f/EPA
   100.0
            United States
            Environmental Protection
            Agency
            Office of Toxic Substance*
            Exposure Evaluation Division
            Washington, DC 20460
EPA 560/5-87-012
February 1988
            Toxic Substances
Chlorinated Paraffins

A Report on the  Findings
from  Two  Field  Studies
Sugar Creek, Ohio
Tinkers Creek, Ohio

Volume II -  Appendix D,
The Quality  Assurance
Project  Plan
1 1
V, / \
^-*~. 	 , 	 ,. W*^A**-' 	 "V 	 -'" '--' -
1 1 1 1 1 1 1 1 1 1 1 1
                10    15     20    25
                  RETENTION TIME (MINUTES)
                         30
      35

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                         SECTION 1.0
                                                 Section No.: 1.0
                                                 Revision No.: 4
                                                 Date: 10/16/86
                                                 Page 1 of 1
                 CHLOROPARAFFIN ENVIRONMENTAL

                         FIELD STUDY



                QUALITY ASSURANCE PROJECT PLAN
                EPA/MRI CONTRACT NO.  68-02-4252
                    WORK ASSIGNMENT NO. 53

              EPA/BATTELLE CONTRACT NO. 68-02-4243
Approval for:
Midwest Research Institute
Eaul C. Constant
Program Manager
Date
          Approval for:
          Battelle Columbus Division
                rean ChessoE^     0  Date
               Project Manager
Carol L. Green             Date
Quality Assurance Officer
           imona Maye'r ' '^/f   Dae'
          Quality Assurance
           Administrator
                       Approval for:
              Environmental Protection Agency
         V^   'Jl'Mfr
 bsep*i J A Rreen
 reject Officer
MRI Contract
68-02-4252
Date
Cindy R. Stroup
Project Officer
Battelle contract
68-02-4243

                  'ETleen ReillyAWiedow  Date
                  EPA Quality Assurance
                    Officer
                               Date

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                LIST OF PLAN HOLDERS
MIDWEST RESEARCH INSTITUTE: P.Constant, J. Hosenfeld,  D.  Steele,
                            C. Green, Tom Janszen  (PEI)

BATTELLE COLUMBUS DIVISION: J. Chesson, R. Heath,  R. Mayer

ENVIRONMENTAL PROTECTION AGENCY:

                            J. Breen, C. Stroup, T. Murray,
                            C. Bass, S. Shapley, E. Reilly-Wiedow,
                            J. Glatz.

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   SECTION 2.0

TABLE OF CONTENTS
Section No.:  2.0
Revision No.: 3
Date: 10/16/86
Page 1 of 1
Section
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
11.0
12.0
Appendix
Appendix
Appendix
Appendix
Appendix
Heading Pages Revision Date
Title Page 1
Table of Contents 1
Project Description 2
Project Organization 9
and Management
Personnel Qualifications 2
Facilities, Equipment,
Consumables and Services 3
Experimental Design and 14
Data Generation
Data Processing 2
Data Quality Assessment 3
(Objectives)
Corrective Action 3
Documentation and Reporting 2
References 1
A - Field Study and Sampling
Design for Sugar Creek
B - Field Study and Sampling
Design for Tinkers Creek
C - Analytical Method
D - Validation Procedures for Analytical
Method
E - PEI Qualifications
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10/16/86
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10/16/86
10/16/86
10/21/86
10/16/86
10/16/86
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9/12/86
10/16/86
11/11/86
11/18/86
9/12/86

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                              3                   Section No.:  3.0
                                                  Revision No.  3
                         SECTION 3.0              Date: 10/16/86
                                                  Page 1 of 2
                     PROJECT DESCRIPTION

     The Environmental Protection Agency/Office of Toxic
Substances (EPA/OTS) under the Existing Chemicals Program has
initiated simple field studies to screen selected waterbodies
for the presence of chlorinated paraffins (CPs). The information
gained from these field studies will be coupled with other
environmental and health studies and collectively contribute to
a risk assessment for this chemical.

     Studies conducted by both the U.S and Europe have found
CPs in environmental samples including sediment, tissue, water
and soil. However, the validity of the analytical methods
used to quantify these samples has been debated fostering a
continuing effort to solve significant analytical and inter-
ference problems.  Therefore, a critical first step to the
development of the field studies discussed in this Project
Plan was to develop and validate an analytical method
capable of measuring these constituents in different environ-
mental matrices. A complete description of this effort
and the analytical method of choice is provided in Appendix C.

     The objective of this field study effort is to collect
information that will help EPA determine, preliminarily, if
chlorinated paraffins exist in the water environment, i.e.
the water column (including suspended material), the sediment
and in biological tissue, and at what environmental levels.
Because chlorinated paraffins are used predominantly in the
lube oil business, this study is designed based on the assump-
tion that if CPs exist in the aquatic environment they will
most likely be found in waters receiving discharge from CP
manufacturers, processors of lubricating oils, and users of
these oils. Therefore, for the purposes of this study, two
areas have been selected for study and will,  therefore,
represent the water environment as expressed in the statement
of objective. The first is Sugar Creek in Dover Ohio; the second
is Tinkers Creek in Bedford, Ohio. Chlorinated paraffins will
be identified by chain length categories and will be quantified
in four environmental matrices.

3 .1  Scope of Work


     The scope of work will consist of the following subtasks:


     1.  Develop and field validate the analytical method
         for determining CPs of differing chain lengths for
         water column, suspended solids, sediment and tissue.

     2.  Develop a QA/QC project plan and a field study and
         sampling design for the sites selected. or the
         study. Combine these to form one document.

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                                              Section No.: 3.0
                                              Revision No.: 3
                                              Date: 10/16/86
                                              Page 2 of 2
     3-  Conduct a preliminary site visit (reconnaissance
         survey) of the study sites.

     4.  Finalize the study and sampling design with information
         obtained from the preliminary site visit.

     5.  Collect field samples at the sites selected for the
         study following the protocol expressed in this QAPP.

     6.  Perform the necessary laboratory analysis of the samples
         collected in the field.

     7.  Analyze data; prepare results and conclusions.

     8.  Write and submit draft and final reports.
     Subtasks 2, 3, 4, 7 and 8 will be developed cooperatively
by Exposure Evaluation Division's Field Studies Branch and
Design and Development Branch and their respective contractors,
Midwest Research Institute and Battelle Columbus Division.
Subtask 5 will be completed by Midwest Research Institute and
its subcontractor, PEI Associates.  Subtasks 1 and 6 will be
completed by MRI. The experimental design of the field study
will be developed by the Design and Development Branch and its
contractor, Battelle Columbus Division.

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                              5                   Section No.:  4.0
                                                  Revision No:  3
                         SECTION 4.0              Date: 10/16/86
                                                  Page 1 of 9
             PROJECT ORGANIZATION AND MANAGEMENT
       This project is being conducted as part of OTS1 Existing
Chemicals Program.  Focus and direction for the study is
provided by a Technical Team of OTS experts.  The field study
will be conducted largely by the Midwest Research Institute
and its contractor PEI Associates under contract to the Field
Studies Branch.  The experimental design, data analyses and
results and conclusions for the study will be developed by
the Design and Development Branch and its contractor, Battelle.

The overall project organization chart is shown in Figure 4.1.

4.1    Midwest Research Institute;

       The MRI project organizational chart is shown in
Figure 4.2.


4.1.1  Project Management

       Mr. Paul Constant will represent management and serve as
program manager.  He will be assisted in this effort by Mr.
John Hosenfeld.  Together they will:

  o    Assure that all necessary resources are available.

  o    Assure that the Quality Assurance Manager (QAM)/Quality
       Assurance Coordinator (QAC) is fully informed and involved
       in the project.

  o    Assure that all personnel are informed of project QA policy.

  o    Review all communication from the QAM/QAC regarding the
       project.

  o    Assure that any problems, deviations, etc. reported by
       the QAM/QAC receive immediate corrective action.

4.1.2  Quality Assurance Manager/Quality Assurance Coordinator

       Ms. Carol Green, Quality Assurance Manager,  will
represent QA management.  She will be assisted by Mr. Jack
Balsinger who will serve as QAC.  Together they will:

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                                                 Section No.:  4.0
                                                 Revision No.:2
                                                 Date:  9/12/86
                                                 Page  2 of 9
Experimental
Concept by DDE
and its Contractor
BATTELLE
Analytical Protocol
by FSB and Its
Contractor
MRI
              Conduct
              Reconnaissance
              Study & Collect
              Samples for Method
              Validation by MRI/
              PEI AND BATTELLE
                                            1
 Experimental
 Design by DDB
 and BATTELLE
     Method
     Validation by
     FSB and MRI
                                            T
                  Prepare
                  QAPP by FSB &
                   DDB
                  APPROVE QAPP
           Conduct Field Study
           and Perform Analysis by
           FSB and MRI/PEI


Transmit Field Study
Results to ECAD
     FIGURE 4-1  - Overall  Project  Organization

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                                              Section No.: 4.0
                                              Revision No.: 2
                                              Date: 9/12/86
                                              Page 3 of 9
                  DIRECTOR OF
                  K.C OPERATIONS
                               PROGRAM MANAGER
                                 P. Constant
                               DEPUTY PROGRAM
                                 MANAGER
                                 J. Hosenfeld
QUALITY ASSURANCE
      MANAGER

       C. Green

 QUALITY ASSURANCE
   COORDINATOR

  J. Balsinger
  QUALITY CONTROL
    COORDINATOR

      R. Ayling
SUBCONTRACTOR
     PEI
                              WORK ASSIGNMENT
                                   LEADER

                                  D. Steele
  Figure 4-2 MRI Project Organizational Chart

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                                                   Section No.:  4.0
                                                   Revision No.:  2
                                                   Date:  9/12/86
                                                   Page  4 of 9
   o   Assure that all QA policies and procedures  are  available
       and understood by project staff by conducting training
       courses.

   o   Assure MRI Management that the facilities,  equipment,
       personnel, methods, records and controls  are  consistent
       with project objectives/requirements by conducting or
       directing inspections and/or audits.  These inspection/
       audit results are reported to project  and MRI Management.
       Corrective action is requested in these reports.

   o   Help prepare the project QA plan.

   o   Reinspect or audit to assure that appropriate corrective
       actions were implemented.  Report unresolved  corrective
       actions to MRI's Associate Director of K.C. Operations
       and the Senior Vice President for resolution.

   o   Review and audit data reports and supporting evidence
       prior to submission to EPA.

   o   Prepare and direct the preparation of  QA reports  to be
       submitted to EPA.

4.1.3  QC Coordinator

       Mr. Randy Ayling will serve as QCC.  He will:

   o   Conduct systems audit(s) and report findings to the QAM/QAC.

   o   Prepare performance audit samples.

   o   Review notebooks, chromatograms, printouts, and other  hard
       copy information during systems audits.

   o   Report audit findings to project leader and program management
       after QAM/QAC approval.

4.1.4  Work Assignment Leader

       Mr. David Steele will be the work assignment leader. He
       will:

   o   Help prepare the project QA plan.

   o   Be responsible for training staff where required.

   o   Be responsible for sample receipt and  traceability.

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                                                Section No.:  4.0
                                                Revision No.:  2
                                                Date:  9/12/86
                                                Page 5 of 9

   o   Enforce instrument calibration and maintenance  procedures.

   o   Maintain document control of lab and sampling data/ notebooks,
       records, and other hard copy information.

   o   Review and approve all data prior to submittal  to EPA.

   o   Review/validate raw data (e.g., notebooks, forms, strip
       charts, etc.).

   o   Ensure that any deviations from protocol are approved and
       documented.

   o   Be responsible for analytical data traceability.

   o   Take correction action on any problems and communicate  them
       in writing to the QAC/QAM, the QCC, and the program and
       department managements.

   o   Prepare and submit monthly and triannual reports.

   o   Prepare and submit other reports as requested by the  work
       assignment manager in conjunction with project  staff.


4.2  PEI Associates


 The PEI project organizational chart is shown in Figure 4-3.

4.2.1  Project Management

   Mr. Les lingers will represent management and serve  as Program
Manager.  Mr. Unger's  responsibilities are:

  o  Assure that all necessary resources are available.

  o  Assure that the Quality Assurance Manager(QAM)/ Qualty Assurance
     Coordinator (QAC) is fully informed and involved  in the
     project.

  o  Assure that all personnel are informed of project QA policy.

  o  Review all communication from the QAM/QAC regarding the
     project.

  o  Assure that any problems, deviations, etc. reported by the
     QAM/QAC receive immediate corrective action.

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                            10
                                                        Section No.:4.0
                                                        Revision No.: 2
                                                        Date:  9/12/86
                                                        Page 6 of 9
                            MR I
                      PEI SENIOR MGMT
    DIRECTOR
  ENVIRONMENTAL
   MEASUREMENT
    DIVISION
  DIRECTOR
ENVIRONMENTAL
  ANALYSIS
  DIVISION
QUALITY ASSURANCE
 MANAGE R/QUALITY
    ASSURANCE
   COORDINATOR
    T. Wagner
   PROGRAM
   MANAGER

  L. Ungers
   QUALITY
   CONTROL
 COORDINATOR

  C. Zimmer
     WORK
  ASSIGNMENT
    LEADER

  T. Janszen
              FIGURE 4.3 - PEI ORGANIZATIONAL  CHART

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                            11
                                            Section No. :  4.0
                                            Revision No.  1
                                            Date:  9/12/86
                                            Page 7 of 9

4.2.2  Quality Assurance Manager/ Quality Assurance Coordinator

     Mr. Thomas Wagner, Quality Assurance Manager, will
represent QA management.  Mr. Wagner's responsibilities  are:

     o  Assure that all QA policies and procedures are available
        and understood by project staff by conducting training
        courses.

     o  Assure PEI Management that the facilities, equipment,
        personnel, methods, records and controls are consistent
        with project objectives/requirements by conducting
        or directing field sampling efforts.

     o  Help prepare the QA project plan.

     o  When necessary, assure that appropriate corrective actions
        were implemented. Report unresolved corrective actions
        to PEl's Program Manager.

     o  Review reports and supporting evidence prior to  submission
        to MRI.

     o  Prepare and direct the preparation of QA reports to be
        submitted to MRI.

4.2.3.  QC Coordinator

     Mr. Charles Zimmer will serve as QCC.  He will:

     o  Review notebooks, and other hard copy information during
        the performance of the work assignment.

     o  Report findings to the Project Leader and  program
        Management after QAM/QAC approval.

4.2.4   Work Assignment Leader

     Mr. Thomas Janszen will be the work assignment leader.   He
     will:

     o  Help prepare the QA project plan.

     o  Be responsible for training staff, where required.

     o  Be responsible for sample collection and transport of
        these samples to MRI.

     o  Maintain document control of sample collection,  notebooks,
        records, and other hard copy information.

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                           12                Section No.:  4.0
                                             Revision No.:  2
                                             Date:  10/16/86
                                             Page  8 of 9

     o  Review and approve all data prior  to  submittal to  MRI.

     o  Review/validate raw data (e.g.,  notebooks,  forms,  strip
        charts,  etc.)

     o  Ensure that any deviations from protocol  are approved
        and documented.

     o  Take corrective action on any problems  and  communicate
        them in writing to the QAM/QAC,  the QCC and the Program
        and Department Management.

     o  Prepare and submit monthly and triannual  reports.

     o  Prepare and submit other reports as requested by  the
        Work Assignment Manager in conjunction  with Project
        staff.


4.3    Battelle Columbus Division

       The Battelle Columbus Division project organizational  chart
       is shown in Figure 4-4.

4.3.1  Project Management

       Dr. Jean Chesson will represent management  and serve as
       program manager.

4.3.2  Quality Assurance Administrator

       Ms. R.  Mayer will represent QA management.

4.3.3  Work Assignment Leader

       Dr. J.  Chesson is the work assignment  leader.  She  will
       be assisted by  Mr. Robert Heath,  Consultant  to Battelle.
       Responsibilities include:

   o   Help prepare the QA plan.

   o   Prepare the experimental designs.

   o   Participate in  the reconnaissance survey.

   o   Contribute to the field activities.

   o   Review/validate data collected in the  field; formulate results,

   o   Analyze data.

   o   Contribute data analyses, results and  conclusions  to the
       final report.

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                           13
                         Section No. :  4.0
                         Revision No.  2
                         Date:  10/16/86
                         Page  9 of 9
                            DIRECTOR
                       BATTELLE COLUMBUS
                           DIVISION
PROJECT
MANAGER
J.  Chesson
INFORMATION &
ENGINEERING
SYSTEMS
                           QAA
                           R. Mayer
 TASK LEADER

 J. Chesson
R. Heath
Consultant
 Figure 4-4 Battelle Columbus Division Project
            Organizational Chart

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                              14                  Section No.: 5.0
                                                  Revision No.: 2
                                                  Date: 9/12/86
                                                  Page 1 of 2
                          SECTION 5
                   PERSONNEL QUALIFICATIONS

5.1  Midwest Research Institute

     Mr. Paul C. Constant, and Mr. John Hosenfeld will serve as
program manager and deputy manager, respectively.  Mr. Hosenfeld
will assist Mr. Constant.  Their credentials were previously
submitted in the proposal for this contract.  Mr. David Steele
will serve as the Work Assignment Leader.  Mr. Steele has served
as Work Assignment Leader on Tasks 39 and 42 during the previous
contract and is Work Assignment Leader on Task 53 of the present
contract.  His credentials were submitted in the proposal for
this contract.

     Ms. Carol Green will be the Quality Assurance Manager.  She
has served in this capacity since May 1983.  Her credentials were
previously submitted in the proposal for this contract.

     Mr. Jack Balsinger will be the Quality Assurance Coordinator.
He has been assigned to the QA Unit since June 1985.  His
credentials were previously submitted in the proposal for this
contract.

     Mr. Randy Ayling will serve as Quality Control Coordinator.
He is skilled in extraction techniques and mass spectral analyses
and has functioned as a Quality Control Coordinator on the previous
contract.

5.1.1 PEI Associates

     Mr. Les Ungers will serve as Program Manager for PEI.  Mr.
Ungers is a certified industrial hygienist.  His credentials were
submitted in the proposal for this contract.

     Mr. Tom Janszen, a biologist, will serve as the Work Assign-
ment Leader for PEI.  His credentials are contained in Appendix E.

     Mr. Tom Wagner will serve as the Quality Assurance Manager
and the Quality Assurance Coordinator.  His credentials are
contained in Appendix E.

     Mr. Charles Zimmer will serve as Quality Control Coordinator
for PEI.  His credentials are contained in Appendix E.

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                          15
                                             Section No.:  5.0
                                             Revision No. :  3
                                             Date:  10/16/86
                                             Page 2 of 2
5.2   Battelle Columbus Division

     Dr. Jean Chesson will serve as the Battelle Program Manager
and Task Leader. Her credentials can be found in the Battelle
contract.

     Ms. Ramona Mayer will serve as the Battelle Quality Assurance
Administrator.  Her credentials can be found in the Battelle
contract.

     Mr. Robert G. Heath will assist the work assignment leader.
He is a senior biometrician with thirty years experience and
managed the design and operation of several surveys and field
studies.  Mr. Heath is currently retired from government
service and is employed as a consultant to Battelle.

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                             16                   Section No. : 6.0
                                                  Revision No. :  3
                                                  Date: 10/16/86
                                                  Page 1 of 3

                         SECTION 6.0

                 MIDWEST RESEARCH INSTITUTE'S
       FACILITIES, EQUIPMENT, CONSUMABLES AND SERVICES

6.1  Facilities

     Sample preparation will be performed in MRI lab 315 W
designated in part for this project.  This laboratory is
equipped with the fume hoods, and analytical balance and the
volumetric glassware required to carry out this task.  Mass
spectral analyses and data processing will be performed in
one of MRI's mass spectrometer facilities (MRI Lab 144N).

6.2  Equipment

     The sampling equipment used on this task include:

     1.  0.5 gal glass jugs with teflon lined caps

     2.  0.5 Liter glass jars with teflon lined lids

     3.  Coolers

     4.  Clam rakes

     5.  Stainless steel sediment scoop

     6.  Floating platform (two canoes rafted together) for
         deep water sampling

     7.  Ekman dredge sampler

     8.  Kemmerer water column sampler

     9.  Hip waders

    10.  Transport vehicle with trailer hitch

    11.  100 ft. tape measure and 6 ft. folding ruler

    12.  Strapping Tape

    13.  Thermometer

    14.  Bubble pack packaging material

    15.  MRI address labels

    16.  Topographic maps

    17.  Stopwatch, logbook, camera,  indelible pens

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                           17
                                              Section No.: 6.0
                                              Revision No.:  2
                                              Date: 10/16/86
                                              Page 2 of 3

     The major piece of analytical equipment to be used on
this project is a Finnigan 4000 Gas Chromatograph/ Mass
Spectrometer system.  This system is equipped with a fused
silica capillary column, a negative chemical ionization source
and a J & W on column injector.  The system will be interfaced
to an Incos 2400 data handling system.

     The mass scale will be calibrated daily, in the negative
ion mode, using perfluorotributyl amine (FC-43) prior to
sample analysis.  For reproducibility of the relative abundance
measurements, the abundance ratio of the m/z 414: m/z 633 ions
will be adjusted to 1:3 ( + 10% ).

6-2.2  - Maintenance of the analytical equipment used in this
         task will be done according to manufacturers' specifi-
         cations and at their recommended frequency.  This is
         summarized in Table 6.1

6.3    Consumables

       - 0.45 micron filters (Millipore)
       - Hexane, non spectro grade (Burdick & Jackson)
       - Iso-octane, high purity (Burdick & Jackson)
       - Sulfuric acid, reagent grade (MCB)
       - Sodium Sulfate, ACS reagent grade
       - Alumina Woelm B, activity grade 1  (Woelm Pharma)
       - Silica gel, chromatography grade

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                          18
                      Section No.:  6. 0
                      Revision No.:  2
                      Date: 10/16/86
                      Page 3 of 3
                    TABLE 6.1 MAINTENANCE
Equipment
    Service
Frequency
1. Finniqan MAT 4000
2.  Incos Data System;
change forepump oil
change differential
 pump oil
clean ion source
bake out vacuum
 chamber
repair electronic
 components
repair or replace
 jet separator

change air filter on
 disk drive
align disk drives
repair or replace
 electronic components
                                                 as needed

                                                 as needed
                                                 as needed

                                                 as needed

                                                 as needed

                                                 as needed
                                                 6  months
                                                 as needed

                                                 as needed

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                             19                    Section No.:  7.0
                                                   Revision No.: 3
                                                   Date: 10/16/86
                                                   Page 1 of 14
                           SECTION 7.0

             EXPERIMENTAL DESIGN AND DATA GENERATION
7.0  INTRODUCTION

     Chlorinated paraffins (CXH/ 2x-y2)c-*-y) have been reported
to be toxic to mussels and rainbow trout at concentrations as
low as a few parts per billion.  Chlorinated paraffins are used
in several commercial products primarily as lubricating oil
additives (50% of total 1984 consumption).

     There is little available information on levels of CPs in
the environment.  Only three previous studies have been obtained:
two performed for Diamond Shamrock Corporation at Houston, Texas
and the Grand River, Ohio and a third by ICI Limited at numerous
sites in Great Britain [1,2,3].

     While there is some debate over the precision of the
analytical method used in these studies, they indicate that environ-
mental levels are found in the parts per billion range in the
water column and parts of per million range in sediment and biota.
Also, these studies indicate that CPs are widely distributed in
the environment.  For instance, CPs were found in foods and human
tissues and were detected upstream from any possible influence of
a CP manufacturing plant.

     Quantitation of CPs is complicated by the diverse nature of
the structures and potential interferences from other organochlorine
compounds.  Commercial CPs consist of mixtures of linear saturated
hydrocarbons with different chain lengths (C^g to C3Q), degrees
of chlorination (30-70 percent), and distribution of chlorine atoms
along the chain. Many positional isomers exist for each chemical
formula.

     The picture which emerges from these assessments is of a
contaminant that historically has been difficult to measure
analytically.  Further, while believed to be transported to the
environment primarily through the wastewater discharges
associated with CP manufacturing and use in the lube oil
industry, some data indicate that other transport mechanisms
are possible.

     We expect to find that due to its low aqueous solubility and
low vapor pressure, CPs will be relatively chemically stable in
the environment.  Further, we expect to find that most CPs will
rapidly adsorb to solids and settle to the substrate.

     Extensive effort has been given to developing an analytical
method capable of measuring these toxicants in different environ-
mental matrices.  A complete description of the analytical method
of choice and its validation are provided in Appendices C and D.

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                            20
                                                  Section No.:  7.0
                                                  Revision No.  2
                                                  Date: 10/16/86
                                                  Paqe 2 of 14
7.1  Study Objective
     The objective of this effort is to collect information
that will help EPA determine, preliminarily, if chlorinated
paraffins exist in the water environment ,i.e the water
column (including suspended material), the sediment and in bio-
logical tissue and at what environmental levels.   Because
chlorinated paraffins are used predominantly in the lube oil
business, this study is designed based on the assumption that
if CPs exist in the aquatic environment, they will most
likely be found in waters receiving discharge from CP manu-
facturers, processors of lubricating oils and users of these
oils.  Therefore, for the purposes of this study, a selection
of these receiving waters will represent the water environment
as expressed in the statement of objective.  The  first site
to be addressed is a site receiving discharge from a CP
manufacturer.  The second site is a site representing a user
of the lube oils.

7.2 Experimental Design

     The experimental design for this study has necessarily been
developed without the knowledge of the frequency  of occurrence
of residues in the study areas or the statistical parameters
of such residues. The design has also been developed with the
expectation that the precision and accuracy of the analytical
method (concurrently being determined) will be acceptable.
The design calls for the collection of water, sediment, and
tissue samples from a specified number of sampling stations.
These stations are deployed in the receiving water upstream of
and downstream from an identified industrial discharge point and
at designated locations within the plants' wastewater treatment
processes.

     The experimental design has been developed to meet the study
objective of screening the specified aqueous environment for the
presence of CP residues at the time of the individual field
studies.   As such, it is not a statistically-designed sample
survey of CP residues in the designated watersheds.

     The design allows for the data to be analyzed, at least
initially, using non-parametric statistical methods.  In particular,
the data for each medium should lend itself to a  Kruskel - Wallis
one way analysis of variance to determine whether statistically
significant differences exist among station residue levels.  Other
non-parametric measures of the consistency of results among data
sets are possible [4].

     All samples will be collected and handled using procedures
fully approved by EPA.

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                         21
                                             Section No.:  7.0
                                             Revision No.:  2
                                             Date: 10/16/86
                                             Page 3 of 14


     The design calls for the collection of a minimum of three
individual grab or composite samples of water and three
individual grab or composite samples of sediment at specified
locations (stations).

     The design also calls for the collection of mussels,  where
available.  It is anticipated that 8 to 10  small to medium
mussel specimens will be required to compose a sample.  Where
mussels are not available, efforts will be made to collect
invertebrate larval tissue. Fish may be collected if no other
biota are available.

     To enhance study efficiency snd minimize analytical costs,
analyses will be conducted in a logical sequence of sets and
subsets.  Three sets are to be constructed such that the first
set consists of the first samples of each type of medium
collected at each of the designated stations, the second set
comprises the second samples of each medium and so forth.
Subsets comprise all samples of a given medium within a set.
The decision to analyze a given set will depend on the analyti-
cal outcome of the previous sets.  The order of analyses of
subsets will be decided by the MRI analyst.

     As a partial measure of method validity, QC field samples
are included in this design.  In addition to providing a measure
of possible residue degradation during shipping and storage,
these samples also provide limited measures of method precision,
accuracy, and the probability of false negative outcomes.  (See
section 7.7).

     This experimental design is translated to the Sugar Creek
area in Appendix A; it is translated to the Tinkers Creek area
in Appendix B.

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                                                 Section No.:  7.0
                             22                  Revision No.:  3
                                                 Date: 10/16/86
                                                 Page 4 of 14
7.3    Site Specific Sampling Plans.

       o See Appendix A for the field sampling plan for Sugar Creek
         Dover, Ohio.

       o See Appendix B for the field sampling plan for Tinkers
         Creek, Bedford, Ohio.

7.3.1  Water Column Data.

       o Water Column samples will be limited by the field
         team's physical access to the stream.

       o For shallow waters,  collection will be achieved using
         a hand held, one half gallon glass jar. The
         jar will be submerged in the stream at mid-depth
         until all air is replaced by a water sample.

       o For deep waters,  collection will be achieved using
         a Kemmerer water sampler. These samples will
         be depth-integrated with collections made near the
         bottom, at mid-depth and near the surface.

       o See Appendices A and B for more detail.

7.3.2  Suspended Solids Data.

         The water samples will be filtered using a
         0.45 micron Millipore filter and the suspended
         solid fraction extracted and analyzed separately.

7.3.3  Sediment Data

       o Sediment samples will be limited by the field team's
         physical access to the stream.

       o For shallow waters,  collection will be achieved
         using a hand-held stainless steel scoop.

       o For deeper waters, collection will be achieved using
         an Ekman dredge sampler.

       o Sediment will be transferred to 500 ml. glass jars
         with teflon lined lids.

       o See Appendices A and B for more detail.

7,3.4  Tissue from mussels will be collected using a hand-held
       "clam rake". Larval samples will be collected by
       dredging and sieving or manually by overturning rocks
       and rubble. Any fish collection will be done with nets.

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                      23                  Section No.:  7.0
                                          Revision No.:  1
                                          Date:  9/12/86
                                          Page 5 of 14


7.3.5  Sample Preservation and Transportation


       Field samples will require no preservative.
       All sample jars will be stored in coolers and out of
       direct sunlight. They will be transported in ice-filled
       coolers with sufficient packaging material to reduce
       the possibility of breakage.   Any mussels collected
       during the field survey will  also be placed in an
       ice-filled cooler.  This is expected to help keep the
       mussels alive while being transported to  the MRI
       laboratory in Kansas City, Missouri. Upon arrival at
       the MRI laboratory all unhealthy or dead  mussels  will
       be discarded before analysis. All water,  sediment, and
       mussel samples will be shipped via commercial airlines
       or by overnight delivery service.

7.4    Field Quality Control

       Monitoring of toxic substances requires special  quality
       control procedures beyond those necessary for monitoring
       conventional parameters because toxicants generally occur
       in trace concentrations.  The most up-to-date sampling
       and handling procedures recommended by EPA for a  number
       of toxic and conventional parameters are  detailed in a
       recent publication [5].

       Monitoring for chlorinated paraffins requires even more
       demanding quality control procedures because of  the
       potential for contamination.  During this  study special
       precautions will be made to avoid this contamination.
       These include: using polythene gloves in  the field
       and in the laboratory to avoid possible contamination
       by the hands, avoiding seals  and paints which may
       contain CPs and avoiding PVC and plastic  materials which
       may contain CPs.

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                           24
                                            Section No.: 7.0
                                            Revision No.:  3
                                            Date: 10/16/86
                                            Page 6 of 14

       A Field Study Site Observation Sheet (Figure 7.2) will
       be filled out for each sampling station deployed in the
       field.  The field study crew will use this sheet to
       describe each sampling station site, weather conditions,
       and the like. Also, for each sample collected at a station,
       the field study crew will fill out the information
       required on Sample Data Sheets (Figures 7.3 and 7.4). The
       field study crew will use these sheets to record sample
       information such as the time of collection, depth of
       sample collection and the like.

       All samples will be uniquely identified with preprinted
       barcode labels.  Additionally, a data base will be
       used to record each sample as it arrives in the lab
       and to track the samples.  Data will also be recorded
       in laboratory notebooks on approved forms and on strip
       charts.

7.5    Sample Traceability

       The MRI sample traceability protocol will be followed for
       sample tracking for this project.  Traceability records
       will start with sample collection when samples are trans-
       ferred to the laboratory by the completion of the lower
       portion of the Sample Data Sheets.  The data base associated
       with the barcode traceability system will be used to record
       and monitor all sample transfers, all staff associated
       with transfers, and the date/time of all transfers.

7.5.1  Barcode labels

       Uniquely numbered barcode labels (printed as a set of 6)
       will be used to physically track samples for this project.
       One of the labels will be affixed to the sample container;
       and a second will be affixed to a Sample Data Sheet. The
       remaining labels will be affixed to subsamples as needed.

7.6    Laboratory Analysis Procedures

       See Appendix C for the analytical protocol.  A flow
       chart of the steps involved in the analytical method is
       shown in Figure 7.5.

7.7    Quality Control Checks

       Spiked water samples will be prepared at two stations in
       the Sugar Creek site(Stations B and LI) and two stations
       at the Tinkers Creek Site (Stations A and D). Water
       samples will be spiked at 50 ppb. The water sample collected
       from station LI at the Sugar Creek site will be taken
       at mid-depth for spiking.

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                              25
                                                   Section No.:  7.0
                                                   Revision No.:  2
                                                   Date: 9/12/86
                                                   Page 7 of 14
        FIGURE 7.2   FIELD STUDY OBSERVATION SHEET
Site ID: 	 Date: 	 Time:

   Signature:	 Title:	


Sampling Station Description:	
Weather Conditions:
Personal Observations
Dover CP production during Field Study: 	Ibs.

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              26
                 Section No.: 7.0
                 Revision No. :  2
                 Date: 9/12/86
                 Page 8 of 14
FIGURE 7.3    SAMPLE DATA SHEET
SUGAR CREEK
Field Study: DOVER, OHIO
Station ID:
Field:
Flow (cfs) :
Calculated :
Sample No.




i
1



Type of Sample
1 = water
2 = sediment
3 = mussel








Contract Number Date (Mo/Da/Yr)
68-02-4252
Work Assignment No. Substance Monitored:
Chlorinated Paraffin
Samples collected by:
Comp.
or
Grab








Samples relinquished to:


Temp.
C








Time








Depth
(ft)








Remarks








by: _on:
( Date )
   to:
by:
on:
                                                 (  Date )

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                                27
                         Section No.:  7.0
                         Revision No.:  2
                         Date:  9/12/86
                         Page 9 of 14
                  FIGURE 7.4
SAMPLE DATA SHEET
TINKERS CREEK
Field Study: BEDFORD, OHIO
Station ID:
Field:
Flow (cfs) :
Calculated:
Sample No.








Type of Sample
1 = water
2 = sediment
3 = larvae








Contract Number Date ( Mo/Da/ Yr)
68-02-4252
Work Assignment No. Substance Monitored:
Chlorinated Paraffin
Samples collected by:
Comp.
or
Grab








Temp.
C








Time








Depth
(ft)








Remarks








Samples relinquished to:

                     to:
        by:
        by:
on:

on:
(Date )

(  Date )

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                                    28
  Section No.:  7.0
  Revision No.: 2
  Date: 9/12/86
  Page 10 of 14
                               Sediment
                               (~ lOOg)
        Filter
                  Suspended
                   Solids
                       Dry ,  Soxhlet
                       Extraction with Hexane
Extract with Hexane
                        Column Chromatography:
                        H2S04/Silica Column,
                        Alumina Column
                                  T
         Biota
          /v lOOg)
Homogenize,
Dry,
Extract with Hexane

H2S04/Silica Slurry
Cleanup
                         Concentrate to
                               Analyze
               FIGURE  7.5   SCHEMATIC OF ANALYTICAL METHODS

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                                            Section No.: 7.0
                    29                      Revision No. 4
                                            Date: 11/14/86
                                            Page 11 of 14

These QC field samples will be collected in three 4-liter
glass jugs and transferred to one-half gallon glass
jugs for spiking.  Separate sets of 4 liter jugs will
be provided for stations B and LI.  Homogenization and
spiking will be done according to the following
procedure.

The four liter glass jugs will be pre-marked in the lab-
oratory at the 3-liter level.  The one-half gallon jugs
will be pre-marked in the lab at the 475, 950, and 1425
mL levels.  In the field, the 4-liter jugs will be
filled to the marks (3L) with water sample.  The first
jug will be shaken thoroughly and the contents poured
into the one-half gallon jugs to the first mark (475 mL).
The second and third 4-liter jugs will be used to fill
the one-half gallon jugs to the second and third marks
respectively.  Two of the four samples for each station
will be spiked at the 50 ppb level.  This will be done
by adding 1.0 mL of a chloroparaffin standard (approx-
imately 70 ug/mL each cell) in methanol.  The remaining
field QC samples will be spiked at the same level after
they are returned to the laboratory.

Extraction and analysis of the 8 QC samples (4 samples
from each of two stations), constituting 16 analyses
(8 filtrate and 8 suspended solids fractions) will be
done at the same time the field samples are analyzed
(see Appendix A, Table 5 and Appendix B,  Table 5)

In addition to these field QC samples, trip QC samples
will be prepared as follows:

Two samples of laboratory deionized water (volume = 1425 Ml)
will be prepared for each of the four QC stations,
i.e. stations LI and B (Sugar Cr.) and stations A and D
(Tinkers Cr.).  These samples will then be transported
to the field.  At each of the designated QC stations a
set of two of these samples will be removed from the
cooler and one of these per QC station will be selected,
at random, and spiked at 50 ppb (a total of 4 samples).
The other sample from each set of two will be returned
to the laboratory and analyzed along with its spiked
counterpart (a total of 4 samples).

Just prior to analysis, an additional sample per QC station
(a total of 4 samples) will be prepared,  again using
laboratory deionized water, and spiked at 50 ppb.

Because the rate of adsorption of CPs to suspended
solids may differ between environmental and spiked
samples and between field-spiked and laboratory-spiked

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                              30                Section No.:  7.0
                                                Revision No.  2
                                                Date:9/12/86
                                                Page 12 of 14

        samples, CP recovery will be expressed in a weight/volume
        basis (ug/1) after summing the weights of CP in the
        filtered water sample and its respective solids. (It
        is similarly meaningful to express CP residues in
        water samples in the same wayr especially when comparing
        residues in samples containing different amounts of  suspended
        solids.   For example, residue levels  in the solids
        of two samples might be quite similar on a weight
        CP/weight solids basis, whereas total weight of CP
        would be considerably greater in the  water sample
        having the higher concentrations of suspended  solids).


7.7.1  General

       New lots  of reagents are checked prior to use,  or current
       lots of reagents are checked when method blank  problems
       are experienced.


7.7.2  The control checks that will be utilized are the
       following:

       Performance Sample;   Prior to sample analysis

       Method Blanks;   One per sample batch  analyzed

       Daily Standards; One before and after  sample analysis
                        for precision and accuracy as  described
                        in Section 9.0.

7.7.3  Calibration

       The GC/MS system will be calibrated prior to sample
       analysis  over a range which covers the sample concen-
       trations. The initial validation will  be checked daily
       with a midpoint calibration standard at the beginning  of
       the sample run.

7.7.4  Definitions

7.7.4.1  Method  Blanks;  Procedural blanks are carried
                         through the entire procedure  to check
                         for contamination. These will consist of
                         distilled water for  water field samples,
                         sodium sulfate for sediment and mussels,
                         and blank filters for suspended solids.

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                             31                Section No.:  7.0
                                               Revision No.  2
                                               Date:9/12/86
                                               Page 13 of 14
7.8    MRI Systems and Performance Audits

7.8.1  Systems Audits:   Systems audits by the QCC/QAC shall include:

          Inspecting facilities and equipment for adequacy,  appro-
          priateness,  and safety during use.

          Reviewing actual practices versus written procedures and
          protocols.

          Inspecting the records of maintenance and calibration.

          Inspecting QC practices.

          Assisting/conducting data audit prior to report submittal.

          Preparing and submitting a report with recommended correc-
          tive actions to the QAM, and after approval,  to the
          work assignment leader and program manager.

          Conduct additional audits as directed by the QAC/QAM.

          Assisting/preparing QA report for the EPA's  work assignment
          manager.


7.8.2  Analytical Performance Audits

       The performance audit sample is designed to check the operation
       of the analytical equipment.  Several blind performance samples
       will be independently prepared by the QCC and submitted for
       analysis before and during the analysis of the  regular samples.
       Performance audit samples will also be analyzed if (1) the
       QCC/QAC believes the analysis procedure has changed,  (2)
       analytical problems are suspected, or (3) the MRI work assign-
       ment leader or the EPA work assignment manager  requests samples
       All audit findings will be reported to the project leader  and
       program management by the QAM.  A summary of the audits will
       be provided to the EPA work assignment manager.

7.8.3  Field Performance Audit

       A Battelle representative will be in the field  to ensure
       compliance with the sampling protocol and will  write  a trip
       report.

7.8.4  QAC/QAM Audits

       Additional audits will be conducted or directed by the QAC/QAM
       as follows:

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                  32               Section No.:  7.0
                                   Revision No.  2
                                   Date: 10/21/86
                                   Paqe 14 of 14
Schedule and conduct additional audits as needed,  e.g.,
staff credentials, quality control data and practices.

Review and approve the report and supporting evidence for
accuracy and QA compliance prior to report submittal to
EPA.

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                                33
                                                      Section No.:  8.0
                                                      Revision No.  1
                                                      Date:9/12/86
                            SECTION 8.0               Page 1 of 2
                          DATA PROCESSING

8.1    Collection

       Data collection by MRI will utilize both manual and computerized
       acquisition systems.  All activities shall be legibly recorded
       using permanent ink in the project notebook or on worksheets.
       Each person who records data shall sign and date each sheet.
       Strip charts, magnetic tapes,  etc., shall be labeled with a format
       identifier, project number, date, the ID(s) of the instrument, and
       the name of the person responsible for the data.  Custody of  the
       original data media will be the responsibility of assigned project
       staff until archived.

8.2    Data Reduction

       Standard data reduction procedures with built-in checks will  be
       used.  For example, if an integrator or computer is used to cal-
       culate concentrations, the standards used to generate the curve
       must be back-calculated using the curve to ensure satisfactory
       curve fitting over the anticipated range.  In addition, all
       sample manipulations (e.g., weighing, dilution, concentration,
       etc.) must be clearly documented.

8.3    Data Validation

       The MRI work assignment leader will be responsible for assuring
       data validity which will include:

          Validating all equations and computer programs and documenting
          the validation.

          Validating and checking electronic data transfer.

          Proofreading manual data transfers.

          Screening data for consistency by a second project staff
          member.

          Checking calculations.

          Performing outlier checks.

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                               34                  Section No.: 8.0
                                                   Revision No. 2
                                                   Date:  9/12/86
                                                   Page 2 of 2


          Examining QC data and QC checks.

          Maintaining records of reviewing,  proofing,  and validation.

          Examining data/information for completeness,  representativeness,
          and comparability.

8.4    Storage

       Original data will be documented in laboratory notebooks,
       on printed paper,  as strip chart recordings,  or or magnetic tape
       or disk.  Permanent storage of work assignment data in the
       formal project file and hard copy from magnetic media will be
       archived (SOP-QA7).  The storage location of magnetic media will
       be reported.

8.5    Data Analysis

       MRI will provide a copy of final analytical data,  QC data, and
       chronological order of analysis to Battelle Columbus
       Division for statistical analysis.  Included in the report
       will be all protocol deviations and assumptions.  Battelle
       will provide statistical analysis of these data.

8.6    Results and Conclusions

       Battelle will develop the results and conclusions  based on the
       analyses of the data.  This should include a discussion of
       the limits and appropriate uses of the data and possible uses
       of the data which are not statistically supportable.

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                              35                  Section No.: 9.0
                                                  Revision No. 2
                                                  Date: 9/12/86
                                                  Page 1 of 3
                         SECTION 9.0

             DATA QUALITY ASSESSMENT (OBJECTIVES)
     The objectives for instrument precision and accuracy are
30% instrument precision (stability) over an analysis period and
100 jf 10% accuracy for the daily calibration check.

     The objective of precision for this method will be to
obtain chloroparaffin concentrations for replicate spike samples
which have range percent of less than 30% of each other.
The objective for accuracy will be to obtain chloroparaffin
concentrations which have percent difference of less than 30% of
the actual chloroparaffin concentrations.  Average recovery
efficiencies for chloroparaffins using spiked matrices should
fall within the range of 70-130% to yield meaningful data.

     These precision, accuracy and recovery values will be
obtained from the validation work which in turn will be based
upon the experimental design.

9.1  Analytical Precision

     Precision is determined by performing replicate analysis.
For data sets with a small number of points (2 < n < 8), the
estimate of precision will be expressed as range percent (R%).

                      R% = xi -x 2 x 100
     Where X^ = highest concentration value determined
           X2 = lowest concentration value determined

           X = mean concentration value of the set
     and
                n   X^
           X =      ~
     Where Xj_ =ith determination
            n = number of determinations.

     The detection limit (EDL) for the analytical system
will be defined as three times the signal to noise level of the
analytical instrument.

     The limit of quantitation (LOQ) for the analytical system
will be defined as ten times the signal to noise level of the
analytical instrument.

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                              36               Section No.: 9.0
                                               Revision No. 3
                                               Date:ll/14/86
                                               Page 2 of 3

     As an alternative, the estimate of precision may be
expressed as percent relative standard deviation (% RSD):
                            /_ (X- X)

              R.S.D. =    /
                                n - 1

                                  ~            X 100
                                  X

Where n = number of replicate determinations.

                           n
                           1  Xi
               X = mean = i=l
                            n

The precision of the analytical system, which includes instru-
ment stability during analysis, will be monitored by analyzing
the midpoint standard at the beginning and end of each day's
analysis and plotted on a control chart.

9.2  Accuracy

     The  accuracy (A%) of the analytical method will be
established by performance samples and the daily midpoint
standards.  The initial daily midpoint standard will be plotted
on control charts and monitored.

               A% = F x 100
                    A

     Where F = found weight or concentration of chemical
           A = actual weight or concentration of chemical

9.3  Recovery

     Recovery (RE%) will be calculated from the results of the
spiked sample and unspiked sample analyses.


                  RE (%) =  S - U   x  100
                              A

     Where,   S = concentration of the spiked sample
              U = concentration of the unspiked sample
              A = concentration of the added standard

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                          37                Section No. :  9.0
                                            Revision No.  2
                                            Date: 9/12/86
                                            Page 3 of 3


9.4  Traceability of Instrumentation

     All collection and measuring instrumentation will have a
unique identification number.  Maintenance/calibration and use
logs will be maintained.

9.5  Traceability of Samples

     All samples will have a unique identification number
along with information on field site,  monitoring location,
collection device, etc.  The samples will be labeled with
adhesive bar code labels to identify the samples and trace them
through the sampling and analytical procedures.

9.6  Traceability of Data

     Data will be documented and filed to allow complete
reconstruction from initial field records to data archiving.

9.7  Completeness

     Due to the variety of data points available per field
test site, every effort will be made to maintain a level  of data
completeness that will assure meaningful data. Data complete-
ness (C%) will be determined from the number of values which
fall within the instrument accuracy and precision objectives:
            C% = Number of acceptable values  x  100
                   Total number of values

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                                38                  Section No. 10.0
                                                    Revision No. 2
                           SECTION 10.0             Date:9/12/86
                                                    Page 1 of 3

                         CORRECTIVE ACTION


Midwest Research Institute

For those subtasks performed by MRI,  the MRI work assignment leader
has primary responsibility for taking corrective action; if he is
unavailable, the program manager,  and/or the QAC/QAM shall be contacted
for instructions.  Some of the types of problems and corrective
actions to be taken are listed below.  Unresolved problems are reported
by the QAM to the Associate Director of K.C. Operations and to the
Senior Vice President for resolution.


10.1 Performance/Systems Audits

     If problems are detected during an audit:

        The auditor shall notify the person responsible, the work
        assignment leader, and the QAC/QAM of the problem(s) and any
        action(s) he has taken.

        The work assignment leader and the person responsible shall
        correct the problem, then notify the QAC/QAM.

        The auditor shall then prepare, and after QAC/QAM approval,
        send a problem/action taken memo to the program manager and
        the work assignment leader.


10.2 Loss of Data

     The work assignment leader shall investigate the problem then
perform one of more of the following actions:

        If the problem is limited in scope, the problem/action taken
        is documented in the notebook; the work assignment leader
        then prepares and sends a problem/action memo to the QAC/QAM,
        and the program manager.

        If a large quantity of data is affected, the problem/action
        taken is documented in the notebook; the work assignment
        leader then prepares and sends a problem/action memo to the
        QAC/QAM, project manager,  and the EPA work assignment manager.

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                                39
                                               Section No. :  10.0
                                               Revision No.:  1
                                               Date:9/12/86
                                               Page 2 of 3
10.3 Significant QA Problems
     In general, the work assignment leader shall identify technical
problems.

        The work assignment leader prepares and sends a problem memo
        to the QAC/QAM and program manager; if the problems are
        significant, the action is determined collectively.

        The action taken is documented in the notebook.

        The problem and action taken is reported to the EPA work
        assignment manager.


PEI Associates
For the subtasks performed by PEI Associates, the PEI work assign-
ment leader has primary responsibility for taking corrective
action.  If he is unavailable, the PEI Program Manager, and/or the
QAM/QAC shall be contacted for instructions.  Some of the types
of problems and corrective actions to be taken are listed below.
Unresolved problems are reported by the QAM to the PEI Associates
Director for resolution.  All corrective actions should be reported
to MRI.

10.3  Loss of samples

The work assignment leader shall investigate the problem and then
perform one or more of the following actions:

    o  If the problem is limited in scope, the problem/action
       taken is documented in the notebook.  The work assignment
       leader then prepares and sends a problem/action memo to
       the QAM/QAC and the Program Manager.

    o  If a large quantity of data is affected, the problem/action
       taken is documented in the notebook.  The work assignment
       leader then prepares and sends a problem/action memo to the
       QAM/QAC, Program Manager, and the EPA Work Assignment
       Manager.

10.4  Significant QA Problems

In general, the Work Assignment Leader shall identify technical
problems.

    o  The Work Assignment Leader prepares and sends a problem memo
       to the QAM/QAC and Program Manager.  If the problems are

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                             40                 Section No.: 10.0
                                                Revision No.: 2
                                                Date: 10/16/86
                                                Page 3 of 3
        significant, the action is determined collectively.

     o  The action taken is documented in the notebook.

     o  The problem and action taken are reported to the MRI
        Work Assignment Manager.


Battelle Memorial Institute
     For the subtasks performed by Battelle Columbus Division,
the Battelle Work Assignment Leader has primary responsibility
for taking corrective action.  If he is unavailable, the Program
Manager, and/or the QAA shall be contacted for instructions.

     In general, the Work Assignment Leader shall identify
technical problems.

     The Work Assignment Leader prepares and sends a memorandum
to the Program Manager and the QAA.  If the problems are
significant, the action is determined collectively.

     The action taken is documented.  The problem and action
taken are reported to the EPA Work Assignment Leader.

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                         41               Section No.: 11.0
                                          Revision No.:  2
                                          Date: 9/22/86
                                          Page 1 of 2
                     SECTION 11.0

             DOCUMENTATION AND REPORTING
11.1  Documentation

      o  Original (raw) documentation shall be recorded in
         permanent ink.

      o  A hard copy of original computerized data,  which is
         reported, will serve as the official copy.

      o  Initials may be used in place of signatures if they are
         readily traceable.

      o  Manual corrections of original data will be performed
         as follows:  Draw a single line through the incorrect
         entry so that the original entry remains legible.  Add
         the correct entry; then explain, initial,  and date the
         correction.

      o  New information may be added to original data if it is
         initialed and dated.

      o  All deviations from standard operating procedures (SOPs),
         procedures, and protocols will be documented.

      o  Assumptions will be documented.

      o  Strip charts, magnetic tapes, etc., will be labeled with
         a format identifier, the date, the ID(s) of the sampling
         equipment,  and the name of the person responsible for
         the data recording equipment.

11.2  Document Control

      o  Original sampling data will be documented and stored in
         laboratory notebooks, approved forms, on printer
         paper, on magnetic tape, and as strip chart recordings.

      o  The location of all original data will be documented by
         the work assignment manager until the files are archived.


11.3  QA Reports tc> Management

      The QAC/QAM, in cooperation with the work assignment leader,
      shall identify critical phases of the project which will be
      subject to inspection.  The inspection will include a
      review of:

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                             42                   Section No.: 11.0
                                                  Revision No.: 1
                                                  Date:9/12/86
                                                  Page 2 of 2

     o  Staff credentials.

     o  Equipment maintenance and calibration records.

     o  Equipment performance.

     o  Documentation practices.

     o  Recordkeeping practices.

     o  Adherence to protocols, SOPs, and QA plan.

     o  Assessment of data accuracy, precision, and completeness.

     The results of inspections and audits will be reported
quarterly by the QAM to Program MRI management; summaries
will be reported to the EPA work assignment manager.

11.4 Report Design

     Progress, interim draft final, final reports, and QA
     summary reports will be submitted in accordance with the
     provisions for reporting in the contract.  Verbal status
     reports will be made biweekly to the EPA work assignment
     manager.

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                            43
Section No.:  12.0
Revision No.:  1
Date: 9/12/86
Page 1 of 1
                       SECTION 12.0

                       REFERENCES
1. Campbell, Ian and George McConnell. 1980. Chlorinated Paraffins
   and the Environment. 1. Environmental Science and Technology,
   Vol. 14, Number 10, October 1980.
2.  Letter from Alan E. Ramm to Jack Borror dated 11-21-78 concerning
   sediment and biota sampling.


3.  Letter from Alan E. Ramm to Jack Borror dated 7-19-77 concerning
   results of Chlorowax investigations in Grand River.


4.  Segal, S., Non-parametric Statistics,  1956, McGraw-Hill.
5. U.S. Environmental Protection Agency, 1982, Test Methods - Technical
   Additions to Methods for Chemical Analysis of Water and Wastes.
   Office of Research and Development, Cincinnati, Ohio, EPA 600/4 -
   82-055, December 1982.

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               APPENDIX A






FIELD STUDY DESIGN AND SAMPLING PROTOCOL




                  FOR




              SUGAR CREEK




              DOVER, OHIO

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                             A-l
                APPENDIX A - TABLE OF CONTENTS








Section           Heading                   Revision       Date






1.0     Description of the Study Area                    9/12/86



2.0     Waste Inputs                                     9/12/86



3.0     Reconnaissance Survey                            9/12/86



4.0     Field Study Design                               9/12/86



5.0     References                                       9/12/86

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                              A-2
1.0  Description of the Study Area

    Sugar Creek is located in east central Ohio.  From its
source in Wayne County near Wooster, Ohio, it flows south,
southeast toward its confluence with the Tuscarawas River.
Near Beach City, Ohio, Sugar Creek is impounded; here it
recharges the aquifer supplying the city of Canton's well
field.

    The drainage basin of Sugar Creek is largely rural.  It is
classified by the Ohio EPA as a warm water habitat.  The focus
of this field study is on the lower 4 miles of Sugar Creek from
below Strasburg to the mouth.  A map/schematic of this segment
of Sugar Creek is given in Figure 1.1.

    According to the 1986 State of Ohio Section 305(b) report
[1] chemical/physical and biological conditions measured in
the lower 4 miles of Sugar Creek in 1983 were generally good.
Dissolved oxygen, conductivity, ammonia-N and nutrient concen-
trations were not indicative of any stress from sewage or other
oxygen demanding wastes.  Numerous pollution sensitive macro-
invertebrates were collected at RM 1.8, and fish community
health was good at two sites (RM 3.6 and 0.2).  The chemical
data did reveal a transient  influence from acid mine drainage
when runoff from small tributaries to lower Sugar Creek occurred
during low stream flow in Sugar Creek.  The water quality measured
in the mainstem was not severly degraded during these events,
and it is unlikely that chemical perturbations reached
problematic magnitudes or frequencies based upon the relatively
healthy benthos and fish faunas collected in Sugar Creek.
However, Ceriodaphnia bioassays of Sugar Creek water collected
at river mile(RM)T78 (immediately downstream from Goettge
Run) did show reduced production of young.  These findings
combined with a reduction in sensitive macroinvertebrate species
collected at RM 0.6 suggest the possibility of localized chronic
pollution stress from acid mine drainage in lower Sugar Creek.
It is likely that Goettge Run and the other small tributaries
to Sugar Creek between the Beach City dam and the Tuscarawas
River are impacted by abandoned strip mine land and may not be
attaining their potential aquatic life uses (Ohio EPA 1986) .

    The Ohio Department of Natural Resources reported two fish
kill incidents in 1983 and 1984 in Sugar Creek.  Also, Twenty-
one wild animals died as a result of unknown causes.

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                A-3
FIGURE 1-1   SUGAR  CREEK STUDY AREA

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                             A-4
    The mean annual stream flow for this segment of Sugar
Creek is approximately 330 cfs.  Low flow for the area is
approximately 30-50 cfs.  Sugar Creek is about 50-75 feet wide
and averages 1-2 feet in depth throughout this segment of the
river.  As it approaches its confluence with the Tuscarawas
River, its depth increases to 8 feet.  A variety of fish and
macroi nvertebrates are reported to populate the area.  The creek
bottom is a combination of gravel and sand.  Access to the creek
is limited.  There are no public water intakes along this stretch
of Sugar Creek.

2.0  Waste Inputs

    The only point source discharges to this segment of Sugar
Creek are from Dover Chemical Plant (RM 1 .8 )  and the City of
Strasburg wastewater treatment plant (RM 7.3).  Acid mine drainage
from Goettge Run (RM 1.8) is a principal nonpoint source of
pollution.

2.1     Dover Chemical Corporation

    Dover Chemical Corporation is the outfall of interest to
this study.  Dover Chemical Corporation is a major manufacturer
of chlorinated paraffins, producing 21% of the total U.S. production
    Dover Chemical is located at 15^  and Davis Streets in Dover,
Ohio.  At present Dover Chemical continuously pumps approximately
2.2 mgd of water from 2 of their 4 wells and discharges 1.6-1.8
mgd of water.

    The 1980 production outputs for Dover Chemical are as follows:


    Product and By-Product               Annual Quantity

    Chlorinated paraffins (liquid)          6,100 tons
    Chlorinated paraffins (resin)           5,100 tons
    Hydrochloric Acid                      18,000 tons
    Sodium Hypochlorite                     2,766 tons.

    The Standard Industrial Code (SIC) for Dover Chemical is 2861 .

    The Dover Chemical plant employs about 90 people and is
currently operating 24 hours a day 10 days on and 4 days off.

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                               A-5
2.1.1   Chlorinated Paraffins Process Description

    At the Dover Chemical plant chlorine gas and paraffin is
continuously reacted to form the chlorinated paraffin.   Sometimes
carbon tetrachloride is used in this process as a solvent, or to
remove free chlorine from solution.  After the chlorine and
paraffin is reacted it is passed through a degasser to vaporize
the carbon tetrachloride.  The carbon tetrachloride is then
condensed and reused while the freed chlorine is used to produce
sodium hypochlorite.  After the chlorinated paraffin has passed
through the degasser it is deposited on a conveyor belt for water
cooling with well water until hardened.  When it is  solidified
the chlorinated paraffin resin is ground, screened, and stored
for sale.

    Two dry dust, collectors are used to collect the resin dust
from the grinding operation, and are sold for use in making resin.
The water used for cooling is sent to their treatment   system.
When the cooling water is  sprayed against the underside of the
conveyor belt to cool the paraffin product on top of the belt, it
is likely that some water contact with the product or product
residue may occur.

    Liquid  chlorinated paraffins are manufactured in a batch-
reaction kettle.  After reaction the chlorinated paraffins are
sent through a degasser for removal of free chlorine gas from
solution vessels and used to make muriatic acid (HC1).  The other
product of this reaction is chlorine gas which is used to make
sodium hypochloride (bleach).  Sometimes the concentrations of
both by-product's gasses are too low to form their end products
and are water scrubbed.  This scrubbing water is then sent to the
water treatment system.

    A typical process flow diagram for the manufacture of
chlorinated paraffins is shown in Figure 2.1.

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                                       A6
N-PARAFFIN
  SOLVENT
                                                    TO ATMOSPHERE
, 	 
^ 7Z





~\

V. 	 -*
/

-

COOLING 




MATER \


1





VENT GASES ^
Y
(HCL + CL2 + | Vv'
CHLORINATED ! L_
1





REACTOR





CL  !!5

PARAFFIN) j
* SOLVENT *^ 	 "
\ HCL
} COOLING STORAG
WATER


^
        (CHLORINE GAS\
                  STABILIZER-
STABILIZER

      SOLVENT
      STRIPPER
                          LIQUID RESINOUS
                           CP     CP
                                                                    SALE
                                      rO
                                         BAG
                  COOLING
                   HEAT
                 EXCHANGER
                                                                        DRUM
                        SOLVENT
     Fipure 2.1.  Process flow diagram for  the manufacture of
                        chlorinated paraffins.
         Source   PEI  1984

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                            A-7


2.1.2   Dover Chemical Wastewater Treatment Process

    Wastewater consists of non-contact cooling water, boiler
blowdown ion exchange regenerant (deionizer for boiler makeup
water), scrubber water and floor drainage.  All wastewaters with
the exception of non-contact cooling   water enters a 10,000
gallon settling tank and overflows to a limestone bed for
neutralization.  This first settling tank is equipped with both a
rotating oil skimmer and a continuous belt skimmer.  Oil and
grease accumulated by the skimmers is transferred to a separation
tank.  The aqueous portion is returned to the first settling tank.
Solids from the first tank are pumped to a 20,000 gallon tank for
further separation.  This tank is occasionally drained of the
aqueous layer which is subsequently passed through an activated
carbon bed prior to pumping to the first settling tank.  Water
passing through the limestone bed flows to the second settling tank
which is equipped with an oil boom and underflow weir prior to
discharging over a four foot rectangular weir with end contractions.
Non-contact cooling water enters the second settling tank.  The
point just after this weir is designated outfall 601.  The discharge
flows several yards through a pipe before it  is discharged into a
narrow canal.  This canal then carries the wastewater to a lagoon.
Discharge from the lagoon flows through a small unnamed ditch via
outfall 001 and then to Sugar Creek.

    The Dover chemical surface impoundment lagoon is owned by the
company.  It contains a captive population of fish, frogs and
turtles.  The impoundment has been known to overflow; however, no
incidents have occurred in the past 2 years.  The impoundment is
approximately 9 acres in area and is more than 30 feet deep in places

    A simple schematic of the Dover Chemical Wastewater Treatment
Process is given in Figure 2.2.

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                             A-9


3.0 Reconnaissance Survey


     On August 12 and 13, 1986 MRI and PET personnel and Robert
Heath, consultant to Battelle Memorial Institute conducted a
reconnaissance survey of the Sugar Creek area.  The objectives of
this reconnaissance visit were twofold:  (1) to collect field
samples to test the analytical method for CPs developed and
enhanced by MRI in order to estimate its recovery efficiency and
precision and (2) to study the Sugar Creek/Dover area in
preparing the final study design for the monitoring study in this
area.

     In support of the first objective, water and sediment
samples were collected from three sites (stations) in Sugar
Creek.

  o  Site A  -  Downstream from Dover Chemical at Tuscarawas
                Road.

  o  Site B  -  Under the bridge which carries the road to
                Winfield, upstream of Dover Chemical.

  o  Site K  -  Route 39 downstream from Site A, just above the
                confluence with the Tuscarawas River.

     Sufficient water and sediment samples were collected to
allow for a series of analyses aimed at validating the analytical
method (See Appendix D). Mussels were not collected due to the lack
of a permit.  A short follow-up visit will be made to collect
mussel samples.


     In support of the second objective,  the team was able to
meet and discuss the area with EPA State personnel, visit and
walk the Sugar Creek, and visit and walk the Dover Plant itself.
Permission was granted by Dover Chemical Plant personnel to
collect whatever samples from their plant necessary for the
study.  They only requested that samples collected be split and
shared with Dover Chemical and that any photographs taken be made
available to Dover Chemical.  Several photographs of the area
were taken and are available under separate cover.

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                             A-10
4.0  FIELD STUDY DESIGN

      The design for this study has necessarily been developed
without the knowledge of the frequency of occurrence of residues
in the study area(s) or the statistical parameters of such
residues.  The design has also been developed with the expectation
that the precision and accuracy of the analytical method (which
is concurrently being determined) will be acceptable.

        The design calls for a total of eight (8) sampling
stations; four stations in Sugar Creek and four in the discharge
waterway: The station locations are shown in Figures 4.1, 4.2 and 4.3

 Station ID                       Location

                         In the Dover Chemical Plant settling
   LI                    lagoon near the lagoon's effluent.

                         In the Dover Chemical Plant settling
   L2                    lagoon near the influent from the
                         plant discharge.

                         In the Dover Chemical Plant settling
   L3                    lagoon near the middle of the lagoon.


   D                     In the lagoon discharge ditch immediately
                         above the point of discharge into Sugar Cr.

   B                     Sugar Creek under road to Winfield

   B1                    Sugar Creek just upstream of the Dover
                         Chemical Discharge ditch.

   A1                    Sugar Creek just downstream from the Dover
                         Plant discharge ditch but upstream of
                         Goettge Run.

   K                     Downstream from the Dover Plant discharge
                         and just upstream of the confluence of
                         Sugar Creek and the Tuscarawas River.


     The design requires the collection of a minimum of three
individual grab or composite water and sediment samples at each
of the eight stations.  It also calls for the collection of
mussels at all four Sugar Creek stations.  While mussels are
not expected to habitate the lagoon or the drainage ditch, mussel
samples will be collected at these stations, if possible. As
mentioned, each mussel sample is a composite of the flesh of
8 to 10 individual specimens.  The samples and analyses Comprising
each set are shown in Tables 1 through 4.

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                          A-1 1
FIGURE 4.1  Locations  of  sampling sites at Dover Chemical  and
                       in  Sugar Creek.

-------
                       A-12
FIGURE 4.2 Location  of sample points  at Stations A'  and B'

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                              A-13
^^
LU
UJ
ca
  .
ff.
CJ

oo

DOVER
CHEMICAL
SURFACE
IMPOUNDMENT
@
(0)
l 1
OUTFALL ""^ //
001 //
^


>


^ INFLUENT
^ CANAL


DISCHARGE
  DITCH
W

I
                               FIGURE  4.3


           Location of  sampling  points  in the Dover Chemical impoundment.

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                              A-14
                                Table 1
                        SAMPLES TO BE COLLECTED
PLANT DISCHARGE WATERWAY
Set I Set II
Station LI L2 L3 D LI L2 L3 D
Medium:
Water 1111 1111
Sediment 1111 1111
Mussel 1111 -- 	
QC Water 1* - 	
Set HI
LI L2 L3 D
1111
1111
SUGAR CREEK
Set I Set II
Station B B'A'K B B'A'K
Medium:
Water 1111 1111
Sediment 1111 1111
Mussels 1111 ___-
QC Water i*__- ____
Set III
B B1 A1 K
1111
1111
*Composite water sample 4-times volume of field samples.

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                              A-15






                                Table 2






                          POTENTIAL ANALYSES
PLANT DISCHARGE WATERWAY
Stations
Medium:
Filtered Water
Suspended Solids
Sediment
Mussels
QC Water
QC Filtrate
Set I
LI L2
1 1
1 1
1 1
1 1
2 -
2 -
Set II Set III
L3 D LI L2 L3 D LI L2 L3
11 1111 111
11 1111 111
11 1111 111
11 __ 	 ___
	 2- 	 ___
	 2- 	 ___
D
1
1
1
SUGAR CREEK
Stations
Set I
B B.'
Set II Set III
A1 K B B1 A1 K B B1 A1
K
Medium:
Filtrated Water  1111     1111      1111



Suspended Solids 1111     1111      1111



Sediment         1111     1111      1111



Mussels          1111     ___-      ____



QC Water         2_--2---      ____



QC Filtrate      2---     2  -  -  -      ____

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                A-16
                 Table 3
          TOTAL SAMPLES BY SETS
(Plant Waterway and Sugar Creek Combined)
Medium
Water
Sediment
Mussels
QC Water
All Samples
Set I
8
8
7
2
25
Set II
8
8
0
0
16
Set III
8
8
0
0
16
All Sets
24
24
7
2
57

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               A-17
                 Table 4
         TOTAL ANALYSES BY SETS
(Plant Waterway and Sugar  Creek Combined)
Medium
Water (filtrate)
Suspended solids
Sediment
Mussels
QC Water (filtrate)
QC Suspended solids
Potential
Analyses
Set I
8
8
8
7
4
4
39
Set II
8
8
8
0
4
4
32
Set III
8
8
8
0
0
0
24
All Sets
24
24
24
7(+7)
8
8
95

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                            A-18
     To enhance study efficiency and minimize analytical costs,
analyses will be conducted in a logical sequence of sets and
possibly subsets.  Three (3) sets are to be constructed such that
the first set {set I) consists of the first samples of each type
of medium collected at each of the eight stations. The second
set (set II) comprises the second samples of each medium,  etc.
Subsets comprise all samples of a given medium within a set.

      Samples will be analyzed sequentially by sets and by
subsets within sets (see table 5).  Analytical data from Set I
will be evaluated to determine the need for analysis of Set II.
Similarly, a decision to analyze set III would depend on the
combined outcomes of set I and II.

The order of analyses of subsets within sets will be decided by
MRI.  Priority will be given to the analysis of samples collected
from stations B, B1, A1, D, and K.  Decisions on whether to
continue analyses will be made at various points during the
analytical process.

     Within subsets, the extracted field samples and their
respective QC blanks and spikes should be quantified in random
order "blind" to the GC/MS operator.

4.1     Parameter Coverage

        In addition to CP determinations, Temperature (C), Flow
        (cfs), and Depth (feet) will be recorded for each sample.

4.2     Sample Collection

        All samples will be collected and handled using procedures
        fully approved by EPA. A replicate set of samples will
        be provided to Dover Chemical Corp. for their independent
        analysis.

4.3     Sampling Preparations

        All water column and sediment samples will be collected in
        glassware which has undergone the following cleaning steps:

        o   Remove surface residuals.

        o   Hot soapy soak to loosen and flotate most of residue.

        o   Hot water rinse to flush away flotated residue.

        o   Soak with deep penetrant or oxidizing agent to destroy
            traces of organic residue.

        o   Hot water rinse to flush away materials loosrened by deep
            penetrant soak.

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                          A 19

                         TABLE 5

            PROPOSED SEQUENCE OF ANALYTICAL RUNS*
                   BY SETS AND SUBSETS
     Run
     No.     Subset
     1.    Filtered water   8 field samples  + 4  QA field  samples**

Set  2.   Suspended Solids  8 field samples  + 4  QA field  samples**
 I
     3.     Sediment        8 field samples

     4.     Mussels         7 field samples
     5.    Filtered water   8 field samples + 4  QA field  samples**

Set  6.   Suspended Solids  8 field samples + 4  QA field  samples**
II
     7.     Sediment        8 field samples

     8.     Mussels         7 field samples (assuming  mussels  available)
     9.    Filtered water   8 field samples

    10.   Suspended Solids  8 field samples
Set
III 11.     Sediment        8 field samples

    12.     Mussels         NA
*  Analyses within each run are to be made in random sequence  which
   is unknown (blind)  to the operator.

** QA field samples collected from stations B and LI.

   Method blanks will  be analyzed with each run

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                             A-20
        o   Rinse with deionized water to remove metallic deposits
            from the tap water.

        o   Rinse with high purity methanol followed by the high
            purity methylene chloride.

        Glassware will be handled using polythene gloves to avoid
        contact with hands.
4.4  Water Column

    All water column samples collected at stations A',BfB'  and K
will be a composite of single grab samples collected from at
least three equidistant points along a stream transect.
Each 0.5 gallon glass jar will be triple rinsed with stream water
at the location the sample is to be collected.  The jar will then
be submerged in the stream until all air is replaced by a water
sample. The water sample depth will be half way between the
surface and the bottom of the stream.  The samples collected along
the stream transect will be composited to form a single sample.

     Water samples collected at station D will be collected as
a single grab in 0.5 gallon glass jars.

    Water samples collected at stations LI, L2 and L3 will be depth
integrated with discrete samples collected from three depths per
station: near the bottom, at mid-depth and near the surface.

    Field QA water samples will be collected as described in
section 7.7.

    All jars will be capped with teflon-lined lids.  Water samples
will require no preservative.

Each sample jar will be labeled with a barcode label.

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                          A-21

4.5  Sediment Samples

    All sediment samples will be collected in 500 ml. qlass
jars. At stations A1, B, B1 and K a stainless steel scoop will be
used to remove sediment from the same equidistant points along
the stream transect that the water column samples were collected.
These discrete samples will then be composited to form a single
sample.

    At station D a stainless steel scoop will be used to remove
sediment from that sample location.

    At stations LI, L2 and L3 sediment samples will be collected
using an Ekman dredge sampler.

    Large rocks will be removed before placing the sample in the
jars. All jars will be capped with teflon-lined lids.  Sediment
samples will require no preservation.  Each sample jar will be
labeled with the same information as described above.  The stain-
less steel scoop and the Ekman dredge sampler will be triple
rinsed with distilled water prior to filling a sample collection
jar.

4.6  Tissue Samples

    Mussel samples will be collected from the Sugar Creek stations
in one of two manners, depending upon the depth of the stream.
Generally, where the stream is 6 inches or less in depth, the
mussels will be collected by hand.  In areas where water depth
exceeds 6 inches, a clam rake will be utilized to collect samples
as visual observations will not be possible. If mussels cannot
be found at a given Sugar Creek station after 2 hours of samp-
ling, mussel sampling will be aborted at that station.

    Mussels are not expected to habitate the lagoon or the drainage
ditch. However, if there is evidence that mussels exist in the
lagoon, sampling of mussels will be conducted only if, after 15
minutes of sampling, a sufficient number of specimens are collected
to warrant further investigation.

Unhealthy or dead mussels will be discarded.  All live mussels
will be placed on ice in coolers.

    In accordance with the permit obtained for the Sugar Creek
area from the Ohio Department of Natural Resources, no more than
10 mussel specimens will be collected from each of the stations
deployed in the receiving water proper.  Also, following ship-
ment to the lab, the shells will be removed from the specimens
collected from the field and shipped back to the State of Ohio
thus fulfilling the requirements of the permit.


4.7   Sample Preservation And Transportation


    All sample jars will be kept in coolers out of direct sunlight

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                            A-22

and transported in ice-filled coolers with sufficient packaging
material to reduce the possibility of breakage.  Any live mussels
collected during the study will also be placed in an ice-filled
cooler.  This is expected to keep the mussels alive while being
transported to the MRI Laboratory in Kansas City.  All water,
sediment, and mussel samples will be shipped via commercial
airlines or by overnight delivery service, to MRI's Kansas City
Laboratory.

     Upon arrival at the MRI laboratory, the samples will be
logged in and separated into sets as described above.  The first
set to be analyzed, will be extracted within the first seven (7)
days from date of collection.  The remaining samples will be
refrigerated until extraction.  All samples will be analyzed
within thirty (30) days from date of collection.

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                            A-23
5.0  References
1. 1986 State Section 305(b)  report for the State of Ohio - draft,


2. PEI Associates,  Inc. 1984,  Exposure Assessment of Chlorinated
   Paraffins, Washington,  DC

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                              Appendix B
                              Chloroparaffin field study
                              Date: 10/16/86
               APPENDIX B

FIELD STUDY DESIGN AND SAMPLING PROTOCOL

                  FOR

             TINKERS  CREEK

             BEDFORD, OHIO

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                             B-l
                APPENDIX B - TABLE  OF  CONTENTS
Section           Heading                    Revision        Date



1.0      Description of the Study Area                     10/14/86



2.0      Waste Inputs                                     10/14/86



2.1      Description of the CP cutting  oil  user            10/14/86



3.0      Reconnaissance Survey                            10/14/86



4.0      Field Study Design                               10/14/86

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                               B-2
1.0   Description of the Study Area

     Tinkers Creek is located in Northeast Ohio.  From its source
it flows south and then to Northeast toward its confluence with
the Cuyahoga River.

     The drainage basin of Tinkers Creek is largely industrialized
and urban.  The focus of this field study is on the upper reaches
of Tinkers Creek and tributaries in the Walton Hills area.  A
map/schematic of this segment of Tinkers Creek is given in Figure
1.1.

     The tributaries to Tinkers Creek in the study area are small
surface streams 3 to 5 ft wide and several inches deep at the
point where they flow under Egbert Road.  These streams have
gravel and silt bottoms and are easily accessed at this point.
Deerlick Run, at the point of its confluence with Tinkers Creek
is 8 to 10 feet wide, 6 inches deep and has a shale bedrock and
coarse gravel bottom.  Tinkers Creek, at it confluence with its
tributary Deerlick Run, is about 50 feet wide, 1 to 3 feet deep
and has a coarse gravel and shale bedrock bottom.  Deerlick Run
and Tinkers Creek have relatively steep gradients; several water-
falls and rapids are present in this area. Flow is estimated at
100 - 150 cfs. (During the spring, Tinkers Creek has Class V
Whitewater.)  During summer low flow conditions about 80 percent
of the volume of Tinkers Creek is contributed by upstream sewage
effluents.  The Ohio EPA (OEPA) reported that no mussels would be
found in any of these streams.

     Several oil spills and industrial releases have impacted
these tributaries in recent years.  OEPA previously has conducted
monitoring and toxicity studies on these streams.  Their studies
indicate the presence of stream pollution from many sources in
this area, termed the Deerlick Run Drainage Network.

2.0  Waste Inputs

     In the study area, there are at least 17 industrial facil-
ities (e.g, chemical manufacturers, metal fabricators, concrete
plants, drum recyclers, etc.) and two hazardous waste sites
(S.  K.  Wellman's electroplating sludge pond which is currently
being closed and American Steel Drum Recyclers which was previously
cleaned-up by EPA) located in the close proximity to each other.
(Figure 2-1)  Many of these facilities have nonpoint discharges
to the same tributaries to Tinkers Creeks that are influenced by
the point source discharger in the area that is a supposed CP
lube oil user.

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-------
     . (tbiSAWttf

ctfauai (e.fTo c
         lOr/OF  7

-------
                               B-5

2.1  The CP User

     A metal-working industry located in the study area is a
supposed user of cutting oils containing chlorinated paraffins
as an additive.

     This Company operates a plant that manufactures clutch and
brake friction materials for trucks and heavy equipment.  While
OEPA officials could not confirm that CPs are used in the process,
other sources of information indicate that these oils are
used.  Process wastewaters discharge to the city of Bedford's
POTW.  Pollutants including heavy metals (mainly copper), ammonia,
oil, grease, and acids and bases are present in the process
wastewater.  Noncontact cooling water and storm water are discharged
from the plant property through NPDES outfalls to a discrete
conveyance  (i.e., a small surface stream) that flows a distance
of about 2 km before it enters Tinkers Creek.  It is likely that
ground water carrying contaminants from past waste management
practices (i.e., surface impoundments) located on-site also
enters this tributary to Tinkers Creek.  This company employs
about 250 employees.

     The tributaries impacted by this plant and the other point
source dischargers originate immediately upgradient of these
sites.  Storm sewer outfalls, runoff, ground water and nonpoint
source discharges are the sources of flow.  There are no
non-impacted upstream control sites.  Tinkers Creek is impacted
by POTW and industrial outfalls upstream of its confluence with
Deerlick Run.

3.0  Reconnaissance Survey

     On October 1 and 2, 1986, a site reconnaissance was conducted
in the study area by Tom Janszen and Bob Hoye of PEI.  Additionally,
a meeting was held with Ohio EPA representatives on October 2 to
discuss their knowledge of the operations conducted at this
facility, the physical setting of this and other plants in the
area and their discharges to surface waters.  The purpose of the
visit was to gather the information necessary to make a decision
regarding sampling of surface waters, sediments and mussels for
CP analysis.

     The PEI representatives were able to meet with the Ohio EPA
but were able to obtain only limited information about the proposed
sampling area.  They obtained one toxicity evaluation report for
the area which is available under separate cover.

     The PEI representatives were also able to visit the proposed
site, photograph prospective sampling sites, and evaluate the
hydrology of the area.

-------
                           B-6
     Their efforts produced the following information about the
area.

     o   There is no indication of mussels or any oter macro-
         invertebrates or fish in the proposed study area.  In
         the best judgement"of the Reconnaissance Team, it is
         unlikely that mussels will be found in the area.

     o   Because Tinkers Creek flows through the Cleveland
         Metroparks Bedford Reservation in the proposed study
         area, permission to take samples from Tinkers Creek and
         Deerlick Run must be obtained from the Metroparks
         Administration.

     o   No special sampling gear will be required if the field
         study is implemented.

     o   Streams in the study area are generally accessible
         especially at the sample locations desicribed later in
         this Appendix.

     o   Stream samples collected in this area  will likely
         contain a variety of organic and metal constituents from
         past and current operations in the area.

     o   Sediment samples will be limited to gravel and rock
         although some silt may be obtainable from the upstream
         tributaries to Deerlick Run.

4.0  Field Study Design

     The design for this study has necessarily been developed
without the knowledge of the frequency of occurrence of residues
in the study area(s) or the statistical parameters of such
residues.  The design has also been developed with the expectation
that the precision and accuracy of the analytical method  (which
is concurrently being determined) will be acceptable.

     The design calls for a total of 6 samplings stations; 2
stations in Tinkers Creek, one on Deerlick Run at its confluence
with Tinkers Creek, and one each on Hukill Tributary, Ferro
Tributary and South Branch at Egbert Road.  The station locations
are shown in Figures 4.1, 4.2 and 4.3.  A seventh sample  station
will be established to capture a sample of the process wastestream
(or wastewater sludge if a wastestream sample cannot be collected)
from the plant effluent of the supposed CP cutting oil user.

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                                              Figure 4.1  Tinkers Creek area

                                                            and  sampling  stations
     "'  '.'. "* ''*''''" -;*: ' -'-'<-''*.-".-  --"'" "'---:: .1. .' 
P/uK/u Cv.fttMef
                fa fro nor. (^IBW
                 /?l5r/ppp 7 ^      V

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                       B-8
                           DIRECTION
                            OF FLOW
                                            Not to scale
Figure 4.2 Location of Sampling  Stations A through C at
  the confluence of Tinker's  Creek  and Deerlick Run.

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B-9
                                              en
                                              o
                                              o

                                              in
                                              c
                                              o

                                              t-J
                                              (D
                                              ->
                                              00

                                              01
                                              (O
                                              oo
                                              c
                                              o
                                              IO
                                              (J
                                              o
                                              __1

                                              n

                                              ^j-
          SOUTHWEST  BRANCH

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                               B-10


  Station ID                              Location

     A                           Tinkers Creek immediately
                                 upstream of Deerlick Run
                                 Confluence

     B                           Tinkers Creek immediately
                                 downstream from Deerlick Run
                                 confluence

     C                           Deerlick Run at its confluence
                                 with Tinkers Creek

     D                           Hukill Tributary downstream
                                 from Wellman discharge and at
                                 Egbert Road

     E                           Ferro Tributary at Egbert Road

     F                           South Branch at Egbert Road.

     G                           A representative site to capture
                                 the process wastestream (or sludge)

     The design requires the collection of a minimum of three
individual grab or composite water and sediment samples at each
of the stations.  The samples and analyses comprising each set
are shown in Tables 1 through 4.

     To enhance study efficiency and minimize analytical costs,
analyses will be conducted in a logical sequence of sets and
possibly subsets.  Three (3) sets are to be constructed such that
the first set (set I) consists of the first samples of each type
of medium collected at each of the stations.  The second set
(set II) comprises the second samples of each medium, etc.

     Samples will be analyzed sequentially by sets and by subsets
within sets (see table 5).  Analytical data from Set I will be
evaluated to determine the need for analysis of Set II.  Similarly,
a decision to analyze set III would depend on the combined outcomes
of sets I and II.

     The order of analyses of subsets within sets will be decided
by MRI.  Decisions on whether to continue analyses will be made
at various points during the analytical process.

     Within subsets, the extracted field samples and their
respective QC blanks and spikes should be quantified in random
order "blind" to the GC/MS operator.

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                                 B-ll








                                 Table 1



                         SAMPLES TO BE COLLECTED

Station
Medium:
Water
Sediment
Tissue**
nr> TT-,-^>V-***


A
1
1
1
i


B
1
1
1
TIN!
Set I
C D E
111
111
111
i _
CERS CREEK

F G*
1 1
1 -
1 -
AND TR]

A
1
1
1
[BUT?
Set
B C
1 1
1 1
1 1
WIES
II
D E F G*
1111
111-
111-


A
1
1
1

Set
B C
1 1
1 1
1 1

III
DBF
111
111
111


G*
1
-
-
*   If accessible



**  Subject to availability



*** Conposite water sample 4 times volume of field samples

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                            B-12




                             Table 2

                      TOTAL SAMPLES BY SETS
Medium
Water
Sediment
Tissue
QC Water
Set I
6
6
6
2
Set II
6
6
0
0
Set III
6
6
0
0
All Sets
18*
18
6
2
All sanples          20           12            12             44*


*  An additional three (3)  sanples may be added  if a process wastewater
   sanple can be obtained

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                                    B-13
)                                   Table 3
                              POTENTIAL ANALYSES
                        TINKERS CREEK AND TRIBUTARIES
Stations
Medium:
Filtrate
TSS
Sediment

i issue
/*Y- T.T_ i_ -. .-.

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                                B-14



                               Table  4

                        TOTAL ANALYSES BY SETS

                     TINKERS CREEK AND TRIBUTARIES
Medium
Water (filtrate)
TSS
Sediment
Tissue
QC water (filtrate)
QC water (TSS)
Pbtential
Analyses
Set I
6
6
6
6
4
4
32
Set II
6
6
6
0
4
4
26
Set III
6
6
6
0
0
0
18
All Sets
18*
18*
18
6
8
8
74
* If a process wastewater sample can be obtained,  this  number will  increase by
  three (3)  .

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                                B-15
                              Table  5

                 PROPOSED SEQUENCE OF ANALYTICAL RUNS*
                        BY SETS AND  SUBSETS
Set I
Set II
Set III
Run
No.
1
2
3
4
5
6
7
8
9
10
11
12
Subset
Filtered water
TSS
Sediment
Tissue
Filtered water
TSS
Sediment
Tissue
Filtered water
TSS
Sediment
Tissue

6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples
6 field samples

+ 4 QC field samples **
+ 4 QC field samples **

(subject to availability)
+ 4 QC field samples **
+ 4 QC field samples **

(subject to availability)



(subject to availability^
* Analyses within each run  are  to be made  in randan sequence which is unknown
  (blind) to the operator.

**  OA field samples collected  from stations A and D
    Method blanks will be analyzed  with each run

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                               B-16

4.1  Parameter Coverage

     In addition to CP determinations,  Temperature (C),  Flow
(cfs),  and Depth (feet) will be recorded for each sample.

4.2  Sample Collection

     All samples will be collected and  handled using procedures
fully approved by EPA.

4.3  Sampling Preparations

     All water column and sediment samples will be collected in
glassware which has undergone the following cleaning steps:

     o   Remove surface residuals.

     o   Hot soapy soak to loosen and flotate most of residue.

     o   Hot water rinse to flush away  flotated residue.

     o   Soak with deep penetrant or oxidizing agent to destroy
         traces of organic residue.

     o   Hot water rinse to flush away  materials loosened by deep
         penetrant soak.

     o   Rinse with deionized water to  remove metallic deposits
         from the tap water.

     o   Rinse with high purity methanol followed by the high
         purity methylene chloride.

     Glassware will be handled using polythene gloves to avoid
     contact with hands.

4.4  Water Column

     All water column samples collected at stations A, B & C will
be a composite of single grab samples collected from at least
three,  but if possible five or more equidistant points along a
stream transect.  Each 0.5 gallon glass jar will be triple rinsed
with stream water at the location the sample is to be collected.
The jar will then be submerged in the stream until all air is
replaced by a water sample.  The water sample depth will be half
way between the surface and the bottom of the stream.  The samples
collected along the stream transect will be composited to form a
single sample.

     Water samples collected at station D, E, F and G will be
collected as a single grab in 0.5 gallon glass jars. These"should
be collected near midstream.

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                               B-17
     Field QA water samples will be collected as described in
Section 7.7.

     All jars will be capped with teflon-lined lids.  Water
samples will require no preservative.

Each sample jar will be labeled with a barcode label.


     If, in the judgement of the field crew, more water should
be collected in order to facilitate a more successful total
suspended solids analysis, additional samples should then be
collected.  Conversely, if, in the judgement of the field crew,
additional sample collection will lend little towards this end,
then no additional water samples should be collected.


4.5  Sediment Samples

     All sediment samples will be collected in 500 ml. glass
jars.  At stations A, B and C a stainless steel scoop and/or
Ekman dredge will be used to remove sediment from the same equi-
distant points along the stream transect that the water column
samples were collected.  These discrete samples will then be
composited to form a single sample.  If sediment is not available
at these points, the most representative sample possible will be
obtained from these sites and the precise location will be docu-
mented.

     At stations D, E and F a stainless steel scoop and/or Ekman
dredge will be used to collect sediment.

4.6  Tissue Samples

     Attempts will be made to collect biological organisms from
the stream bottom at stations A, B, C, D, E and F.  Sediment
scoops will be seived using a U.S. Standard No. 30 Sieve and
invertebrate larval forms (esp., chironomid larvae) will be
collected for analysis, if available. If dredging and sieving is
not appropriate given the nature of the stream, then collections
should be made manually by overturning rocks and rubble.  If
sufficient biological organisms cannot be found over 2 hours of
sampling at any given station further biological collection will
be abandoned.
4.7  Sample Preservation And Transportation

     All sample jars will be kept in coolers out of direct sunlight
and transported in ice-filled coolers with sufficient packaging
material to reduce the possibility of breakage.  All water,
sediment, and tissue samples will be shipped via commerci-al
airlines or by overnight delivery services, to MRI's Kansas City
Laboratory.

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                            B-18


     Upon arrival at the MRI laboratory,  the samples will be
logged in and separated into sets as described above.  The first
set analyzed,  will be extracted within the first seven (7) days
from date of collection.  The remaining samples will be refrigerated
until extraction.  All samples will be analyzed within thirty (30)
days from date of collection.

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   APPENDIX C




ANALYTICAL METHOD

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                          TABLE OF CONTENTS
Section             Heading            Revision

   1.        Scope and Appication
   2.        Summary of Method
   3.        Definitions
   4.        Interferences
   5.        Safety
   6.        Apparatus and Equipment
   7.        Reagents and Standard
              Solutions
   8.        GC/MS Performance Criteria
   9.        Quality Control Procedures
  10.        Sample Preservation and
              Handling
  11.        Sample Preparation and
              Extraction
  12.        Cleanup Procedures
  13.        Instrumental Procedures
  14.        Data Reduction
      Date

November 11, 1986
November 11, 1986
November 11, 1986
November 11, 1986
November 11, 1986
November 11, 1986

November 11, 1986
November 11, 1986
November 11, 1986

November 11, 1986

November 11, 1986
November 11, 1986
November 11, 1986
November 11, 1986

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SCOPE AND APPLICATION

This method provides procedures for the detection and semiquantitative
measurement of chlorinated paraffins in water,  suspended solids,  sedi-
ment and mussel tissue.  Chlorinated paraffins  measured with this method
are C10-C12, 50-60%, Cl; C14-C17, 50-60%; and C20-C30, 40-50% Cl.

SUMMARY OF METHOD

Figure 1 presents a schematic of the analytical procedures for deter-
mining chlorinated paraffins in water, sediment, suspended solids, and
mussel tisse.  The method requires sample preparation, extraction of
chlorinated paraffins, cleanup, concentration,  and determination by
high resolution gas chromatography/negative chemical ionization mass
spectrometry/selected ion monitoring (HRGC/NCIMS/SIM).

DEFINITIONS

3.1    Concentration Calibration Solution

       Solutions containing known amounts of analytes.  These calibra-
       tion solutions are used to determine instrument response of the
       analytes as a function of mass.

3.2    Sample Batch

       A sample batch consists of up to 10 environmental samples of
       the same matrix, one laboratory method blank, and two internal
       quality control samples (one spiked and one unspiked).  Addition-
       al QC samples (e.g., field QC samples, trip QC samples) may be
       added to a sample batch where appropriate.

3.3.   Laboratory Method Blank

       This blank is prepared in the laboratory through performing all
       analytical procedures except addition of a sample aliquot to
       the extraction vessel.  A minimum of one laboratory method blank
       will be analyzed with each batch of samples.

3.4    Laboratory Method Spike

       This sample consists of an aliquot of matrix to which an known
       amount of analyte is added.  All analytical procedures are per-
       formed on this spike.  A minimum of one laboratory spike is ana-
       lyzed with each batch of samples, where appropriate, to monitor
       recovery for that batch.

3.5    Field QC Samples

       A sample collected in the field, homogenized, and divided into
       four aliquots.  Two of the aliquots are spiked in the field
       (field spikes) and two are left unspiked (field blanks).  The

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                  Suspended
                  Solids
Extract with Hexane
                                 Sediment
                                 (~100g)
          1
                       Dry
                       Soxhtet Extraction with Hexane
Column Chromatography
H2SO4/S?lica Column
Alumina Column
                           Concentrate to S
                                 Analyze
                                          Biota
                                          ~100g)
                                Homogenize,,
                                Extract wifh Hexane
                                H2SO4/Silica Slurry Cleanup
         Figure 1   Prooosed  extraction  and clean-un procedures
                       for chlorinated oaraffins.

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             field blanks are spiked in the laboratory at the  same  level  as
             the field spikes,  analyzed,  and compared to the field  spikes to
             monitor analyte behavior during transportation and  storage.

      3.6    Trip QC Samples

             Blank matrix samples prepared in the laboratory,  taken and main-
             tained on the sampling trip.   Half of the samples are  spiked in
             the field and the  remaining half left unspiked.   The samples
             are transported, stored, and analyzed in the laboratory in the
             same manner as the environmental samples.  These  samples are
             used to monitor contamination of the environmental  samples.
             For this method, deionized water served as the trip sample
             matrix.

      3.7    Performance Sample

             A standard solution of analytes prepared by the work assignment
             QCC at a concentration unknown to the analyst. This sample  is
             analyzed by the analyst and the results reported  to the QCC  for
             evaluation.  This  sample is designed to measure instrument per-
             formance.

4.    INTERFERENCES

      Chemicals which elute from the HRGC column within the retention time
      windows of the chloroparaffins and produce ions within the mass ranges
      scanned are potential interferences.  Because low levels (sub ppb)  of
      chlorinated paraffins are anticipated, the elimination of  the inter-
      ferences is essential. High purity reagents and solvents  must be used
      and all equipment must be throughly cleaned.  Because chlorinated paraf-
      fins are used as plasticizers, contact with plastics (except  polyethylene)
      must be avoided.  Polyethylene gloves should be worn during sample  pre-
      paration to avoid contamination of the samples.  Laboratory method  blanks
      must be analyzed to demonstrate the absence of contamination  that would
      interfere with the measurement of the chlorinated paraffins.   Column
      chromatographic procedures are used to remove co-extracted sample com-
      ponents;  these procedures must be performed carefully to  minimize  loss
      of chlorinated paraffins  during attempts to increase their concentra-
      tion relative to other sample components.

5.    SAFETY

      5.1    The toxicity or carcinogenicity of each reagent used in this
             method has not been precisely defined; however, each chemical
             compound should be treated as a potential health  hazard.  Chloro-
             paraffins have been shown to be carcinogenic. From this view-
             point, exposure to these chemicals must be reduced  to  the lowest
             possible level by  whatever means available.

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      5.2    All laboratory personnel will be required to wear laboratory
             coats or coveralls,  polyethylene gloves,  and safety glasses.
             The neat standards,  stock,  and working solutions  will  be  handled
             only in a Class A fume hood or glove box.   When manipulating
             stock standards or working  solution, the  analyst  is advised  to
             place the solution vials in a secure holder (sample block or
             glass beaker)  to prevent accidental spills.

      5.3    If stock or working  standards are spilled,  absorb as much as
             possible with  absorbent paper and place in a container clearly
             labelled as chlorinated paraffin waste.  Solvent  wash  all con-
             taminates surfaces with acetone and absorbent paper.

      5.4    If handling of these compounds results in skin contact, immedi-
             ately remove all contaminated clothing and wash the affected
             skin areas with soap and water for at least 15 min.

      5.5    Disposal of Laboratory Wastes

             All laboratory wastes (solvents and absorbents) will be disposed
             of as hazardous wastes.

6.     APPARATUS AND EQUIPMENT

      6.1    High Resolution Gas  Chromatograph/Negative Chemical lonization
             Mass Spectrometer/Data System.

             6.1.1    The GC must be equipped for temperature  programming,
                      and all required accessories must be available,  such
                      as syringes, gases,  and a fused  silica capillary column.
                      The injector must  be an on-column injector capable  of
                      allowing direct injection with a fused silica syringe.
                      When  using  this method, a l-|Jl injection volume  is  recom-
                      mended.  Since this  method does  not employ an internal
                      standard, injection volumes for  all extracts, blanks,
                      and calibration solutions must be consistent.

             6.1.2    High  Resolution Gas  Chromatograph-Mass Spectrometer
                      Interface

                      It is recommended  that the HRGC  column be fitted
                      directly into the  MS ion source.   If an  interface is
                      used, all components should be glass or  glass-lined
                      stainless steel.  The interface  components should be
                      compatible  with 300C temperature, and should be appro-
                      priately designed  so that the separation of the  chlori-
                      nated paraffins which is achieved in the gas  chromato-
                      graphic column is  not appreciably degraded.  Cold spots
                      and active  surfaces  (adsorption  sites) in the interface
                      may cause sample losses.

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       6.1.3    Mass Spectrometer

                The mass spectrometer must be equipped with a negative
                chemical ionization source and associated hardware,  and
                must be operated in the selected ion monitoring mode
                with a total cycle time of 3 s or less.

       6.1.4    Data System

                A dedicated hardware or data system is required to con-
                trol the rapid selected ion monitoring process and to
                acquire the data.  Quantitation data (peak areas) and
                SIM traces must be acquired during the analysis.  Quanti-
                tations are reported based on computer generated peak
                areas.

6.2    HRGC Column

       A 30-m x 0.25-mm ID fused silica capillary column coated with
       DB-5 (0.25 (Jm) is used for analysis of chloroparaffins.

6.3    Miscellaneous Equipment

       6.3.1    Nitrogen evaporation apparatus with variable flow rate.

       6.3.2    Balance capable of accurately weighing to 0.01 g.

       6.3.3    Balance capable of accurately weighing to 0.0001 g.

       6.3.4    Water bath equipped with concentric ring cover and
                capable of being temperature controlled.

       6.3.5    Stainless steel spatulas or chemical spoons.

       6.3.6    Magnetic stirrers and stir bars.

6.4    Glassware

       6.4.1    Separatory Funnels, 2 L

       6.4.2    Kuderna-Danish (KD) apparatus

       6.4.3    Soxhlet apparatus

       6.4.4    Erlenmeyer flasks

       6.4.5    Minivials

                2-mL borosilicate glass with conical-shaped reservoir
                and screw caps lined with teflon@-faced silicone disks.

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       6.4.6    Powder funnels - glass

       6.4.7    Chromatographic columns for the silica and alumina
                chromatography - mini champagne columns wit 30 ml
                reservoirs (Supelco).

       6.4.8    Carborundum boiling chips; extracted for 6 h in a
                soxhlet apparatus with benzene and air dried.

       6.4.9    Glass Wool, silanized (Supelco); extracted with
                methylene chloride and hexane and air dried.

       6.4.10   Glassware Cleaning Procedure

                The glassware will be cleaned using the procedures
                outlined in Appendix B, section 4.3.

REAGENTS AND STANDARD SOLUTIONS

7.1    Column Chromatography Reagents

       7.1.1    Alumina Woelm B, (Woelm Pharma) activated at 130C for
                48 h or longer.

       7.1.2    Silica Gel

                High purity grade, type 60, 70/230 mesh; extract the
                silica gel in a Soxhlet apparatus with methylene chlor-
                ide for 10 h (minimum of two cycles per h).  Air dry
                and activate by heating in a foil-covered glass contain-
                er for at least 24 h at 130C.

       7.1.3    Silica gel impregnated with 40% (by weight) sulfuric
                acid.  Add 2 parts (by weight) concentrated sulfuric
                acid to 3 parts (by weight) silica gel (extracted and
                activated) in a glass screw cap bottle.  Tumble for
                5 to 6 h, shaking occasionally until free of lumps.

       7.1.4    Sulfuric Acid, Concentrated; ACS grade, specific
                gravity 1.84.

7.2    Sodium sulfate, granular, anhydrous.  Extract with methylene
       chloride for 16 h (minimum of 2 cycles per h), air dry and then
       muffle for longer than 4 h; in a shallow tray at 400C.  Let
       cool in a desiccator and store in a 130C oven.

7.3    Solvents

       High purity, distilled in glass; methylene chloride, hexane,
       diethyl ether, acetone and isooctane.  High purity solvents are
       dispensed from teflon squirt bottles.

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      7.4    Concentration Calibration Solutions

             Three Chloroparaffin standard materials  (Paroil  142,  Paroil  152,
             and Paroil 1160)  are required.   Portions  of the  standards  are
             accurately weighed and dissolved in  isooctane  to produce  concen-
             tration calibration solutions at the concentrations  shown  in
             Table 7.1.

8.     GC/MS PERFORMANCE CRITERIA

      Single run limited mass  range selected ion  monitoring analyses of the
      chlorinated paraffins are carried out with  the  instrumental  conditions
      and parameters outlined  in Table 8.1.   Eleven mass ranges,  given  in
      Table 8.2 are monitored  during each run.

      8.1    Tuning and Mass Calibration

             The mass spectrometer is tuned on a  daily basis  prior to  sample
             analysis using perfluorotributylamine (FC-43).   For  reproduci-
             bility of the relative abundance measurements, the abundance
             ratio of the m/z  414: m/z 633 ion will be adjusted to 1:3  ( 10%).

      8.2    Initial Calibration for Clorinated Paraffin Analysis

             Initial calibration is required before any samples are analyzed
             for chlorinated paraffins.   Initial  calibration  is also required
             if any routine calibration does not  meet  the required criteria
             listed in Section 8.3-

             8.2.1    Tune and calibrate the instrument with  FC-43 as  outlined
                      in Section 8.1.

             8.2.2    The five concentration calibration solutions listed in
                      Table 2  will be analyzed for the initial calibration
                      phase.

             8.2.3    Using the HRGC and MS conditions in Table 8.1 and the
                      SIM monitoring parameters given  in Table 8.2, analyze
                      1 pL of  each of the five concentration  calibration
                      solutions.

             8.2.4    Compute  the response factors for each mass  range  using
                      the computational method in Section 14.2.

             8.2.4    Calculate the mean RF and the standard  error.

      8.3    Criteria for Acceptable Initial Calibration

             8.3.1    The standard error of the mean  RFs for  the  five  cali-
                      bration  standards must be less  than 30%.

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               Table 7.1.   Concentration Calibration Solutions
                           Concentration in calibration solutions (pg/mL)
    CP                  CS1         CS2         CS3         CS4         CSS


Paroil 142              100          50          20          10          1

Paroil 152              100          50          20          10          1

Paroil 1160             100          50          20          10          1
                                     8

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         Table 8.1.   HRGC/NCIMS Operating Conditions for CP Analysis
Mass spectrometer
     Mode:
     lonization gas:
     Ionizer pressure:
     Electron energy:
     Emission current:
     Electron multiplier voltage:
     SEV:
     Source temperature:
     Overall SIM cycle  time:
negative chemical ionization
methane
0.7 torr
70 eV
0.3 mA
-1700 V
10"7
170C
3 s
Gas chromatograph

     Column coating:
     Film thickness:
     Column dimensions:
     Helium linear velocity:
     Helium head pressure:

     Injection type:
     Injector temperature:
     Interface temperature:
     Injection size:
     Initial temperature:
     Initial time:
     Temperature program:
DB-5
0.25 urn
30 m x 0.25 mm ID
~ 25 cm/s
8 psi

on-column
ambient
300C
1 ML
80C
2 min
80C to 320C at 10C/min

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                Table 8.2.   SIM Mass Ranges for CP Analysis
                                  Nominal
Mass range                     scan time (s)                        CP cell


 324-329                           0.34                             C10-C12
 359-364                           0.34
 367-372                           0.34
 393-401                           0.34
 401-420                           0.35                             C14-C17
 441-454                           0.34
 477-488                           0.36
 498-503                           0.36                             C20-C30
 514-518                           0.34
                                    10

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             8.3.2    The SIM traces for all ions  used for quantitation must
                      present a signal-to-noise (S/N)  ratio of  1  3.

      8.4    Routine Calibration

             Routine calibration must be performed at  the beginning  of every
             day before actual sample analyses are performed and  after all
             samples for the day are analyzed.  Additional calibration during
             the day may be employed if instrument instability  is suspected.

             8.4.1    Inject 1 [JL of concentration calibration  solution CS2
                      as the initial calibration check on each  analysis day.

             8.4.2    Compute the RF for each ion  range in the  concentration
                      calibration solution.

      8.5    Criteria for Acceptable Routine Calibration

             8.5.1    The measured RF for all cells must be within  30%  of
                      the average mean calculated  in section 8.1.6.2.

             8.5.2    If this criterion is not met, a  second attempt will be
                      made before repeating the entire initialization process.
9.     QUALITY CONTROL PROCEDURES

      9.1    Summary of QC Analyses

             9.1.1    Initial and routine calibration and instrument per-
                      formance checks.

             9.1.2    Analysis of a batch of samples  with accompanying QC
                      analysies:  up to 10 environmental samples  of one
                      matrix type plus  QC analyses  including one  method
                      blank, and one spiked blank.  Additional  QC samples,
                      including field spikes,  field blanks,  trip  spikes and
                      trip blanks may be included in  a batch of samples.

      9.2    Performance Evaluation Solutions

             Prior to sample analysis,  a solution provided by the work assign-
             ment quality control cooridinator containing known amounts of
             chlorinated paraffins will be analyzed.   The accuracy of measure-
             ment for performance evaluation samples  should be  in the range
             of 70-130% of true value.

      9.3    Laboratory Method Blanks

             A minimum of one laboratory method blank is generated with each
             batch of samples.  A method blank is generated by performing
                                    11

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             all steps detailed in the analytical  procedure  using  all  rea-
             gents,  standards,  equipment,  apparatus,  glassware,  and  solvents
             that would be used for a sample analysis.   For  sediment,  sus-
             pended  solids, and biota samples,  the matrix  is omitted.  Deion-
             ized water is substituted for environmental water.

             9.3.1    An acceptable method blank exhibits  no positive  response
                      in the characteristic ion ranges monitored.

                      9.3.1.1    If the above criterion  is not met,  solvents,
                                 reagents, apparatus, and  glassware  are
                                 checked to locate and eliminate the source
                                 of the contamination before any further
                                 samples are extracted and analyzed.

                      9.3.1.2    If new batches of reagents  or solvents con-
                                 tain interfering  contaminants,  they will be
                                 purified  or discarded.

      9.4    Spiked  Samples

             9.4.1    Method Spikes

                      A minimum of one method spike is generated with  each
                      batch of  samples.  A method  spike  is generated by per-
                      forming all steps detailed in the  analytical procedure
                      using all reagents,  standards,  equipment,  apparatus,
                      glassware, and solvents that would be  used for a sample
                      analysis.  For sediment,  suspended solids, and biota
                      samples,  the matrix  is omitted.  Deionized water is
                      substituted for environmental water.  These  samples
                      are spiked with known amounts of chlorinated paraffins
                      prior to  extraction.

             9.4.2    Field Spikes

                      Field spikes will be analyzed using  the method at the
                      frequency specified  in the experimental design contained
                      in the main body of  the QAPP.

             9.4.3    Trip Spikes

                      Trip spikes will be  analyzed using this method at the
                      frequency specified  in the experimental design con-
                      tained in the main body of the QAPP.

10.    SAMPLE PRESERVATION AND HANDLING

      Water and sediment samples will be maintained at 8C or lower  until
      extraction.  Mussel samples will be  maintained at  -20C until  extrac-
      tion.  Sample  extracts will be stored at 8C or less until analysis.
                                    12

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11.    SAMPLE PREPARTION AND EXTRACTION

      11.1   Extraction of  Water Samples

             11.1.1    Filter water  through a  0.45  M  filter  (Type HA, Millipore,
                      47 mm) in a millipore filtration apparatus.  Use a 2 L
                      suction flask to receive  the filtrate.  Use  suction by
                      aspiration to facilitate  the process.

             11.1.2    Rinse the sample jar with a  250-mL portion of the fil-
                      trate and pass  through  the filter again.  Note:  For
                      samples with  a  large amount  of particulate,  more than
                      one filter may be needed  if  filtration becomes slow.

             11.1.3    Measure the volume  of the filtrate in a 500-mL graduated
                      cylinder and  pour back  into  the sample jar.

             11.1.4    Transfer the  filter to  a  clean 4 oz jar using forceps.

             11.1.5    Transfer 1000 mL of the filtrate into a 2-L  separatory
                      funnel.

             11.1.6    Add 60 mL of  hexane, stopper,  invert  and vent the funnel.
                      Shake the funnel for 2  min vigorously enough to form
                      an emulsion.

             11.1.7    Allow the phases to separate,  drain the aqueous phase
                      into  a 1000-mL Erlenmeyer flask and the hexane phase
                      into  a 250-mL Erlenmeyer  flask.

             11.1.8    Transfer the  aqueous phase back into  the 2-L separatory
                      funnel and add another  60 mL of hexane to the 1000 mL
                      Erlenmeyer to rinse the flask. Add the rinse to the
                      separatory funnel and shake  again for 2 min.

             11.1.9    Repeat step 11.1.7.

             11.1.10   Discard the aqueous phase.

             11.1.11   Add enough anhydrous sodium  sulfate to the hexane
                      extract to remove the water  (10-20 g).

             11.1.12   Transfer the  hexane extract  to a 250-mL Kuderna Danish
                      (KD)  flask equipped with  either a 5-  or 10-mL receiver.
                      Complete the  transfer with three rinses of hexane,
                      10-20 mL each.

             11.1.13   Add several carborundum chips  and place a 3-ball Snyder
                      column into position.

             11.1.14   Concentrate the hexane  to about 5 mL  on a steam bath.
                                    13

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       11.1.15  Transfer the concentrated hexane extract to a 4-dram
                vial using a pasteur pipette.   Complete the transfer
                with three rinses of hexane (about aO.5 mL each).

       11.1.16  Proceed to the sulfuric acid/silica cleanup (Section 12.1)

11.2   Extraction of Sediment Samples

       11.2.1   Transfer the sediment sample (~ 1 kg)  to a clear pyrex
                baking dish (12 in x 12 in x 2 in) with a stainless
                steel spatula.

       11.2.2   Drain and discard the excess water.

       11.2.3   Dry the sediment by placing in an oven (65-70C) for
                48-60 h.   Stir the sediment occasionally to facilitate
                drying and to break up large clumps.

       11.2.4   Break the sediment into a fine powder  using a mortar
                and pestle if necessary.   Remove large rocks with a
                pair of forceps.

       11.2.5   If necessary, sift the sediment through a screen to
                remove particles greater than 1 mm.

       11.2.6   Weigh 100 g (+/- 0.1 g) of the sediment into a clean
                8 oz jar.

       11.2.7   Add 100 g (+/- 0.1 g) of anhydrous sodium sulfate to
                the sediment sample and mix with a spatula.

       11.2.8   Load the sediment/sodium sulfate mixture into a Soxhlet
                flask containing a pad of glass wool.

       11.2.9   Add 200 mL of hexane to a 200-mL round bottom flask,
                add several carborundum chips and extract the sample
                for 16 h.

       11.2.10  Allow the apparatus to cool and manually cycle any
                remaining hexane in the sediment.  Remove the 250-mL
                flask from the apparatus.  Discard the sediment.

       11.2.11  Transfer the hexane to a 250-mL KD flask.  Complete
                the transfer with three 10-mL rinses  of hexane.  Con-
                centrate to about 5 mL and transfer to a 4-dram vial
                using a Pasteur pipette.   Complete the transfer with
                three 0.5-mL rinses of hexane.  Cap with a teflon-
                lined lid.

       11.2.12  Proceed to the sulfuric acid/silica cleanup (Section
                12.1).
                              14

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11.3   Preparation and Extraction of Mussel Samples

       11.3.1   Open the mussel with a sharp knife by cutting the
                muscles attached to the shell next to the hinge.

       11.3.2   Scrape and transfer the tissue to a tared 500-mL  beaker.

       11.3.3   Drain off any residual water and remove any plant tissue.

       11.3.4   Open and add enough mussels to obtain at least 100 g
                of tissue.

       11.3.5   Homogenize the tissue in a Waring blender.   A homo-
                geneous viscous liquid should be obtained.

       11.3.6   Transfer the tissue homogenate to a clear pyrex
                dish (12 in x 12 in x 2 in) using a stainless steel
                spatula.

       11.3.7   Slowly add 3 times the sample weight of anhydrous
                sodium sulfate to the homogenate, stirring frequently
                with a spatula.

       11.3.8   Allow the mixture to dry until it is free flowing.
                This step may take several days.

       11.3.9   Load the tissue/sodium sulfate mixture into a Soxhlet
                flask to an equivalent weight of 100 g of mussel  tissue.
                Extract for 16 h with 450 ml of hexane.

       11.3.10  Cool and remove the round bottom flask.  Discard  the
                tissue/sodium sulfate mixture.

       11.3.11  Add 10-20 g of anhydrous sodium sulfate to dry the extract.

       11.3.12  Add 20 g of 40% (w/w) sulfuric acid on silica gel, and
                let stand for 1 h with occasional swirling.

       11.3.13  Transfer the extract to a 250-mL KD flask.   Complete
                the transfer with three 20-mL rinses of hexane. Concen-
                trate to about 5 mL.

       11.3.14  Transfer the concentrated extract to 4-dram vial.  Com-
                plete the transfer with three 0.5-mL rinses of hexane.

       11.3.15  Concentrate the extract to about 0.5 mL with a gentle
                stream of nitrogen.  Cap with a teflon-lined lid.

       11.3.16  Proceed to the alumina cleanup step.  (Section 12.2.)
                              15

-------
12.    CLEANUP PROCEDURES .

      12.1   Sulfuric Acid/Silica Cleanup

             12.1.1    Prepare the columns (champagne  minicolumns  with  30-mL
                      reservoir,  Supelco  Inc.)  by inserting  a  small  pad  of
                      pesticide-grade  glass  wool  (DCMS  treated, Alltech
                      Associates).

             12.1.2    Rinse  the  columns and  glass wool  with  three aliquots
                      each of acetone  and hexane  in that order.

             12.1.3    Add  1.0 g  of 40% (w/w) sulfuric acid/silica to the
                      column. Layer about 1 cm of anhydrous sodium  sulfate
                      on top of  the bed.

             12.1.4    Wet  the column with enough  hexane to saturate  the  bed.
                      DO NOT ALLOW THE COLUMN TO  DRAIN  FAR ENOUGH TO EXPOSE
                      THE  BED OF SILICA.

             12.1.5    Transfer the sample to the  column using  a pasteur
                      pipette.   Complete  the transfer with three  0.5-mL
                      rinses of  hexane.   Collect  the  eluent  in a  6-dram
                      vial.

             12.1.6    Allow  the  sample extract  to flow  through the column
                      and  add 5  mL of  hexane to the column.

             12.1.7    Allow  the  column to run dry and rinse  the tip  with
                      about  1 mL of hexane into the vial.

             12.1.8    Concentrate the  eluate to about 0.5 mL with a  gentle
                      stream of  nitrogen.  Cap  with a teflon-lined  lid.

      12.2   Alumina Cleanup

             12.2.1    Prepare the columns as described  for  the sulfuric  acid/
                      silica columns (Section 12.1.1).   Use  1.0 g of basic
                      alumina prepared as described in  Section 7.1.1.

             12.2.2    Wet  the column with enough  hexane to  saturate  the  bed.
                      DO NOT ALLOW THE SOLVENT  LEVEL  TO FALL BELOW THE TOP
                      OF THE ALUMINA BED.

             12.2.3    When the solvent level has  reached the bed, add  the
                      sample extract with a  pasteur pipette.

             12.2.4    Measure 10 mL of 1% (v/v) diethyl ether  in  hexane into
                      a graduated cylinder.   Complete the transfer of  the
                      sample extract to the  column with three  rinses of the
                      1% ether in hexane  mixture  when the sample  extract has
                                    16

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                      completely drained into the alumina bed.   Add the re-
                      maining 1% ether in hexane.  Collect the  eluate  in a
                      4-dram vial.

             12.2.5   When the 1% ether in hexane has reached the top  of the
                      bed, add 10 ml of 50% diethylether in hexane to  the
                      column.  Collect the eluate in a fresh 4-dram vial.
                      Discard the 1% ether eluate.

             12.2.6   After the 50% ether in hexane fraction has completely
                      eluted and the column drained dry, rinse  the tip of
                      the column with about 1 mL of hexane and  concentrate
                      the sample to about 0.5 mL with a gentle  stream  of
                      nitrogen.

             12.2.7   Transfer the sample with a pasteur pipette to a  2-mL
                      conical reaction vessel (Supelco).  Complete the trans-
                      fer with one rinse of hexane and two rinses of acetone
                      (about 0.5 mL each).  Reduce the sample to dryness with
                      a gentle stream of nitrogen.

             12.2.8   Cap with a teflon-lined lid and store for analysis by
                      mass spectroraetry.

             12.2.9   Prior to analysis, the analyst will add a 50 (JL  (or
                      other volume) aliquot of isoctane to the  sample  and
                      sonicate for 30 sec.

13.    INSTRUMENTAL PROCEDURES

      13.1   Once routine calibration criteria are met, the instrument is
             ready for sample analysis.  Prior to the first sample, a  blank
             injection of isooctane will be analyzed to document system
             cleanliness.  If any evidence of system contamination is  found,
             corrective action must be taken and another isooctane blank ana-
             lyzed.

      13.2   The typical daily sequence of injections is shown in Table 13.1.

14.    DATA REDUCTION

      In this section, the procedures for data reduction are outlined  for
      the analysis of chlorinated paraffins in environmental samples.

      14.1   Quantitative Calculations

             14.1.1   Calculation of Response Factors

                      Response factors for each mass range are  calculated
                      from the data obtained during the analysis of concen-
                      tration calibration solutions using Equation 14.1.
                                    17

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   Table 13.1.  Typical Daily Sequence for CP Analysis





1.   Tune and calibrate mass spectrometer with FC-43.



2.   Inject concentration calibration solution.



3.   Inject isooctane blank.



4.   Inject samples.



5.   Inject concentration calibration solution.
                           18

-------
                           ET _    Astd                        -
                                Cstd x Vstd

                Where:
                  Astd is computer generated area for a mass range
                  Cstd is the concentration of the standard (ng/pL)
                  Vstd is the volume of sample injected in ((JL)

       14.1.2   Calculation of Chlorinated Paraffin Concentrations

                Chlorinated paraffin concentrations will be calculated
                for each mass range using Equation 14.2.

                                              .              EQ.  14.2
                      /-.     *.       /  i_ \     Aex x Vex
                      Concentration (ppb) = 5=	rp:	r:
                                     **     RF x Vinj x M
                Where:
                  Aex is the computer generated area of the mass range
                    in the extract
                  RF is the response factor calculated in Equation 14.1
                  Vinj is the volume of extracted injected ((JL)
                  Vex is the final volume of the extract (|JL)
                  M is the mass of sample taken for analysis (g)

14.2   Estimated Method Detection Limit

       Estimated method detection limits must be calculated in situa-
       tions where (1) no response is noted for a specific mass range
       and (2) where a response is quantitated as a trace value, that
       is, where the response is between 3 and 10 times the signal to
       noise ratio.  These two cases are discussed below.

       14.2.1   For samples in which no signal is detected above the
                baseline, calculate the estimated minimum detectable
                concentration.  The background a is determined by
                integration the ion abundances for the mass ranges in
                the appropriate regions and relating the area to an
                estimated concentration that would produce that area.
                The formula is given in Equation 14.3.

                                                         EQ. 14.3
                           r-nr -   x     x
                           ^    RF x Vinj x M
                Where:
                  EDL is the estimated detection limit  (ppb)
                  Aex is the computer generated area of the mass range
                    in the extract
                  RF is the response factor calculated  in Equation 14.1
                  Vinj is the volume of exract injected (pL)
                  Vex is the final volume of extract (pL)
                  M is the mass of sample taken for analysis (g)
                              19

-------
             14.2.2   If a response for a specific mass  range  is  quantated
                      as a trace value [signal to noise  is  greater than or
                      equal to 3 (a) but less  than 10 (or)],  the analyst must
                      also provide an estimated method detection limit.
                      This is accomplished by  using the  average observed
                      signal to noise on either side of  the  response and
                      calculating as given in  Equation 14.3.

15.    REPORTING AND DOCUMENTATION

      Data will be reported for each individual sample.   Concentration values
      or estimated detection limits will be reported for each  mass range moni-
      tored.   Raw data,  calculations, etc, will be maintained  in a format as
      to allow a complete external data reviewed.
                                    20

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                 APPENDIX D
VALIDATION PROCEDURES FOR THE ANALYTICAL METHOD

-------
              D-l
APPENDIX D  TABLE OF CONTENTS
HEADING
Summary
Experimental Design
Analytical Procedures
Data Reduction
Data Quality Assessment
REVISION
 DATE






11/18/86






11/18/86






11/18/86






11/18/86






11/18/86

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                          D-2
1.0  Summary

The method validation phase of this work was designed to assess the
precision, accuracy, and recovery of the method.  Matrix samples,
(except mussel tissue, which was obtained commercially) for the
validation were obtained from Sugar Creek (Dover,  Ohio) sampling
stations A and B during a reconnaissance trip conducted on
August 12, 1986.  Station A is located downstream from the
Dover Chemical Plant and station B is located upstream. Station B
samples provided the basis for method assessment,  while station A
samples were run to obtain a preliminary indication of downstream
CP  levels.


2.0 Experimental Design

The experimental design for the method validation phase of this
study is outlined in Table 2.1.  The design is broken down into
two phases.  The first phase was designed to measure background
(LO) levels of CPs in the matrices, and to provide a basis for
setting spiking levels (LI - L3) for phase II.  The phase II
analyses were used to assess method accuracy, precision, and
recovery.  A batch of samples consists of four validation samples
and associated quality control samples.  A laboratory method
blank and a spiked control sample for water and a laboratory
method blank for sediment have been incorporated.   Since a
control sediment was not available, spiked control sediments were
not included in the design.


3.0 Analytical Procedures

The validation samples were analyzed according to the procedures
detailed in Appendix C.


4.0 Data Reduction

Data will be reduced according to the procedures outlined in
Appendix C.


5.0  Data Quality Assessment

Precision, accuracy and recovery will be determined for three
spiking levels for each of the three cells.


     5.1   Precision

           Precision will be assessed as relative standard deviation
           within each cell.  Precision will be expressed as relative
           standard deviation as defined in Section 9.1 of the QAPP.

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 22-Aug-96
      D-3

  TABLE 2.1

fIRI  PROJECT No.  a853-A(OD CHLOROPARAFFINS
METHOD VALIDATION

A :  WATER
                           (upstreaa)
               (downstream)
  Method
   Blank
(distilled
                                                                               Spike
                                                                              Control
                                                                             (distilled

PHASE
=33333=3=3
I
II
II
II
Total *

Batch No.
3==333===3S3=a
1
2
3
4
o-f analyses:
B' Pool
LO LO
333333333333333333
2X 2X
IX
IX
-
2 4
"A"
LI
= 3 = 32
-
IX
IX
IX
3
Pool
L2
133333:
-
IX
IX
IX
3

L3
13=3=3333
-
IX
IX
IX
3
water)
SO
=33333=33333
IX
IX
IX
IX
4
 water)
SI
333333=33333=
IX
IX"
IX
IX
4
B :  SEDIftENT
                           (upstreaa)
              (downstream)
 Method
  Blank

Batch No.

5
6
7
8
TotaL
B" Pool
LO LO
3333=3333=3333333=
2X 2X
IX
"
IX

2 4
A"
LL
S3333
-
IX
IX
IX
3
Pool
L2
=3333:
-
IX
IX
IX
3

L3
S33333
-
IX
IX
IX
3
(no sediaent)
SO
.~~~~
IX
IX
ix
IX
4
      I
     II
     II
     II
Note 1 : IX = single analysis ; 21 * replicate analyses.

Note 2 : Each sample in the above table ,  whether in the uatrix
         (e.g., riverwater or sediaent) or not, wilL go through
         the extraction process.

Note 3 : One solvent blank and one calibration check at the
         the L2 spiking level will be run  per day
         for instruaent check,                                 .. _

Note 4 : Spiking level St -for the distilled water spike check
         will be 10 tiaes the estiaated LOQ (i.e., 5 ppb for water).

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                    D-4
5.2   Accuracy
      The accuracy of the method will be assessed within each
      cell.  Accuracy will be expressed as A% as defined in
      Section 9.2 of the QAPP.
5.3   Recovery
      Recovery will be assessed within each cell.   The measure
      of recovery will be percent recovery as defined in
      Section 9.3 of the QAPP.

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    APPENDIX E
PEI QUALIFICATIONS

-------
     PEI Associates, Inc.
                          LESLIE J. UNGERS, C.I.H.
                            Senior Staff Expert
EDUCATION:
     B.A., Zoology, Miami University, 1973
     M.S., Industrial Hygiene, College of Medicine, University of Cincinnati,
      1984

PROGRAM QUALIFICATIONS:

0    Certified Industrial Hygienist

0    Senior Industrial Hygienist for PEI specializing in protection,  surveil-
     lance and monitoring of workers handling hazardous wastes and toxic
     substances

0    Experienced in the collection of water sediment, biota and other
     limnological samples.

0    Experienced in the management of field studies involving chain of
     custody and sample QA

0    Working knowledge of EPA and OSHA regulations and NIOSH recommendations
     as they apply to the ambient and work environment

RELEVANT EXPERIENCE:

Mr. Ungers is a Board-Certified Industrial Hygienist (No. 2302) with more
than 12 years of experience in the identification, evaluation, and control  of
workplace and environmental hazards.  As Group Leader of PEI Associates' Risk
Assessment Group, he is responsible for managing and conducting industrial
risk assessment projects and audits for both the government and the private
sector.  He is an adjunct professor at the University of Cincinnati,  College
of Mathematics and Applied Sciences.  He is a full-member of the American
Industrial Hygiene Association and a member of the American Academy of Indus-
trial Hygiene.

Field Investigations

Mr. Ungers has directed a number of investigations and chemical reviews for
the U.S. Environmental Protection Agency's Office of Toxic Substances.  He
has been instrumental in promoting the success of the EPA's interagency
efforts with NIOSH.  His past experience in conducting field investigations
of water and sediment quality at inland lakes and streams, conducting NIOSH
surveys and control technology efforts has been helpful to EPA in its
formulation of cost-effective industry-specific investigations.  Several
years ago, Mr. Ungers was instrumental in assisting OTS with the development
of a methodology assessing the relative importance of toxic chemicals.

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     PEI Associates, Inc.
Leslie J. lingers (continued)

Industrial Site Surveys

Mr. Ungers has conducted over 200 site surveys.   These efforts have allowed
him to gain an understanding of a wide range of  chemical  and manufacturing
operations, including inorganic minerals processing,  paint and surface  coat-
ing formulation, organic chemical manufacturing, food processing,  microelec-
tronics, and semiconductor fabrication.  His experience in these industries
has focused on the identification of potentially hazardous unit operations
that may contribute to the release of toxic substances into the workplace or
surrounding environment and result in real  or potential violations of OSHA
Health and Safety Standards.

Industrial Hygiene

Mr. Ungers has conducted industrial hygiene monitoring at a variety of  indus-
trial processes.  This experience includes  monitoring workers for  exposures
to organic solvents (e.g., methyl ethyl ketone,  butyl acetate, benzene,
xylene) at paint manufacturing operations.   He has also assessed worker
exposure to a number of toxic substances, including organic solvents, toxic
gases, and flammable and pyrophoric gases.   This work has required him  to
determine the sources of occupational exposure and to define worker activ-
ities prior to establishing a monitoring scenario.  During these investiga-
tions Mr. Ungers has been responsible for ensuring the quality of  sampling
data collected in the field.  Mr. Ungers1 OTS-related experience in this area
includes using his industrial field experience in estimating potential  routes
of exposure to workers involved in processes for which little or no monitor-
ing data are available.

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     PEI Associates, Inc.


                               THOMAS J. WAGNER
EDUCATION:

     Five years graduate work toward Ph.D.  in Analytical  Chemistry,  University
      of Minnesota, 1971
     B.A., Chemistry, Thomas More College,  1966

QUALIFICATIONS:

Mr. Wagner has over 20 years' experience in analytical  chemistry and 8 years
in technical project management.  He has been with PEI  for 8 years.   For the
past 7 years he has served as the Quality Assurance Coordinator for  the
Environmental Measurement Division.  Previously he was  Project Manager and
Senior Group Chemist.  In the past, he has  taught analytical  chemistry and
instrumental analysis at the University of Cincinnati.  Mr.  Wagner has an
extensive background in both wet chemical methods and instrumental techniques
such as atomic absorption, gas chromatography, ion chromatography, infrared
spectroscopy, nuclear magnetic resonance, and mass spectroscopy.  He is a
member of the American Chemical Society, including both the Analytical and
Environmental Divisions.

RELEVANT EXPERIENCE:

Quality Assurance

As Quality Assurance Coordinator, Mr. Wagner has served as Quality Assurance
Officer for two previous SSCD (DSSE) contracts.  When required for these pre-
vious contracts, he has developed and monitored the QAPP's under the "Interim
Guidelines and Specifications for Preparing Quality Assurance Project Plans,
QAMS 005/80," which included plans for the testing of a Solid Waste  Reduction
Plant for Washington, D.C., and VE observations during Stationary Source
Inspections and Test Observations.  Mr. Wagner has revised the quality assur-
ance plan for PEI's laboratory, written quality assurance plans for  the
Emission Measurement Group and Ambient Monitoring Group,  written chain-of-
custody procedures for sampling and analysis, and administered performance
audit programs.  He has also written sections in Volumes  2 and 3 of  the U.S.
EPA "Quality Assurance Handbook for Air Pollution Measurement Systems," and
conducted quality assurance and VOC sampling and analysis workshops  for
government personnel and private contractors.

Mr. Wagner is Program Manager for PEI's contract for Quality Assurance Tech-
nical Support to the Water Engineering Research Laboratory (WERL).  Under
this contract he has conducted numerous Technical System  Audits and  Data
Quality Audits nationwide and directed the development of a "Quality Assur-
ance Procedures Manual for WERL Project Officers."

Source Testing

Mr. Wagner has participated in the project design and developed and monitored
QAPP's for the Collaborative Test of EPA Method 6B, the Air Curtain Hood Test

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    ' PEI Associates, Inc.
Thomas J. Wagner (continued)

Program at the Asarco Copper Smelter in Tacoma,  a full-scale  scrubber  charac-
terization study of large utility boilers, the Comparison Study of EPA Methods
16 and 16A, the Comparison Study of EPA Methods  15 and 15A, Development of  a
Source Test Method for Chromium Speciation, and  the Comparison study of EPA
Method 5, 5B, and 5F for fluidized catalytic Cracking units and oil burning
utilities boilers.  Mr. Wagner assisted in the design and was the QA Officer
for the laboratory and field validation studies  of the Volatile Organic
Sampling Train (VOST).

Field Monitoring and Analytical Support

Mr. Wagner has participated in the project design and developed and monitored
QAPP's for the Philadelphia Aerosol Field Study, the Toxicity Treatability
Assessment of Iron and Steel Industry Wastewaters, Assessing  Hazarous  Waste
Contamination of Locally Grown Agricultural Products, and the ambient  air
monitoring during the hazardous waste cleanup at the Chem-Dyne site.   He has
managed projects involving the evaluation of new analytical techniques for
screening ambient particulate samples for polynuclear aromatic hydrocarbons
and the development of an alternate analytical procedure for  EPA Method 5F.
Mr. Wagner is the Quality Assurance Officer for  a toxic monitoring project
for an industrial client.  This project involves the monitoring of two
inorganic and five organic compounds in the ambient air at five sites.  As  a
senior staff chemist, he improved the technique  for trace metal analyses by
atomic absorption in solid waste leachate samples and developed a method for
measuring hydrocarbon emissions from a stationary source. He also supervised
the laboratory effort for a full-scale scrubber  characterization study
involving both trace organic and trace metal analyses in gaseous, liquid, and
solid effluents.

Technical Support

Mr. Wagner has developed lectures for workshops  on quality assurance  for
emission testing based on Volume III of the Quality Assurance Handbook for
Air Pollution Measurement Systems:  Stationary Source Specific Methods and
for VOC Sampling and Analysis Workshop. EPA-340/l-84-001b.He has also
prepared lectures for advanced training and special topics in emission testing
workshops.  Mr. Wagner has participated in the presentation  of 18 workshops
nationwide and has presented papers at national  symposia, including the 1986
EPA/APCA Symposium on Measurement of Toxic Air Pollutants.

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      ' PEI Associates, Inc.
                               Thomas A.  Janszen


EDUCATION:     B.S., Biology, Rockhurst College, 1972
               M.S., Biology, Old Dominion University,  1974


RELEVANT EXPERIENCE:

Mr. Janszen is a Group Leader and a Project Director/Manager  in  PEI's  Waste
Management Division with more than 11 years of experience.  Mr.  Janszen was
the project manager for collecting mollusk samples over a three-mile section
of the Ohio River near Cairo Illinois.  Mr. Janszen was the project manager
and lead field sampler for collecting monthly water and sediment samples  over
a period of two years from a lake in Virginia Beach, Virginia.   Mr. Janszen
also collected extensive numbers of sediment samples from the Great Dismal
Swamp over a one year period.

During the past eight years, he has managed or played a key technical  role  in
over 40 solid and hazardous waste projects totaling over $3,000,000.
Mr. Janszen is the project manager for preparing three  chemical  agent  treat-
ment and storage RCRA Part B's for the Department of Defense. He is also  the
project manager for preparing a RCRA Part B for one of  the nation's largest
offsite industrial hazardous waste storage and treatment facilities.
Mr. Janszen was directly responsible for the design of  the container storage
area at this facility, which will store as many as 13 different  types  of
incompatible waste at one time.  Mr. Janszen was also responsible for  the
complete design of an indoor hazardous waste pile to be operated at this
facility.  This particular facility will  also be permitted to store and treat
almost all hazardous wastes listed in 40 CFR 261.

Mr. Janszen is currently directing the performance of 150 liability audits  of
hazardous waste TSD facilities around the United States for DOE.  Mr.  Janszen
is also PEI's key senior advisor on a RCRA Subtitle D implementation project
being performed for OSW.  Mr. Janszen was the Quality Assurance  Officer for a
RCRA Part B developed for a high-technology computer firm.  He performed  over
50 technical reviews of Part B applications (including  15 land disposal
facilities).  Mr. Janszen has also managed the development and presentation
of land disposal RCRA Part B workshops across the country.  These workshops
were presented to Federal and state agency personnel and industrial  per-
sonnel.  Additionally Mr. Janszen has developed hazardous waste  training
programs for several industrial clients who manage hazardous  wastes.   He  also
assisted in the development of a model Part B application to  be  used  in
workshops and seminars for industry and EPA.

Mr. Janszen's more than 100 site inspections at a wide variety of industrial
facilities have involved evaluations of facility compliance  and  assessments
of technology related to hazardous waste handling, treatment, storage, and
disposal procedures; fugitive dust control; air pollution control; and vola-
tile organic compounds.  He has also conducted interim status inspections at
land disposal facilities.

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      PEI Associates, Inc.
Thomas A. Janszen (continued)

Mr. Janszen played a key technical role in PEI's development of the most
extensive and detailed Part B checklist used for reviewing Part B's for
completeness and technical adequacy.  This checklist is now widely used by
many U.S. EPA Regions and many state agencies.

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       PEI Associates, Inc.
                               ROBERT L. HOYE
EDUCATION:
     B.S., Zoology, Ohio University, 1974
     M.S., Environmental Science, University of Cincinnati,  1979

RELEVANT EXPERIENCE:

Mr. Hoye is a Group Leader in PEI's Waste Management Division.  He  has 9
years of experience in conducting RCRA related solid and  hazardous  waste
management studies and assessments.  Mr.  Hoye has  acted as Project  Manager,
Task Manager, and/or principal researcher on projects dealing with  data base
development, industry wide solid waste assessments,  waste characterization
studies, environmental monitoring of groundwater and surface waters,  evaluation
of solid and hazardous waste management practices, development  of multimedia
sampling and analysis protocols and manuals, and the impact  and costs of
existing and alternative waste control technologies.  Mr. Hoye  has  managed  or
conducted over 100 site inspections and sample acquisition visits throughout
the country and managed ground water and surface water monitoring at  eight
waste disposal facilities.

Mr. Hoye recently managed a study for EPA's Office of Radiation Programs  to
estimate radon-222 emissions and associated health risks  from uranium mills
and associated tailings piles.  As part of this effort he is preparing a
Background Information Document (BID) in support of EPA regulations that  will
be promulgated.  He also completed a study of heap leaching  of  gold ores  with
cyanide which focused on conceptual control practices.

During past projects Mr. Hoye developed and implemented sampling  plans, data
management systems, QA/QC plans including field sampling  protocols, following
EPA guidelines (SW-846).  He managed the installation of  groundwater  and
surface water monitoring stations and collection of periodic samples  at
several sites.  He is familiar with DOT regulations and EPA  guidelines per-
taining to shipping of environmental and hazardous waste  samples.

Mr. Hoye was Project Manager of a waste characterization  and industry overview
study of the nonferrous smelting and refining industry.  This  large volume
waste related study, conducted for EPA-OSW in response to RCRA, involved  site
investigations, sample collection, and waste characterization  at  24 facilities.
Mr. Hoye was Assistant Project Manager of a RCRA-mandated multi-mi 11 ion-
dollar multi-year study of solid waste and disposal technology  in the mining
industry.  During this project, Mr. Hoye conducted surveys of waste disposal
technologies, managed waste characterization sampling studies  at  over 65
sites and assessed environment impacts by conducting eight case studies  that
involved groundwater and surface water monitoring.  This  study  also included
evaluation of control technologies and the cost associated with these ancil-
lary /mi tigative practices.

Mr. Hoye managed hydro!ogical assessment of two waste disposal  impoundments
for the Bureau of Mines.  In addition, he has conducted assessments of municipal
waste collection and disposal systems in several midwestern  cities.  Mr.  Hoye
has experience in conducting limnological field studies including collection
of fish by electroshocking, nets, rotenone, and collection  of benthos and
sediment samples.

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    ' PEI Associates, inc.
                              BARBARA B. LOCKE
EDUCATION:
     M.S., Environmental Science, Indiana University, 1983
     B.A., Biology, Stephens College, 1980

RELEVANT EXPERIENCE:

Ms. Locked has over 4 years experience in sampling hazardous wastes and other
environmental media.  She sampled lake sediments on the Great Lakes to deter-
mine outfall compliance while employed with the EPA-Great Lakes National
Program Office.  As part of this effort she utilized an Ekman Dredge,  Ponar
Dredge, and Core Sediment sampling equipment in industrial harbor areas of
the Great Lakes.  She collected the samples, packaged them for shipment,
utilized EPA chain-of-custody procedures and wrote up trip reports containing
exact sample locations to be used in enforcement proceedings.  Furthermore,
Ms. Locke sampled stream sediments for possible radiation contamination
around a DOE facility in Wedon Springs, Missouri.  She selected the sample
locations, collected the samples, and wrote the subsequent report of results.
Ms. Locke also conducted a pre-strip mining environmental assessment in which
she collected water, soil, sediment, flora and fauna samples.  Additionally,
she performed stream transects, volumetric flow measurements, and collected
groundwater samples.  She has collected soil samples suspect of TCDD and PCB
contamination and she conducted several field investigations to check for
leaking underground petroleum storage tanks.  She is thoroughly familiar with
the use of personal protective equipment levels B, C, and D.

As a member of the cleanup crew on a $1.2 million emergency Superfund site in
Gary, Indiana, Ms. Locke developed and implemented a sampling and analysis
plan involving the cleanup of over 65,000 drums.  In this capacity, she was
responsible for the sampling (including compositing operations), record-
keeping, chain-of-custody, manifesting, transportation, and disposal of all
waste and waste samples.  Under the same EPA contract, Ms. Locke has served
as Response Manager and Site Engineer for several emergency cleanup operations.

As part of a State-initiated study, Ms. Locke recently completed an in-depth
analysis of deli sting hazardous wastes under the RCRA regulations.  She
evaluated the history of deli stings granted and the future potential (under
the 1984 Solid Waste Amendments) for delisting specific wastes.  Also under
this study, she evaluated proposed alternative treatment technologies for the
metal plating industry.  The evaluation included cost considerations, technical
feasibility, and market research.

Ms. Locke was been extensively involved with hazardous waste management under
RCRA and CERCLA for the last 3 years.  She was responsible for coordinating
and writing major portions of Part B applications for 6 multi-operating TSD
facilities,including incinerators, landfills, waste piles, surface impound-
ments, and container and tank storage.  Furthermore, she recently completed
an independent audit for one of the largest hazardous waste landfills in the

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    ' PEI Associates, Inc.
Barbara B. Locke (continued)

county.  As part of this effort, she completed on-site inspections and record
reviews of the operating procedures.  The result of this effort was a state
ordered regulatory compliance report (including compliance with the 1984
Solid Waste Amendments).  As a result of the 1984 Solid Waste Amendments,  Ms.
Locke recently revised and updated closure plans for partial  closure (scheduled
to begin immediately) of a commercial incineration facility.   The plans
included closure of 7 surface impoundments on outdoor container storage and
waste pile area, and above- and below-ground storage tanks.  She will continue
to meet with State and Federal EPA personnel throughout the planned closure
operations.

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     PEI Associates, Inc.
                               JUDY L. MCARDLE
EDUCATION:
     B.S.E., Environmental Engineering, Purdue University,  1983
     B.S., Natural Resources and Environmental Science,  Purdue University,
      1983

RELEVANT EXPERIENCE:

Ms. McArdle is an environmental engineer in PEI's  Waste  Management Division
with 3 years of experience in RCRA- and TSCA-related studies.  As  part  of the
EPA/OSW large-volume waste studies under Section 8002 of RCRA, Ms. McArdle
helped prepare an industry profile of the copper smelting/refining industry.
The profile provides data on the number, size, location, and operating  status
of smelters/refineries across the country as well  as information on the
volume, characteristics, and management of wastes  generated by the industry.
Data gathering efforts involved site visits, sample collection,  and contact
with trade associations and regulatory personnel.   The information is being
used by the EPA to develop regulatory strategies for wastes that are currently
excluded from regulation under Subtitle C of RCRA.

Ms. McArdle is familiar with the use of the Kemmerer water  sampler and  the
Ekman dredge through her involvement in water quality studies of the Wabash
River and numerous lakes and streams in the West Lafayette, Indiana, area.

In support of contemplated regulatory action under TSCA, Ms. McArdle investigated
occupational exposure to methyl chloride and chlorinated paraffins for
EPA/OTS.  These investigations involved  preparation of  industrial process
descriptions, estimation of release rates and exposure levels, and evaluation
of engineering controls.  She has also worked with EPA/ORD's Exposure Assessment
Group to gather information needed to assess occupational and public exposures
to dioxin-related compounds.  This effort entailed summarizing data on  the
physical, chemical, and biological properties of 15 of the  most  toxic congeners;
identifying sources of these compounds in the environment;  determining
release rates; and enumerating exposed populations.

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       PEI Associates, Inc.
                            MICHAEL M. AROZARENA
EDUCATION:
     M.S. Environmental Sciences, University of Cincinnati,  1979
     B.S., Natural Sciences, Xavier University, 1977

RELEVANT EXPERIENCE:

As an environmental scientist with PEI Associates, Mr.  Arozarena has  more
than 7 years of managerial and technical experience in  water/wastewater
monitoring, groundwater monitoring, ambient air monitoring and hazardous
waste management.  Currently, Mr. Arozarena is managing a field monitoring
project in Falls City, Texas, for EPA's Office of Radiation  Programs  (ORP)
involving a comparison of several existing measurement  methods for radon  in
soil gas.  Sampling methods, including Lucas cell alpha scintillation counting,
charcoal adsorption, and alpha track techniques, were compared in order to
determine their ability to characterize the potential of any site to  cause
elevated indoor radon concentrations.  In addition to the collection  of soil
gas samples, Mr. Arozarena collected soil samples to a  depth of 10 feet for
radium-226 analysis, soil moisture content, determination of radon emanating
power, and diffusion coefficients.

Mr. Arozarena has also participated in numerous groundwater  and surface water
monitoring studies for EPA and industrial clients.  He  managed a groundwater
monitoring study for a chemical manufacturing plant investigating the impact
of a superfund landfill, and he has participated in several  wastewater
monitoring projects in fulfillment of NPDES permit application requirements.
He monitored wastewater discharges from two steel facilities in central Ohio
and prepared their applications.  The most recent wastewater sampling project
involved the monitoring of numerous electroplating/metal finishing operations
for a major jet engine manufacturer in Cincinnati.  Sampling and analysis
supported a baseline monitoring report submitted in response to recently
developed pretreatment regulations.

Mr. Arozarena has also collected hundreds of soil samples for EPA and indus-
trial clients.  An intensive soil sampling study was conducted in Texas to
investigate lead and cadmium contamination of soil in the vicinity of secondary
lead smelters.  A large portion of the soil sampling studies for industrial
clients were concerned with the proper closure or decontamination of  surface
impoundments under RCRA.

Recently, Mr. Arozarena completed an air radiation monitoring study for ORP
in central  Florida.  Alpha track detectors, charcoal canisters, high-volume
samplers, and particle sizing samplers were installed at five wet-process
phosphoric acid plants operating phosphogypsum piles.  Data  was collected
over a period of one year and will be used to evaluate  the need for radionu-
clide emission standards for phosphogypsum piles.  Mr.  Arozarena has  worked
with ORP on several other projects.  One study involved the  completion of
site-specific information on all active and inactive phosphogypsum piles  in
the United States.  ORP used this information to determine exposure to

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       PEI Associates, Inc.
MICHAEL M. AROZARENA (continued)


radionuclides of residents in the vicinity of these piles.   He assisted in
the collection of groundwater, surface water and sediment samples at two
chemical manufacturing facilities in Missouri that managed phosphogypsum
piles.  Finally, he provided assistance on an ORP study of radon emissions
and control practices at active uranium mills and associated tailings piles.

He also served as field manager on several ambient air monitoring projects
involving the collection of monitoring data to satisfy prevention of signifi-
cant deterioration (*PSD) permit requirements.  These projects included the
monitoring of total suspended particulates, carbon monoxide, sulfur dioxide,
ozone, nitrogen dioxide, and meteorological parameters.  He was involved in
organizing an ozone monitoring study in the vicinity of Indianapolis, Indiana,
and monitoring oxides of nitrogen, reactive hydrocarbons, and meteorological
parameters in Jeffersonville, Indiana.  Other past ambient air monitoring
projects included field sampling of fugitive dust emissions from various coal
mining operations as part of the development of emission factors, and field
sampling of fugitive chrysotile asbestos emissions at a recreational area in
California.

Prior to coming to PEI  in 1979, he worked for over a year in drinking water
research at U.S.  EPA MERL in Cincinnati, Ohio.  He conducted bench- and
pilot-scale studies for the removal  of parasites from drinking water using
various water treatment processes including coagulation/flocculation/sedimenta-
tion, granular media filtration, and diatomaceous earth filtration.

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50377-IQ>	
 REPORT DOCUMENTATION
      PAGE
                   1. E"O*T HO.
                    560/5-87-012
                                                         1. ftacipxrirt Accvttion No
4. TMk and SutXrtl*
Chlorinated Paraffins:  A report  on the Findings
From  Two Field Studies, Sugar Creek,  Ohio and
Tinkers Creek, Ohio
                                                         i. port Ol
                                                          January 22, 1988
       Murray,Tom and Mary Frankenberry"
Steele, David H.  ; Heath,  Robert GC
                                                          B. rfamwnc OrBil1xi **pi. No.
t. Pvrltmlns Ogrfntratton Mam* and Addran
a)  Exposure Evaluation Division.  OTS
b)  Midwest Research Institute,  425  Volker Blvd.,
    Kansas City, Missouri 64110
c)  Battelle Columbus Division,  2030 M St. N.W.
    Washington. D.C.   20036	
                                                         10- Prvtvct/Tmli/Worli Unit No.
                                                         II.

                                                         c> EPA  68-02-4252

                                                         8> EPA  68-02-4243
It S0entanic Organization Name and AddrMS
    Environmental  Protection Agency
    Office of Toxic Substances
    Exposure Evaluation Division
    401  M St. S.W.,  Washington D.C.  20460
                                                         II. Tjrpa at Report & fHrtod Covered
                                                           Final  Report
                                                           1986 - 1987
                                                         14.
15. Supptemantary Netr*
Joseph J. Breen,  Project Officer  - MRI contract  68-02-4252

Cindy Stroup, Project Officer - Battelle contract  68-02-4243
It Ae*tract (Limit: KO
   This  report presents the results of two field  studies conducted in
   1986  by the Environmental Protection Agency's  Office of Toxic  Substances
   (EPA/OTS) under  the existing  chemicals program to screen selected
   waterbodies for  the presence  of  chlorinated paraffins.  Chlorinated
   paraffins are  saturated straight-chain hydrocarbons ranging  from 10 to
   30  carbons in  length and containing 20 to 70%  chlorine by weight.  The
   information gained from these field studies will  be coupled  with that
   from  other environmental hazard  and environmental exposure studies
   and collectively contribute to an EPA risk assessment for this chemical.

   The report also  develops an analytical method  for chlorinated  paraffins
   in  Different environmental matrices and includes  a rigorous  statistical
   analysis of the  data used to  validate the method.
7. Document AAaty>* - Paaerfeaf
   Chlorinated Paraffins, lubricating oils, survey design,
   HRGC/NCIMS/SIM analytic method,  statistical  assessment of
   method validation studies.
 B. S*wlftr/O*-Cnd Tanns

   Literature review
   Extraction
   Mass spectrometry

 c. COSATI FMd/Croup
                             Chromatography
                             Cleanup
                             Statistical  analysis
 Availability .

   Release Unlimited
                                             It. Caeurtty Ctau (Thit Mapert)
                                              Unclassified
SI. Me af **(
55 plus App.
                                             20. Security Cl>\ (Thit *ift)
                                               Unclassified
                                                                   22.
                                Sa* Initrvction* an fter
                                                                       FOKM 271 (4-77)
                                                                  (Formerly NTlS-35)
                                                                  Dp1rrnnl ol Commtrc*

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