? 

 

2. Sample Bottle Volume: Recommended but not required, 

100 mL (liquids). Sample bottle volume indicated? 

 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Sample holding time prior to analysis: Samples analyzed 

within 48 hours of collection? (40 CFR 136 Table II) 

 

2. Storage conditions: Extract stored between 0 and 6 C. 

Correct storage conditions indicated? 

 

3. Sample Stabilization: Are samples checked for chlorine? 

 How? Are samples treated for chlorine with sodium sulfate?

 

4. Sample pH: Is sample pH adjusted to prior to analysis? 

 What pH criteria is used?

 

5. Hydrogen peroxide: Was hydrogen peroxide present in the 

samples? How was hydrogen peroxide treated?

 

6. Analysis Temperature: Are samples equilibrated to 20 ±3 

°C?

 

7. Seeding: Are samples seeded if required? 

8. Seed Source: If seeded, was seed material source 

documented? 

 

9. Seed Correction: Was the seed correction calculated based 

on average seed control sample results?

 

SECTION E-1. QC INFORMATION – Method Performance 

1. Nitrification Inhibitor: Was nitrification inhibitor added to 

all samples and controls? (CBOD5)

 

2. Nitrification Inhibitor Type: What nitrification inhibitor 

was used?

 

3. Seeding: Were all samples, seed controls, and glucoseglutamic acid (GGA) for CBOD seeded? 

4. Initial Dissolved Oxygen: Was initial DO measured (within 

30 min) of sample dilution preparation? (Should be between 

7 and 9 mg/mL)

 

5. Dilution: Were samples out of calibration range diluted for 

analysis? 

Note: For dilutions >67% of sample, were extra nutrients 

added? 

 

6. Incubation: Are samples incubated for 5 days ± 6 hours? 

7. Are any final DO measurements below 1.0? 

8. Have all samples shown a DO depletion of at least 2.0 mg/L? 

9. Seed Correction: Were seed corrections properly subtracted 

from seeded samples? 

 

10. Was the final BOD of the samples properly calculated?

SECTION E-2. QC INFORMATION – Instrument Calibration 

11. Initial Calibration (ICAL): Was an initial calibration 

reported on day one (1) of analysis? 

 

12. Continuing Calibration Check: Was the dissolved oxygen 
Laboratory Name:________________ CCH Episode #.:__________ SM 5210B Page 3 of 3 

Criterion 

met

STANDARD METHOD 5210 B Reviewer Comment Y N 

(DO) meter calibrated on day five of the procedure? 

13. Calibration Drift Check: Was the DO meter calibration 

checked for drift during and at the end of the sample set? 

 

14. Drift Test Requirements: Did the drift checks agree within 

± 0.2 mg/L?

 

SECTION E-3. QC INFORMATION –Reagent Blanks 

15. Water Quality: Was water type or quality documented? Is 

water aged before use, if so how long? 

 

16. Was water allowed to come to room temperature before 

usage? 

17. Were nutrient and phosphate buffer prepared or purchased? 

18. Was reagent quality verified and documented? 

19. Phosphate Buffer pH: Was this buffer pH= 7.2? 

20. Water Blank: Was a water blank analyzed in each analysis 

batch? Was it ≤ 0.20 mg/L? 

 

21. Glucose-glutamic Acid: Was a glucose-glutamic acid 

standard analyzed with each analysis batch? 

 

SECTION F-1. Method QC 

1. Analysis Time: Was the analysis incubation start and end 

documented? Did it meet method required times? 

 

2. Incubator temperature? Was incubator temperature 

documented? Was it within in specifications? 

 

3. Duplicates: Were duplicates run at every 20 samples? (5%) 

Are duplicates within 30%? 

 
Laboratory Name:________________ CCH Episode #.:__________ HACH Method 8000 Page 1 of 3 

CCH Study Data Review Checklist 

HACH METHOD 8000 COD 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank 1, 2, 3 

Field or Laboratory Duplicate Results 1,2,3 

Initial Calibration Data 2, 3 

Calibration Check Data 2, 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D)-- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F)-- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through F)-- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.
Laboratory Name:________________ CCH Episode #.:__________ HACH Method 8000 Page 2 of 3 

Criterion Met

HACH METHOD 8000 Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Receipt Temperature: Storage in the dark at a temperature 

≤6 C. (40 CFR 136 Table II) 

 Correct receipt and storage conditions indicated? 

 

4. Sample Condition: Sample bottle breakage? Sample 

leakage? 

 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Polyethylene, fluoropolymer, or glass. 

Correct sample container used? 

 

2. Septum/liner/cap: Fluoropolymer lined. 

Correct septum/liner/cap indicated? 

 

3. Sample Bottle Volume: Recommended but not required, 

100 mL (liquids) Sample bottle volume indicated?

 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Sample Stabilization: Were samples stabilized with sulfuric 

acid to pH of less than 2?

Were results corrected for the volume of sulfuric acid added? 

 

2. Were sample vials used that contained Mercury Sulfate for 

chloride stabilization?

 

3. Was the level of chloride interference exceeded for the 

HACH sample vials used? (Table 1 in HACH DR4000 

Procedure)

 

4. Sample holding time prior to analysis: Stabilized samples 

held up to 28 days maximum. Correct hold time indicated? 

 

5. Storage conditions: Extract stored between 0 and 4 C. 

Correct storage conditions indicated? 

 

Maximum analysis holding time: 28 days from collection 

to analysis. Correct analysis time indicated? 

 

6. Homogenization: Were the samples uniform or did samples 

contain solids requiring homogenizing? Was this procedure 

noted in the data? Were samples homogenized for 30 

seconds in a blender?

 

7. Digestion: Was digestion performed on samples before 

analysis? 

 

8. Was the COD reactor preheated to 150 °C? 

SECTION E-1. QC INFORMATION – Method Performance 

1. Initial Demonstration of Performance, Quality Control 

Sample (QCS): Were multiple measurements of a known 

standard (e.g., 100 mg/L analyzed to determine method 

precision? 

 Were the results within ±0.5% of the standard?

 

2. Detection Limit: Was the method detection limit 

determined and ≤ 1% of the calibration range?

 

SECTION E-2. QC INFORMATION – Instrument Calibration 

3. Initial Calibration (ICAL): Was an initial zero reported for 

certified blank vial? 

 

4. Low range: (0-150 mg/L) Was a minimum of 5 points used 

to prepare the initial calibration curve?

 
Laboratory Name:________________ CCH Episode #.:__________ HACH Method 8000 Page 3 of 3 

5. Continuing Calibration Verification (CCV) and Accuracy 

Check: Was the calibration accuracy checked with a zero (0) 

and high range potassium acid phthalate (KPH) standard? 

 

SECTION E-3. QC INFORMATION –Blanks 

6. Colorimetric Blanks: Was a reagent (deionized water) used 

to zero the instrument in absorbance mode? 

 

SECTION F. INSTRUMENT INTERFERENCE 

1. Chloride Interference: Was chloride concentration above 

stabilizer limits for the method?

 
CCH Study Data Review Checklist 

Trace Element Analysis of Water and Wastes EPA Method 200.7 

(Inductively Coupled Plasma Atomic Emission Spectrometry) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank 1, 2, 3 

Instrument Check Sample 1, 2, 3 

Calibration Blank 1, 2, 3 

Quality Control Sample 1, 2, 3 

Initial Calibration Data 2, 3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F) -- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G) -- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks. 

Laboratory Name:________________ CCH Episode #.:_____________ Method 200.7 – Page 1 of 4 
Criterion 

met

EPA METHOD 200.7 REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Sample Condition: Sample bottle breakage? Sample 

leakage?(200.7/8.1) 

4. Sample Hold Time: Were samples analyzed within 180 

days of collection? (CLP contract within 35 days for sample 

receipt?)

SECTION C. SAMPLE INFORMATION 

1. Sample container: Polyethylene, fluoropolymer, or glass 

Correct sample container used? (40 CFR 136 Table II) 

2. Septum/liner/cap: Fluoropolymer lined. 

Correct septum/liner/cap indicated? 

3. Sample bottle volume: Typically 1L. 

Correct sample bottle volume indicated? 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Data Type: Decisions about preservation and pretreatment 

of samples are made before collection. Was information 

provided designating the type of data as dissolved, suspended 

or total metals? (200.7/8.2) 

2. Dissolved Elements: For dissolved elements was the sample 

filtered through a 0.45 um membrane filter soon after 

collection? 

 Was the filtrate acidified with 1 to 1 nitric acid to a pH of 2 

or less? 

3. Suspended Elements: For determination of suspended 

elements was a known volume of unpreserved sample 

filtered through a 0.45 um membrane soon after sampling? 

Was the filter plus suspended material stored in a suitable 

container without preservation for shipment? (200.7/8.2.2) 

4. Total Elements: For the determination of total or total 

recoverable elements was the sample acidified with 1 to 1 

nitric acid to pH of 2 or less after sampling?

5. Dissolved Elements Analysis: Were dissolved elements 

analyzed directly as received or acidified to dissolve 

precipitate? (200.7/9.1)

6. Suspended Elements Analysis: Was the sample digested 

with nitric and hydrochloric acid and filtered prior to 

analysis? (200.7/9.2)

7. Total Elements Analysis: Was a well mixed volume of the 

sample digested with nitric acid and hydrochloric acid and 

filtered prior to analysis? (200.7/9.3)

SECTION E-1. QC INFORMATION – Instrument Performance 

1. Instrument Check Sample: Were the results of the target 

analyte ICS analyzed at a frequency of 10% and within 5% 

of expected value (or within established control)? 

(200.7/12.1.1/7.6.1)

2. Duplicate Sample (DUP): Was a duplicate sample analyzed 

once per analysis batch or SDG. 

Was the RPD of the duplicate <± 20 for samples > 5x 

Laboratory Name:________________ CCH Episode #.:_____________ Method 200.7 – Page 2 of 4 
Criterion 

met

EPA METHOD 200.7 REQUIREMENT Reviewer Comment Y N 

CRDL; ±CRDL for samples <5X CRDL

3. Interference Check Sample: Was a check sample analyzed 

at the beginning, end, and at periodic intervals during a 

sample batch run? (7.6.2) Were results within control limits 

of 1.5 times the STD of the mean value? (200.7/12.1.1) 

4. Serial Dilution Sample: Was one serial dilution sample run 

per batch or SDG? 

 Was serial dilution sample ± 10% of the original results for 

analytes 

 with concentration 50 X the IDL? 

SECTION E-2. QC INFORMATION – Instrument Calibration and Detection Limit 

5. Detection Limit (Contract Required Detection Limit):

Did reported detection limits meet contract required limits 

shown in Table 1 (below)? 

6. Initial Calibration (ICAL): Was a minimum of one blank 

and one calibration standard analyzed (ICAL)? 

7. Initial Calibration Verification (ICV): Was an ICV 

analyzed and did it meet required 90 – 100% of expected 

concentration? Was the ICV from a secondary source? 

8. Continuing Calibration Verification (CCV) : Was CCV 

analyzed daily before samples, after every 10 samples and at 

end of the analysis run? 

Did CCV meet 90-110% of expected concentration 

requirement? 

9. Contract Required Detection Limit Verification Standard 

(CRI): Was the CRI analyzed after initial Calibration 

Verification (ICV) but before sample analysis, and did the 

results meet 65 – 135% of expected concentration?

SECTION E-3. QC INFORMATION –Blanks 

10. Calibration Blank: Was a Calibration Blank prepared and 

used to flush the system between standards and samples? 

(200.7/7.5.1) 

11. Reagent/Method Blank (MB): Was a blank containing all 

reagents prepared and used to evaluate contaminants in 

reagents?(200.7/7.5.2) 

12. Calibration Blank: Was a calibration blank (7.5.1) analyzed 

at a frequency of 10% and within control limits (2STD of 

mean)? (200.7/12.1.1)

SECTION F. RECOVERY OF INTERNAL STANDARDS 

1. Instrument Check Standard (LCS): Was a standard 

containing compatible elements prepared at the midpoint of 

the calibration curve and used to assess continuing 

calibration and instrument performance once per batch or 

SDG? (200.7/12.1.1,7.6,3.7) 

Were LCS results within 80 – 120% of expected values? 

2. Interference Check Sample (ICS): Was a representative 

sample spiked with the elements of interest at 100 ug/L or 5 

times the MDL and used to test matrix interference and 

correction factors? (200.7/12.1.2, 7.6.2,3.8)

Was the ICS run at the start and finish of daily sample runs 

or twice per 8 hours? 

Did ICS results meet 80 – 120% of expected concentration?

3. Matrix Spike Sample (MS): Was one MS analyzed per 

Laboratory Name:________________ CCH Episode #.:_____________ Method 200.7 – Page 3 of 4 
Laboratory Name:________________ CCH Episode #.:_____________ Method 200.7 – Page 4 of 4 

Criterion 

met

EPA METHOD 200.7 REQUIREMENT Reviewer Comment Y N 

batch or SDG? 

Did the results indicate 75 – 125% recovery of expected 

value?

4. Quality Control Sample: Was a secondary source 

calibration sample at 1 mg/L prepared and analyzed to 

confirm calibration accuracy? (200.7/7.6.3/3.9)

SECTION G. DETAILED SAMPLE RAW DATA REVIEW 

1. Sample Results Reporting: Were results reported in units of 

micrograms per liter (ug/L) for water samples?

2. Sample Results: Were the sample results less than five 

times the Method Blank results?

3. Sample Results: Were the sample results at least greater 

than ten times the Method Blank results?

4. Minimum Levels: Were the minimum levels reported by 

the lab comparable to those specified in the method?

5. Duplicate Samples: Were duplicate samples collected? 

Were the RPDs less than 20%?

TABLE 1. Target Analyte List, CAS Numbers, and Contract Required Detection Limits (CRDL) for Metals by ICPAES 

ANALYTE CAS No. CRDL for Water 

(μg/L) 

CRDL for Soil 

(mg/Kg) 

Aluminum (Al) 7429-90-5 200 40 

Antimony (Sb) 7440-36-0 60 12 

Arsenic (As) 7440-38-2 10 2 

Barium (Ba) 7440-39-3 200 40 

Beryllium (Be) 7440-41-7 5 1 

Cadmium (Cd) 7440-43-9 5 1 

Calcium (Ca) 7440-70-2 5000 1000 

Chromium (Cr) 7440-47-3 10 2 

Cobalt (Co) 7440-48-4 50 10 

Copper (Cu) 7440-50-8 25 5 

Iron (Fe) 7439-89-6 100 20 

Lead (Pb) 7439-92-1 3 1 

Magnesium (Mg) 7439-95-4 5000 1000 

Manganese (Mn) 7439-96-5 15 3 

Molybdenum (Mo) 7439-97-6 20 4 

Nickel (Ni) 7440-02-0 40 8 

Potassium (K) 7723-14-0 5000 1000 

Selenium (Se) 7782-49-2 5 1 

Silver (Ag) 7440-22-4 10 2 

Sodium (Na) 7440-23-5 5000 1000 

Thallium (Tl) 7440-28-0 10 2 

Vanadium (V) 7440-62-2 20 4 

Zinc (Zn) 7440-66-6 10 2 
Laboratory Name:________________ CCH Episode #.:_____________ Method 245.7 – Page 1 of 5 

CCH Study Data Review Checklist 

Total Mercury Analysis EPA Method 245.7 

(Cold Vapor Atomic Fluorescence Spectroscopy) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank 1, 2, 3 

Instrument Check Sample 1, 2, 3 

Calibration Blank 1, 2, 3 

Quality Control Sample 1, 2, 3 

Initial Calibration Data 2, 3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F) -- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G) -- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks. 
Laboratory Name:________________ CCH Episode #.:_____________ Method 245.7 – Page 2 of 5 

Criterion Met

EPA METHOD 245.7 REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Sample Condition: Sample bottle breakage? Sample 

leakage? Bottles must be tightly sealed to avoid diffusion of 

atmospheric Hg through the cap threads. (245.7/8.2) 

 

4. Sample Hold Time: Were samples analyzed within 90 days 

of collection? (40 CFR 136 Table II) (CLP contract within 

35 days for sample receipt?) 

 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Fluoropolymer bottles with 

fluoropolymer-lined caps. (Glass may be used if Hg is the 

only target analyte. 

Correct sample container used? 

 

2. Septum/liner/cap: Fluoropolymer lined. 

Correct septum/liner/cap indicated? 

 

3. Sample bottle volume: Typically 1L. 

Correct sample bottle volume indicated? 

 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Data Type: Decisions about preservation and pretreatment 

of samples are made before collection. Was information 

provided designating the type of data as dissolved or total 

mercury? (8.4) 

 

2. Dissolved Elements: For dissolved mercury, samples must 

be accompanied by a blank that was filtered under the same 

conditions. Was the sample filtered through a 0.45 um 

capsule filter soon after collection? 

 

3. Preservation: Was the filtrate acidified with 5 mL/L 

pretested 12 N HCl within 48h of collection? (Or 5 mL/L 

BrCl) (245.7/8.5) (40 CFR 136 Table II) 

 

4. Total Mercury: For the determination of total mercury was 

the sample acidified with 1-to-1 nitric acid to pH of 2 or less 

after sampling?

 

5. Dissolved Elements Analysis: Were dissolved elements 

analyzed directly as received or acidified to dissolve 

precipitate? 

Was KBrO3/KBr added to samples at least 24 hours before 

analysis? (245.7/8.5.2)

 

SECTION E-1. QC INFORMATION – Instrument Performance 

1. Detection Limit (CRDL/MDL): Did reported detection 

limits meet contract required limits shown in Table 1 

(below)? 

 

2. Duplicate Sample (DUP): Was a duplicate sample analyzed 

once per analysis batch or SDG? 

Was the RPD of the duplicate <± 20 for samples > 5x 

CRDL; ±CRDL for samples <5X CRDL or met the criteria 

in Table 2?

 

3. Quality Control Sample: Was a secondary source 

calibration sample at 1 mg/L prepared, analyzed and reported 

to confirm calibration accuracy? (245.7/9.3)

 

4. Initial Precision and Recovery (IPR): Was an initial 
Laboratory Name:________________ CCH Episode #.:_____________ Method 245.7 – Page 3 of 5 

Criterion Met

EPA METHOD 245.7 REQUIREMENT Reviewer Comment Y N 

precision and recovery reported? 

5. OPR: Was an ongoing precision and recovery performed and 

compared to the IPR? Does the recovery of Hg in the OPR 

meet the requirements in Table 2 (below)?

 

SECTION E-2. QC INFORMATION – Instrument Calibration and Detection Limit 

6. Initial Calibration: Was a minimum of one blank and eight 

calibration standards analyzed with each analytical batch 

(ICAL)? 

Was the correlation coefficient, r ≥ 0.995? 

 

7. Initial Calibration Verification (ICV): Was an ICV at the 

midpoint of the ICAL analyzed and did it meet required 80 – 

120% of expected concentration? 

Was the ICV from a secondary source standard? 

Was the ICV analyzed daily, immediately following the 

ICAL and prior to sample analysis? 

 

8. Continuing Calibration Verification (CCV): Was the CCV 

analyzed daily before samples, after every 10 samples and at 

end of the analysis run? 

Did CCV meet 80-120% of expected concentration 

requirement? 

 

9. Contract Required Detection Limit Verification Standard 

(CRI): Was a CRI analyzed after initial calibration 

verification (ICV) but before sample analysis, and did the 

results meet 65 – 135% of expected concentration?

 

SECTION E-3. QC INFORMATION –Blanks 

10. Calibration Blank: Was a Calibration Blank prepared and 

analyzed after it was used to flush the system between 

standards and samples? (245.7/9.1.1.2) 

Was the ICB & CCB analyzed after the ICV & every CCV? 

Were the results less than the required detection limits? 

 

11. Reagent/Method Blank (MB): Was a blank containing all 

reagents prepared and used to evaluate contaminants in 

reagents? 

Was the MB run once per batch or SDG and every 20 

samples? (245.7/9.2.1) 

Was the MB result < Contract Required DL?

 

12. Field Blank/Bottle Blank: Was a field blank and/or bottle 

blank analyzed? Was the field blank data used to correct 

sample results?(245.7/12.4.2)

 

SECTION F. RECOVERY OF INTERNAL STANDARDS 

1. Instrument Check Standard (LCS): Was a standard 

containing compatible elements prepared at the midpoint of 

the calibration curve and used to assess continuing 

calibration and instrument performance once per batch or 

SDG? (245.7/12.1.1,7.6,3.7) 

Were LCS results within 75 – 125% of expected values? 

 

2. Matrix Spike Sample (MS/MSD): Was one MS/MSD pair 

analyzed for every 10 samples? 

Did the results indicate 75 – 125% (or Table 2) recovery of 

expected value? 

 

SECTION G. DETAILED SAMPLE RAW DATA REVIEW 

1. Sample Results Reporting: Were results reported in units of 

micrograms per liter (ug/L) for water samples?

 

2. Sample Results: Were the sample results less than five 
Laboratory Name:________________ CCH Episode #.:_____________ Method 245.7 – Page 4 of 5 

Criterion Met

EPA METHOD 245.7 REQUIREMENT Reviewer Comment Y N 

times the Method Blank results?

3. Sample Results: Were the sample results at least greater 

than ten times the Method Blank results?

 

4. Minimum Levels: Were the minimum levels reported by 

the lab comparable to those specified in the method?

 

5. Duplicate Samples: Were duplicate samples collected? 

Were the RPDs less than 20%?

 
Laboratory Name:________________ CCH Episode #.:_____________ Method 245.7 – Page 5 of 5 

TABLE 1. Target Analyte List, CAS Numbers, and Contract Required Detection Limits for Metals by ICP-AES 

ANALYTE Lowest Water Quality 

Criterion 1

Method Detection Limit 2

 Minimum Level 3

Mercury (Hg) 1.3 ng/L 1.8 ng/L 5.0 ng/L 

1 The lowest water quality criterion is for the Great Lakes System (Table 4, 40 CFR 132). The lowest criterion that is 

applicable nationwide (e.g., outside of the Great Lakes) is 12 ng/L (40 CFR 131.36). 

2 Method detection limit (MDL 40 CFR 136, Appendix B) 

3 Minimum level (ML) of quantitation (see Glossary) 

Table 2. Quality Control Acceptance Criteria for Performance Tests 

Performance Test Acceptance Criterion

Recovery (%) RSD (%) RPD (%)

Initial Precision and Recovery (IPR) 78 - 108 16 —

Ongoing Precision and Recovery (OPR) 76 - 113 — —

Matrix Spike/Matrix Spike Duplicate (MS/MSD) 63 – 111 — 18
CCH Study Data Review Checklist 

Volatile Organic Compounds EPA Method 1624C 

(Isotope Dilution GC/MS) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample No., and 

Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt Checklist) 1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank (includes 

ion abundance ratios) 

1, 2, 3 

Blank Spike Results (OPR) 1, 2, 3 

Labeled Compound Recovery Summary 1, 2, 3 

Matrix Spike/Duplicate Matrix Spike Recovery 

Summaries 

1, 2, 3 

Instrument Performance Check (Resolution) 2, 3 

Initial Calibration Data 2, 3 

Continuing Calibration Data 2, 3 

Windows Defining Mixture/Column Resolution Check 3 

Selected Ion Chromatograms for Each Sample, Blank, and 

Standard 

3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F)-- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G-2)-- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.

Laboratory Name:________________ CCH Episode #.:_____________ Method 1624C – Page 1 of 4 
Criterion met

EPA METHOD 1624C REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Receipt Temperature: Storage in the dark at a temperature 

< 6C. (40 CFR 136 Table II) 

Correct receipt conditions indicated? 

4. Sample Condition: Sample bottle breakage? Sample 

leakage? Air bubbles noted in sample? (1624C/9.1) 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Glass, hermetic seal. 

Correct sample container used? 

2. Septum/liner/cap: Fluoropolymer lined. 

Correct septum/liner/cap indicated? 

3. Sample bottle volume: 25 to 40 mL. 

Correct sample bottle volume indicated? 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Aqueous sample residual chlorine: If an aqueous sample 

contains residual chlorine, 10 mg/40 mL of sodium 

thiosulfate preservative is added to the empty bottle. 

Was residual chlorine measured (Method 330.4, 330.5)? 

Was preservative added? 

2. BTEX Sample Preservation: Were BTEX compounds 

found in the sample? 

If BTEX compounds were reported, was a separate sample 

collected, acidified, and analyzed for these compounds? 

(1624C/9.3)

3. Sample holding time prior to analysis: 14 days 

recommended maximum. Correct hold time indicated? 

4. Storage conditions: extract stored between 0 and 4 C. 

Correct storage conditions indicated? 

5. Maximum analysis holding time: 14 days from collection 

to analysis. (1624C/9.4) 

Correct analysis time indicated? 

SECTION E-1. QC INFORMATION – Instrument Performance 

1. Mass Intensity: Did the analytical system meet the massintensity criteria in Table 4 of Method 1624C for 50 ng 

BFB?(1624C/7.1)

2. Initial Precision and Recovery (IPR): Were two sets of 

four 5-mL aliquots of the aqueous performance standard 

analyzed before blanks and samples?

3. Average Recovery of IPR: Did the average recovery and 

standard deviation of the recovery for the first set of analyses 

meet the requirements in Table 6 of Method 1624C? 

(If yes, Instrument Performance Passes 1624C/8.2.3)

4. Additional Recovery for Failed IPR: Did the average 

recovery and standard deviation of the failed set of analytes 

meet the requirements in Table 6 of Method 1624C?

(If yes, Instruments Performance Passes 1624C/8.2.4) 

5. Detection Limits: Did the analytical system meet the 

minimum levels in Table 3 of Method 1624C for the 

compounds analyzed? (1624C/7.1)

6. Continuing Calibration Verification (CCV)/Ongoing 

Precision and Accuracy (OPA): Was the CCV calibration 

Laboratory Name:________________ CCH Episode #.:_____________ Method 1624C – Page 2 of 4 
Criterion met

EPA METHOD 1624C REQUIREMENT Reviewer Comment Y N 

standard analyzed prior to analyzing samples, blanks? 

(1624C/11.1) 

7. CCV/OPA: Did Concentrations meet the corresponding 

limit for ongoing accuracy in Table 6 of Method 1624C 

before samples were analyzed? (1624C/11.5.1)

SECTION E-2. QC INFORMATION – Instrument Calibration 

8. Initial Calibration (ICAL): Was an initial calibration curve 

with at least five points performed for each analyte? 

(1624C/7.4) 

9. Isotope Dilution Calibration: Was calibration by isotope 

dilution used for compounds for which a labeled analog is 

available? (1624C/7.4) 

10. Internal Standard Calibration: Was calibration by internal 

standard used for compounds for which a labeled analog is 

not available? (1624C/17.5)

11. ICAL RSD: Was the averaged response factor coefficient of 

variation less than 20% for analytes calculated by the isotope 

dilution method? For compounds that did not meet this RSD, 

was the complete calibration curve used? (1624C/7.4.) 

12. ICAL RSD: Was the averaged response factor RSD less 

than 35% for compounds calculated by the internal standard 

method? For compounds that did not meet this RSD, was the 

complete calibration curve used? (1624C/ 7.5) 

13. ICAL levels: Were the unlabeled compounds calibrated at 

the correct level as listed in Table 4 of Method of 1624C? 

(1624C/Table 4) 

14. Labeled Compound Spiking Levels: Were the labeled 

compounds spiked at 20 μg/L level (except acrolein, 

acrylonitrile, acetone, diethyl ether, p-dioxane, and MEK at 

100μg/L). (1624C/6.6) 

SECTION E-3. QC INFORMATION – Method Blanks 

15. Method blanks: Was the level at which the analytical 

system will carry greater than 5 μg/L of pollutant into a 

succeeding blank determined and reported? (1624C/8.5.1) 

16. Ongoing Laboratory Batch Blanks: Was a blank sample 

analyzed after every 8-hour shift? 

Were any of the target compounds or interfering compounds 

found in the blank at > 10μg/L? 

If so, was analysis stopped and contamination eliminated? 

17. Field Blank: Reagent water or other reference 

Was the Field Blank reported? 

Was the Field Blank above the detection limit? 

SECTION F. RECOVERY OF LABELED ISOTOPE DILUTION INTERNAL 

STANDARDS 

1. Recovery of labeled compounds: The recovery criteria of 

each labeled compound are listed in Table 6 of Method 

1624C. 

Did the average recovery % meet the criteria? (1624C/8.3.3) 

2. Recovery of labeled compounds: If recovery criteria of the 

labeled compounds are not met, was sample dilution 

analyzed? (1624C/18.3.3) 

3. Dilution of Samples: Have all samples where EICP area 

exceeds the calibration range been diluted until they are in 

the calibration range?

Laboratory Name:________________ CCH Episode #.:_____________ Method 1624C – Page 3 of 4 
Laboratory Name:________________ CCH Episode #.:_____________ Method 1624C – Page 4 of 4 

Criterion met

EPA METHOD 1624C REQUIREMENT Reviewer Comment Y N 

4. Diluted Sample Reporting: Have diluted samples been 

reported at the least dilute level which is within the 

calibration range? (1624C/13.6.1)

SECTION G-1. DETAILED RAW DATA REVIEW – Compound Identification 

Quality Control 

The following criteria must be met for a GC peak to be 

identified as a volatile organic target: 

1. The Signals: Did the GC peak contain at least five complete 

spectra across the upper half of the GC peak? (1624C/7/2/1) 

2. Characteristic m/z: Did the characteristic m/z stored in the 

spectral library maximize within the same two consecutive 

mass scans? 

3. Mass intensity: Did the corrected relative intensities of mass 

spectral peaks and the GC peak maximum agree within a 

factor of two for all masses stored in the spectral library? 

(1624C12.2.2)

4. Relative Retention Time Between Labeled analog and 

pollutant: Did the relative retention time between analog 

and pollutant meet the requirements in Table 3 of Method 

1624C?

5. OPA/Aqueous Performance Standard: Was an aqueous 

performance standard (Section 6.7.2) analyzed prior to 

calibration? 

Were these results compared to the areas obtained by 

injection 1 μL of the methanolic standard? 

Were water soluble compounds recovered at greater than 

20% 

Were all other compounds recovered from 60 to 110% of 

expected? 

6. Toluene Recovery: Did 100ηg toluene produce area at m/z 

91 or 99 approximately one-tenth that required to exceed the 

linear range of the system? 

7. Absolute Retention Times: The absolute retention times of 

the labeled compounds in the CCV must be within the limits 

given in Table 3 of Method 1624C. (1624C/11.3,12.1.3) 

8. GC resolution: Was the valley height between toluene and 

toluenen-d8 must be less than 10% of the taller of the two 

peaks?

SECTION G-2. DETAILED RAW DATA REVIEW – Sample Results

9. Sample Results: were the sample results less than five 

times the Method Blank results?

10. Sample Results: were the sample results at least greater 

than ten times the Method Blank results?

11. Minimum Levels: were the minimum levels reported by the 

lab comparable to those specified in the method?

12. MS/MSD: if a MS/MSD was reported, were the recoveries 

within ± 50%?

13. Duplicate Samples: were duplicate samples collected? 

Were the RPDs less than 20%?
CCH Data Review Checklist 

Semivolatile Organic Compounds EPA Method 1625C 

(Isotope Dilution GC/MS) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample No., and 

Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt Checklist) 1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank (includes 

ion abundance ratios) 

1, 2, 3 

Blank Spike Results (OPR) 1, 2, 3 

Labeled Compound Recovery Summary 1, 2, 3 

Matrix Spike/Duplicate Matrix Spike Recovery Summaries 1, 2, 3 

Instrument Performance Check (Resolution) 2, 3 

Initial Calibration Data 2, 3 

Continuing Calibration Data 2, 3 

Windows Defining Mixture/Column Resolution Check 3 

Selected Ion Chromatograms for Each Sample, Blank, and 

Standard 

3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F) -- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G-2) -- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.

Laboratory Name:________________ CCH Episode #.:_____________ Method 1625C – Page 1 of 4 
Criterion 

met

EPA METHOD 1625 REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: Entered by analysis laboratory? 

3. Receipt Temperature: Storage in the dark at a temperature 

0 - 6 C. (40 CFR 136 Table II) 

Correct receipt conditions indicated? 

4. Sample Condition: Sample bottle breakage? Sample 

leakage? (1625C/9.1) 

SECTION C. SAMPLE INFORMATION 

1. Sample container: Amber glass, or clear glass protected 

from the light. 

Correct sample container used? 

2. Septum/liner/cap: Fluoropolymer lined. 

Correct septum/liner/cap indicated? 

3. Sample bottle volume: > 1L (liquids), or >0.5 L (solids) 

Correct sample bottle volume indicated? 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Aqueous sample residual chlorine: If an aqueous sample 

contains residual chlorine, 80 mg/L of sodium thiosulfate 

preservative is added to the empty bottle. 

Was residual chlorine measured (Method 330.4, 330.5)? 

Was preservative added? 

2. Sample holding time prior to analysis: Extract samples 

within 7 days of collection. Correct hold time indicated? 

3. Storage conditions: Extract stored between 0 and 4 C. 

Correct storage conditions indicated? 

4. Maximum analysis holding time: 40 days from extraction . 

(1625C/9.3) 

Correct analysis time indicated? 

SECTION E-1. QC INFORMATION – Instrument Performance 

1. Mass Intensity: Did the analytical system meet the massintensity criteria in Table 7 of Method 1625C for 

DFTPP?(1625C/7.1)

2. Initial Precision and Accuracy (IPA): Were two sets of 

four 1-L aliquots of the aqueous performance standard 

analyzed before blanks and samples? (1625C/8.2.1)

3. Average Recovery of IPA: Did the average recovery and 

standard deviation of the recovery for the first set of analyses 

meet the requirements in Table 10 of Method 1625C? 

(If yes, Instrument Performance Passes 1625C/8.2.3)

4. Additional Recovery for Failed IPA: Did the average 

recovery and standard deviation of the failed set of analytes 

meet the requirements in Table 10 of Method 1625C?)

(If yes, Instruments Performance Passes 1625C/8.2.4) 

5. Detection Limits: Did the analytical system meet the 

minimum levels in Table 5 of Method 1625C for the 

compounds analyzed? (1625C/7.3)

6. Continuing Calibration Verification (CCV): Was the CCV 

calibration standard analyzed prior to analyzing samples, 

blanks? (1625C/12.5) 

7. Continuing Calibration Verification: Was the CCV used 

to verify calibration every 20 extracts or less? Was 

Laboratory Name:________________ CCH Episode #.:_____________ Method 1625C – Page 2 of 4 
Criterion 

met

EPA METHOD 1625 REQUIREMENT Reviewer Comment Y N 

Pentachlorophenol recovered > 85%? (1625C/10.8.25)

8. CCV and Ongoing Precision and Accuracy: Did

concentrations meet the corresponding limit for ongoing 

accuracy in Table 10 before samples were analyzed? 

(1625C/12.5.1, 12.7.3)

SECTION E-2. QC INFORMATION – Instrument Calibration 

9. Initial Calibration (ICAL): Was an initial calibration curve 

with at least five points performed for each analyte? 

(1625C/7.4, 7.5) 

10. Isotope Dilution Calibration: Was calibration by isotope 

dilution used for compounds for which a labeled analog is 

available? 

11. Internal Standard Calibration: Was calibration by internal 

standard used for compounds for which a labeled analog is 

not available? (1625C/17.5) 

12. ICAL RSD: Was the averaged response factor RSD less 

than 35% for compounds calculated by the internal standard 

method? For compounds that did not meet this RSD, was the 

complete calibration curve used? (1625C/ 7.5) 

13. Labeled Compound Spiking Levels: Were the labeled 

compounds spiked at nominally 100 μg/L level. 

(1625C/6.14) 

SECTION E-3. QC INFORMATION – Method Blanks 

14. Method blanks: Was the level of the reagent blank greater 

than 10 μg/L (aqueous) or 100 ug/kg (solids)? (1625C/8.5.2) 

If so, was analysis stopped and contamination eliminated?

15. Ongoing Laboratory Batch Blanks: Was a blank sample 

analyzed after every 8-hour shift or 20 samples? 

(1625C/8.5.1) 

16. Field Blank: Reagent water or other reference. Was the 

Field Blank reported? Was the Field Blank above the 

detection limit? 

SECTION F. RECOVERY OF LABELED ISOTOPE DILUTION INTERNAL 

STANDARDS 

1. Recovery of labeled compounds: The recovery criteria of 

each labeled compound are listed in Table 10 of Method 

1625. 

Did the average recovery % meet the criteria? (1625C/8.3.3) 

2. Recovery of labeled compounds: If recovery criteria of the 

labeled compounds are not met, was sample dilution 

analyzed? (1625C/18.4) and guidelines followed for 

reporting? 

3. Dilution of Samples: Have all samples where EICP area 

exceeds the calibration range been diluted until they are in 

the calibration range? (1625C/14.4)

4. Diluted Sample Reporting: Have diluted samples been 

reported at the least dilute level which is within the 

calibration range? (1625C/14.6)

Laboratory Name:________________ CCH Episode #.:_____________ Method 1625C – Page 3 of 4 
Laboratory Name:________________ CCH Episode #.:_____________ Method 1625C – Page 4 of 4 

SECTION G-1. DETAILED RAW DATA REVIEW – Compound Identification 

Quality Control 

The following criteria must be met for a GC peak to be 

identified as a semivolatile organic target: 

1. The Signals: Did the GC peak contain at least five complete 

spectra across the upper half of the GC peak? (1625C/7.2.4) 

2. Characteristic m/z: Did the characteristic m/z stored in the 

spectral library maximize within the same two consecutive 

mass scans? 

3. Absolute Retention Times: Did the absolute retention time 

of 2,2’-difluorobiphenyl fall within 1078 and 1248 seconds? 

(1625C/12.3)

4. Relative Retention Time Between Labeled analog and 

pollutant: Did the relative retention time between analog 

and pollutant meet the requirements in Tables 5 and 6 of 

Method 1625C? (1625C/12.3)

5. GC resolution: Was the valley height between anthracene 

and phenanthrene at m/z 178 (or the analogs at n/z 188) less 

than 10% of the taller of the two peaks?

6. Library Reverse Search: Was a library reverse search 

performed for the compounds of interest? (1625C/5.13.2, 

7.2.5, T3, T4)

SECTION G-2. DETAILED RAW DATA REVIEW – Sample Results

7. Sample Results: Were the sample results less than five 

times the Method Blank results?

8. Sample Results: Were the sample results at least greater 

than ten times the Method Blank results?

9. Minimum Levels: Were the minimum levels reported by 

the lab comparable to those specified in the method?

10. MS/MSD: If a MS/MSD was reported, were the recoveries 

within ± 50%?

11. Duplicate Samples: Were duplicate samples collected? 

Were the RPDs less than 20%?
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 1 of 7 

OW Effluent Guidelines Data Review Checklist 

Tetra- Through Octa-Chlorinated Dioxins and Furans (D/F) EPA Method 1613B 

(Isotope dilution HRGC/MS) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

 Record reviewer comments in the Reviewer Comment section. 

 Record detailed information in the “Comments and Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. Overall Method 1613B Data Package Checklist 

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 1 

Cross reference of Field Sample No., Lab Sample 

No., and Analytical Batch 

1, 2, 3 

Chain-of-Custody Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

1 

Results Summary for Each Sample and Blank 

(includes ion abundance ratios) 

1, 2, 3 

Blank Spike Results (OPR) 1, 2 

Labeled Compound Recovery Summary 1, 2 

Matrix Spike/Duplicate Matrix Spike Recovery 

Summaries 

1, 2 

Instrument Performance Check (Resolution) 1,2 

Initial Calibration Data 1,2 

Continuing Calibration Data 1,2 

Resolution Check 1,2 

Selected Ion Chromatograms for Each Sample, 

Blank, and Standard 

1,2 

Quantitation List 1,2 

Copies of Sample Preparation Work Sheets 1,2,3 

Copies of Run Logs 1,2 

1. COMPLIANCE SCREENING (ERG Sections A through D) -- Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through H) -- Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through I) -- Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks. 
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 2 of 7 

Criterion Met

EPA METHOD 1613B REQUIREMENT Reviewer Comment Y N 

SECTION B. Sample Receipt, Traffic Report

1. Sample Receipt Record: Signatures Complete? 

2. Receipt Date: Entered by Analysis Laboratory? 

3. Samples Listed Correctly and Complete?

4. Receipt Temperature: Storage temperature <6°C but not 

frozen. 

Correct receipt temperature indicated? 

5. Condition: Breakage?/Leakage? 

SECTION C. Sample Handling Information

1. Sample container: Was the correct sample container used?

[Method specifies amber or clear glass bottles wrapped in 

foil or stored in boxes that prevent exposure to light.] 

2. Septum/liner/cap: Was the container cap PFTE lined? 

3. Sample bottle volume: Was the correct sample bottle 

volume used (e.g., 1 liter, 1 quart, 1 pint, or 0.5 liter)? 

4. Sample preservation: Were the samples preserved by 

neutralizing any chlorine residual with 0.008% sodium 

thiosulfate? 

5. Maximum holding time: Were the samples held for 7 days 

or less? 

SECTION D. Sample Preparations/Extract Handling Information

1. Storage temperature - cooled to 6°C? 

Were the samples stored at 6°C (40 CFR 136 Table II) but 

not less then 0°C? 

2. Maximum analysis time: 

Were the samples analyzed within 40 days from day of 

extraction? 

SECTION E. Instrument Parameter Review

SECTION E-1. QC Information – Instrument Performance

1. Instrument Resolution: 

Was the PFK determined resolution greater than or equal to 

10,000? 

2. Instrument Mass Deviation: 

Was the deviation between the exact mass and the 

theoretical mass (Table 3 in 1613B) for each of the three to 

five ions monitored less than 5 ppm. 

3. Mass Drift: 

Did the PFK lock-masses vary by less than +/-20% 

throughout each respective time window (1613B/7.2.1.2)? 

4. Ion abundance ratios: 

Were all labeled and unlabeled PCDDs and PCDFs in the 

calibration standard (CS1) within the QC limits in 1613B 

Table 3A for their respective ion abundance ratios 

(1613B/7.2.2)? Do the ion abundance ratios fall within the 
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 3 of 7 

Criterion Met

EPA METHOD 1613B REQUIREMENT Reviewer Comment Y N 

required limits (see reference table in Method)? 

5. Signal to Noise ratio: 

Are all labeled and unlabeled analytes in the CS1 calibration 

standard detected with signal to noise ratios greater than or 

equal to 10.0? (1613B/7.2.3) 

6. Retention Time: 

Does the absolute retention time of 13C labeled -1,2,3,4-

TCDD exceed 25.0 minutes on the DB-5 column, and the 

retention time of 13C labeled 1,2,3,4-TCDD exceed 15.0 

minutes on the DB-225 column? (1613B/7.2.4) 

7. Resolution: 

Is the height of the valley between the most closely eluted 

isomers and the 2,3,7,8-substituted isomers less than 25% 

(1613B/7.4.2)? 

SECTION E-2.(1613B/10.5) QC Information – Instrument Calibration

8. Was an initial five point calibration curve determined for 

each analyte? 

9. Was the calibration curve determined less than 30 days prior 

to the time the first samples were analyzed? 

10. Was the averaged response factor RSD less than 20% for 

analytes calculated by the isotope dilution method? 

11. Was the averaged response factor RSD less than 35% for 

analytes calculated by the internal standard method? 

12. Labeled Compound Spiking Levels (when all CDD/CDF 

compounds are analyzed):

Were the labeled compounds spiked at the correct nominal 

level?

13C -2,3,7,8-TCDD 100 ng/mL 

13C -2,3,7,8-TCDF 100 ng/mL 

13C -1,2,3,7,8-PeCDD 100 ng/mL 

13C -1,2,3,7,8-PeCDF 100 ng/mL 

13C -2,3,4,7,8-PeCDF 100 ng/mL 

13C -1,2,3,4,7,8-HxCDD 100 ng/mL 

13C -1,2,3,6,7,8,-HxCDD 100 ng/mL 

13C -1,2,3,4,7,8-HxCDF 100 ng/mL 

13C -1,2,3,6,7,8-HxCDF 100 ng/mL 

13C -1,2,3,7,8,9-HxCDF 100 ng/mL 

13C -2,3,4,6,7,8,-HxCDF 100 ng/mL 

13C -1,2,3,4,6,7,8-HpCDD 100 ng/mL 

13C -1,2,3,4,6,7,8-HpCDF 100 ng/mL 

13C -1,2,3,4,7,8,9-HpCDF 100 ng/mL 

13C -OCDD 17-157 200 ng/mL 

37Cl -2,3,7,8-TCDD 10 ng/mL

13. Labeled Compound Spiking Levels (when only 

TCDD/TCDF compounds are analyzed):

Were the labeled compounds spiked at the correct level?

13C -2,3,7,8-TCDD 100 ng/mL 

13C -2,3,7,8-TCDF 100 ng/mL 

37Cl -2,3,7,8-TCDD 10 ng/mL

14. Labeled Compound Recovery in Calibration Standards 
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 4 of 7 

Criterion Met

EPA METHOD 1613B REQUIREMENT Reviewer Comment Y N 

(when all CDD/CDF compounds are analyzed):

Did the spiked 13C isotope recovery meet the following 

criteria? 

13C -2,3,7,8-TCDD 25–164% 

13C -2,3,7,8-TCDF 24–169% 

13C -1,2,3,7,8-PeCDD 25–181% 

13C -1,2,3,7,8-PeCDF 24–185% 

13C -2,3,4,7,8-PeCDF 21–178% 

13C -1,2,3,4,7,8-HxCDD 32–141% 

13C -1,2,3,6,7,8,-HxCDD 28–130% 

13C -1,2,3,4,7,8-HxCDF 26–152% 

13C -1,2,3,6,7,8-HxCDF 26–123% 

13C -1,2,3,7,8,9-HxCDF 29–147% 

13C -2,3,4,6,7,8,-HxCDF 28–136% 

13C -1,2,3,4,6,7,8-HpCDD 23–140% 

13C -1,2,3,4,6,7,8-HpCDF 28–143% 

13C -1,2,3,4,7,8,9-HpCDF 26–138% 

13C -OCDD 17-157% 

37Cl -2,3,7,8-TCDD 35-197% 

15. Labeled Compound Recovery in Calibration Standards 

(when all only TCDD/TCDF compounds are analyzed):

Did the spiked 13C isotope recovery meet the following 

criteria?

13C -2,3,7,8-TCDD 31-137% 

13C -2,3,7,8-TCDF 29-140% 

37Cl -2,3,7,8-TCDD 42–164.% 

SECTION E-3. (1613B/11.0) QC Information – Method Blanks

16. Were Reference matrix method blanks initially 

acceptable?

Ongoing Laboratory Method/Batch Blanks acceptable? 

(Samples on a given 12-hour shift, to a maximum of 20 

samples)? 

Note any 2,3,7,8-substituted CDD/CDF found in the blank at 

greater than the minimum level listed below. 

For Compounds using 13C12 -1,2,3,4-TCDD as the injection 

internal standard: 

2,3,7,8-TCDF 13C -2,3,7,8-TCDF 10 pg/L 

2,3,7,8-TCDD 13C -2,3,7,8-TCDD 10 pg/L 

1,2,3,7,8-PeCDF 13C -1,2,3,7,8-PeCDF 50 pg/L 

2,3,4,7,8-PeCDF 13C -2,3,4,7,8-PeCDF 50 pg/L 

1,2,3,7,8-PeCDD 13C -1,2,3,7,8-PeCDD 50 pg/L 

Compounds using 13C12 -1,2,3,7,8,9-HxCDD as the injection 

internal standard: 

1,2,3,4,7,8-HxCDF 13C -1,2,3,4,7,8-HxCDF 50 pg/L 

1,2,3,6,7,8-HxCDF 13C -1,2,3,6,7,8-HxCDF 50 pg/L 

1,2,3,7,8,9-HxCDF 13C -1,2,3,7,8,9-HxCDF 50 pg/L 

2,3,4,6,7,8-HxCDF 13C -2,3,4,6,7,8,-HxCDF 50 pg/L 

1,2,3,4,7,8-HxCDD 13C -1,2,3,4,7,8-HxCDD 50 pg/L 
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 5 of 7 

Criterion Met

EPA METHOD 1613B REQUIREMENT Reviewer Comment Y N 

1,2,3,6,7,8-HxCDD 13C -1,2,3,6,7,8,-HxCDD 50 pg/L 

1,2,3,4,6,7,8-HpCDF 13C -1,2,3,4,6,7,8-HpCDF 50 pg/L 

1,2,3,4,7,8,9-HpCDF 13C -1,2,3,4,7,8,9-HpCDF 50 pg/L 

1,2,3,4,6,7,8-HpCDD 13C -1,2,3,4,6,7,8-HpCDD 50 pg/L 

OCDF 13C -OCDD 100 pg/L 

OCDD 13C -OCDD 100 pg/L 

17. Method Blank— Were required reagent water blanks 

prepared, and treated as a sample in all respects for the 

purpose of determining if the field or sample transporting 

procedures and environments have contaminated the 

sample? 

Was Field Blank reported? 

Was the Field Blank below the detection limit?

SECTION F. Recovery of C-13 Labeled Isotope Dilution Internal Standards

1. Labeled Standard Recovery: Was recovery of each C-13 

labeled PCDD and PCDF isomer using Method 1613B 

within acceptable range defined in Table 6 of Method 

1613B? 

SECTION G. Instrument Recovery of Internal Standards

1. Internal Standard Recovery: 

Was the sum of the area counts of two masses for each of the 

two instrument recovery internal standards for samples, 

blanks, and standards within a factor of four (-25% to 

+400%) from the sum of the associated average areas from 

the five initial calibration standards? (EPA Region 10 SOP 

for Method 1613B Data Validation) 

Note: When all CDDs/CDFs are analyzed the internal 

standard solution contains 13C12 -1,2,3,4-TCDD and 13C12 -

1,2,3,7,8,9-HxCDD. 

When only 2,3,7,8-TCDD and 2,3,7,8-TCDF are to be 

determined, the standard solution contains 13C12 -1,2,3,4-

TCDD only. 

Was the Internal Standard Recovery Correct? (1613B/15.0)

SECTION H. Performance Evaluation (QA) Samples

1. Field duplicates, transfer blanks, trip blanks, blind spikes, 

blind blanks, and performance evaluation (PE) samples 

should be reviewed during data evaluation. 

If QA samples are included among the field samples for 

measurement by the laboratory, then the data validator 

should refer to the applicable QAPP for any QA 

requirements regarding QA samples. Did the QA samples 

meet the required precision and bias limits? (1613B/9.6-

15.0) 

Results from the measurement of project and regional QA 

samples will reflect upon the ability of the laboratory to 

report analytical results of known and documented quality 
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 6 of 7 

Criterion Met

EPA METHOD 1613B REQUIREMENT Reviewer Comment Y N 

which meet the Precision, Accuracy, and Representativeness 

QA/QC requirements of the QAPP. (Reference, Region 10 

SOP for Data Validation from Method 1613B) 

SECTION I. Detailed Raw Data Review – Compound Identification Quality 

Control

The following criteria must be met for a GC peak to be 

identified as a PCDD or PCDF:

1. Were the signals for the two exact m/z's being monitored 

present, and maximized within plus or minus 2 seconds of 

one another (see 1613B/Section 15.1)? 

2. The signal-to-noise ratio Was the signal to noise (S/N) of 

each of the two exact m/z's greater than or equal to 2.5 for a 

sample extract, and greater than or equal to 10 for a 

calibration standard (see 1613B/Section 15.2)? 

3. The ratio: Was the ratio of the integrated ion currents 

(EICPs) of both the exact m/z's monitored within the limits 

of the method (see 1613B/Section 15.3)? 

4. Relative Retention Times:

Was the relative retention time (RRT) of the peaks 

representing an unlabeled 2,3,7,8 substituted PCDD or 

PCDF within the limits given in the method? The retention 

time (RT) of peaks representing non-2,3,7,8-substituted 

PCDDs or PCDFs must be within the RT windows 

established in the method (see 1613B/Section 15.4)? 

5. Confirmatory Column Analysis:

Was the measurement of 2,3,7,8-TCDF on the primary DB-5 

GC column confirmed by analysis on a confirmatory column 

such as DB-225, SP-2330, DB-DIOXIN, or equivalent? 

Were all QC requirements of the method met on both the 

primary and secondary GC columns (see 1613B/Section 

15.5)? 

6. Non-PCDPE Interferences: 

If non-PCDPE interferences to the measurement of 2,3,7,8-

TCDF on the secondary GC column are present, did the 

laboratory measure 2,3,7,8-TCDF on a third dissimilar GC 

column in order to separate the 2,3,7,8-TCDF peak from the 

non-PCDPE interference peak? 

Did the measurement of 2,3,7,8-TCDF on a third dissimilar 

GC column include full calibration (both initial and 

calibration verification) on the third GC column? 

Did analysis resolve interference? 

7. The identification of a GC peak: Was the identification of 

a GC peak (on either primary or confirmatory GC column) 

as a PCDF made when no signal having a S/N 2.5 at the 

same retention time (± 2 seconds) in the corresponding 

polychlorinated diphenyl ether (PCDPE) channel? 

These criteria require that the laboratory document the EICP 

of all PCDPE m/z's which are scanned (see 1613B/15.3). 

Was EICP documented for all PCDPE m/z’s? 
Laboratory Name:______________ CCH Episode #.:___________ Method 1613B – Page 7 of 7 

8. Retention Time Verification:

Were the retention times of target compounds verified using 

reference standards before identifications were determined 

(see 1613B/15.4)? 

Were retention times verified and correct? 

9. The valley height: Was the valley height between 2,3,7,8-

TCDD and the other TCDD isomers at m/z 319.8965, and 

between 2,3,7,8-TCDF and the other TCDF isomers at m/z 

303.9016 less than 25% on their respective columns (see 

1613B/Section 14.4.2.2)? 
Laboratory Name:________________ CCH Episode #.:_____________ Method 1668A – Page 1 of 5 

CCH Study Data Review Checklist 

Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue 

(Isotope Dilution HRGC/HRMS Method 1668A) 

SECTION A-1. Sample Identifiers

CCH Effluent Guidelines 

Development 

Sampling Episode: 

Laboratory Name: 

Sample Number or Range: 

Data Reviewer signature: Date: 

Instructions: Complete this checklist electronically or using a ballpoint pen. 

Record reviewer comments in the Reviewer Comment section. 

Record detailed information in the Comments in the “Overall Assessment” section for each criterion not (“N”) met. 

SECTION A-2. OVERALL ASSESSMENT OF THE QUALITY OF THE DATA

General Comment Checklist 

Deliverable Requirement 

Required 

for 

Category Present Comments 

Copies of Shipping Documents (Fed-Ex Airbills) 1, 2, 3 

Case Narrative 1, 2, 3 

Table of Contents 3 

Cross reference of Field Sample No., Lab Sample No., 

and Analytical Batch 

1, 2, 3 

Traffic Report Form (including Sample Receipt 

Checklist) 

1, 2, 3 

Sample Calculation (usually just a page copied from 

SOW) 

3 

Results Summary for Each Sample and Blank (includes 

ion abundance ratios) 

1, 2, 3 

Blank Spike Results (OPR) 1, 2, 3 

Labeled Compound Recovery Summary 1, 2, 3 

Matrix Spike/Duplicate Matrix Spike Recovery 

Summaries 

1, 2, 3 

Instrument Performance Check (Resolution) 2, 3 

Initial Calibration Data 2, 3 

Continuing Calibration Data 2, 3 

Windows Defining Mixture/Column Resolution Check 3 

Selected Ion Chromatograms for Each Sample, Blank, 

and Standard 

3 

Quantitation List 3 

Copies of Sample Preparation Work Sheets 3 

Copies of Run Logs 3 

1. COMPLIANCE SCREENING (ERG Sections A through D)--Sample and QC results only; no instrument calibration or performance checks 

2. SUMMARY VALIDATION (ERG Sections A through F)--Sample, QC, calibration & instrument performance results; no raw data 

3. FULL VALIDATION (ERG Sections A through G-2)--Sample, QC, calibration & instrument performance results; includes raw data transcription 

checks & result recalculation checks.
Laboratory Name:________________ CCH Episode #.:_____________ Method 1668A – Page 2 of 5 

Criterion 

met

EPA METHOD 1668A REQUIREMENT Reviewer Comment Y N 

SECTION B. SAMPLE RECEIPT

1. Sample Receipt Record: Signatures complete? 

2. Receipt Date: entered by analysis laboratory? 

3. Receipt Temperature: storage in the dark at a temperature < 

6 C. (40 CFR 136 Table II) 

Correct receipt conditions indicated? 

 

4. Sample Condition: sample bottle breakage? Sample 

leakage? 

 

SECTION C. SAMPLE HANDLING INFORMATION 

1. Sample container: Amber or clear glass bottles – Clear 

glass wrapped in foil or stored in boxes that prevent exposure 

to light. 

Correct sample container used? 

 

2. Spetum/liner/cap: Fluoropolymer lined. 

Correct septum/liner/cap indicated? 

 

3. Sample bottle volume: 1 liter (liquids) or 0.5 liter (solids). 

Correct sample bottle volume indicated? 

 

SECTION D. SAMPLE PREPARATION/EXTRACT HANDLING 

INFORMATION 

1. Hold time for aqueous, solid, semisolid, tissues, or other 

matrices: Extract and analyze within 1 year of collection. 

(1668A/8.5) 

 Correct hold time indicated?

 

2. Sample holding time prior to extraction: Maximum of 1 

year. 

 Correct extraction time indicated?

 

3. Storage conditions: Extracts stored in the dark at <-10 C. 

Correct storage conditions indicated? 

 

4. Maximum analysis holding time for aqueous extractions:

one year at a pH< 9. 

Correct holding time indicated? 

 

SECTION E-1. QC INFORMATION – Instrument Performance 

1. Instrument Resolution: For the PFK molecular leak, the 

resolution must be greater than or equal to 10,000 at m/z 

330.9792. 

Is the instrument resolution provided and sufficient? 

(1668A/10.2.1) 

 

2. Instrument Mass Deviation: The deviation between the 

exact mass and the theoretical mass (Table 7 in Method 

1668A) for each of the two ions monitored must be less than 

5 ppm. (1668A/10.2.2) 

Is the mass deviation documented and acceptable? 

 

3. Mass Drift: Using PFK to provide lock-masses. Each lockmass shall be monitored and shall not vary by more than ± 

20% throughout each respective time window. 

(1668A/10.3.1.2) 

Is mass drift documented and acceptable? 

 

4. Ion abundance ratios: All CB s and labeled compounds in 

the Calibration standard (CS-1) must be within the QC limits 

in Table 8 of Method 1668A for their respective ion 

abundance rations. (1668A/10.3.2). 

Do the ion abundance ratios fall within the required? 

 

5. Continuing Performance and Calibration Verification 
Laboratory Name:________________ CCH Episode #.:_____________ Method 1668A – Page 3 of 5 

Criterion 

met

EPA METHOD 1668A REQUIREMENT Reviewer Comment Y N 

(CCV): Was the CCV (CS-3) and Diluted combined 209 

congener soulution standard analyzed prior to analyzing 

samples, blanks, IPRs, and OPRs? (1668A/15.1 and Table 6 

below) 

Do they meet performance criteria? 

6. CCV Recovery: The CCV (CS-4) recovery limits are listed 

in Table 6 of Method 1668A (1668A/15.3.5) 

Do the recoveries meet acceptance criteria for CCV? 

 

7. Signal to Noise ratio: All labeled and unlabeled analytes in 

the CCV calibration standard must have signal to noise ratios 

greater or equal to 10.0. (1668A/10.3.3) If the S/N ratio is 

indicated, is it greater than or equal to 10.0? 

 

8. Absolute Retention Time: The absolute retention times of 

the labeled compounds in the CCV must be within ± 15 

seconds of the respective retention times in the most recent 

CCV. (1668A/15.4.1.1) 

Are the retention times within specifications? 

 

9. Absolute Retention Time: The absolute retention time of 

CB 209 must exceed 55 minutes. 

 Are the retention times within specifications

 

10. Relative Retention Time: The relative retention time of the 

native and labeled compounds in the CCV must be within 

their respective RRT times listed in Table 2 of Method 

1668A. (1668A/15.4.1.2) 

Are the absolute retention times within specifications? 

 

11. Initial Precision and Recovery (IPR): Was an IPR 

performed prior to analyzing samples and blanks? 

(1668A/9.2.3) 

 

12. IPR Recovery: The IPR recovery limits are listed in Table 6 

of Method 1668A. (1668A/9.2.3) 

Do the recoveries meet acceptance criteria for IPR? 

 

13. Ongoing Precision and Recovery (OPR): Is the OPR 

calibration standard analyzed prior to analyzing samples and 

blanks? (1668A/15.5.1) 

 

14. OPR Recovery: The OPR recovery limits are listed in Table 

6 of Method 1668A. (1668A/15.5.3) 

Do the recoveries meet acceptance criteria for OPR? 

 

15. Sample Dilution: If the SICP area at the either quantitation 

m/z exceeds the calibration range, was the sample diluted to 

bring the concentration within the calibration range and reanalyzed? (1668A/17.5) 

 

SECTION E-2. QC INFORMATION – Instrument Calibration 

16. Initial Calibration (ICAL): Was an initial calibration curve 

with at least five points performed for each compound? 

(1668A/10.4.) 

 

17. Isotope Dilution Calibration: Was calibration by isotope 

dilution used for compounds for which a labeled analog is 

available? (1668A/10.4) 

 

18. ICAL RSD: Was the averaged response factor RSD less 

than 20% for compounds calculated by the isotope dilution 

method? For compounds that did not meet this RSD, was the 

complete calibration curve used? (1668A/10.4.4) 

 

19. Internal Standard Calibration: Was calibration by internal 

standard used for compounds for which a labeled analog is 

not available? (1668A/10.5) 

 
Laboratory Name:________________ CCH Episode #.:_____________ Method 1668A – Page 4 of 5 

Criterion 

met

EPA METHOD 1668A REQUIREMENT Reviewer Comment Y N 

20. ICAL levels: Were the unlabeled compounds calibrated at 

the correct level as listed in Table 5 of Method of 1668A? 

 

21. Labeled Compound Spiking Levels: Were the labeled 

compounds spiked at the acceptable level (conc. in extract) 

listed in Table 3 of Method 1668A?

 

SECTION E-3. QC INFORMATION – Method Blanks 

22. Blank: Was the Method blank extracted with each sample 

batch and analyzed immediately following the OPR?

(1668A/15.6)

 

23. Methods blanks/ Ongoing Laboratory Batch Blanks: 

Note any compounds found in the blank at greater than the 

minimum level listed in Table 2 of Method 1668A. 

(1668A/9.5.2) 

Analysis should not be performed if blank is above minimum 

level or within a factor of 3 of the regulatory limit, whichever 

is greater. 

– Were blank results less than the minimum level 

in1668A -Table 2? (1668A/9.5.2) 

 

24. Field Blank: Reagent water or other reference matrix placed 

in a sample container in the laboratory or the field, and 

treated as a sample in all respects for the purpose of 

determining if the field or sample transporting procedures 

and environments have contaminated the sample. 

Was Field Blank reported? Was the Field Blank above the 

detection limit? 

 

SECTION F. RECOVERY OF LABELED ISOTOPE DILUTION INTERNAL 

STANDARDS 

1. Recovery of labeled compounds: The recovery criteria of 

each labeled compound are listed in Table 6 of Method 

1668A. 

Did the average recovery % meet the criteria? 

(1668A/18.5.1) 

(Note: Background of IUPAC numbers 105, 114, 118, 123, 

156 and 167 are common) 

 

2. Recovery of labeled compounds: If recovery criteria of the 

labeled compounds are not met, was sample dilution 

analyzed? (1668A/18.5.1) 

 

3. Recovery of labeled compounds: If recovery criteria of the 

labeled compounds are not met in the diluted sample, was the 

calibration verified with a CCV standard? (1668A/18.5.2) 

 

4. Recovery of labeled compounds: If the calibration can not 

be verified, was another calibration performed and the 

sample re-analyzed? (1668A/18.5.3) 

 
Laboratory Name:________________ CCH Episode #.:_____________ Method 1668A – Page 5 of 5 

SECTION G-1. DETAILED RAW DATA REVIEW – Compound Identification 

Quality Control 

The following criteria must be met for a GC peak to be 

identified as a CB: 

 

1. The signals for the two exact m/zs being monitored (listed in 

Table 7 of Method 1668A) must be present, and must 

maximize within the same two scans. (1668A/16.1) 

 

2. The signal-to-noise ratio (S/N) of each of the two exact 

m/zs must be greater than or equal to 2.5 for each compound 

in a sample. (1668A/16.2) If, through observation of the 

SICP, the S/N ratio looks questionable calculate an 

approximate S/N using the heights of the signals. Is the S/N 

ratio greater than or equal to 2.5? 

 

3. The ratio of the integrated ion areas of the two exact m/zs 

monitored (listed in Table 7 of Method 1668A) must be 

within the limit in Table 8 of 1668A or ± 15% of the ratio in 

the CS-3 or CCV, if the CCV is more recent. (1668A/16.3). 

 

4. Relative Retention Times: The relative retention time 

(RRT) of the peaks representing a CB must be within the 

window specified in Table 2 of Method 1668A. 

(1668A/16.4) 

 

SECTION G-2. DETAILED RAW DATA REVIEW – Sample Results

5. Sample Results: Were the sample results less than five 

times the Method Blank results?

 

6. Sample Results: Were the sample results at least greater 

than ten times the Method Blank results?

 

7. Minimum Levels: Were the minimum levels reported by 

the lab comparable to those specified in the method?

 

8. MS/MSD: If a MS/MSD was reported, were the recoveries 

within ± 50%?

 

9. Duplicate Samples: Were duplicate samples collected? 

Were the RPDs less than 20%?