Karluss Thomas 

Senior Director 

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 

WASHINGTON, D.C. 20460 

DEC 0 4 2014 

Silicones Environmental, Health. and Safety Center 

American Chemistry Council 

700 2nd Street NE 

Washington, DC 20002 

Re: Quality Assurance Project Plan (QAPP) 

OFFICE OF CHEMICAL SAFETY 

AND POLLUTION PREVENTION 

Testing Consent Order for Octamethylcyclotetrasiloxane (D4) (CASRN: 556-67-2) 

40 C.F.R. 799.5000 

EPA-HQ-OPPT-20 12-0209 

·rhis letter is in response to your October l, 2014, submission of a Quality Assurance Project Plan 

(QAPP) as identified in the April 4, 2014, Enforceable Consent Agreement (ECA) for Environmental 

Testing for Octamethylcyclotetrasi loxane (D4) between the U.S. Environmental Protection Agency and 

five manufacturers of the chemical. While the QAPP as submitted has not fully fulfilled the requirement 

of the ECA, described below are EPA's comments on the submission. In addition, particular deficiencies 

and needs for claritication are identified in the enclosed table. The D4 environmental monitoring 

program may commence after all the issues in this letter and the attached table have been resolved and 

EPA has approved the Study Plan and QAPP. 

Major Comments: 

1. Modifications to the Study Plan (including site specific sampling plans) shall follow procedure 

identified in the ECA and codified in 40 CFR 790.68. Although not a requirement, EPA 

encourages SEHSC to develop and include in the QAPP contingency plans for (a) the major and 

minor Study Plan (including site-specific sampling plans adjustments and schedule changes 

related to potential challenges encountered during tield work activities) and (b) criteria for 

determining if post-implementation notifications to EPA are preferable to pre-implementation 

notifications. 

2. Representatives from both laboratories are required to sign the QAPP; in particular, the project 

manager and the QA manager from each laboratory must sign the QAPP. In addition, the 

database software and how stored information will be recorded, archived and transmitted 

amongst the participants must be described in the QAPP with greater detail and specificity. 

3. Further detail must be provided in the QAPP to describe the data quality objectives (DQOs) for 

the analytics and under what conditions data may be rejected. A procedure for who would be 

responsible for determining how to handle rejected data and considerations for replacement of 

rejected data must be described in the QAPP. The QAPP must also identify where rejected data 

Internet Address (URL) ·http //www epa gov 

Recycled/Recyclable • Pr,nted w1th Vegetable 011 Based Inks on 100% Postconsumer. Process Chlorine Free Recycled Paper 
will be discussed in the final or interim reports. Rejected data must be presented in one of the 

reports, not only in the bulk raw data submission. Please refer to Group A 7, Quality Objectives 

and Criteria for Measurement Data and 85, Quality Control Requirements. 

4. The QAPP states that primary samples will be disposed of by the laboratory 30 days after 

submitting the data package to EPA and the retained samples will be disposed of following QA 

verification. Based on the frequency of Interim and Final Reports, both of these disposal triggers 

will likely occur before EPA has an opportunity to review the raw and summary data from the 

analysis. The QAPP must be revised to allow EPA sufficient time to review this data. 

Deficiencies and Clarifications: 

Deficiencies and needs for clarification were identified by comparing the QAPP to the enclosed table of 

requirements in the ECA and EPA's 2002 QAPP guidance. The identified deficiencies must be 

addressed in a modified QAPP covering the direct discharge and WWTP sites. 

If you have any questions, please contact Heather Njo or my stafTat 202-564-2574 or at 

njo.hcather@epa.gov. 

Enclosure 

Jeff Monis, Deputy Director for Pror:,TTams 

Office of Pollution Prevention and Toxics 
Review Checklist: Quality Assurance Project Plan (QAPP) D4 Environmental Testing Study Versus ECA Requirements and EPA Guidance

Page 1 of 6

EPA 2002 QAPP Guidance ECA Requirement Defficiencies and Clarifications

Group A: Project Management 

A1. Title and approval sheet - Section 2.1 - Page 9

Title:

Organization name:

Dated signature of project manager:

Dated signature of QA officer: Note, signatures and dates will be added when QAPP is approved. It is 

also necessary for a representative of each of the labs to sign the 

QAPP.

Other signatures, as needed: Must add a representative from the laboratories to the QAPP signature 

list.

A2. Table of Contents and Document Control Format - Section 2.2 - 

Page 9 

Includes Table of Contents:

Includes document control format:

A3. Distribution List - Section 2.3 - Page 9 

Includes a list of people who will receive the completed QAPP:

A4. Project/Task Organization - Section 2.4 - Page 9

Identifies key individuals, w/ their responsibilities (data users, decisionmakers, project QA manager, subcontractors, etc.):

A5. Problem Definition/Background - Section 2.5 - Page 11 

Clearly states problem or decision to be resolved:

Provides historical and scientific background info.:

A6. Project /Task Description - Section 2.6 - Page 11 

Lists measurements to be made:

Cites applicable technical, regulatory, or program-specific quality 

standards, criteria, or objectives:

Notes special personnel or equipment requirements:

Identifies the assessment tools needed:

Provides work schedule:

Notes required project and QA records/reports:

A7. Quality Objectives and Criteria for Measurement Data - Sect. 

2.7 - P. 16

States project objectives and limits, both qualitatively and 

quantitatively:

Table 2-6 does not provide the Data Quality Objectives (DQOs), but 

rather summarizes the DQO process for this program. As the QAPP 

and supporting documents address the DQO process for this program, 

Table 2-6 is redundant and unnecessary because the DQOs for this 

program are the performance and acceptance criteria provided in 

Tables 2-7 through 2-9.

(1) See comments under Section B5 below regarding development of 

DQOs for sampling and analytical precision. 

(2) See EPA Comment #(2) under Section B5 below regarding 

developing a DQO for Relative Percent Difference (RPD) between 

pairs of field spikes to these tables.

(3) Please provide info. on how bias will be assessed (i.e., qualitatively 

or quantitatively) and how sensitivity will be assessed (i.e., MDLs, 

LOQ, etc.).

(4) EPA suggests adding depth measurement to Table 2-7. The 

importance of collecting samples at a certain depth was stated, thus 

this info. should be included in the QAPP. EPA suggests adding the 

instrument that will be used to perform this assessment and the 

instruction manual's performance criteria. Additionally, EPA suggests 

adding the instrumentation that will be used for all measurements and 

to add the sensitivity for water quality.

(5) Footnote 1 in Table 2-8 indicates that field spike QC samples that 

do not meet the target limit "will raise questions that must be resolved 

prior to acceptance of the data." Please describe the types of questions 

that may be anticipated, the steps that will be undertaken to resolve 

them, and the criteria that will be considered in evaluating acceptance 

of the data.

(6) The term "Field Blank" in Table 2-8 and throughout the QAPP is too 

vague and inconsistent (e.g., reference material field blank, split 

sample unspiked (field blank), lab water field blank, surface water field 

blank).

A8. Special training/Certification Requirements - Section 2.8 - 

Page 19

Lists special training and certification requirements:

A9. Documentation and Records - Section 2.9 - Page 21

1) An Interim Progress Report is required 180 days after the Effective 

Date of the ECA and every 180 days thereafter until all obligations are 

fulfilled. Interim Progress Reports shall include a summary of work 

completed to date, any proposed changes in protocols or schedule, 

raw data, and any other matters affecting progress of testing.

2) The Final Report is due no later than 150 days following completion 

of the required environmental testing (i.e., collection and analysis of the 

data). The Final Report shall include a description of monitoring 

performed, summary of test results, raw data, laboratory analyses, and 

QA/QC info., as per 40 CFR 792.185.

3) "The Signatory Companies will document all QA/QC work done as 

part of the Testing Program."

4) "The Signatory Companies will electronically submit all of the raw 

data (as defined in 40 CFR 792.3)..."

Describes process and responsibilities for ensuring that the most 

current approved version of the QAPP is available:

Specifies the level of detail of the field sampling and/or lab analysis 

narrative needed to completely describe difficulties encountered:

Gives retention time and location for records and reports: Records shall be retained per 40 CFR 792.195.

Group B: Measurement/Data Acquisition

B1. Sampling Process Design (Experimental Design) - Section 3.1 - 

Page 26

States and characterizes measurements quality objectives as 

applicable action levels or criteria:

Lists info. and records to be included in data reports (eg., raw data, 

field logs, results of QC checks, problems encountered):
Review Checklist: Quality Assurance Project Plan (QAPP) D4 Environmental Testing Study Versus ECA Requirements and EPA Guidance

Page 2 of 6

EPA 2002 QAPP Guidance ECA Requirement Defficiencies and Clarifications

Direct Discharge Sites:

1) Sample Types (App. 1): wastewater treatment effluent, receiving 

stream surface water, receiving stream sediment, receiving stream 

biota.

States sampling network design and rationale:

Direct Discharge Sites:

1) Sample Locations (App. 1): The 4 direct dischargers (Dow Corning 

Carrollton Plant; MPM Silicones Waterford Plant; MPM Silicones 

Sisterville Plant; Wacker Adrian Plant). 

2) Sampling Frequency (App. 1): "Samples shall be taken during two 

testing events at least 3 months apart. The exact duration between 

sampling events for each site shall be determined in a detailed 

Sampling Plan included in the Study Plan and QAPP." 

3) Effluent Sample Locations (App. 4): "At each site, effluent samples 

shall be collected at the regulated compliance point per the WWTP's 

discharge permit."

 4) Surface Water Sample Locations (App. 5): "At each site, surface 

water samples should be collected at approximately the same location 

and roughly the same time as benthic organisms are collected which is 

described in App. 8."

 5) Sediment Sample Locations (App. 7): "At each site, sediment 

samples from the receiving water body shall be collected at 

approximately the same location where benthic organisms are 

collected for D4 analysis as described in App. 8." 

6) Biota Sample Locations (App. 8): "At each site, benthic organisms 

shall be collected as close as reasonably possible to the effluent outfall 

provided adequate mixing of the discharge and receiving water has 

occurred and where adequate benthic organism sample masses are 

obtained."

Identifies sample matrices: Direct Discharge Sites: Sample Matrices (App. 1): wastewater 

treatment effluent, receiving stream surface water, receiving stream 

sediment, receiving stream biota.

Gives appropriate validation study info. for non-standard situations:

B2. Sampling Methods Requirements - Section 3.2 

Influent and Effluent Samples (App. 4): 1) "Influent and effluent 

samples will be collected as grab samples and not composite samples 

due [to] the expected high degree of volatilization of D4 from aqueous 

samples." 2) "For each site, procedures for collecting grab samples of 

influent and effluent will be based on USEPA 2013 (Wastewater 

Sampling, Section 4, Sample Types and Section 6, Manual Sampling, 

pp. 14-15, 20), USEPA 2004 (NPDES Compliance Inspection Manual, 

Section 5B, Sampling Procedures and Techniques, pp. 5-3 to 5-7), 

Knoerr 2013 (Sample Collection section), and APHA 1999 (Part 1060 

Collection and Preservation of Samples, pp. 48-62) if appropriate given 

the site-specific circumstances.

 Surface Water Samples (App. 5): During preparation of the sitespecific Sampling Plans, the physical nature (e.g., width, depth, flow) 

of the receiving water will be determined and used to guide the 

selection of the appropriate method of sample collection. For each site, 

collection procedures for surface water samples shall be based, as 

appropriate to the characteristics of the receiving water, on USEPA 

1994 (SOP #2013, Section 7.3 Sample Collection, pp. 3-4) (USEPA 

1994).

 Sediment Samples (App. 7): 1) During preparation of the site-specific 

Sampling Plans, the physical nature (e.g., width, depth, flow) of the 

receiving water will be determined and used to guide the selection of 

the appropriate method of sample collection. For each site, collection 

procedures for sediment samples shall be based, as appropriate to the 

characteristics of the receiving water, on techniques described in 

USEPA 1994 (SOP #2016, Sections 2-5,7, pp. 1-7) and USEPA (2001) 

(Chapter 3, pp. 3-1 to 3-17)." 2) "Sample collection, storage and 

preparation will follow Powell and Woodburn (2009) w/ each sample 

being placed in a plastic bag, homogenized, then placed directly into a 

glass jar, and then capped.

 Biota Samples (App. 8): 1) Benthic Organism Samples: During 

preparation of the site-specific Sampling Plans, the physical nature 

(e.g., width, depth, flow) of the receiving water will be determined and 

used to guide the selection of the appropriate method of sample 

collection. For each site, collection procedures for sediment samples 

shall be based, as appropriate to the characteristics of the receiving 

water, on techniques described in Powell and Woodburn (2009, 

Sample Collection, p. 9) and USEPA (2003a, Sections 5.2 Sampling 

for Community Samples and 5.3 Sampling for Analytical 

Measurements)." 2) Fish Samples: "During preparation of the sitespecific Sampling Plans, the physical nature (e.g., width, depth, flow) 

of the receiving water will be determined and used to guide the 

selection of the appropriate method of sample collection. For each site, 

collection procedures will be based, as appropriate to the 

characteristics of the receiving water, on USEPA 2003a (Section 7.0 

Procedures, pp. 3-5) and Powell and Woodburn (2009, Sample 

Collection, p. 8)."

Gives sampling locations and sampling frequency: EPA suggests adding sampling locations for sediment and benthic as 

discussed in response to study plan. Not all WWTP are specified as of 

this date, as expected. 

Identifies sample collection procedures and methods: EPA suggests including info. on the headspace left w/in each of the 

sample bottles.

Lists samples required as to type and number: EPA suggests revising the column headings in Table 2-5 to clarify that 

the reported numbers are per site per event (instead of per site). Labels 

for each of the rows at the bottom of Table 2-5 should start w/ the word 

"Total". Additionally, it's confusing that the numbers reported in the 

columns do not sum to the totals listed in the bottom rows. EPA 

suggests revising the table format to better indicate the split between 

the top and bottom of the tables (e.g., double border or shading), and 

adding a footnote to explain how the totals are calculated.
Review Checklist: Quality Assurance Project Plan (QAPP) D4 Environmental Testing Study Versus ECA Requirements and EPA Guidance

Page 3 of 6

EPA 2002 QAPP Guidance ECA Requirement Defficiencies and Clarifications

Lists equipment needed: Presently, only sampling equipment is provided in this section. 

However, Sect. 3.6.1 identified additional equipment that are used to 

determine water depth, scales, electrofishing, etc. The additional 

equipment provided in Sect. 3.6.1 pertain to sampling and therefore 

should be included in the list of equipment provided.

Identifies support facilities:

Identifies individuals responsible for corrective actions:

Describes process for preparation and decontamination of sampling 

equipment:

Influent and Effluent Samples (App. 4) and Surface Water Samples 

(App. 5): "Immediately prior to each sampling event at each site, the 

laboratory that will analyze the samples shall prepare clean (new, 

never used) glass sample containers in sufficient numbers for all 

[influent and effluent or surface water] samples to be analyzed for D4, 

for all QA samples, and for retain samples. The sample containers will 

be prepared by pre-washing w/ hexane, adding low density 

polyethylene (LDPE) sorbent into the containers, providing 

polytetrafluoroethylene (PTFE) tape to assist in sealing the containers 

(as described in Knoerr 2013, Sample Collection section), as well as 

providing labels. The laboratory will ship all sample containers w/ 

adequate packing materials in coolers to each site. The coolers will 

also contain chain-of-custody forms that will accompany the sample 

containers from the laboratory to the field and back to the laboratory."

Sediment Samples (App. 7) and Biota Samples (App. 8):

Same as above, except where underlined: "...shall prepare clean (new, 

never used) pre-weighed glass sample containers in sufficient 

numbers...The sample containers will be prepared by pre-washing w/ 

hexane, providing polytetrafluoroethylene (PTFE) tape to assist in 

sealing the containers, as well as providing labels..."

Influent and Effluent Samples (App. 4), Surface Water Samples (App. 

5), and Sediment Samples (App. 7): "Sealed sample containers will be 

packed into coolers w/ blue-ice or water ice, and taken back to the 

laboratory or shipped back to the laboratory using an overnight express 

shipping company." 

Biota Samples (App. 8): 1) Benthic Organisms: "Benthic organisms will 

be separated from the sediment and five composite samples shall be 

prepared by randomly dividing the collected organisms into glass 

containers and freezing prior to shipment. Prior to preparing composite 

samples, the taxa represented in the sample will be noted at the lowest 

level possible. Frozen samples will be packed into coolers w/ dry ice 

and taken back to the laboratory or shipped back to the laboratory 

using an overnight express shipping company." 2) Fish Samples: 

"Individual fish will be doubly bagged using polyethylene bags and 

frozen prior to shipment. Composited fish will be placed in sample 

containers and frozen prior to shipment. Frozen samples will be packed 

into coolers w/ dry ice and taken back to or shipped back to the 

laboratory using an overnight express shipping company."

B3. Sample Handling and Custody Requirements - Section 3.3 

Notes sample handling requirements: Special Considerations for D4 (Appendices 4, 5, 6, 7, and 8): 

"Specific requirements for collecting and handling...samples aimed at 

preventing sample contamination by sources of D4 that are not specific 

to the WWTP or direct discharge site shall be specified in the Study 

Plan and QAPP."

Information is presented w/in the QAPP. However, page 31 indicates 

that sample container, minimum sample volume, preservation and 

maximum storage requirements are presented in Table 3-2. Table 3-2 

shows the analytical methods. Need to make sure that tables and 

figures are referenced consistently throughout the document.

Notes chain of custody procedures, if required: The chain-of-custody procedures provided for Field QC samples is 

confusing and incomplete. Section 3.3.2.1 of the QAPP states "COC 

forms will not identify field QC samples, such as field blanks or field 

spike samples. Field QC samples will be designated following the 

procedures presented in Section 3.2.5.2 of the QAPP." However, 

Section 3.2.5.2 of the QAPP does not exist. Section 4.0 of SOP 100 

(Field Sample Custody) states "COC forms will not identify field QC 

(QC) samples, such as field blanks or field spike samples. Field QC 

samples will be designated following the procedures presented in 

Section 3.5.1 of the QAPP." However, Section 3.5.1 of the QAPP does 

not discuss custody of QC samples. Please describe how custody of 

field QC samples will be maintained and documented.

B4. Analytical Methods Requirements - Section 3.4 - Page 38

Influent, Effluent, and Surface Water Sample Analysis for D4 

(Appendices 4 and 5)

"The commercial laboratory will validate a method for the analysis of 

D4 in the...samples that shall be adapted from the analytical method 

specified in Knoerr (2013)...the water sample and the LDPE sorbent 

are solvent extracted and processed for analysis w/ GC-MS."

"During method development, the Knoerr (2013) analytical method for 

D4 achieved a matrix-specific MDL of 0.037 μg/L which shall be 

achieved for influent and effluent testing. The specific level of detection 

shall be based on the LOQ which shall be 3 times the MDL.

 

 

"Influent, Effluent, and Surface Water Sample Analysis for TOC 

(Appendices 4 and 5):

"The TOC analyses shall follow procedures equivalent to APHA 1999 

Part 5310, Total Organic Carbon (TOC)."

Describes selection and preparation of sample containers and sample 

volumes:

Sample hold time is not provided in this section, however, it is 

mentioned as a stability study in section 3.4.4. EPA suggests providing 

how long each sample will be stored from sampling until analysis in this 

section.

Describes preservation methods and maximum holding times:

Identifies analytical methods to be followed (w/ all options) and 

required equipment:

As previously mentioned under QAPP Element B2 Sampling Methods 

Requirements, EPA suggests including info. on sample headspace. 

Specifically, will there be headspace in the extracted sample vial ready 

for analysis and how long will the sample wait in the autosampler 

before being analyzed. Any effects to the measurements caused by 

wait time in the auto sampler before analysis shall be described.
Review Checklist: Quality Assurance Project Plan (QAPP) D4 Environmental Testing Study Versus ECA Requirements and EPA Guidance

Page 4 of 6

EPA 2002 QAPP Guidance ECA Requirement Defficiencies and Clarifications

Sediment Sample Analysis for D4 (Appendix 7):

"The commercial laboratory will validate a method for the analysis of 

D4 in sediment samples that shall be adapted from the analytical 

method specified in Powell (2010)."

"The method for analyzing D4 in sediment reported by Powell (2010) is 

deemed the appropriate method for achieving an MDL up to 3.7 ng/g 

(wet weight, ww) and shall be achieved for sediment. The specific level 

of detection shall be based on the LOQ which shall be 3 times the 

MDL. All measurements of D4 concentration in sediment shall include 

sufficient info. to perform a wet weight to dry weight conversion and 

shall report concentrations in terms of dry weight." 

Sediment Sample Analysis for TOC (Appendix 7):

"Following the general procedures of Powell and Woodburn (2009, 

Characterization of Sediments, p. 10) these additional samples shall be 

analyzed by carbon coulometry or an equivalent method for total 

carbon, total inorganic carbon, and total organic carbon, and loss-onignition for total water content and total organic matter content."

Biota Sample Analysis for D4 (Appendix 8):

"The commercial laboratory will validate a method for the analysis of 

D4 in biota samples that shall be adapted from the analytical method 

specified in Powell and Woodburn (2009, Analysis of Cyclic Volatile 

Methylsiloxane (cVMS) Materials section, Extraction of Fish and 

Benthic Macroinvertebrates sub-section, p. 13, and QC, p. 14). The 

Powell and Woodburn (2009) analytical method involves extraction of 

aliquots of homogenized biota samples and QA samples followed by 

quantification using GC-MS."

"The method for analyzing D4 in biota reported by Campbell 2010; 

Durham 2010a and 2010b; Kaj 2005; Powell 2010a and 2010b; and 

Powell and Woodburn (2009) is deemed the appropriate method for an 

MDL of 0.2 to 3.0 ng/g (wet weight, ww). An MDL up to a value not 

exceeding 3.0 ng/g (wet weight, ww) shall be applied for biota. The 

specific level of detection shall be based on the LOQ which shall be 3 

times the MDL." Biota Sample Analysis for Lipids (Appendix 8):

"Lipid analysis will be performed on two ground rainbow trout field 

blanks. The method for analysis of lipid content of the composited 

benthic organism samples will be the same as used for fish. 

Procedures equivalent to Powell and Woodburn (2009) 

Characterization of Fish and Benthic Macroinvertebrates, p. 11 shall be 

used to measure liquid contents in the benthic organism samples."

Provides available validation and/or performance info. for non-standard 

methods:

Identifies individuals responsible for corrective actions: This is not covered in the QAPP. EPA suggests adding text that 

specifies the responsible party for corrective actions.

Specifies needed laboratory turnaround time if important to project 

schedule:

This is not covered in the QAPP. EPA suggests adding text that 

specifies the lab analysis turnaround time.

B5. QC Requirements - Section 3.5 - Page 41

Influent, Effluent, and Surface Water Samples (Appendices 4 & 5):

1) "Grab samples 3, 4 and 5 will be divided to provide two duplicates 

for analysis of D4. The duplicate samples shall be processed and 

analyzed as individual samples for D4. Duplicate samples are used to 

evaluate between-sample variability and precision."

2) "Grab samples 6 and 7 will serve as retain samples."

3) "Grab samples 1 and 2 will serve as field blank/field spike samples. 

The field blank/field spike samples will be split into two parts. One part 

will be analyzed for D4 as is (field blank) and the second part will be 

spiked w/ a known amount of D4 and then analyzed (field spike). The 

field blank/field spike samples will be used to evaluate contamination 

bias resulting from sample collection, processing, transport, storage 

and analysis. During each...sampling event at a given site, two 

laboratory blanks will also be prepared. The two laboratory blanks shall 

be created from two samples of laboratory-grade water having 

concentrations of D4 below the Limit of Quantification (LOQ) and shall 

be taken into the field and processed like [a]...sample. The laboratory 

blanks will be used to evaluate contamination bias resulting from 

collection, processing, transport, storage, and analysis of samples."

Sediment Samples (Appendix 7):

1) "Sediment samples 3, 4 and 5 will be divided to provide two 

duplicates for analysis of D4."

2) "Sediment samples 6 and 7 will serve as retain samples."

3) "Sediment samples 1 and 2 shall be split, one half of each sample 

shall be spiked in the field w/ a known amount of D4...Two reference 

sediment samples having concentrations of D4 below the LOQ for this 

matrix shall be taken into the field and processed like sediment 

samples."

Identifies QC procedures and frequency for each sampling, analysis, or 

measurement technique, as well as associated acceptance criteria and 

corrective action:

(1) EPA suggests adding a discussion of QC requirements for duplicate 

investigative samples, including the development of DQOs for 

sampling and analytical precision, as appropriate. Section IX.A of the 

ECA requires the submission of a QAPP prepared in accordance w/ 

EPA guidance (USEPA Guidance for QA Project Plans, QA/G-5). 

Section 2.2.5 of EPA QA/G-5 describes the purpose of QC and 

provides guidance on the content for QC for field sampling programs 

including blanks, spikes, and split samples. For example, Section 2.2.5 

of EPA QA/G-5 states "Replicate samples and split samples are 

commonly used to denote the level of precision in the measurement or 

collection system." Duplicate investigative samples are clearly a critical 

QC element of the sampling process design for this program 

regardless of their identification as "Study Samples" versus "QA 

Samples" w/in the ECA. For example, per the ECA, "Duplicate samples 

are used to evaluate between-sample variability and precision." (Note 

that Section 5 of the SOPs prepared for this program correctly identify 

the following as Field QA/QC Samples: split (duplicate) samples, 

unspiked field blanks, and spiked field blanks.) 

(2) Section 3.5.1.2 of the QAPP (Field Spikes) states "the RPD for 

each pair of field spikes will then be calculated by using the results of 

the spiked samples. The calculated %R and RPD will be compared to 

the target QC limits in Tables 2-8 and 3-4." EPA suggests adding the 

acceptance criterion for RPD between pairs of field spikes to these 

tables. 

(3) Overall the QAPP must clearly discuss acceptance criteria, DQO, 

criteria for rejecting data and corrective actions.
Review Checklist: Quality Assurance Project Plan (QAPP) D4 Environmental Testing Study Versus ECA Requirements and EPA Guidance

Page 5 of 6

EPA 2002 QAPP Guidance ECA Requirement Defficiencies and Clarifications

Biota Sample Analysis for D4 (Appendix 8):

Benthic Organism Samples

1) "Samples 1, 2 and 3 shall be divided into three parts. Two of the 

parts will serve as duplicates for D4 analysis and one part will be 

analyzed for lipid content."

2) "Samples 4 and 5 will be retained for analysis as needed."

Fish Samples

1) "For each of the two species, five individual fish or composited 

samples shall be prepared and frozen. In the laboratory three of the 

samples shall be thawed, homogenized and divided into three parts. 

Two of the parts will serve as duplicates for D4 analysis and one part 

will be analyzed for lipid content."

2) "Two of the five samples will be retained for analysis as needed."

Applies to both Benthic and Fish Samples:

"During each sampling event at a given site, two field blanks and two 

field spikes will be prepared as follows. Rainbow trout tissue purchased 

from a commercial fish hatchery will be ground into a homogeneous 

mixture. Samples of the ground rainbow trout will be prepared in the 

laboratory prior to sample collection and shipped to the field. Prior to 

shipping to the field, the ground rainbow trout samples will be analyzed 

and shown to have concentrations of D4 below the LOQ for this matrix. 

Serving as field blanks, two reference ground rainbow trout samples 

will be opened during preparation of the composite samples of benthic 

organisms...In addition, two of the ground rainbow trout samples shall 

be spiked in the field w/ a known amount of D4."

Referenced procedures used to calculate QC statistics (precision and 

bias or accuracy):

B6. Instrument/Equipment Testing, Inspection and Maintenance 

Requirements - Section 3.6 - Page 44 

Identifies acceptance testing of sampling and measurement systems:

Describes equipment preventive and corrective maintenance:

Notes availability and location of spare parts:

B7. Instrument Calibration and Frequency - Section 3.7 - Page 45

Identifies equipment needing calibration and frequency for such 

calibration:

Notes required calibration standard and/or equipment:

Cites calibration records and manner traceable to equipment:

B8. Inspection/Acceptance Requirements for Supplies and 

Consumables - Section 3.8 - Page 46 

States acceptance criteria for supplies and consumables:

Notes responsible individuals:

B9. Data Acquisition Requirements for Non-direct Measurements - 

Section 3.9 - Page 47

Identifies type of data needed from non-measurement sources (eg., 

computer databases and literature files) along w/ acceptance criteria 

for their use:

Direct Discharge Sites: Sample Timing (Appendix 1):

1) "Samples shall be collected during normal plant operations and 

during such times that effluent flow rates from the wastewater 

treatment system are representative of the normal plant operations."

2) "Samples shall be taken during typical weather conditions and not 

until at least 3 days after an unusual weather event such as a heavy 

rain storm. Samples shall be collected at a time when the rate of D4 

release is expected to be representative of the typical rate of release of 

D4 for that site."

Additional Measurements:

1) "Total effluent flow rate shall be recorede and reported." (Appendix 

1)

2) "The date and time of the most recent precipitation occurrence for 

each sapling event will be recored" (Appendices 4 and 5)

Sufficient info. is not provided in the QAPP regarding data quality, 

acceptance criteria, use of data, and data limitations. EPA 

recommends addressing uncertainties surrounding how the team will 

determine if the timing of a sampling event is acceptable, plant 

operations are "normal", and weather conditions are "typical". Please 

provide historical plant operation data, including process upsets for 

each plant. Please provide weather data for each plant . Please include 

a statement and sufficient supporting summary data to indicate what 

are considered "normal" plant operations.

“Samples shall be collected during normal plant operations and during 

such times that effluent flow rates from the wastewater treatment 

system are representative of the normal plant operations.” This need 

would be met if SEHSC submitted info. that both plant operations 

relevant to D4 were normal, effluent flow rates were representative 

preceding (by three days) and during the time of each sampling event. 

This could be accomplished by a succinct, written narrative of the 

associated process operations along w/ strictly necessary supporting 

process data. Any abnormal equipment or operating conditions that 

might have an impact on D4 effluent concentrations or flows should be 

clearly identified and explained. 

Describes any limitations of such data:

B10. Data Management - Section 3.10 - Page 47 

Describes standard record keeping, data storage, and retrieval 

requirements:

Further details on the database software and how the electronically 

stored data will be transmitted to the participants is needed. A version 

number for the database software and a description of how it will meet 

record keeping needs should be included in the QAPP.

Checklists of standard forms attached to QAPP:

Describes data handling equipment and procedures used to process, 

compile, and analyze data (e.g., required computer hardware and 

software):

Describes process for assuring that applicable info. resource 

management requirements are satisfied:

Group C: Assessment/Oversight

C1. Assessments and Response Actions - Section 4.1 - Page 51

(1) EPA recommends including info. regarding how the assessment of 

compliance w/ the SOPs will be recorded (i.e., checklist or other 

recording mechanism). The checklists provided in App. J for each 

event do not have a place to indicate compliance w/ each of the SOP 

bullets; only compliance w/ SOP 102 and 30 are recorded in the 

checklist. EPA suggests adding the other SOPs to the checklist.

Lists required number, frequency, and type of assessments w/ 

approximate dates and names of responsible personnel (assessment 

include but are not limited to peer review, management systems 

review, technical systems audits, performance evaluations and audits 

of data quality):

(3) Overall the QAPP must clearly discuss acceptance criteria, DQO, 

criteria for rejecting data and corrective actions.
Review Checklist: Quality Assurance Project Plan (QAPP) D4 Environmental Testing Study Versus ECA Requirements and EPA Guidance

Page 6 of 6

EPA 2002 QAPP Guidance ECA Requirement Defficiencies and Clarifications

 (2) EPA recommends having a checklist for performing GLP audits 

prior to going into the field to ensure that audits are performed 

consistently and to have documentation of this. The checklist should be 

included in the QAPP appendices and contain a description of 

expectations, similar to the info. provided in Tables 5-1 and 5-2. 

(3) Sect. 4.1.1.2 does not describe how an internal laboratory audit will 

be performed and what methods will be used to perform the audit. EPA 

suggests including a checklist of what systems will be audited as well 

as a description of the expectations, similar to the info. provided in 

Tables 5-1 and 5-2.

Identifies individuals responsible for corrective actions:

C2. Reports to Management - Section 4.2 - Page 56 

1) An Interim Progress Report is required 180 days after the Effective 

Date of the ECA and every 180 days thereafter until all obligations are 

fulfilled.

2) The Final Report is due no later than 150 days following completion 

of the required environmental testing (i.e., collection and analysis of the 

data).

Results of performance evaluations and audits: The Signatory Companies will document all QA/QC work done as part 

of the Testing Program.

EPA suggests adding the frequency.

Results of periodic data quality assessments: The Signatory Companies will document all QA/QC work done as part 

of the Testing Program.

EPA suggests adding the frequency.

Any significant QA problems: The Signatory Companies will document all QA/QC work done as part 

of the Testing Program.

EPA suggests adding the frequency.

Preparers and recipients of reports: EPA suggests specifying who will prepare the documents and who will 

receive them in a table or list w/in the document.

Group D: Data Validation and Usability

D1. Data Review, Validation, and Verification - Section 5.1 - Page 

58 

States criteria for accepting, rejecting, or qualifying data: EPA suggests adding a statement that specifies if analytical data does 

not fall w/in the acceptance criteria, the data will be reported but 

flagged. The flags that will be used should be specified w/in the 

document. EPA also suggests including references to the table(s) that 

contain the acceptance criteria. Add discussion on corrections if min. 

sample size problems arise from rejected or destroyed samples. 

Includes project-specific calculations or algorithms:

D2. Validation and Verification Methods - Section 5.2 - Page 59 

Describes process for data validation and verification:

Identifies issue resolution and responsible individuals:

Identifies method for conveying these results to data users:

D3. Reconciliation w/ User Requirements - Section 5.3 - Page 60

Describes process for reconciling project results w/ DQOs and 

reporting limitations on use of data:

Although it's mentioned who communicates/reports to whom, it is not 

clear how ERM is going to provide project status reports (e.g., monthly 

reports or monthly meetings). This info. should be included in this 

section.

Project status:

Lists required number, frequency, and type of assessments w/ 

approximate dates and names of responsible personnel (assessment 

include but are not limited to peer review, management systems 

review, technical systems audits, performance evaluations and audits 

of data quality):