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TRANSCRIPT
HERCULES/VERTAC OFF-SITE STUDYFINAL REPORT
Prepared For
HERCULES INCORPORATEDWILMINGTON. DELAWARE
PreparedBy:
rr CORPORATIONFIELD ANALYTICAL SERVICES
KNOXVILLE, TENNESSEE
MAY 1990
HERCULES/VERTAC OFF-SITE STUDY
FINAL REPORT
(FOR TOTAL TCDD AND 2A7.8-TCDD)
JACKSONVILLE, ARKANSAS
IT ANALYTICAL SERVICES APPROVALS:
Name: Dana S. SimeriyTitle: Project Manager
Name: William A. Trippet nTitle: Program Director, Field Analytical Services
Signature: (l)^M^—/l- ' / ' A / ' "K-
CONTENTS
LIST OF TABLESLIST OF FIGURES
iiiv
1.0 INTRODUCTION 1-1
2.0 SAMPLING AND ANALYTICAL PROGRAM 2-12 . 1 Overall Sampling Program 2-12.2 Analytical Program 2-12.3 Common Practices 2-1
2 . 3 . 1 Field Chain-of-Custody and Related Documentation 2-22 . 3 . 2 Transfer of Custody to Analytical Laboratory 2-3
3.0 SOIL AND SEDIMENT STUDY 3-13 . 1 Sample Location Determination 3-13.2 Sample Collection, Handling, and Documentation 3-2
Procedures3 . 2 . 1 Soil Sampling 3-23.2.2 Sediment Sampling 3-23.2.3 Sample Handling 3-33.2.4 Sample Documentation 3-33-2.5 Field Split Sample Collection 3-3
3.3 Sampling Analysis/Archive Strategy 3-43.4 Analytical Results 3-4
3 . 4 . 1 2,3,7,8-TCDD Results 3-43.4.2 Total Dioxin Results 3-53.4.3 Partial Priority Pollutant List Results 3-53.4.4 Field Split Sample Results 3-6
3.5 Statistical Analysis of Dioxin in Soil/Sediments 3-6Over Time
4.0 WOOD DUCK STUDY 4-14 . 1 Sample Location Determination 4-14.2 Hood Duck Sample Collection 4-1
4 . 2 . 1 Authorization for Collection 4-14.2.2 Collection Events 4-24.2.3 Collection Procedures 4-2
4.3 Sample Preparation and Analysis/Archive Strategy 4-34.4 Analytical Results of Hood Duck Study 4-4
5.0 AQUATIC BIOTA SURVEY 5-15 . 1 Sample Collection Locations 5-15.2 Sample Collection Procedures 5-15.3 Sample Preparation and Analysis/Archive Strategy 5-25.4 Analytical Results of Aquatic Biota Study 5-35.5 Statistical Analysis of Aquatic Biota Results 5-3
ANA2537CON05/15/90 F3
CONTENTS (Continued)
6 . 0 FIELD QUALITY CONTROL REPORT6 . 1 Sampling Quality Control Activities
6 . 1 . 1 Sample Handling6 . 1 . 2 Sampling Equipment6 . 1 . 3 Field Travel Blanks6 . 1 . 4 Equipment Rinsate Samples6 . 1 . 5 Glove Blanks6 . 1 . 6 Field Duplicates
6 . 2 Summary of Field Quality Control6 . 3 Corrective Actions
Page
6-16-16-16-16-16-26-26-26-36-3
7.0 DIOXIN ANALYSES QUALITY CONTROL REPORT 7-17 . 1 Analytical Quality Assurance Objectives 7-1
7 . 1 . 1 Accuracy 7-17 . 1 . 2 Precision 7-17 . 1 . 3 Completeness 7-17 . 1 . 4 Comparability 7-2
7.2 Calibration Procedures and Frequency 7-27 . 2 . 1 Instrument Performance 7-27.2.2 Calibration Procedures 7-2
7 . 2 . 2 . 1 Total Dioxins 7-27.2 . 2 . 2 Isomer-Specific TCDD 7-3
7.3 Analytical Procedures 7-37 . 3 . 1 Soil/Sediment Sample Preparation 7-47.3.2 Fish Sample Preparation 7-4
'' 7.3.3 Duck Sample Preparation 7-57.3.4 High Resolution Gas Chromatography/High 7-5
Resolution Mass Spectrometry7.4 Data Reduction, Validation, and Reporting 7-67.5 Laboratory Quality Control Samples and Results 7-7
7 . 5 . 1 Standards 7-77.5.2 Blanks 7-77. 5 . 3 Matrix Spike/Matrix Spike Duplicate Samples 7-77.5.4 Surrogate Spike Samples 7-87.5 . 5 Quality Control Sample Results 7-8
7 . 5 . 5 . 1 Method Blank Results Summary 7-87 . 5 . 5 . 2 Matrix Spike/Matrix Spike Duplicate 7-9
Results
8.0 PARTIAL PRIORITY POLLUTANT ANALYSES QUALITY CONTROL REPORT 8-1
APPENDICES
A. SAMPLE CUSTODY AND DOCUMENTATION FORMSB. SAMPLING METHOD DIAGRAMC. STATISTICAL SUPPORT DATAD. PROJECT DATABASE MANAGEMENTE. ANALYTICAL QUALITY CONTROL SUMMARIESF. PRIORITY POLLUTANT ANALYSES CASE NARRATIVE
ANA2537COM ii05/15/90 F3
TABLES
FollowsNumber
1 Soil and Sediment Sampling Locations 3-1
2 Analysis Strategy for Soils and Sediments 3-4
3 Comparison of 1987 2,3,7,8-TCDD Results for Vertac 3-4Off-Site Soil and Sediment Samples with SamplesCollected in 1984
4 Vertac Off-Site Total Dioxin Results for Soil and 3-5Sediment Samples Collected During 1987
5A Vertac Off-Site Sediment Field Information for Samples 3-5Analyzed for Partial Priority Pollutants
5B Vertac Off-Site Analyses for Partial Priority Pollutants 3-5
6 Vertac Off-Site 2,3,7,8-TCDD Results for Soil and 3-6Sediment Samples Split with EPA
7 Vertac Off-Site Wood Duck Dioxin Results for Samples 4-4Collected During July 1987
8 Dioxin Analysis of One Wood Duck Collected West of 4-4Highway 15, Near Anderson Aviation Vertac Off-SiteStudy Area, Jacksonville, Arkansas
9 Vertac Off-Site Wood Duck Dioxin Results for Samples 4-5Collected During January 1988
10 Fish Sampling Locations 5-1
11 Vertac Off-Site Dioxin Analyses Results of Fish Samples 5-3Collected During 1987
12 Field Quality Control Sample Summary 6-3
13 Vertac Off-Site Results for Soil and Sediment Quality 6-3Control Samples: Blanks, Rinses, and Background.Collected 1987
14 Vertac Off-Site Dioxin Results for Soil and Sediment 6-3Duplicate Samples Collected in 1987
15 Vertac Off-Site Dioxin Results of Fish Quality Control 6-3Samples Collected During 1987
16 Precision and Accuracy Objectives 7-1
17 Laboratory Quality Control Sample Summary 7-7
ANA2537CON iii05/15/90 F3
TABLES (Continued)
FollowsNumber-
18 Vertac Off-Site Dioxin Results for Soil and Sediment 7-9Matrix Spike (MS) and Spike Duplicates ( M S D ) , 1987
19 Vertac Off-Site Dioxin Results for Hood Duck Matrix 7-9Spike (MS) and Spike Duplicate (MSD) Samples Collectedin 1987 and 1988
20 Vertac Off-Site Dioxin Results of Fish Matrix Spike (MS) 7-9and Spike Duplicate (MSD) Samples Collected During 1987
21 Sample Summary Table . 8-2
ANA2537CON iv05/15/90 F3
FIGURES
FollowsNumber
1 Overview - Sampling Area 2-1
2 Soil/Sediment Sample Locations 3-1
3 Detail - Soil/Sediment Sample Locations (Oxidation 3-1Ponds, Aeration Basin, and Outfall Ditch)
4 Detail - Soil/Sediment Sample Locations (Rocky Branch, 3-1Redmond Road, and Hwy. 167)
5 Detail - Soil/Sediment Sample Locations (Bayou Meto, 3-1Hny. 1 6 7 , and Bayou Meto/Rocky Branch Confluence)
6 Detail - Soil/Sediment Sample Locations (Bayou Meto, 3-1Missouri Pacific RR Track, and Hwy. 1 6 1 )
7 Detail - Soil/Sediment Sample Locations (Hwy. 161 and 3-1Bayou Meto)
8 Detail - Soil/Sediment Sample Locations (Bayou Meto and 3-1Hwy. 391)
9 Wood Duck Sample Locations 4-1
10 "' Fish Sample Locations 5-1
ANA2537CON v05/15/90 F3
1 . 0 INTRODUCTION
Dioxin [specifically, 2,3,7,8-tetrachlorodibenzo-p-dioxin (2 , 3 , 7 , 8 - T C D D ) ]
contamination has been observed in the geographic area surrounding the Vertac
plant site near Jacksonville, Arkansas. This contamination is apparently the
result of routine operation of the Vertac plant, which is no longer in use.
Previous investigations of these "off-site" areas have detected dioxin in
wildlife and sediments at varying levels, primarily along the Bayou Meto andRocky Branch Creek. In June 1987 Hercules Incorporated commissioned IT
Corporation ( I T ) , a subsidiary of International Technology Corporation, toconduct a study to assess the currently existing levels of suspected dioxin
contamination in the Vertac off-site area. The findings of that study arepresented in this report.
Before initiation of the off-site assessment, reports of the previous
investigations by other organizations were carefully reviewed and an extensive
site walk of the entire area was undertaken. Samples collected as part of
this investigation were intended to represent current environmental conditions
of sample locations selected in the previous studies.
The objective of this investigation was to augment existing information with
current data in an effort to determine if a trend toward degradation and/ordispersion of dioxin in soils, sediments, and biological tissues in the Vertac
off-site areas is developing. The analytical results from this program willbe compiled with existing information to help provide the necessary data for
ascertaining the presence or absence of dioxin, thus allowing an informedresponse to the overall situation.
To accomplish this objective, the project encompassed a complete, systematic
approach for sample collection, documentation, sample chain-of-custody, and
coordination of sample analysis with the analytical laboratory. The three
sample matrix types included in this study were soils/sediments, wood ducks(Aix sponsa), and various fish species. For comparison purposes, areas
previously sampled for soils/sediments were sampled again, though a greaternumber of samples were collected from some locations. As many biological
specimens as possible were collected from the approximate locations of
ANA25371 1-109/12/89 F2
previous studies. Those samples considered "duplicates" of previous samples
(based on location for soils/sediments and location, size, and species for
biological specimens) were analyzed for total dioxins (the total of ail
tetra-, penta-, hexa-, hepta-, and octa-chlorinated isomers) and isomer-
specific 2,3,7,8-TCDD. Other sampies collected and not limned lately analyzed
have been archived for possible analysis at a later time.
The specific sampling program and analytical results for samples of each
matrix type have been reported as independent sections in this document,
though an overview of the plan and common factors to all matrix types are
described in the section immediately following.
ANft25371 1-209/12/89 F2
2,0 SAMPLING AND ANALYTICAL PROGRAM
2 . 1 OVERALL SAMPLING PROGRAM
Selection of specific sampling locations was based on a directed rather than a
random approach. Documented locations of samples collected during previous
studies were reviewed and identified as closely as possible. The previous
locations of primary interest for this program were those where dioxin was
detected at levels close to or greater than 1 part per billion ( p p b ) in thecase of soils/sediments, and greater than or equal to 25 parts per trillion
(ppt) in the case of wildlife samples. An overview of the entire targetedsampling area is provided in Figure 1 .
2.2 ANALYTICAL PROGRAM
Each sample designated for analysis was analyzed for total polychlorinateddioxins (Cl^-Clg) and 2,3,7,8-TCDD at the IT Analytical Services (ITAS)
Special Analysis Laboratory (SAL) in Knoxviile, Tennessee, except samplessplit with the U . S . Environmental Protection Agency (EPA) (see Sections 3.2.5
and 3 . 4 . 4 ) . All samples were analyzed using high resolution mass spectrometry
instrumentation to achieve the best possible detection limits. Brief
descriptions of the analysis procedures used for each matrix type may be found
in Section 7.3 of this document.
2 . 3 COMMON PRACTICES
Collection of all three sample matrix types involved common sample custody anddocumentation practices. These practices ensure the integrity of the sample
from collection to data reporting. Routine ITAS sample custody procedures aredesigned to satisfy legal requirements for evidence; samples processed as a
part of this program were handled as if each sample were to be directly
involved in litigation.
The sample custody procedures used for this program conform to the guidelines
of EPA's Test Methods for Evaluating Solid Waste (SW-846). The Sampling
Coordinator had overall responsibility for sample custody in the field.
ANA25372 2-109/12/89 F2
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2 . 3 . 1 Field Chain-of-Custody and Related DocumentationBefore collecting samples in the field, the Sampling Coordinator issuednumbered sample tape to the field samplers. Each sample container (Jar orwrapped specimen) was labeled with a unique sample number as it was collected;complete sample documentation consisted of the following:
• A field collection log was completed as each sample was collected.This form contains field sample location descriptions and all otherpertinent sample information for documentation of each sample.Individual forms were used'for wildlife specimen samples andsoil/sediment samples. These forms are provided in Appendix A ,Figures 1 and 2.
• At least one photograph was taken showing the sample location,including the best available reference points.
• A chain-of-custody record ( C / C ) , also provided in Appendix A , Figure3, was initiated by the Sampling Coordinator for each group of tensamples or less to track the transfer of samples from collection inthe field to receipt at the laboratory. The original of the C/Crecord accompanied the samples at all times; a copy of each form wasmaintained in the field for the duration of the sampling effort.
• A request for analysis <R/A) form (Appendix A , Figure t) was alsoinitiated in the field for each group of samples shipped to thelaboratory. The original R/A form accompanied the samples to the
" laboratory, with a copy maintained in the field.
The completed field collection forms (Appendix A , Figures 1 and 2) weremaintained by the Sampling Coordinator in the field for the duration of thesampling effort. Upon demobilization, they were incorporated into the centralproject file in Knoxville, Tennessee and became an important part of thepermanent sample documentation record. At a minimum, the followinginformation was included on the appropriate form for each sample:
• Sample number, both on bottle (or wrapped specimen) and data sheet• Sample location ( i . e . , station, river mile, highway number, e t c . )• Sample description• Sample date and time• Depth sampled or measurements and weight of specimen
Pertinent observations/descriptions• Names of sampling personnel.
ANA25372 2-209/12/89 F2
As a final step, each sample location was clearly identified on a master planmap.
2 . 3 . 2 Transfer of Custody to Analytical LaboratorySamples under custody for transport to the analytical laboratory were
accompanied by all original and completed C/C records and R/A forms. Theserecords were used to cross check the accuracy and completeness of eachshipment, to note the condition of each sample when received, and to prescribethe analyses to be performed or the disposition of a sample into archive.Shipment records have been maintained on file, as they constitute an extensionof the chain-of-custody during commercial shipment.
Any inconsistencies or problems with a sample shipment were reported to theSampling Coordinator or designee for immediate resolution.
When any/all problems were solved, the official custody of the samples wasaccepted by the laboratory by signing the C/C record. Samples were thentracked through the laboratory by routine, laboratory-specific procedures.
ANA25372 2-309/12/89 F2
3.0 SOIL AMD SEDIMENT STUDY
Soil and sediment samples were collected from 49 separate locations, including
a background site, as identified in Table 1 . A total of 200 soil/sediment
samples (excluding quality control samples) were collected in the off-site
areas. All soil/sediment sample locations are indicated in Figure 2. Detailsof the location and results of individual samples are given in Figures 2
through 8.
3 . 1 SAMPLE LOCATION DETERMINATIONCharts, maps, and sample location descriptions from a Remedial Investigation/
Feasibility Study (RI/FS) of the Vertac off-site areas performed in 1984 and1985 were used as the basis for determining the soil/sediment sample locations.
The RI/FS program and results are reported in the Offsite Remedial Investiga-
tion, Final Report, Volumes I and I I . December 1 , 1985 and Vertac Offsite
Feasibility Study Final Report Volume I , June 1986, both prepared for EPA.
The reference sample numbers listed in Table 1 are those used in the RI/FS.
IT site maps were constructed by referencing U . S . Geological survey maps,
Arkansas state and local maps, flood insurance rate maps, and Martinez Mappingand Engineering maps prepared for the RI/FS reports. Sample locations were
also confirmed via verbal communication with a member of the FieldInvestigation Team (FIT) that conducted the previous sampling. Every effort
was made to verify each location and sampling point. Where physical
conditions had changed, attempts were made to select the most probable area of
sediment/soil deposition which would best represent the presence or absence of
contamination. When there were conflicts between the maps and the RI/FS
sample descriptions, conclusive decisions were made by the FIT representative.
Some sample descriptions used in the IT analytical tables and database werechanged from the RI/FS wording to be either more descriptive or shortened to
accommodate the existing database format. Some conditions necessitated the
change of a sample's characteristic, such as a previously collected soil
sample being collected as a sediment sample due to a higher water level than
the period of previous sampling. These changes were described fully on the
collection log form.
ANA25373 3-109/12/89 F2
Table 1 . Soil and Sediment Sampling Locations
Location NumberReferenceSample # Location Description
7
8
9
10
11
12
13
14
15
F006 Mouth of outfall ditch and Bayou Meto
F014 Approximately 500 yards east of Highway 167 bridgeand 100 feet east of the confluence of Bayou Meto aiits east-to-northeast branch
F046 Bayou Meto cross section 25 feet downstream frommouth of the STP outfall ditch, left bank, 150 feetfrom water's edge, surface 2 feet above water level
F047 Bayou Meto cross section 25 feet downstream frommouth of the outfall ditch, left bank, 12 feet fromwater's edge, surface 1 foot above water level
F059 Approximately 400 feet east of power lines on northbank Bayou Meto, 12 feet from water
FO&0 Approximately 400 feet east of power lines on northbank of Bayou Heto, 7 feet from water
F061 Approximately 400 feet east of power lines in BayouMeto on Worth bank, 1 foot above water surface
F063 Approximately 400 feet east of power lines on southbank of Bayou Meto, 1 foot above water level
F069 Approximately 300 yards east of Highway 167 bridgefrom Bayou Meto
F071 340 feet northwest of Highway 161 bridge in BayouMeto
F085 Approximately 750 feet south of Lake Dupree locatedin woodland
F104 Approximately 100 feet northwest of RB in abandonedstream channel; sample taken parallel with Sample MlF051
F105 Approximately 100 feet northwest of RB in abandonedstream bed
FS025 Just south of Bayou Meto, 1/2 mile from Highway 161
FS040 Dry creek bed bottom, approximately 500 feetsoutheast of railroad tracks
ANA2537A09/12/89 F2
Table 1 . (Continued)
ReferenceSample »Location Number Location Description
16
17
18
19
20
21
22
23
-24
25
26
27
28
29
30
31
N026 Near the West Lane dead end
N030 20 feet from west and east banks of RB, 120 feet or a220° azimuth from sampling point to manhole No. 10(9)3and No. 1010 Q
S002 Center of south oxidation pond in5009 North oxidation pond, southwest corner approximate] yM
50 feet from each bank
5010 South oxidation pond, 50 feet east of outfall ditct
3011 South oxidation pond along the southern edge(incorrect description)a
Center of north oxidation pond (correct descriptior)
5012 South oxidation pond along the southern edge
5013 Southeast corner of south oxidation pond
5014 North oxidation pond, southeast corner approximately50 feet from each bank
5018 Northeast corner of'aeration basin
5019 Middle of aeration basin
5020 Southwest corner of aeration basin
BACKGROUND Take Highway 167/67 north to AFB exit, west on AFBRoad approximately 1/4 mile, 50 feet off road and ;feet north of drain culvert
F010 Intersection of RB creek and Highway 167 sampledcenter, beside bridge on west side of highway.
F051 RB cross section; 200 yards south-southwest fromRedmond Road bridge near water's edge on north banh
F052 RB cross section; 200 yards south-southuest fromRedmond Road bridge in middle of stream bed.
ANA2537A09/12/89 F2
Table 1 . (Continued)
ReferenceSample fLocation Number Location Description
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
F057 RB cross section; approximately 600 feet south ofHighway 167 bridge in RB, midstream sediment layer:
F064 RB approximately 200 yards from Highway 167 bridge CT»and 100 feet downstream from pipe crossing RB, middleof stream bed.
F065 RB depth sample; 8 feet from south bank on sand barapproximately 30 feet southwest of small stream '•''entrance leading to sewage treatment plant. C
F067 1400 feet at 278° from south end of Dupree Park.
F013 50 feet northwest of Bayou Meto bridge at Highway167.
F017 50 feet northwest of MPRR bridge in Bayou Mefco.
F018 Approximately 40 feet northwest of Highway 161 bridgein Bayou Meto.
F068 On Bayou Meto, southeast of Highway 167,approximately 3 feet from water (no sand barspresent).
F070 1400 feet south of Lake Dupree in Bayou Meto.
F076 Approximately 1100 feet north of Intersectingrailroad tracks and dirt road.
F078 Approximately 800 feet southeast of MPRR bridge inBayou Meto.
F077 Approximately 800 feet due west of MPRR in BayouMeto.
F102 Approximately 1 mile north of northwest corner ofShuffield Lake.
F016 Approximately 905 feet south of Lake Dupree locatedin woodland 50 feet west of Bayou Meto.
FS044 No description, see map 7-1.
ANA2537A09/12/89 F2
Table 1 . (Continued)
ReferenceLocation Mumber_____Sample #____________Location Description
47 Bayou Meto at Interstate 40.
48 Bayou meto at Highway 79.
49 FS056 No description.
^The location description in the RI/FS report was found to be incorrect basedon location maps and confirmation by the FIT representative. The IT samplewas collected at the location described in the correct description. Theoriginal description remains in this table and subsequent tables in relationto sample number SOU for comparability with the previous reports.
ANA2537A09/12/89 F2
0 2 5 7 1 1
0 2 5 7 1 2
0 2 5 7 1 3
0 2 5 7 1 4
0 2 5 7 1 5
0 2 5 7 1 6
0 2 5 7 1 7
3 . 2 SAMPLE COLLECTION, HANDLING, AND DOCUMEMTATIOM PROCEDURESSamples were collected according to the guidelines described in EPA SW-846,
Test Method for Evaluating Solid Waste, where applicable.
In ail cases, all necessary and appropriate steps were taken to ensure thateach sample was representative of the location from which it was taken, free
from cross contamination, and fully documented with respect to location, its
condition, appearance, and nature at the time of its collection.
3 . 2 . 1 Soil Sampling
Soil samples were collected using a 2-inch diameter bucket auger. At each
location, four separate samples were collected in 3-inch depth increments.
The auger and sample handling tools were cleaned between each 3-inch incrementto avoid cross contamination. A new clean pair of latex or vinyl gloves was
donned for handling each sample.
The sample was removed from the auger with a clean stainless steel spatula andplaced on an aluminum pan. The soil was homogenized and placed into a
-precleaned sample jar equipped with a teflon lined lid.
3 . 2 . 2 Sediment SamplingSediment samples were collected using a U . S . BMH-53 piston-type bed material
hand sampler with a 2-inch by 14-inch-long stainless steel sample barrel (seeAppendix B , Figure 1 ) . While being held in a fully vertical position, the
sampler was firmly pressed into the stream bed material to the desired depth( 1 2 inches or refusal) to collect four 3-inch increment samples of the
"surface" sediment and the "bottom" sediment. The piston retracted from theforce of the bed material and airtight seal prevented the sediment from
falling out of the sample barrel as the sampler was removed. The sample was
then extracted in the specific increments into wide-mouth, pre-cleaned, sample
jars equipped with Teflon"-lined lids. The sediment sampler was cleanedbetween each sample to avoid cross contamination, and a new pair of gloves was
donned before handling each sample.
ANA25373 3-209/12/89 F2
3.2.3 Sample HandlingBefore shipment or release of the samples by the sample team, each samplecontainer was sealed with custody tape for resistance bo tampering during
shipment. Ice chests were used to ship samples under cooled conditions andwere also sealed with custody tape.
3.2.4 Sample Documentation
A sample label with the sample number written in Indelible ink or a pre-nunbered label tape number was attached to each sample jar and Jar cap. Each
3-inch sample increment from the same location was identified with the sameprimary number ( e . g . , WH1240) with an added letter indicating the depth
increment ( e . g . , A , B , C , e t c . ) . C/C, R/A, and sample collection log forms
were completed as described earlier in Section 2 . 3 .
3.2.5 Field Split Sample Collection
As requested by the U . S . Department of Justice, split soil and sedimentsamples were collected at a target frequency of 5 percent of the total number
of samples collected for this matrix type. The choice of which samples to be
split was determined by a FIT representative from the EPA Off-site Remedial
Investigation conducted in 1984. Ecology and Environment Incorporated ( E & E ) ,
selected by EPA, served as the FIT organization.
After selection by the FIT representative, the appropriate sample was
collected as usual, homogenized and then divided into two equal portions, putinto two identical Jars, and sealed with Teflon-lined caps. One sample of the
split sample pair was assigned a normal IT sample number and submitted foranalysis of total dioxins and isomer-specific 2,3,7,8-TCDD at the ITAS SAL in
Knoxville, Tennessee. The second sample of the split sample pair was assigned
the same IT sample number (an " S " suffix was added later in the IT
database). The custody of this sample was then transferred to the FITrepresentative who was responsible for its submifctal for analysis at a second
analytical laboratory designated by EPA and approved for Contract Laboratory
Program (CLP) analysis for dioxin. The laboratory contracted by E&E was
requested to perform isomer-specific (2,3,7,8-TCDD) dioxin analysis only.
ANA25373 3-309/12/89 ?2
3.3 SAMPLIHG ANALYSIS7ARCHIVE STRATEGY
Sample cores collected at each location contained multiple samples subdividedby depth. The samples selected for immediate dioxin analysis, as shown in
Table 2 , represent those depths that most closely match the samples analyzed
from these locations during the previous studies showing concentrations of
around 1 ppb or greater of 2,3,7,8-TCDD. In addition, the 0- to 3-inch
increment (notated subsample A ) was always selected for analysis. The
remaining core sections were held in archive status in the laboratory.
As requested by Hercules Incorporated, sediment samples collected from thenorth and south oxidation ponds and those collected from the aeration basin
were analyzed for a partial list of priority pollutant compounds. The
analytical methods used are described in Section 8.0.
3.4 AMALYTICAL RESULTS
The results of the dioxin analyses of the soil and sediment samples and theresults of the selected samples analyzed for a partial list of priority
pollutant compounds are presented in this section. Complete EPA CLP datapackages have been prepared; the original data packages are on file at
Hercui-es Incorporated, and another complete copy is maintained at the IT-
Knoxvllle office.
3 . 4 . 1 2.3.7.8-TCDD Results
A total of 81 soil and sediment samples were analyzed for isomer-specific2,3,7,8-TCDD. In Table 3 the results of these 1987 analyses have been
compared with analytical results of the soil/sediment samples collected in the1984 study. The abbreviations used in the table are defined as follows:
SE = SedimentSO == SoilQ = Qualifierppb = parts per billion = ug/kg.
Qualifiers
J = Compound detected but below the contract-required detectionlimit. The value given is an estimate.
U = Compound analyzed for but not detected. The value given isthe detection limit.
ANA25373 3-409/12/89 F2
T
Location NumberFigure 2
1
2
3
4
5
6
7
8
9
10
11
-12 '
13
14
15
16
17
18
19
20
21
22
23
24
ANA2537B09/12/89 F2
r^
able 2. Analy
Matrix'1
Type
SE
SO
SO/SE1'
SO/SE1'
SO
SO
SO
so
SO/SE5
SE
SO
so
soso
so
so
so
SE
SE
SE
SE
SE
SE
SE
sis Strategy for
Reference SampiIT Sample M
F006/WH1247A
F014/WH1241A
F046/WH1246A
F047/WH1245A,
F059/WH1228A,
F060/WH1229ft,
F061/WH1230A,
F063/WH1235A,
F069/WH1240A,
F071WH1242A,
F085/WH1226A,
F104/WH1237A
F105/WH1236A,
FS025/WH1232A
FS040/WH1234A
N026/WH1224A,
N030/HH1225A,
S002/WH1248A,
S009/WH1258A,
S010/WH1254A,
S011/WH1259A,
S012/WH1253A,
S013/WH1252A,
S014/WH1260A,
/•
Soils anc
e No./0.
B, C
C
B
B
B, C
D
D
C
C
, C
C
C
C
D
D
D
G
J
F
•
Sedime
Sam
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
0-3
nts
pie
i-n
in
in
in,
in,
in,
in,
in,
in,
in,
in,
in
in,
in,
in
in,
in,
in,
in,
in,
in,
in,
in,
in,
Increments ftnalyz
3-6 in, 6-9 in
6-9 in
3-6 in
3-6 in
3-6 in, 6-9 in
9-12 in
9-12 in
6-9 in
6-9 in
6-9 in
6-9 in
6-9 in
6-9 in
9-12 in
9-12 in
9-12 in
18-21 in
27-30 in
15-18 in
id
^—
0-Jr~-^-i(M0
Location NumberFigure 2
25
26
27
28
29
30
31
32
33
34
35
-36 -
37
38
39
40
41
42
43
44
45
46
47
48
ANA2537B09/12/89 F2
/-^
Matrix3
Type
SE
SE
SE
SO
SE
SO
SO/SE1'
SE
SE
SO
SE
SE
SE
SE
SO
SE
SE
SE
SE
SE
SO/SE"
SO
SE
SE
-S
Table 2. (Continued)
Reference Sample No./IT Sample Ho.
S018/WH1267A, E, F
S019/WH1269A, G
S020/WH1264A, E
WH1222A, B, C, D
F010/WH1283A
F051/WH1279A
F052/WH1280A
F057/WH1287A
F064/WH1282A
F065/WH1281A
F067/WH1285A
F013/WH1308A
F017/WH1300A
F018/WH1298A
F068/WH1309A
F070/WH1305A
F076/WH1313A
F078/WH1299A
F077/WH1304A
F102/WH1292A
F016/WH1312A
FS044/WH1296A
I40/WH1291A
HWY79/WH1290A
Sample
0-3 in,
0-3 in,
0-3 in,
Background composite
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
0-3 in
ncrements
12-15 in,
18-21 in
12-16.5 in
Analyz
15-18
'd
In
<M(Mr~LFI
C\J0
Table 2. (Continued)
Location Number ^fatrixa Reference Sample No./Figure 2___________Type________IT Sample No._______Sample Increments Analyz
49 SO FS056/WH1301A 0-3 in
Matrix types: SO = soil; SE = sediment. *Reference sample was soil; IT sample was taken at same location; there was a sedimentto change in conditions.
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TBBLE 5[lOTmlSBM OF 1(17 ;,1,7,1 TCDD HESIIITS FIB VWtIl CFtSITE SOIL MD SEDIhEHT SWIES IITH SfltlflES COELECTEI IH 1984
PIOJECT 4i00)l> 1
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SE
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SESE
DIOXIH371 ItOl | BN1IS
( 8 ppb
1.) ppb7,iB ppb
.022 ppb.57 « ppb
.Wf ppb
.2 ppb
1.; ppbi ppb
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. 1 « ppb
.41 ppb1 . » 1 « ppb
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l.i ppb).< ppb
.01 11 ppb
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1 1 DobI.I PIIU
l.i ppb
DRTE SMPLE
ll-SEP-17
11-SEP-t;11-Blll-M
17-SEM715-lttt-M
17-SiP-87
15-HUE-84
19-SEP-17ll-MC-14
19-SEP-17
ll-IIUC-14
19-SEP-1711-11111-14
19-SEP-17
K-fllG-14
2D-SEP-17li-MG-14
;0-SEf-«7
li-IIDC-U
19-SEM7li-IIU-B4
19-SEP-B?
K-llllt-14
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lEPIHg OF HKE
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SOTTtPE
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21-SEP-1721-SEP-17
ll-SEP-17
14-BCT-17u-mt-u
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SE [ORKEI OF S OlIBIITIOH FIKD
2.2 HD«I« gXIOftllOH POHD, KOtIHEBSI UWH IIPPRDX 50ft («OH (MH Wm» OXIMTIOK POM) SE CBtNEIi APPRDX. SO' FRDH ERCH BMK.
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10.7 H1BBLE IF »(8«T10» USIMIIIDDLE OF «EHTln« RASItt.
10.7 HieDLE OF IERITION MSIH
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0 M/MMENBEII M WK 1/4(1 1 OF J «IHD[«.S OF [UEIERIS IT flFB e«W1
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Any differences between the 1984 and 1987 sample descriptions are due to
changes in wording only; the actual sampling locations were reproduced as
closely as possible (see Section 3 . 1 ) . A statistical analysis of the change
in dioxin concentration in the Vertac off-site soils and sediments over timeis presented in Section 3 . 5 .
3.4.2 Total Dioxin Results
The 81 soil/sediment samples analyzed for 2,3i7,8-TCDD were also analyzed fortotal dioxins (Cly-Clg). Table 4 presents the results of these analyses. The
abbreviations defined above also apply to Table 4.
3 . 4 . 3 Partial Priority Pollutant List Results
Twenty-one sediment samples collected from the north and south oxidation ponds
and the aeration basin (see Figure 3) were analyzed for selected compoundsfrom the priority pollutant compound list. These compounds, along with their
abbreviations, are as follows:
• Toluene (CAS No. 108-88-3)• 2-chiorophenol (CAS No. 95-57-8), 2CLPHENO• 4-chlorophenol (CAS No. 106-48-9), 4CLPHENO• 2,4-dichlorophenol (CAS No. 120-83-2), 24CLPHEN• 2,6-dichlorophenol (CAS No. 87-65-0), 26CLPHEN• 2,3,6-trichlorophenol (CAS Mo. 933-75-5), 236CLPHE• 2,4,5-trichlorophenoi (CAS No. 95-95-4), 245CLPHE• 2,4,6-trichlorophenol (CAS No. 88-06-2), 246CLPHE• 2,4-D [(2,4-dichlorophenoxy) acetic acid] (CAS No. 94-75-7), 24D• 2,4,5-T [2,4,5-trichlorophenoxy) acetic acid] (CAS No. 93-76-5), 245T• Silvex (2-(2,4,5-trichlorophenoxy) propionic acid] (CAS No. 93-72-1),
245TP.
The results of the partial priority pollutant analyses are presented in Tables
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WA = Water
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3 . 4 . 4 Field Split Sample Results
Forty-eight soil and sediment samples were selected to be split in thefield. Table 6 presents the isomer-specific (2,3,7,8-TCDD) dioxin results forall the split samples and the corresponding original samples (when data areavailable). In addition to the abbreviations defined earlier in Section 3 . 4 . 1 ,the following apply to Table 6 :
E&E Data Qualifier
X = Sample spiked with standard compound to determine recovery ofanalyte from sample matrix; the original sample was not analyzed(this result should not be used for split comparison).
In the table, those samples designated with a suffix "S" appended to the ITfield sample number are the samples transferred to the FIT representative andanalyzed by a subcontracted laboratory. Those samples without the " S " wereanalyzed by the IT SAL.
Mot all samples selected to be split were part of the IT analytical plan foranalysis (see Section 3.3 and Table 2 ) ; therefore, for some of the splitsamples, the IT original sample is not listed. These samples are currentlystored in archive status.
3.5 STATISTICAL ANALYSIS OF DIOXIM IM SOIL/SEDIMEMTS OVER TIME
To assess the possible degradation or dispersion of 2,3,7,8-TCDD (TCDD) in theVertac off-site soils and sediments, a statistical analysis of all availablesoil and sediment data was conducted. Soil and sediment data are availablefrom two sampling events - one in August 1984 and the other in September andOctober of 1987. As previously described, the 1987 samples were collected inclose proximity to the locations of those collected in 1984. Appendix Ccontains the actual statistical test results.
ANA25373 3-609/12/89 F2
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»[RT«[ OFFSIIE ;,},7,t TIBC 1ESOLTS FOII Sill MD, SEDIHEIIT SWIiS SfllT KITH EPBriOJECT 41DO;g
MEKSDWILIE, MKmSttS
WIE Smr IIOKIII DEFTK IKTtll LBCIUBm/MUKEII TTPE 2)71 KDD ( UIIITS t»T[ SBWIEt If HCE DEPTH LOUTIOH OESMtPHM I, LOCtIIW tESCBIFTlBH |[OHI ] REFERENCEI
'i record stiected.
The statistical analysis of soil and sediment data involved a comparison of1987 TCDD concentrations to 1984 TCDD concentrations via the Wilcoxin SignedRank Test (Hollander, M. and Wolfe, D. A . , Nonparametric Statistical Methods,John Wiley and Sons, Inc., New York, 1973). In this application, the WilcoxinSigned Rank Test tests that the null hypothesis that the median change in TCDDconcentration from 1984 to 1987 is greater than or equal to zero ( i . e . , TCDDconcentrations increased over time), against the alternate hypothesis that themedian change in TCDD concentration from 1984 to 1987 is less than zero ( i . e . ,TCDD concentrations decreased over time). Generally speaking, if the nullhypothesis is rejected, it is reasonable for one to believe that the 1987 soiland sediment TCDD concentrations are significantly less than the 1984 soil andsediment TCDD concentrations.
Differences were calculated between the 1984 and 1987 soil and sediment TCDDconcentrations (see Appendix C, Table 1 ) . The Hilcoxin Signed Rank Test wasapplied to the differences. The result of the Wilcoxin test was that the nullhypothesis is rejected at the a= 0.05 level of significance. The 0.05 levelof significance implies that the probability of concluding that the TCDDconcentration decreased in 1987, when in fact if increased, is 0.05. Becausethe null hypothesis is rejected, it is reasonable for one to conclude the 1987TCDD concentrations are significantly less than the 1984 TCDD concentrations.
A point estimate of the magnitude of the difference between 1987 and 1984 TCDDconcentrations is -0.40 ppb. This implies that a TCDD concentration taken in1987 at a given location is, on the average, 0.40 ppb less than the TCDDconcentration observed in the same location in 1984. A 95 percent confidenceinterval for the magnitude of the difference is (-0.745, -0.205) ppb. Thisimplies the true, but unknown, median difference between TCDD concentrationsobserved in 1987 and 1984 is highly likely to be contained in the interval
(-0.745, -0.205) ppb. It is not unreasonable to believe the median decreasein TCDD concentration from 1984 to 1987 is as great as 0.74 ppb or as littleas 0.20 ppb.
ANA25373 3-709/12/89 F2
4.0 WOOD DUCK STUDY
To determine the current levels of suspected dioxin contamination in wildlifeliving in the Vertac off-site areas, 23 resident wood ducks (Aix sponsa) werecollected from several locations along the Bayou Meto and White River Wildlife
Refuge. Analysis for total dioxins and 2,3,7,8-TCDD uas performed on 18 woodducks.
4 . 1 SAMPLE LOCATION DETERMINATIONFor comparison purposes, locations for duck specimen collections were selectedbased on sample locations described in the Arkansas Game and Fish Commission,Wildlife Management Division's Project Completion Report, titled: Polychlorin-ated Dibenzodioxins and Dibenzofurans in Resident Wood Ducks (Aix sponsa) FromBayou Meto and White River national Wildlife Refuge. October 3, 1986, preparedby G. A . Perkins and S. C. Yaich. G. A . Perkins was consulted and maps weremarked to confirm the collection areas described in the report. The threelocations, identified as "Highway 1 5 " , "Slick MeCollum's reservoir nearHighway 1 6 5 " , and "White River National Wildlife Refuge" in the above statedreport, are indicated, along with each sample number and analytical resultfrom this study, in Figure 9 . The White River National Wildlife Refugelocation was selected as the background sample collection point.
The IT report changed some location descriptions from those in the previousstudy to depict the terminology or landmarks from the reference maps used. Inselecting each actual sample location, nesting and roosting sites at or verynear the Bayou Meto waterway were sought, so as to collect specimens whichwould be valid representatives for this comparative study. Adult females andimmature ducks were considered the most desirable specimens because ducks inthese categories typically spend the most consistent tiae in the same area.
4.2 WOOD DUCK SAMPLE COLLECTION
4 . 2 . 1 Authorization for CollectionBefore any biological sample collections, local, state, and federalauthorities were consulted and arrangements made to obtain the necessarypermits. Wood duck sampling required scientific collection permits from the
ANA25374 4-109/12/89 F2
0 2 5 7 4 5
U . S . Department of Interior, Fish and Wildlife Service and the Arkansas State
Game and Fish Commission and a special use permit from the U . S . Department ofInterior at the White River National Wildlife Refuge. An Arkansas small game
hunting license with an Arkansas Game and Fish Commission waterfowl hunting
and conservation stamp and a U . S . Department of Interior migratory bird
hunting and conservation stamp were also obtained before any collection
activities. State and federal wildlife officers were contacted and given an
overview of the activities and areas designated for collection. On someoccasions, either due to accessibility or convenience, private hunting clubs
were utilized after requesting permission from the owners or propertymanagers.
4. 2 . 2 Collection Events
Two wood duck collection events were completed - one in 1987 and one in early1988 - in the same general areas of the Bayou Meto ranging from Jacksonville
to Stuttgart, Arkansas and southeast to the White River National Wildlife
Refuge. The 1987 collection began July 6 and was completed on July 1 6 , 1987
with a total of nine ducks collected. The original sampling plan hadprojected that sample collection would commence on or about mid-June; however,
due to-unforeseen difficulties and the time necessary to obtain scientificcollection permits, the trip was delayed. As a result, most of the immature
wood ducks were flighted and had greatly expanded their apparent daytimefeeding area. Considerable effort was expended to locate and collect these
ducks at dusk and dawn periods at the precise locations identified in previouscollection reports.
4 . 2 . 3 Collection Procedures
All wood ducks were collected by routine stalking methods typically used insport hunting. The ducks were shot with twelve-gauge shotguns with No. 4
steel shot. The specimens were immediately placed in a cooler with wet or dry
ice and the time and location were recorded on a specimen collection sheet.
Immediately upon arrival at the established base location, the ducks were
marked by attaching metal tags and scribed sample numbers to each leg with a
self-locking nylon strap. The duck's weight and size were recorded on the
specimen collection sheets. The samples were put into "zip-loc" bags, placed
in coolers, and covered with dry ice pellets for overnight shipment to the
ANA25374 4-209/12/89 F2
laboratory. C/C and R/A forms were completed and the originals shipped alongwith the samples.
4.3 SAMPLE PREPARftTIOH AND AMflLYSIS/ARCHIVE STRATEGYUpon receipt of the samples at the laboratory, the identification on the C/Cform was confirmed with that on each specimen submitted and the condition uponreceipt noted. The R/A form was checked to see which samples were to beprepared for analysis. Laboratory personnel were instructed to cut the still-frozen ducks sagittally and to assign each bilateral portion a unique samplenumber. For example, WH1010R and WH1011L are the sample numbers of the rightand left portion of the same duck. The half duck sample was regarded as awhole duck analysis since each half contained all the body parts in the sameproportion as in a whole duck.
A sample selected for analysis was processed through a decontaminated meatgrinder until uniformly homogenized (including the bill and foot). A 25-gramaliquot was removed and analyzed for total dioxins and 2,3,7,8-TCDD. Theremaining homogenized portion and the intact half was stored frozen in archivestatus for future analysis as necessary.
The initial analysis strategy was for one of the two half samples of each duckselected as a comparison sample (based on its collection location, age, andsize relative to the samples collected in the previous study) to behomogenized and analyzed. If, upon examination of the results, a sampleshowed significant levels of dioxin, the retained half of the duck was to behomogenized, cooked, and analyzed to assay any changes that might occur indioxin concentrations during the cooking process. The cooking procedureconsisted of wrapping a homogenized portion in aluminum foil which had beenpierced to allow any exudate to be collected away from the sample. The samplewas then placed in a small convection oven, preheated at 350°F, and cooked for
1 hour.
ANA25374 4-309/12/89 F2
4.4 ANALYTICAL RESULTS OF HOOD DUCK STUDY
The results of the dioxin analyses (2,3,7,8-TCDD and total dioxins) of the
first nine wood ducks collected in July 1987 are presented in Table 7. The
abbreviations used in the table are defined as follows:
WD == Wood duckQ = QualifierU = Compound analyzed for but not detected; value given in the
detection limitppb = Parts per billion = vg/kg.
fts apparent in the table, only one sample showed significant levels of
dioxin. This wood duck had been collected as it was approaching a beaver dam
pond west of Highway 15 near Anderson Aviation on July 15, 1987, at dusk. Theright half of this specimen, identified as sample number WH1016R, had a
reported level of .300 ppb of 2,3,7,8-TCDD. Therefore, its opposite half,sample number WH1017L, was selected to be analyzed after undergoing the
cooking procedure (Section 4 . 3 ) .
During the cooking procedure, the laboratory manager observed that
approximately 2 milliliters of what appeared to be lipid drippings were exuded
from the sample. The results of analysis after cooking showed no 2,3,7,8-TCDDat a detection limit of .0018 ppb. Due to the unlikelihood that such a
significant reduction would occur after cooking, a decision was made to
reanalyze, in duplicate, aliquots of both the uncooked half (sample numbers:
WH1016RR1 and WH1016RR2) and the cooked half (sample numbers: HH1017LC1 andWH1017LC2) for 2,3,7,8-TCDD. The results were all positive but low, not more
than .0048 ppb 2,3,7,8-TCDD in either duplicate of the uncooked or cookedportions (see Table 8 ) .
It was also noted fron the results of the first nine wood duck analyses that
the ducks collected from the background location, the White River National
Wildlife Refuge, showed positive concentrations of 2,3,7,8-TCDD ranging from
1 ppt to 9 Ppt.
AMA25374 4-409/12/89 F2
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I IIIICK DIOXIN BESIIITS FOR SMPLES COLLECTED OUIIHC JUL( 1917PMJECT 41101)0 I
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Table 8. Dioxin Analysis of One Wood Duck Collected West ofHighway 15, Near Anderson Aviation Vertac Off-Site Study ftrea
Jacksonville, Arkansas
Sample Number Date Collected 2,3,7.8-TCDD
WH1016R
WH1016RR1
WH1016RR2
WH1017L
WH1017LC1
HH1017LC2
July 15, 1987
July 15, 1987
July 15, 1987
July 15, 1937
July 15, 1987
July 15, 1987
.300
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Uncooked
Uncooked
Uncooked
Cooked
Cooked
Cooked
ANA2537H05/15/90 F3
Due to the original results of sample WH1016R and the positive concentrationsin the background samples, an additional wood duck collection event wasconducted in January 1988 along the Bayou Meto west of High 15, near AndersonAviation and in the White River Wildlife Refuge. Also, two sediment grabsamples were collected in the White River Wildlife Refuge in an attempt tolocate the source of 2,3,7,8-TCDD in the ducks collected there.
Nine wood ducks were collected and analyzed for dioxin. Table 9 presents theresults of dioxin analyses performed on the January 1988 samples. All showeither none detected or no more than 10 ppt 2,3,7,8-TCDD. One of the sedimentgrab samples (WH135D collected in the White River Wildlife Refuge wasanalyzed for 2,3,7,8-TCDD; the result was none detected at a detection limitof 0.0034 ppb.
ANA25374 4-509/12/89 "2
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.5.0 AQUATIC BIOTA SURVEY
An investigation into the levels of total dioxins and 2,3,7,8-TCDD in fish
from Lake Dupree and Bayou Meto was conducted as part of this three-pronged
project. The objectives of this investigation were to:
• Document current levels of total dioxin and isomer-specific 2,3,7,8-TCDD in fish from Lake Dupree and Bayou Meto.
• Provide data for comparison with data collected during a previousaquatic biota survey of the same area.
• Provide data on total dioxin and 2,3,7,8-TCDD levels in edibleportions of fish to help assess potential endangerment to humansthrough consumption of fish.
5.1 SAMPLE COLLECTIOH LOCflTIOMS
Sixty-four fish of varying species were collected from Lake Dupree on August 13,
1987. This location was selected to serve as the indicator for the extent of
apparent dioxin contamination in the immediate Jacksonville, Arkansas area.
In addition, eight sample locations were selected along the Bayou Meto
waterway. These locations stretch from the northernmost at the Cato bridge,
north^of Jacksonville, to the southernmost sample location at the Bayou Meto
Wildlife Management Area. These eight locations were selected based on
previously sampled locations described by CH?M Hill and reported in the
Offsite Remedial Investigation, Final Report. Volume II , December 1, 1985,
prepared for EPA. Background fish samples were collected from the LaGrue
Bayou Channel at Peckerwood Lake, which flows parallel to the Bayou Meto
several miles to the east, outside the expected contamination area. The ten
fish sampling locations are identified in order from northernmost to
southernmost in Table 10 and are located on the map in Figure 10 along with
individual sample numbers and results.
5.2 SAMPLE COLLECTION PROCEDURES
All scientific collection permits and fishing licenses were obtained before
sample collection. Fish collection methods included the use of gill nets, bag
nets, angling, and electroshocklng. The choice of method was dependent on
expediency and approval by the Arkansas Game and Fish Commission. Immediately
upon collection, each fish was identified, measured, and weighed. I dent ifi-
ANA25375 5-109/12/89 F1
Table 10. Fish Sampling Locations
Station Number Location Description
8
9
10
Bayou Meto at Cato bridge
Bayou Meto at Rocky Branch confluence
Lake Dupree
Bayou Meto at Highway 391
Bayou Meto at Highway 15
Bayou Meto at Highway 31
Bayou Meto at lower confluence with big ditch,just above Highway 79
Bayou Meto at Highway 152 bridge
Bayou Meto at wildlife refuge
Peckerwood Lake at LaGrue Bayou Channel
ANA2537J09/13/89 F2
0 2 5 7 5 3
cation was made using .The Audubon Society Fish Guide to Morth American Fishes,
Whales, and Dolphins, November, 1983 and How to Know the Freshwater Fishes, by
Samuel Eddy, 1957. The fish were also classified according to feeding
behavior (i.e., bottom feeder versus predator versus plankton feeder).
Upon identification, a metal tag was scribed with a sample number and attached
to the specimen with a self-locking nylon tie. Each fish was then wrapped in
aluminum foil, the sample number was written on the outside with indelible
markers, and the specimen was placed in an insulated cooler with dry ice. The
samples were frozen and kept frozen until laboratory analysis. The specimen
collection log and C/C and R/A forms were completed and the appropriate
originals shipped with the sample via overnight delivery to the laboratory.
5.3 SAMPLE PREPARATION AMD ftMALYSIS/ARCHIVE STRATEGY
Upon receipt of the samples at the laboratory, the identification on the C/C
form was confirmed with that on each specimen submitted and the condition upon
receipt was noted. The R/A form was checked to see which samples were to be
prepared for analysis. The R/A form included a suffix at the end of each
sample number designating the portion of fish to be analyzed, as follows:
• WF = whole fish« WFMF = whole fish minus filets• RFMS = right filet minus skin• LFHS = left filet with skin« FMS = filets minus skin• FWS = filets with skin• COMP = composite of smaller fish• C = sample was cooked before being analyzed.
A filet was considered to be the "edible" portion removed from one side and
ideally did not contain any part of the visceral tissue. A filet "with skin"
included the intact scales when possible. A "whole fish minus filets"
required that both filets be removed; if only one filet was analyzed, the
remaining filet was identified by the original sample number and stored frozen
for future analysis, if necessary. One composite analysis was performed on
three small similar fish collected at the same location.
ANA25375 5-209/12/89 F1
A sample portion selected for analysis was processed through a decontaminatedmeat grinder to be uniformly homogenized. A 10-gram aliquot was removed andanalyzed for total dioxins (Cl^-Clg) and 2,3,7,8-TCDD. The remaininghomogenized portion was stored frozen for possible future analysis.
Two fish samples were selected for analysis following cooking. The cookingprocedure consisted of wrapping a homogenized portion in aluminum foil whichhad been pierced to allow any exudate to be collected away from the sample.The sample was then placed in a small convection oven preheated to 350°F andwas cooked for 1 hour.
Fish were selected for analysis by the Project Manager, based on theircomparability with the specimens collected in the previous studies accordingto their size, weight, species, feeding habit, and location of collection. Atotal of 219 fish were collected over a 9-day period; results have beenreported for 49 separate analyses of whole fish or prepared portions.
5.4 ANALYTICAL RESULTS OF AQUATIC BIOTA STUDY
Table 11 and Figure 10 present the results of total dioxins (Cly-CIo) and2,3,7-r8-TCDD analyses on the selected fish collected from the Vertac off-siteareas. The samples and results are ordered by collection locations from northto south along the Bayou Meto from Cato bridge to the Wildlife Refuge, withthe background samples collected at Peckerwood Lake listed last. The
following abbreviation definitions apply to the table (see Section 5.3 forsample number suffix definitions):
• Q s qualifier (analytical)• ppb = parts per billion ug/kg• U ; compound analyzed but not detected; value given is the
detection limit.
5.5 STATISTICAL AMALYSIS OF AQUATIC BIOTA RESULTSTo assess possible change in levels of 2,3,7,8-TCDD over time or over distancefrom the Vertac site, a statistical analysis of all available fish data wasconducted. Fish data are available from sampling events held in 1979, 1980,1981, 1984, and 1987. These data were collected from 14 locations. A listing
ANA25375 5-309/12/89 F1
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of the data is shown in Appendix C. The statistical analysis included a testfor trend over time at each of the 14 locations and a test for overall spatialtrend.
The test for trend over time at each location was carried out via the WilcoxinRank Sum Test or the Kruskal Wallis Test. Both tests are nonparametrie tests( i . e . , a test statistic is calculated based on the ranks of the TCDDconcentrations instead of the actual TCDD concentrations). A nonparametricapproach was taken because the TCDD concentrations for a given year at a givenlocation generally did not follow a normal distribution.
For each location, the nonparametrie tests, named above, test the nullhypothesis that the concentration of TCDD is. the same for the different timeperiods observed, against the alternative hypothesis that the concentration ofTCDD is not the same for the different time periods observed. The results ofthe test show that samples collected from Bayou Meto at Highway 79 havedifferent concentrations over time. This difference appears to be a decreaseover time. The test could not be carried out at the following threelocations: Lagrue Bayou/Peckerwood Lake, Benson Bridge, and Highway 11 due toinsufficient data. The remaining ten locations showed no change over time.The large number of "no change" results could in part be caused by the smallamount of data collected during each time period. See Appendix C fortabulated statistical tests results for each of the 14 locations.
The test for overall spatial trend was carried out using data collected in1987. The Mann-Kendall test for trend was used to test the null hypothesisthat the concentrations of TCDD in fish remain constant as distance from thesite increases versus the alternative hypothesis that the concentrations ofTCDD in fish decrease as distance from the site increases. The data used toperform this test are presented in Appendix C. These data present eachlocation along with the average concentration of TCDD found in fish from the
location. The average concentration considered all nondetected results asone-half the detection limit. The results of the test show that theconcentration of TCDD in fish does decrease as distance from the siteincreases ( i . e . , the null hypothesis is rejected at the a= 0.05 level ofsignificance).
ANA25375 5-409/12/89 F1
.6.0 FIELD QUALITY CONTROL REPORT
The quality assurance (QA) goal for this program was to ensure that all
information, data, and documentation are technically sound, statistically
valid, and properly documented. To accomplish this goal, certain field
quality control (QC) activities were performed along with the regular field
sample collection activities described in earlier sections. A description of
these QC activities and a summary of the ensuing results are presented in this
section.
6.1 SAMPLING QUALITY CONTROL ACTIVITIES
6.1 .1 Sample Handling
Upon completion of each day's activities, all sample documentation was
verified and the samples were prepared for shipment to the laboratory.
A C/C form (Appendix ft, Figure 3) was initiated before samples left the
site. The C/C acted as the primary transmittal form from sampling personnel
to laboratory personnel, and was signed when samples were relinquished by and
received by involved personnel at the time of each transfer.
6.1.2 Sampling Equipment
Sampling apparatus, where used, was thoroughly cleaned before beginning each
sampling event by washing with laboratory-approved detergent followed by a
distilled water rinse and a final hexane rinse. Clean latex gloves were worn
during all equipment cleaning operations and were changed between each sample
taken to avoid cross contamination. All soil/sediment samples were placed in
precleaned glass sample containers with Teflon-lined screw caps.
6.1.3 Field Travel Blanks
Field travel blanks were submitted for analysis at a target frequency of 5
percent (1 blank for every 20 soil/sediment and fish samples) or a minimum of
one blank for each day that samples were collected, whichever is greater.
ANA25376 6-109/12/89 F2
Each blank consisted of a 40-ml glass vial filled with pesticide-grade hexaneat the laboratory, transported to the field, and included with each shipmentof site samples to the laboratory for analysis.
The purpose of the blank was to monitor potential cross contamination of thesamples during handling and shipment.
Field travel blanks were prepared in association with soil/sediment and fishsamples. When the number of blanks significantly exceeded 5 percent due todaily submittals, a portion of them were designated for archive, pendinginitial sample results. When taken, this option was recommended by the ITASProject Manager, approved by the OC Officer, and authorized by the HerculesProject Manager before implementation.
6 . 1 . 4 Equipment Rinsate SamplesTo verify the effectiveness of the equipment cleaning procedure, an aliquot ofthe final hexane rinse was collected at a target frequency of 5 percent, orone for each soil/sediment sampling day. These rinsates were only collectedin association with the soil/sediment samples, as these are the only sample
: matrix,where sampling equipment was involved.
6 . 1 . 5 Glove BlanksIn addition to equipment rinsates, glove blank QC samples were prepared andsubmitted for analysis. Preparation of a glove blank sample consisted ofdonning a clean pair of latex gloves normally used during sample collection,soaking a sterile gauze pad in hexane, and wiping the latex gloves thoroughlywith the wet gauze pad. The pad was then put into a clean Teflon-lined screwcap glass jar, given a unique sample number, and shipped to the laboratorywith regular field samples for analysis. A target frequency for glove blanks
was not established before project initiation; however, they were submitted atregular intervals during the soil/sediment sample collection events.
6 . 1 . 6 Field DuplicatesDuplicate samples were prepared at randomly selected soil/sediment samplinglocations to achieve a frequency of 5 to 10 percent of the total samples
ANA25376 6-209/12/89 F2
collected for this matrix type. The duplicate was assigned a separate andunique sample number, so that its identity was blind to the analyticallaboratory.
6 . 2 SUMMARY OF FIELD QUALITY CONTROL
Table 12 summarizes the actual number of field QC samples collected during thedefined sampling program compared with the total number of non-QC samples foreach matrix. In each case the targeted frequency was met or exceeded.
Only selected field samples collected were submitted for analysis (seeSections 3 . 3 , t . 3 , and 5.3 for the analysis/archive strategies of eachmatrix); therefore, only the corresponding QC samples were submitted foranalysis to maintain the target frequencies as defined in Section 6 . 1 . The
analytical results of the field QC samples submitted for analysis arepresented by matrix type in Tables 13 through 15.
The following abbreviations apply to the tables:
• SO = Soil• WI : Gauze wipe pad
'• LI = Liquid• SE = Sediment• Q == Qualifier• U = Compound analy2ed but not detected; value given is the detection
limit.
6 . 3 CORRECTIVE ACTIOHSOne anomaly was observed in the field QC data. The results of the analyzedglove blanks showed relatively high levels of total octachloro-dioxins (octa-CDD) compared with all other soil/sediment samples analyzed (see Table 1 2 ) .As soon as these anomalous results were reported, corrective action began.
First, an investigation into the source of the contamination was initiated.Samples from the two brands of gauze pads used in the preparation of gloveblanks and the brand of latex gloves used during collection were extracteddirectly in hexane and analyzed for total dioxin. The results of both brandsof gauze were none detected at adequate detection limits; however, the gloveextract showed total octa-CDD that exceeded the instrument's linear range(approximately 1,320 ng/sample). Upon receiving the results, the project
ANA25376 6-309/12/89 F2
Table 12. Field Quality Control Sample Summary
Total No. No. of Field No. of No. of No. ofof Samples Travel Glove Equipment Field
Sample Matrix Collected____Blanks____Blanks Rinsates Duplicates
Soil/sediment 200 15 6 13 10
Wood ducks 23 0 0 0 0
Fish 219 12 0 0 0
ANA2537L09/13/89 F2
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management distributed, a directive requiring the discontinuation of this brandof gloves in all field activities (for health and safety reasons as well assample integrity reasons).
Because the general sample collection procedure does not involve directcontact between the gloves and the field sample and because the equipmentrinsate samples were all "non detected" for 2,3,7,8-TCDD and very low forocta-CDD, it is believed that the soil and sediment data collected while usingthe anomalous gloves have been affected minimally or not at all.
ANA25376 6-409/12/89 F2
7.0 . DIOXIN ANALYSES QUALITY CONTROL REPORT
As with the sampling program, the QA goal for the analytical program has been
to ensure that all information, data, and documentation are technically sound,
statistically valid, and properly documented. Specific QA objectives have
been defined for this program. To meet the objectives, the QA program
includes the use of approved calibration procedures and analytical methods and
the analysis of special QC samples. The objectives, procedures, and resultsof the Hercules/Vertac analytical QA program are described in this section.
7 . 1 ANALYTICAL QUALITY ASSURANCE OBJECTIVES
The accuracy, precision, completeness, and comparability discussions thatfollow include and represent the objectives set by IT for this project.
7 . 1 . 1 Accuracy
Accuracy is defined in QAMS-005/80 as the degree of agreement of a
measurement (or average of measurements of the same thing) with an accepted
reference or true value. The project objectives for accuracy were to providedata within the guidelines set forth in Table 1 6 .
7 . 1 . 2 Precision
Precision is defined in QAMS-005/80 as a measure of mutual agreement amongindividual measurements of the same property, and is best expressed as
relative percent difference (RPD) under prescribed similar conditions. Theproject objectives for precision were to provide precision data within the
guidelines set forth in Table 1 6 .
7 . 1 . 3 CompletenessCompleteness is a measure of the amount of valid data obtained compared to the
amount expected to be collected under normal correct conditions. It is
usually expressed as a percentage. The completeness objective has been
^AMS-OOS/SO, "Interim Guidelines and Specifications for Preparing QualityAssurance Project Plans," Office of Monitoring Systems and Quality Assurance,Office of Research and Development, U.S. EPA, Washington, D.C. 20460,December 29, 1980.
ANA25377 7-105/15/90 F3
Table 1 6 . Precision and Accuracy Objectives
Analysis Matrix
Precision(Expressedas RPD)
SurrogateAccuracy(Expressed as
% of True Value)
SpikeAccuracy(Expressed as% Recovery)
Total dioxins
Isoaier-specific(2,3,7,8-TCDD)
Wildlife
Soil/sediment
Wildlife
Soil/sediment
±50
±50
±50
±50
60-140
60-140
60-140
60-140
60-140
60-140
60-140
60-140
ANA2537P09/13/89 F2
calculated on those samples reaching the laboratories intact, not the total
number of samples collected, since breakage during transit can occur for whichthe laboratories are not responsible.
The goal of this Qfl program was to generate valid data .for at least 90 percent
of the samples analyzed.
7 . 1 . 4 Comparability
Comparability expresses the confidence with which one data set can be compared
to another. To achieve comparability in this project, the data generated havebeen reported using units of vg/kg (pp b ) or ng/kg ( p p t ) , as appropriate.
Analytical results are comparable to that produced from similar laboratories
using the same instrumentation and methodology.
Standard reference materials have been used to document traceability of
calibration standards and allow comparison of data across laboratoriesperforming analyses.
7.2 CALIBRATIOH PROCEDURES AND FREQUENCY
7 . 2 . 1 Instrument Performance
ftt the outset of 2,3,7,8-TCDD analysis, a performance check on each instrumentwas made to demonstrate compliance with manufacturer's specifications.
7.2 . 2 Calibration Procedures
7 . 2 . 2 . 1 Total Dioxins
The analytical approach employed by ITAS for the determination of total
dioxins is considered semi-quantitative due to the lack of availability of all
dioxin isoner standards. The standard analyzed each shift consisted of:
2,3,7,8-TCDD ^C^.S^.S-TCDD1,2,3,7,8-PeCDD "C-l,2,3,7,8-PeCDD1,2,3,4,7,8-HxCDD •-'C-1,2,3,^,7,&-HxCDD1 , 2 , 3 , 4 , 6 , 7 , 8 , - H p C D D 'y-1,2,3^.6,7,S-KpCDDOCDD ^C-OCDD
3'C1-2,3,7,8-TCDD (surrogate).
ANA25377 7-205/15/90 F3
Response factors were calculated for each compound in the standard relative to
the corresponding -C isomer (internal standard) from each congener group; thesame response was assumed to be applicable to all isomers in each congener
group. A 5-point calibration plot was run in triplicate. The mean response
factors obtained from the 15-point calibration were used for all subsequent
calculations. The shift standard analyzed on the same day as the samples hadto produce a response factor within 30 percent of the multi-point to be
acceptable. ^d-TCDD was used to calculate the accuracy of the method,expressed as surrogate recovery.
7 . 2 . 2 . 2 Isomer-Specific TCDD
For isomer-speelfic analyses, a seven-isomer performance mixture containingthe six most closely eluting TCDD isomers was run at the beginning and end of
each 8-hour shift to demonstrate satisfactory resolution of the targetcompound. In addition, an initial 5-point calibration plot was run in
triplicate before sample analysis. The mean response factors obtained fromthis 15-point calibration were used for all subsequent calculations. The
daily calibration standard, analy2ed on the same day as the samples, had toproduce a response factor within 10 percent of the 15-point calibration. If
the response observed from the calibration standard was outside the expectedconcentration by >10 percent upon two successive Injections, a new calibration
curve was established before continuing with sample analyses.
7.3 ANALYTICAL PROCEDURESAll sample analysis for total and isomer-specific dioxin was performed at the
ITAS SAL in Knoxvllle, Tennessee (except for the analysis of the split samplestransferred to the EPA FIT). Sample preparation and analysis procedures were
performed using modifications of EPA Method "Determination of 2,3,7,8-TCDD in
Soil and Sediment", RCRA Method 8280. In an effort to generate data
comparable to previous studies of the Vertac off-site areas, wood duck sampleswere prepared according to the method "Determination of Part-per Trillion
Levels of Polychlorinated Dibenzofurans and Dioxins in Environmental Samples"(Smith et a l . ; Analytical Chemistry, 1984, 56, 1830), with appropriate
modifications as used in the previous work (see Section 7 . 3 . 3 ) . All sampleshave been analyzed using high resolution gas chromatography/high resolution
ANA25377 7-305/15/90 F3
mass spectrometry (HRGC/HRMS) instrumentation to achieve the best possibledetection limits.
A brief description of the analysis procedure used for each sample matrix is
outlined below. Detailed laboratory standard operating procedures (SOPs) maybe provided on request.
7 . 3 . 1 Soil/Sediment Sample PreparationA weighed aliquot of each soil sample (usually 10 grams) was transferred to a
jar and spiked with the internal standard/surrogate spike mixture, composed ofthe following ^C-labeled compounds: 2,3,7,8-TCDD, penta-CDD, penta-CDF,
hexa-CDD, hexa-CDF, hepta-CDD, hepta-CDF, and octa-CDD, as the internalstandards and 3'C1-2,3,7,8-TCDD as the surrogate. This spike solution is used
for the analysis of total dioxins, isomer-specific 2,3,7,8-TCDD, as well astotal furans; therefore, it includes chlorodibenzo-p-furans ( C D F ) . Each
sample was allowed to stand overnight for equilibration, followed by a 3-hour
Jar extraction with a methanol/hexane mixture. Extracts were filtered and
concentrated in preparation for selected cleanup steps. To aid in the removalof chemical interferences, samples were cleaned up using dual column
chromatography consisting of an acid-modified silica gel column followed by aneutral alumina column. Final extracts were concentrated to near dryness and
raised to 50 ill with isooctane.
7. 3 . 2 Fish Sample Preparation
Using the routine ITAS procedures for preparation of biological samples, a
weighed aliquot, usually 10 grams, of each macerated fish sample and a sodiumsulfate blank were weighed into separate jars, spiked with the internal
standard/surrogate mixture, and blended with 20 grams of sodium sulfate.After thorough mixing, 150 ml of acetonitrlle was added and the samples shaken
using a platform shaker for 3 hours. The resulting extract was filtered into
a flask and concentrated down to approximately 1 ml. To aid in the removal of
chemical interferences, samples were cleaned up using silica gel/alumina
column chromatography. Detailed descriptions of the cleanup techniques can be
found in Option A of EPft, Region VII protocol for "The Determination of2,3,7,8-TCDD in Soil and Sediment", revised September 1983. Final extracts
were concentrated to near dryness and raised to 50 pi with isooctane.
ANA25377 7-405/15/90 F3
For internal laboratory comparison, two fish samples were prepared by theSmith et al. enrichment procedures as well as the procedures describedabove. The results indicated negligible differences between the twoextraction/cleanup procedures.
7 . 3 . 3 Duck Sample PreparationTwenty-five grams of ground homogenized duck halves (either right or left duckhalf cut longitudinally) and 25 grams of sodium suifate (a blank) were weighedinto separate Jars. The samples and blank were spiked with the internalstandard/surrogate mixture and allowed to stand overnight for equilibration,followed by an extraction with a cyclohexane/methylene chloride mixture for 3hours on a platform shaker. The extract was carried through the Smith et al.enrichment procedure before being concentrated to near dryness and the volumeraised to 50 ul with isooctane.
In the 1984 procedure published by Smith et al. tissue samples are spiked withisotopic marker compounds and processed in a two-part enrichment procedure.In Part I , a mixture of the sample and sodium suifate is subjected to solventextraction and the extract, in the same process, is passed through a series ofsilica-based adsorbents and then through the carbon/glass fiber adsorbent. InPart II, following a change of solvent to hexane, the sample is applied to asecond series of adsorbents contained in two tandem columns. The extract isthen reduced in volume for instrumental analysis. The modification of theprocedure, as determined from the previous wood duck study, was the additionof the "pre-extraction" step using a cyclohexane/methylene chloride mixturementioned above. The purpose of the modification was to disperse fat intosolution to prevent clogging of the enrichment columns.
7.3. 1* High Resolution Gas Chromatography/High Resolution Mass SpectrometryThe prepared sample extracts were analyzed using HRGC/HRMS scanning in theselected ion monitoring mode for enhanced sensitivity. The column used forisomer-specific analysis was a 60-meter SP-2331 fused silica column. Fortotal dioxin congener analysis (Cli(-Clg), a 30-meter DB-5 column was used. Asample-specific detection limit was calculated as 2.5 times the signal tonoise ratio in the elution window for each congener (or 2,3,7,8-TCDD, for
ANA25377 7-505/15/90 F3
isomer-specific data).when a "not detected" (ND) is reported. A detection
limit of 1 to 5 ppt is typical for soil and sediment samples (based on a10-gram aliquot). For biological samples, the target detection limit was lessthan or equal to 10 ppt. However, due to the complexity of some of the samplematrices, the detection limit may have been higher.
7.4 DATA REDUCTION. VftLIDATIOM, AND REPORTING
At all ITAS facilities, the continuing operational objectives are directed atproviding quality results and service from the receipt of the sample throughthe data report. Data interpretation is performed by experienced personneland thoroughly reviewed by the QC Coordinator. The laboratory QA/QC planadheres to the stringent U . S . EPA dioxin CLP dioxin QA/QC plan. As part ofthis program, the laboratory has received a 99 out of 100 percent rating on anEPA Performance Evaluation sample analyzed for dioxin in soils. Additionally,IT continues to receive high marks on Performance Evaluation samples submittedby EPA and other regulatory agencies during ongoing projects as part of theagency's auditing procedures.
Each data package submitted as part of this program has contained thefollowing items:
• Results of the initial calibration including all selected ion currentprofiles (SICP), as well as results of calculated response factorsfor that multi-point.
• Completed sample data sheets with appropriate SICPs and spectraattached. The rounding rules found in Section 7 . 2 . 2 , "Handbook forAnalytical Quality Control in Water and Waste-water Laboratories",EPA 600/t-79-019 were applied to all data. Each SICP and spectrumincludes computer-generated header information indicating instru-mental [gas chromatograph/mass spectrometer (GC/MS)] operatingparameters during data acquisition.
• SICPs generated during each performance check solution analysis andeach concentration calibration solution analysis.
» A chronological list of all analyses performed. If more than oneGC/MS system was used, a chronological list was required for eachsystem. The list provides the sample number and (if appropriate) thecontractor laboratory sample number for each sample and blank,concentration calibration solution, and performance check solution.This list also specified the date and time that analysis was begun.All sample/blank analyses performed during an 8-hour period were
ANA25377 7-605/15/90 F3
accompanied by two performance check solution analyses - onepreceding and one following sample/blank analyses. If multipleshifts were used, the ending performance check sample analysis fromone 8-hour period serves as the beginning analysis for the next 8-hour period.
7.5 LABORATORY QUALITY COMTROL SAMPLES AND RESULTS
The attainment of the analytical QA goal and objectives for this project wasdependent upon the operation of the laboratory in accordance with a program
which systematically ensured the precision and accuracy of analyses by
detecting errors and preventing their recurrence or measuring the degree of
error inherent in the methods applied.
The routine internal QC program included the analysis of calibration and check
standards, blanks, matrix spike/matrix spike duplicate (MS/MSD) samples, and
surrogate spike samples.
7 . 5 . 1 StandardsAnalytical instruments were calibrated daily using certified standards when
possible. The highest purity standards commercially available, usually 98percent, were used for calibration and check standard solutions.
7.5.2 Blanks
Nanograde quality solvents were used for the analyses performed for thisproject. Each lot of solvent was checked to ensure its suitability for the
intended analysis.
To demonstrate that all analytical materials ( i . e . , reagents, glassware, andsolvents) were free from interferences, a method blank was assigned to each
batch of 20 samples (or less) of each matrix and was extracted, analyzed, and
reported following the identical procedures used for the accompanying
samples. Table 17 lists the number of samples and method blanks analyzed foreach matrix.
7.5.3 Matrix Spike/Matrix Spike Duplicate Samples
In accordance with CLP requirements, an MS/MSD pair was prepared for each
batch of 20 samples (or less) of each matrix. The sample to be spiked and
ANA25377 7-705/15/90 F3
Table 17. Laboratory Quality Control Sample Summary
Total No. No. of No. ofSample Matrix_____of Samples_______Method Blanks_____MS/MSD Pairs
Soil/sediment 82 14 6
Wood ducks 18 6 2
Fish 49 8 4
ANA2537Q09/13/89 F2
duplicated was selected at random by the laboratory at the time the samples
were logged in. The total number of matrix spike duplicate pairs analyzed foreach matrix during this project is listed in Table 17.
The results of these samples demonstrate the precision and accuracy of the
Vertac project sample results. The project objectives for precision andaccuracy are listed in Table 1 6 .
7 . 5.4 Surrogate Spike Samples-3-7-"C1-TCDD was spiked into every sample analyzed for dioxin. The ensuing
result was used to calculate the accuracy of the method, usually reported as a
percent. The surrogate percent accuracy target range was the same as that formatrix spike percent accuracy, 60 to 140 percent.
7.5.5 Quality Control Sample Results
Volume I of each data package submitted to the client by the laboratory
contained a QA/QC discussion section and tables presenting the mean surrogate
percent 'accuracy of all samples included in the data package and the resultsof MS/USD samples, along with the corresponding precision and accuracy
calculations. Copies of this supporting information are included in AppendixE.
7 . 5 . 5 . 1 Method Blank Results Summary
A total of 37 method blanks were analyzed during the course of this project,
far exceeding the target frequency. Of these blanks, four were positive for
2,3,7,8-TCDD; however, all four showed a concentration of less than or equalto .0052 ppb. These values were in the range of the expected detection limit
of 2,3,7,8-TCDD in soils and well below the expected detection limit ofbiological samples. Of the project samples associated with these positive
blanks, the majority of those that were positive for 2,3,7,8-TCDD had
concentrations two to three orders of magnitude higher than the blanks.
A more difficult situation was found in the high resolution analysis of the
total dioxins (Clh-CIa). Of the 37 blanks, 24 were positive for at least onetotal congener. However, of these 24 blanks, 20 had concentrations less than
0.020 ppb. Again in this case, of the project samples associated with the
ANA25377 7-805/15/90 F3
positive blanks, the majority of those that were positive had concentrations
several orders of magnitude greater than that in the blanks. This situationwas noted early in the project and stricter cleaning procedures were
Instituted. Due to the sensitivity of the higher resolution procedures andthe nature of the biological samples, resolving the blank situation took
time. But the situation did improve and the last six blanks analyzed in theproject tested negative for total dioxins.
7 . 5 . 5 . 2 Matrix Spike/Matrix Spike Duplicate Results
Table 18 presents the results and the corresponding field information of thesoil/sediment samples spiked in duplicate with a standard dioxin solution.
The calculations for precision and accuracy are defined and the results arepresented in the QA/QC report tables found in Appendix E. Tables 19 and 20
list the results and field information for the matrix spike pairs of the wood
ducks and fish samples, respectively. Again, see Appendix E for precision and
accuracy calculations.
AMA25377 7-905/15/90 F3
M Da« D! fly 1mi 11
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8.0 PARTIAL PRIORITY POLLUTANT ANALYSES QUALITY COMTROL REPORT
Nineteen sediment samples along with three trip blanks were submitted forpartial priority pollutant (PPP) analysis at ITAS, located on Middlebrook Pikein Knoxville, Tennessee. Thirty-eight other sediment samples collected forPPP analysis were submitted for storage at the laboratory under archivestatus. The ITAS laboratory has qualified as an EPA CLP laboratory fororganics analysis.
The compounds requested for analysis are a subset of the EPA's CLP TargetCompound List. The requested parameters are listed below:
• Volatiles
Toluene
• Semivolatiles
2-chlorophenol4-chlorophenol2,4-dichlorophenol2,6-dichlorophenol2,316-tr ichlorophenol
'' 2,4,6-trichlorophenol2,4,5-trichlorophenol
• Herbicides
2,4-D [(2,4-dichlorophenoxy) acetic acid]2,4,5-T [(2,4,5-trichlorophenoxy) acetic acid]Silvex [2-(2,4,5-trichlorophenoxy) propionic acid, 2 , 4 , 5 - T P ] .
The volatlles analyses were performed by purge and trap and GC/MS. The semi-volatiles, or base, neutral, acid ( B N A ) extractables, analyses were performedby direct injection of the sample extract onto a capillary column GC/MS
system. Both GC/MS analyses followed EPA CLP protocol, revision 7/87. The QCprogram is explicitly defined in the CLP document. QC samples analyzedinclude surrogates and internal standards in every sample, a method blank forevery 20 samples (or less) of a matrix, and an MS/MSD pair for every 20samples (or less) of a matrix. The QC sample target frequencies were met orexceeded in every case for the analyses performed. The limits used foraccuracy (as determined by percent recovery of a matrix spike) and precision
ANA25378 8-109/12/89 F2
(as determined by relative percent difference between the spike duplicateresults) were those given in the EPA CLP protocol for each compound spiked.Explanation of the QC results is given in the Case Narrative of the CLP datapackage (see Appendix F ) .
The herbicide analyses were performed by packed column GC. Because the CLPprotocol does not include criteria for herbicide analysis, the CLP protocolfor pesticide analysis was approximated for data reporting and packaging. Thesamples were analyzed for phenoxyacetic acid herbicides in accordance with aroutine ITAS procedure with modifications in the run sequence to more closelyapproximate the CLP pesticide method. References for the ITAS procedure arelisted in the Case narrative presented in Appendix F.
QC samples analyzed during herbicide analyses include method blanks, one foreach batch of samples extracted, not to exceed 20 samples; a matrix spike orspiked blank, one for every 20 samples; and a matrix spike duplicate or aduplicate sample, one for every 20 samples. The targeted frequencies were metor exceeded in each case. At this tine, there are no established criteria forherbicide analysis precision and accuracy.
Table 21 presents a sample summary table for partial priority pollutantsevaluation. ' '
ANA25378 8-209/12/89 F2
ITAS Project Code:Purchase Order NumberCase Name:
Field Number
WH1261A-P
WH1266A-P
WH1271A-P
WH1248A-P
WH1248C-P
WH1252A-P
WH1252J-P
WH1253A-P --
WH1253A-P ( R E )
WH1254A-P
WH1254D-P
WH1254D-P (MS)
WH1254D-P (USD)
WH1258A-P
WH1258D-P
ANA2537R09/13/89 F2
^
Table 21
ITFK 40036: 480030
Hercules/Verta
ITAS Number
DD7590DD7587
DD7591DD7588
DD7592DD7589
DD7593DD7593
DD7594CD7594
DD7595DD7595
DD7596DD7596
DD7597DD7597
DD7597R
DD7598DD7598
DD7599DD7599
DD7599 MS
DD7599 MS
DD7599 MSD
DD7599 MSD
DD7600DD7600
DD7601DD7601
. Sample Sumi
1C
Matrix
WaterWater
WaterWater
WaterWater
SoilSoil
SoilSoil
SoilSoil
SoilSoil
SoilSoil
Soil
SoilSoil
SoilSoil
Soil
Soil
Soil
Soil
SoilSoil
SoilSoil
/~\
nary Table
Concentration
-
-
LowLou
LowLow
MediumLou
LowLou
MediumLou
Lou
LowLow
LowLow
Low
Low
Low
Low
MediumLow
LowLow
Analysis
BNA, HERBVO
BNA, HERBVO
BNA, HERBVO
BNA, HERBVO
BNA, HERBVO
BNA, HERBVO
BNA, HERBVO
BNA, HERBVO
VO
BNA, HERBVO
BNA, HERBVO
QC-MS-BNA,HERBOC-MS-VO
QC-MSD-BNA,HERBQC-MSD-VO
BNA, HERBVO
BNA, HERBVO
m
r^-in(M0
Field Number I
WH1259A-P
WH1259D-P
HH1260A-P
WH1260A-P (MED)
WH1260F-P
HH1264A-P
HH1264A-P (MED)
WH1264E-P
WH1267A-P
WH1267A-P (MED)
WH1267F-P
WH1269A-P
WH1269A-P (MS)
WH1269A-P (MSD)
WH1269G-P
WH1269G-P (RE)
Abbreviations: BNA =HERB ==VO =MS =MSD =RE =
ANA2537R09/13/89 F2
/^
Tabi
TAS Number
DD7602DD7602
DD7603DD7603
DD7604DD7604
DD7604
DD7605DD7605
DD7606DD7606
DD7606
DD7607DD7607
DD7608DD7608
DD7608
DD7609DD7609
DD7610DD7610
DD7610 MS
DD7610 MSD
DD7611DD7611
DD7611 R
Semi volat lies.PhenoxyacefcieVoiatiles.Matrix spike.Matrix spike dRerun.
Le 21. (Continued
Matrix
SoilSoil
SoilSoil
SoilSoil
Soil
SoilSoil
SoilSoil
Soil
SoilSoil
SoilSoil
Soil
SoilSoil
SoilSoil
Soil
Soil
SoilSoil
Soil
acid herbicides.
uplicate.
^
)
Concentration
MediumLow
LowLow
MediumLow
Medium
LowLow
MediumLow
Medium
LowLow
LowLow
Medium
LowLow
MediumLow
Medium
Medium
LowLow
Low
Analysis
BNA, HERBVO
BMA, HERBVO
BNA, HERBVO
VO
BNA, HERBVO
BNA, HERBVO
VO
BNA, HERBVO
BNA, HERBVO
VO
BNA, HERBVO
BNA, HERBVO
QC-MS-BNA
QC-MSD-BNA
BNA, HERBVO
VO
</Y"
rLT
CVc
APPENDIX A
SAMPLE CUSTODY AMD DOCUMENTATION FORMS
ANA2537APA08/31/89 F1
03r^. ^-\
SPECIMEN COLLECTIUN LOG DATE'T I M E -PROJECT NAME: HERCULES/VERTAC
LOCATION: JACKSONVILLE, ARKANSAS
PROJECT #480030.01.06.01
SAMPLE lS>
Specimen Type
Species
Collection Method
Preservation Method
OBSERVATIONS /SKETCH/ADDITIONAL COMMENTS
.Age
Sex
Weight
Length
Girth
Station No.
River Mile
Sample Location Description
Prep Lab AU = Austin CE ° Cerritos DI = Directors ED s Edison FM s FAS MobileHK = Middlebrook PI = Pittsburgh SC ° Santa Clara
Analysis Request: 01 = 2.3,7,8 TCDO 02 » Total PCDD/DF03 = Total and ISOHER specific PCDD/DF04 °
Film Roll No.
Sample Team
Frame No.
(Initials)Prepared By_ Ck'd By
( In i t ia l s )
FORM * D84625-F34 / R 1 [7/671
Figure 1
^ SAMPLE COLLECTION LOG
03SAMPLE 9
PROJECT NAME: HERCULES/VERTAC
LOCATION: ARKANSASPROJECT # 480030.0Z.07.01
DATE'
TIME' 1
Sample Location Description_
Purpose: PR * Predecon DE " Decon Rl = 1st Resample R2 = 2nd Resample FI = FinalVF " Verification EC •' Equipment Check RH = Routine MonitoringGC = General Characterization UI ° Well Installation
Sample Type; AI - A i r BU z Bulk CH = Chip CO = Core LI ' Liquid 01 = On (Liquid)SE = Sediment SO = Soil UI = Wipe HA = Hater
Composite? Y/N Conp. descr1ption_
Sample Attitude: 01 ° Horizontal 02 = Vertical 03 = Both
[— — Stetch/Coimient?Elevation
Depth of Take
X-Axis ,
Y-Axis
Area or Volune Sampled
Floor/Area
Room
Zone
Equipment
QA/QC Code
OA/OC Partner
Lab: AU =MK =
F1o(000102030405
QBLQGSQRI
Aust in CEMiddlebroc
or/Area Code
BasementFirst
QA/qc° Blank° Spike= Equipment Rinse
E = Cerritos 01 ' C3k PI = Pittsburgh
EquilMient Code
01 ' Wal l 07 -02 - Ceil ing 0803 = Floor04 = Equipment 0905 = Vent System 10 -06 = Ambient Air 11 -
12 -CODE
QRE = RewipeQDU = DuplicateORI6 = Original of QA/OC
'irectors ED = EdisonSC ' Santa Clara
= Cabinet/Desk= Exterior Pipes
Beams, Duct= Doors
: sample
FM ° FAS Mobile
Analysis Request: 01 s PCB 02 s! PCOD/PCDF 03 = 04 s
Analysis Status: 01 s Priority 02 = Analyze 03 = Hold
Film Roll No._____ Frame No.______
Sample Team_______________ Prepared By_(Initials)
FORM It- 0846Z5-F8, Rl 0/87)
Figure 2
RNATIONALMOLOGYDHATION CHAIN-OF-CUSTODY RECORD
R/A Control No.
C/C Control No,
PROJECT NAME/NUMBER
SAMPLE TEAM MEMBERS -
LAB DESTINATION
CARRIER/WAYBILL NO.
SampleNumber
SampleLocation and Description
Dale and TimeCollected
SampleType
ContainerType
Condition on Receipt(Name and Date)
DisposalRecord No
Special Instructions:
Po isible Sample Hazards;
SKiNATURES: (Name, Company, Date and Time)
1. Relinquished By:
Received By;-
3. Relinquished By:
Received by:
2. Relinquished By:
Received By:
4. Relinquished By:
Received By:-
WHI re - To accompany samplesYELLOW-Field copy Figure 3
0 2 5 7 8 8
L J, J INTE1 U • TECILUCOR
PROJECT NAME
PROJECT NUM
PROFIT CENTE
PROJECT MAN/I
BILL TO
PURCHASE OR
Sample No.
KNATIOMALINOLOGY Bcrniccrcrtn AMAIVCIC R/ACoPORATION ] REQUEST FOR ANALYSIS
C/C Co
= DATE SAMPLES SHIPPED
BER LAB DESTINATION
R NUMBER '' LABORATORY CONTACT
tGER SEND LAB REPORT TO
DATE REPORT REQUIRED
DER NO. PROJECT CONTACT
PROJEC
Sample Type Sample Volume Preservative
^T CONTACT PHONE NO.
Requested Testing Program
ntrol No. 19 5 7 2 8
ntrol No.
Special Inslruclkms
TURNAROUND TIME REQUIRED: (Rush must be approved by Ihe Laboratory projecl Manager) OC LEVEL: (Levels II and III subjecl to surcharge: profect-specii'c requirements must besubmitted lo lab bofore beginning work.)
Normal____ Bush ___ i (Subjecl to rush surcharge.) I____ II____ III____ I rojecl Specific____
POSSIBLE HAZARD IDENTIFICATION: (Please indicate II sample(s) are hazardous materials and/or susprcled 10 conlain high levels ol hazardous substances.)
Non-hazard____ Flammable____ Skin Irritant____ Highly Toxic____ Oil »r
SAMPLE DISPOSAL:
Return lo Client .
(Please indicate disposition of sample following analysis. Lab will charge lor packing, shipping, archive and disposal.)
Disposal by Lab ____ Archive ____ (Indicate number of months.)
(Please SpecUr)
FOR LAB USE ONLYReceived by .
WHITE • Original, to accompany samplesYELLOW - Field copy
0 2 5 7 8 9
APPENDIX B
SAMPLIHG METHOD DIAGRAM
ANA2537APA08/31/89 F1
r> ^PISTON-TYPE BED-MATERIAL HAND SAMPLER, US BMH-53
This sampler is used to collect a sample from thebed of a shallow stream which may be waded.
The sampler contains a cylinder 2 Inches indiameter and 8 inches long which is pressed Intothe stream bed to collect the sample. A piston islocated inside the cylinder. The overall length ofthe sampler Is 46 inches. A handle for pressingthe cylinder into the bed is located at the top ofthe sampler frame. The piston rod with a handle
on its upper end passes through the sampler frame.The piston is retracted when the cylinder is pressedinto the bed material. The suction created by thepiston holds th° «i""r>i« in the cylinder. The sampleis pushed out of the cylinder by the piston.
N•1 Wight 8 Lb«. (4 kg)Shipping Weight 25 Ltx. (11 kg)Shipping Container—4"x4"xSO" (JO cu. tt.)
MANUFACTURED BY:
PRODUCT16121 484-8427
MANUFACTURING CO.MAPLEWOOD INDUSTRIAL PARK
2515 HIGHWAY 61 NO. ST. PAUL. MN S510S
Figure 1
APPENDIX C
STATISTICAL SUPPORT DATA
ftNA2537APA08/31/89 F1
D. Simeriy
J. Christman
STATISTICAL ANALYSIS OF SOILAND SEDIMENT DATA FROM VERTAC
May 12, 1988
Project No. t80030.02.05.05
In order to assess the current levels of 2 , 3 , 7 , 8 TCDD (TCDD) towarddegradation or dispersion, a statistical analysis of all available soil andsediment data was conducted. Soil and sediment data are available from twosampling events, one in August 1984 the other in September and October of1987. The 1987 samples were collected in close proximity to those collectedIn 1984.
The statistical analysis of soil and sediment data includes a comparison of1987 TCDD concentrations to 1984 TCDD concentrations. The specific interestbeing is it reasonable to conclude that the 1987 TCDD concentrations are lowerthan the 1984 TCDD concentrations. As mentioned above, the 1987 samples werecollected in close proximity to those collected in 1984. This being the case,the 1987 soil and sediment samples were compared to the 1984 soil and sedimentsamples via the Wilcoxin signed Rank Test ( 1 ) . In this application, theWilcoxin Signed Rank Test tests the null hypothesis that the median change inTCDD concentration from 1987 to 1984 is greater than or equal to zero againstthe alternate hypothesis that the median change in TCDD concentration from1987 to 1984 is less than zero. Generally speaking, if the null hypothesis isrejected it is reasonable for one to believe that the 1987 soil and sedimentTCDD concentrations are significantly less than the 1984 soil and sedimentTCDD concentrations.
Table 1 presents the 1984 and 1987 soil and sediment TCDD concentrations alongwith their respective differences. The Hilcoxin Signed Rank Test was appliedto the column of differences. The result of the Wilcoxin test is the nullhypothesis is rejected at the a= 0.05 level of significance. The 0.05 levelof significance implies that the probability of concluding the median changein TCDD concentration from 1987 to 1984 is less than zero when in fact themedian change is greater than or equal to zero is 0.05. Since the nullhypothesis is rejected, it is reasonable for one to conclude the 1987 TCDDconcentrations are significantly less than the 1984 TCDD concentrations.
A point estimate of the magnitude of the difference between 1987 and 1984 TCDDconcentrations is -0.40 ppb. This implies that a TCDD concentration taken in1987 at a given location is one the average, -0.40 ppb less than the TCDDconcentration observed in the same location in 1984. A 95 percent confidenceinterval for the magnitude of the difference is ( - 0.745, - 0.205) ppb. This
ANA25371tr C-109/13/89 F2
implies the true, but unknown, median difference between TCDD concentrationsobserved in 1987 and 1984 is highly likely to be contained in the interval( - 0.745, - 0.205) ppb. It is not unreasonable to believe the median changein TCDD concentration from 1987 to 1984 is as great as - 0.74 ppb or as littleas - 0.20 ppb.
The Hilcoxin test was used as a test for degradation over time. It can beconcluded that there is a significant difference between the concentration of .TCDD observed in 1984 and 1987 soil and sediment samples. The magnitude ofthis difference appears to be - 0.40 ppb. A test for dispersion or decreasing -TCDD concentration as distance of the site increases can be carried out if I""desired. iTi
(M0
Reference
1 . Hollander, M. and Wolfe, D. A . ( 1 9 7 3 ) . Nonparametric Statistical Methods.John Wiley and Sons, I n c . , Mew York.
ANA25371tr C-209/13/89 F2
STATISTICAL ANALYSIS OF FISH DATA FROM VERTAC
To assess the current levels of 2,3,7,8-TCDD toward degradation or dispersion,a statistical analysis of all available fish data was conducted. Fish areavailable fron sampling events held in 1979, 1980, 1981, 1984, and 1987.These data were collected from 14 locations. A listing of the data is shownin Table C-1. The statistical analysis Includes a test for trend over time ateach of the 14 locations and a test for overall spatial trend.
The test for trend over time at each location was carried out via the WilcoxinRank Sum Test or the Kruskal Wallis test. Both tests are nonparametric tests,i . e . , a test statistic is calculated based on the ranks of the TCDDconcentrations instead of the actual TCDD concentrations, ft nonparametricapproach was taken because the TCDD concentrations for a given year at a givenlocation generally did not follow a normal distribution.
The nonparamefcric tests named above test, for a given location, the nullhypothesis that the concentration of TCDD is the same for the different timeperiods observed against the alternative hypothesis that the concentration ofTCDD is not the same for the different time periods observed. The results ofthe test for each of the 14 sample locations are presented in Table C-2.Table C-2 shows that samples collected at the Bayou Meto at Highway 79 havedifferent concentrations over time. The test could not be carried out at the
following three locations: Largrue Bayou/Peckerwood Lakes, Benson Bridge, andHighway 1 1 . The remaining ten locations showed no change over time. Thelarge number of "no change" results could in part be caused by the smallamount of data collected during each time period.
The test for overall spatial trend was carried out using data collected in
1987. The Mann-Kendall test for trend was used to test the null hypothesisthat the concentrations of TCDD in fish remain constant as distance from thesite Increases versus the alternative hypothesis that the concentrations ofTCDD in fish decreases as distance from the site increases. The data used toperform this test are shown in Table C-3. These data present each locationalong with the average concentration of TCDD found in fish from the loca-tion. The average concentration considered all non-detect results as one-half
ANA2537STAT C-309/13/89 F2
Table C-1. Vertac Soil and Sediment Data Collected in 1984 and 1987
1987 SampleNumber
HH1247AHH1241AHH1246AHH1245AWH1245BWH1245CWH1228AWH1228CWH1229AWH1229BWH1230AWH1230BWH1235AWH1235BWH1235CWH1240AWH1240D
WH1242A
WH1226AWH1226CWH1237AWH1236AWH1236CHH1232AHH1233AHH1233CHH1232CHH1234AWH1224AWH1224C
ANA2537CA09/13/89 F2
1987 TCDDConcentration
(ppb)
0.45000.80001.20000.50000.60000.68000.49001.70000.53000.75000.85000.64000.34000.12000.33000.29000.0065
0.1800
0.09800.00460.97000.64000.85000.12000.22000.54000.52000.46000.12000.0110
" '- "' • •' ^
1987Qualifier
U
1984 SampleNumber
F006AF014AF046AF047AF047BF047C
F059CF060AF060BF061AF061BF063AF063BF063CF069A
F069XF071AF071X
F085CF104A
F105C
FS025C
FS040A
N026C
1984 TCDDConcentration
(Ppb)
0.740.742.003.501.102.10
1.301.101.520.540.780.811.201.100.53
0.880.311.10
1.581.70
1.50
1.08
0.90
3.01
n 9 ^ 7 Q ^
1984Qualifier
JJ
JJ
Difference1987 - 1984
(PPb)
-0.29000.0600
-0.8000-3.0000-0.5000-1.4200
0.4000-0.5700-0.77000.3100
-0.1400-0.4700-1.0800-0.7700-0.2400-0.2400
-0.1300
-1.5754-0.7300
-0.6500
-0.5400
-0.4400
-2.9990
Table C-1. (Continued)
1987 SampleNumber
HH1225AWH1225CWH1248AWH1248C
WH1258A
WH1254AWH1254D
WH1259AHH1259D
WH1253AWH1253G
WH1252AWH1252J
WH1260A
WH1267AWH1268EWH1267EWH1267FHH1269AWH1269G
WH1264AHm264EWH1265EWH1222ABCD
1987 TCDDConcentration
(DDb)
6.80001.30000.02200.0059
1.2000
0.41000.0061
1.50000.0100
1.3000.0290
1.10000.0150
1.8000
2.90001.50001.30001.70007.60001.9000
2.70000.80000.46000.0230
1987Qualifier
U
U
U
ll
19811 SampleNumber
N030CS002A
S002XS009AS009XS010A
S010XS011A
S011XS012A
S012XS013A
S013XS014AS014XS018A
S019A
S019XS020A
1984 TCDDConcentration
(DDb)
7.580.57
0.203.000.701.98
0.343.60
0.980.92
0.441.30
0.151.800.5137.90
16.20
2.086.50
1984Qualifier
U
UU
U-2.1000
UU
U
U
U
Difference1987 - 1984
(DDb)
-6.2800-0.2630
-1.8000
-0.5800
0.8400
-0.200
0.000
-35.000
-8.600
-3.800
ANA2537CA09/13/89 F2
0 2 5 7 9 7
Table C-1. (Continued)
1987 SampleNumber
HH1283AWH1279AWH1280AWH1287AHH1282AWH1281AHH1285AHH1286AWH1308AWH1300AWH1298AHH1309AWH1305AWH1313AHH1299AWH1304AWH1292AWH1312AHH1296AWH1297AWH1291AWH1290A
WH1301AWH1302A
1987 TCDDConcentration
(DDb)
0.86000.00490.09800.52000.04600.63000.33000.36000.02100.25000.14000.03601.03001.00000.18000.22000.21000.41000.00550.00340.00410.0610
0.06800.0570
1987Qualifier
UU
1984 SampleNumber
F010AF051AF052AF067AF064AF065AF067A
F013AF017AF018AF068AF070AF076AF078AF077AF102AF016AFS044
FS056
1984 TCDDConcentration
(DDb)
0.160.050.170.410.150.110.22
0.270.340.790.470.100.370.250.390.610.860.09
0.06
1984Qualifier
UU
U
UU
U
U
Difference1987 - 1984
(DDb)
0.700-0.020.0.0130.110
-0.1040.5750.110
-0.246-0.090-0.255-0.1990.9300.630
-0.070-0.170-0.370-0.450-0.042
ANA2537CA09/13/89 F2
0 2 5 7 9 8
Table C-2. Results of the Kruskal Wallis/Wilcoxin Rank Sum Test
Sample Location
Bayou Meto at the Cato Bridge
Rocky Branch confluence with Bayou Meto
Bayou Meto 2.5 miles below Rocky Branch
Bayou Meto at Highway 31
Bayou Meto at Highway 152
Bayou Meto at Wildlife Management Area
Bayou-Tleto at Highway 79
Lake Dupree
Bayou Meto at Highway 15
Lagrue Bayou/Peckerwood Lake
Highway 161
Highway 13
Benson Bridge
ANA2537CB09/12/89 F2
Sample Dates
19841987
19841987
19841987
19791980198119841987
1979198119841987
19841987
19791980198119841987
198019811987
19791987
1987
19791980
19791981
1981
Test Results
Accept Ho
Accept Ho
CT-'Accept Ho
1 ~Accept Ho I-T'.
CM0
Accept Ho
Accept Ho
Reject Ho
Accept Ho
Accept Ho
InsufficientData
Accept Ho
Accept Ho
InsufficientData
Table C-2. (Continued)
Sample Location___________________________Sample Dates Test Results
Highway 11 1979 Insufficient1980 Data1981
Accept Ho implies the null hypothesis is accepted, i . e . , there is no change over 0time. 0
rr-Reject Ho implies the null hypothesis is rejected at the a= .05 level of _'significance, i . e . , there is a change over time.
Insufficient data implies there is not sufficient data points to carry out the test.O
ANA2537CB09/12/89 F2
Table C-3. Data Used in Mann-Kendall Test for Trend
Sample Location Mean TCDD(ascending order from site)_______________Concentration in Fish (ppb)
Bayou Mefco at the Cato Bridge 0.400
Rocky Branch's confluence with Bayou Meto 0.500
Lake Dupree 0.709
Bayou Meto 2.5 miles below Rocky Branch 0.766
Bayou Meto at Highway 15 0.081
Bayou Meto at Highway 31 0.094
Bayou Meto at Highway 79 0.020
Bayou Meto at Highway 152 0.208
Bayou Meto at Wildlife Management Area 0.033
Lagrue Bayou/Peckerwood Lake 0.003
ANA2537CC09/13/89 F2
the detection limit. The results of the test show that the concentration of
TCDD in fish does decrease as distance from the site increases, i . e . , the nullhypothesis is rejected at the a = 0.05 level of significance.
References
Hollander, M. and Wolfe, D. A. (1973). Nonparametric Statistical Methods.John Wiley and Sons, Inc., Hew York.
Gilbert, Richard 0. (1973). Statistical Methods for Environmental PollutionMonitoring. Van Nostrand Reinhoid Company, Inc., New York.
ANA2537STAT C-409/13/89 F2
APPENDIX D
PROJECT DATABASE MANAGEMENT SYSTEM
ANA2537APD09/13/89 F2
PROJECT DATABASE MANAGEMENT SYSTEM
A Relational Database Management System (RDMS) was used as a sophisticated
means for organizing, storing, maintaining, calculating, combining, and
retrieving sample information for the Hercules/Vertac Off-Site study. Sample
and analytical data were entered into the system as soon as they were receivedand routinely screened for accuracy and status changes.
Several years of experience in environmental data management have helped IT
Corporation ( I T ) Field Analytical Services (FAS) to determine the set of• information necessary for compilation to allow flexible reporting capabilities
and evaluation of analytical results. The basic field sample information isinitially recorded on a sample or specimen collection log (see Appendix A ) .
The collection log form is designed to ensure that ail necessary field
information is appropriately recorded. This field log is then used to enter
the sample data into the computer so that the field information can be linkedto the analytical results as soon as they are available. The sample or
specimen collection log is considered generic and may contain slots that donot apply to every project; therefore, the collection log headings that are
applicable to the Hercules/Vertac Off-Site project are given and defined inTable D-1.
The data management work station consists of an IBM-compatible AT micro-
computer with fixed disk drives and associated peripherals. Data com-
munications is accomplished as needed through micro-computer modem link-ups
via normal telephone service lines.
The database developed for this project uses the ORACLE Relational DatabaseManagement System (RDBMS) spreadsheet. The ORACLE RDBMS has the ability to
store vast amounts of information in tables, while keeping records available
for instant use or update and can export data from work stations directly to
other computers running ORACLE software. Some of the other system capabili-ties include the use of forms for data entry/editing, ad-hoc report writing,
and formal report generation utilities. The system established for theHercules/Vertac Off-Site project allows the operator to create, modify, and
remove tables and views, add, delete, and update rows of data, construct
ANA2537APD D-109/13/89 F2
queries to select data from tables, and to build and modify reports. The
reports that have been created for this project reflect the most often needed
formats which generate the most information about the sample.
For improved space efficiency, abbreviations and codes are used in the data
reports; these along with other report definitions are listed in Table 0-2.
A data report is generated from the RDBMS by writing a query, which is arequest of the database for the specific data to be included in the report.
In the query, the conditions or criteria that the data must meet arespecified. Typically, specific conditions used for a Hercules/Vertac Off-Site
report are sample number range, project number, sample analysis request,
analysis complete or not, etc. From these conditions, the exact data are
gleaned from the database and captured in the query.
Also in the query, the columns of data are specified and placed in the orderthat the report will display them. In a Hercules/Vertac Off-Site report, the
primary key is the sample number. The column containing this information isusually listed first on all reports.
The sample number is used to link the two tables (Field Sample or Field
Specimen and Analytical Results) that contain the information entered into thedatabase. The field sample table contains the physical information about the
sample entered from the sample collection log, such as description/location,
time of collection, sample type, and analysis requested.
The second table or results table contains the analytical information. In
this table all analytical results are entered and stored to be linked with thedescription information for each sample in the query.
Columns are selected in the query to be displayed in the reports and are
selected from each of the two tables. The controlling factor that limits thenumber of columns is the printer width size. Most of the Hercules/Vertac Off-
Site reports use the full width of the wide printer capacity, since theinformation stored in the database for each sample is extensive.
ANA2537APD D-209/13/89 F2
Once the query has been defined, the report format is established. The reportformat is matched to the query by use of a common file name established at thebeginning of the query assembly.
In the report format, a title for the report is created. Other parameters
such as line and page size are also established. The report format is wheredecisions are made on how the data specified by the query are sorted. Commonsort characteristics used in the Hercules/Vertac Off-Site reports are as ,^5follows: 0
• Sort by sample number in numeric order• Sort by reference number, sample number• Sort by sample type, data collected• Sort by analysis requested, sample type.
Sorting is done primarily on three characteristics with a primarycharacteristic followed by secondary characteristics, each of which is asubset of the preceding sort request.
For very detailed reports, four or more sorts may be accomplished as long as
the last sort is a valid subset of all of the preceding sorts.
ANA2537APD D-309/13/89 F2
Lfi
(M0
Table D-1. Applicable Collection Log Headings and Definitions
I . SAMPLE COLLECTION LOG
Sample Number
A unique alpha numeric identification assigned to each sample at the timeof collection.
Date/Time
The date and time the sample was collected.
Sample Location/Description
Brief, but concise, comment to describe the location of sample collectionincluding a reference to a pertinent structure or position.
Purpose
State of remediation at the time the sample was collected.
GC
General characterization; samples collected as part of a generalassessment of the extent of possible contamination.
Sample Type
"
Air; air monitoring samples.
BU
Bulk; samples of a loose solid material.
CH
Chip; samples of a large or permanent fixture in which small portionswere removed or chipped off.
CO
Core; samples collected as a cross section and examined at intervals,other than soil or sediment.
LI
Liquid; any liquid sample that is not water or oil.
ANA2537D-105/15/90 F3
Table D-1. (Continued)
SE
Sediment; sample of material deposited by water.
SO
Soil; sample of soil.
WI ffl— 0Wipe; sampled by wiping a pre-determined area with a solvent soaked CCpad that will cause the components of interest to be absorbed by the LP;wiping medium, p i
WA • °
Water; sample of water.
Composite
Y
Yes; sample is made up of materials collected from more than onesample point and combined into one sample. ,'
No sample is composed of materials collected only from one samplepoint.
Sample Attitude
The direction the sample is collected.
°1
Horizontal.
02
Vertical.
OS
Both horizontal and vertical.
Elevation
Used for sediment samples as the depth of water below which the sample wastaken.
ANA2537D-105/15/90 F3
Table D-1. (Continued)
Depth of Take
Applicable to samples that are taken at specific depth below the surfacein cores and water.
Area or Volume Sampled
Amount of sample collected ( i . e . , total cm for wipe, total m3 for air,total volume in ml for liquid and soils/sediments).
QA/QC Code
QBL
Blank; a sample of material and container that have followed the samepath unopened or altered to show that there was no extraneouscontamination.
ODD
Duplicate; two separate samples for the purpose of determiningdegrees of variation of the sample area ( i . e . , the wipe sampling oftwo adjacent areas, two adjacent soil samples) in as nearly identicalconditions as possible.
~~ PRIG
Original sample of a QA/QC sample pair for comparison; such as withQDU samples.
QRI
An equipment rinsate; a sample collected by pouring solvent oversample collection equipment after cleaning; used to determine ifcross-contamination is occuring.
II. SPECIMEM COLLECTION LOG
Only those headings unique to the specimen log are listed; all other havethe same definition as in the sample log.
Specimen Type
The common name of the biological specimen ( i . e . , wood duck, whitecrappie, e t c . ) .
The genus and species as determined from a field identification guide.
ANA2537D-105/15/90 F3
Table D- 1 . (Continued)
Collection Method
A word or brief statement describing how the specimen was collected( i . e . , shotgun, electroshocking, gill net, e t c . )
Preservation Method
Method of preservation. Choices were wet ice and dry ice. 0
—————————————————————————————————————————————————————————————— CO
NOTE: Headings not defined are considered self-explanatory. IT)CM
0
ANA2537D-105/15/90 F3
Table D-2. Analytical Results Abbreviations, Codes, and Definitions
Result Sample Ho.
A unique alphanumeric identification assigned to each sample at the tine ofcollection.
Dioxin Units
Concentration units for dioxins, either isomer-specific or totals, such asng/m for wipes; ng/m3 for air; ng/sample for QC blank and ppb for bulks andsoils.
Q
Qualifiers.
U
Compound analyzed for but not detected, value given is the detectionlimit.
E
Compound exceeds calibration range of instrument.
D
Compound analyzed at a secondary dilution factor.
J
Compound detected but below the contract required detection limit. Thevalue given was an estimate.
Spiked compound used to determine the recovery of the analyte from thesample matrix.
B
Compound was found in method blank.
M
High detection limit for that compound due to interferences from thesample matrix, dilution was required to distinguish the compound ofinterest from the background interference.
ANA2537D-209/13/89 F2
Table D-2. (Continued)
2.3.7.8-TCDD
Concentration of the 2,3,7,8 isomer of tetra-chlorodibenzo-p-dioxin.
Tetra-CDD
Smn of concentrations of the tebrachlorodibenzo-p-dioxin isomers.
Pentra-CDD(M
Sum of concentration of the pentachlorodibenzo-p-dioxin isomers.LPt
Hexa-CDD CM0
Sum of concentration of the hexachlorodibenzo-p-dloxin isomers.
Hepta-CDD
Sum of concentration of the heptachlorodibenzo-p-dioxin isoraers.
Octa-CDD
Concentration of octachlorodibenzo-p-dioxin.
Toluene
Concentration of toluene.
2-Chlorophen
Concentration of 2-chlorophenoi.
4-Chlorophen
Concentration of 4-chlorophenol.
2.4-Dichlorophe
Concentration of 2,4-dichlorophenol.
2,6-Dichlorophe
Concentration of 2,6-dichlorophenoi.
2.3.6-Trichloroph
Concentration of 2,3,6-trichlorophenol.
ANA2537D-209/13/89 F2
Table D-2. (Continued)
2.4.5-Trichlot-oph
Concentration of 2,4,5-trichlorophenol.
2.4.6-Trichloroph
Concentration of 2,4,6-triehlorophenol.
2.4-D
Concentration of 2,4-dichlorophenoxy acetic acid. COin
2.4.5-T CM
Concentration of 2,4,5-trichlorophenoxy acetic acid.
2,4,5-TP
Concentration of 2,4,5-trlchlorophenoxy prioprionic acid.
MS/MSD
Matrix spike and matrix spike duplicate samples prepared and analyzed todetermine analytical accuracy and precision. -
ANA2537D-209/13/89 F2
APPENDIX E
ANALYTICAL QUALITY CONTROL SUMMARIES
ANA2537APE09/13/89 F2
This appendix contains, the Quality Assurance/Quality Control (QA/QC) summaries
for each batch of Vertac off-site samples analyzed by the IT-Special Analysis
Laboratory. These summaries and the corresponding tables were originally
reported in Volume I of each results data package released by the laboratory.
NOVEMBER 4. 1987 — BATCH REPORT
QC/QC
Table E-1 lists the results of the QA/QC samples. In all cases, precision and
accuracy are within the limits established for acceptance of dioxin/
dibenzofuran data.
DECEMBER 17. -1987 — BATCH REPORT
QA/QC
Tables E-2 and E-3 list the results of the QA/QC samples. Precision and
accuracy are within established EPA limits for 2,3,7,8-TCDD for all samples in
this report. IT Internal Qft limits were not met for the accuracy of higher
chlorinated congeners of one matrix spike duplicate pair, J4677. The PeCDD,
HxCDD, and HpCDD spike accuracies were out of limits (see Table E-3). Failure
to meet limits in this case is due to matrix effects in the higher
congeners. TCDD precision and accuracies for this pair are well within QA
limits. The other matrix spike duplicate pair, J4655R, however, is well
within QC limits for all congeners'indicating no procedural problems in the
laboratory.
Two problems were encountered with this analysis. The first problem was that
some of the laboratory blanks showed detectable amounts for dioxins.
Realizing that this is a problem, IT is currently investigating various means
to refine the procedures. However, due to the sensitivity of the HRMS
equipment, it will take some time to eliminate all sources of possible cross
contamination. With regards to the data, the majority of the positive samples
were 2 to 3 orders of magnitude higher than the blanks. This leads IT to
believe that these values are valid. The second problem encountered was with
spike accuracies for one of the matrix spike/matrix spike duplicate pairs
analyzed.
ANA2537APE E-109/13/89 F2
Due to the high octa d.ioxin levels encountered with the first samples of this
project, the calibration range was extended with the second initialcalibration from 500 pg/ul to 3,000 pg/ul.
The isomer-specific surrogate calibration for 10-27-87 is outside acceptable
IT QC limits of j;10 percent (-12 percent). IT feels that this error does not
affect the data for the following reasons: ( 1 ) this response factor deals
solely with the Cl surrogate compound; the native 2,3,7,8-TCDD RF was withinthe limits and ( 2 ) the reported value was only 2 percent outside the range
(this should not be a major problem especially since the acceptance window forthis RF is 30 percent of the totals analysis).
DECEMBER 29. 1987 — BATCH REPORTQA/QC
Tables E-4 through E-9 list the results of the QA/QC samples. Precision and
accuracy are within established U . S . Environmental Protection Agency ( E P A )
limits for 2,3,7,8-TCDD for all samples in this report. The total dioxin TCDD
spike recovery for sample J4800 was slightly high at 142 percent; however, noEPA limits have been established for total congeners.
During the analysis of these samples, two problems were encountered. The
first one is low-level positive results for some of IT'S laboratory blanks.This has been a recurring problem and has been discussed in previous
reports. In most cases, the blank is much lower than the sample; however,
this is not true in all cases. Since the levels in these other samples (and
corresponding blanks) are very low, IT does not feel this creates a majorproblem with the data. IT is currently trying new procedures to correct this
problem. The second problem was high spiked analyte recovery for sample J4800for HpCDD and OCDD.
In keeping with the unpredictable nature of biological samples, extremely high
spike, accuracies were seen for HpCDD and OCDD in J4800. IT believes that thisis a function of lack of sample homogeneity and selective absorption of spike
by biological tissues.
ANA2537APE E-209/13/89 F2
Several of the 259/322.ratios of native TCDD were above the normal acceptance
range. This problem is attributable to high sample load of biological
samples, which may have caused interferences to be slowly baked off the
instruments flight tube during the runs of samples and standards for thisproject. The lower molecular weight of 259 makes it prone to interferences.
Since 259 is used as a confirmation ion only and is not used in thecalculation of 2,3,7,8-TCDD, high ratios for 259/322 do not invalidate
results.
FEBRUARY 24. 1968 — BATCH REPORT
QA/QC
Tables E-7 through E-9 list the results of the QA/QC samples. Precision andaccuracy are within established EPA limits for 2,3,7,8-TCDD for all samples in
this report.
It is very difficult to obtain sample homogeneity with biological matrices andthis difficulty is reflected in the low spike recoveries obtained for sample
J4963 (Table E-7) for penta-octa-dioxin and the poor precision exhibited byheptadioxin.
Progress has been made on the problem of blank contamination. Although some
blanks are still positive for OCDD, the level is lower and other congeners arenow not detected. This is an imporvement over previously submitted work.
Several of the 259/322 ratios of native TCDD were above IT'S normal acceptance
range. This problem is attributable to high sample load of biological
samples, which may have caused interferences to be slowly baked off the
instrument's flight tube during the runs of samples and standards for thisproject. The lower molecular weight of 259 makes it prone to interferences.
Since 259 is used as a confirmation ion only and is not used in thecalculation of 2,3,7,8-TCDD, high ratios for 259/322 do not invalidate
results.
ANA2537APE E-309/13/89 F2
APRIL 4, 1988 — BATCH REPORT
QA/QC
Tables 10 and 11 list the results of the QA/QC samples. Precision and
accuracy are within established EPA limits for 2,3,7,8-TCDD for all samples inthis report.
The 259/322 ratio was high (above IT established acceptance range) for several
samples and standards in this project. The 259 mass is lower than other 03masses monitored making it prone to interferences. (Jo calculations on —
congeners are made using 259. It is used as a confirmation ion only. c0
inCM
High spike accuracy for the higher chlorinated congeners on the BB0153 matrix Qspike duplicate pair is attributable to the difficulty in obtaining sample
homogeneity with biological samples.
JUNE 10. 1988 — BATCH REPORT
QA/QC
Table 12 lists the surrogate results for this analysis. In all cases,surrogate accuracy is within the limits established for acceptance of dioxin
data.-
ANA2537APE E-409/13/89 F2
Table E-1. QA/QC Report Vertac Off-Site 2,2,7,8-TCDDNovember 4, 1987
Surrogate Percent Accuracy
Number of Data Points = 36
Mean Percent Accuracy = 112?
Range: 86 - 1 1 9 ) 6
EPA Range ^ 60-140)1
Precision of Duplicates
Spike Value ( b ) =
Spike Dup. Value ( a ) =
Precision = a-b x 100 % =a+b2
EPA Range = t 50;
Accuracy of Spike
Orig. Value ( a ) =
Observed Spike Value ( b ) =
Spike Level ( c ) =
bAccuracy = a+c x 100? ^
EPA Range == 60-140?
Soil WH1222ABCD Soil WH1235AJ4611 J1630
0.093 0.'48
0.10 0.46
7.2 % -4.2!(
J4611 J4630
ND 0.34
0.093 0.48
0.10 0.10
93% 109?
ANA2537APE109/13/89 F2
Table E-2. QA/QC Report Vertac Off-SiteDecember 17, 1987
Surrogate Percent Accuracy for 2 , 3 , 7 , 8 -
Number of Data Points = 50
Mean Percent Accuracy = 109?
Range = 79 - 120?
EPA Range = 60-140?
Precision of Duplicates
Spike Value ( b ) =
Spike Dup. Value ( a ) =
a-bPrecision = a+b x 100)1 s
2
-EPA Range = j: 50?
Accuracy of Spike
Orig. Value ( a ) ==
Observed Spike Value ( b ) .s
Spike Level ( c ) s
Accuracy = b x 100% :a+c
EPA Range = 60-1 to;
o EPA Range has been established foro EPA Range has been established for
ANA2537APE209/13/89 F2
-TCDD
Sample Mo
2 , 3 , 7 , 8 -TCDD
0.37
0.42
13»
a
2 , 3 , 7 , 8 -TCDD
0.29
0.37
0.10
95?
b
these analytes. ITthese analytes. IT
. J4655R
TCDD
0.64
0.82
25?
a
TCDD
0.55
0.64
0.10
98?
b
Sedinif
PeCDD
0.18
0.20
10?
a
PeCDD
0.079
0.18
0.10
100?
b
QA/QCQA/QC
'nt WH1240A
HxCDD
0.15
0.14
- 6 . 9 ?
a
HxCDD
0.044
0.15
0.10
104?
b
limits + 50?limits 60-140?
HpCDD
0.23
0.23
0.0?
a
HpCDD
0.12
0.23
0.10
104?
b
0CMCOIP,
CM0
OCDD
2.3
2.2
-4.4?,
a
OCDD
2.0
2.3
0.10
110?
b
Table E-3. QA/QC Report Vertac Off-SiteDecember 17, 1987
Surrogate Percent Accuracy for 2,3
Number of Data Points = 50
Mean Percent Accuracy = 103)1
Range == 89-114?
EPA Range = 60-140?
Precision of Duplicates
Spike Value ( b ) =
Spike Dup. Value ( a ) =
a-bPrecision = a+b x 100; =
2
-EPA Range ; 50?
Accuracy of Spike
Orig. Value ( a ) =
Observed Spike Value ( b ) ;
Spike Level ( c ) =
Accuracy = b x 100? =a+c
EPA Range : 60-140?
^See QA/QC section of report for a''No EPA Range has been established"No EPA Range has been established
ANA2537APE309/13/89 F2
,7,8-TCDD
Sample Mo
2 , 3 , 7 , 8 -TCDD
0.10
0 . 1 1
9 . 5 ?
b
2 , 3 , 7 , 8 -TCDD
ND
0.10
0.10
100?
c
discussion of these valifor these analytes. ITfor these analytes. IT
. J4677 ;
TCDD
0.093
0.094
1 . 1 ?
b
TCDD
ND
0.093
0.10
93?
c
Sedlrnei
PeCDD
ND
HD
a
b
PeCDD
ND
ND
0.10
a
c
ies.QA/QCQA/QC
it HH12591
HxCDD
ND
ND
a
b
HxCDD
0.019
ND
0.10
a
c
limits + 50?limits 60-140?
3
HpCDD
0.055
0.055
O.O?
b
HpCDD
0.065
0.055
0.10
33?'1
c
T—
CM.-"Y';
U"'!
CM0
PC DP
8.3
8.2
-1.2?,
b
OCDD
8.8
8.3
0.10
93?
c
Table E-4. QA/QC Report Vertac Off-Site - December 29, 1987
Surrogate Percent Accuracy for 2,3,7,8
Number of Data Points ; 59
Mean Percent Accuracy =; 107?
Range = 87-138
EPA Range = 60-140
Precision of Duplicates
Spike Value (b) =
Spike Dup. Value (a ) =
Precision - a-b x 100)1 =a+b2
EPA Range = ^50%
Accuracy of Spike
Orlg. Value (a) =
Observed Spike Value (b ) =
ANA2537APE409/13/89 F2
-TCDD
%
%
2,3,7,8-TCDD
0.11
0.10
-9.5?
a
2,3,7,8-TCDD
0.0049
0.11
Sample H(
TCDD
0.095
0.098
3.1?
a
TCDD
ND
0.095
'.. .
i. J4764 Sol
PeCDD
0.098
0.095
-3.1?i
a
PeCDD
0.0028
0.098
0 2
1 WH1279A
HxCDD
0.11
0.10
-9.5?
a
HxCDD
ND
0.11
5 8 2 2
HpCDD
0.15
0.16
6.4
a
HpCDD
0.054
0.15
OCDD
1.2
0.93
-25il
a
OCDD
1.0
1.2
Table E-4. (Continued)
Precision of Duplicates
Spike Level ( c ) =
Accuracy = b x 100)1 =a+c
EPA Range = 60-110?
2,3,7,8-TCDD TCDD PeCDD HxCDD HpCDD OCDD
0 .10 0.10 0 . 1 0 0 .10 0 .10 0 . 1 0
105? 95)6 95)1 1 1 0 ? 97? 109)1
b b b b b b
''No EPA Range has been established for these analytes. IT QA/QC limits j:505i."No EPA Range has been established for these analytes. IT QA/QC limits 60-110?.
ANA2537APE109/13/89 F2
0 2 5 8 2 3
Table E-5. OA/QC Report Vertac Off-Site - December 29, 1987
Surrogate Percent Accuracy for Total D
Number of Data Points = 59
Mean Percent Accuracy = 105?
Range = 97-105
EPA Range = 60-110
Precision of Duplicates
Spike Value (b ) =
Spike Dup. Value (a) =
Precision - a-b x 10051 ;a+b
2
EPA Range = ^50%
Accuracy of Spike
Orig. Value (a) ==
Observed Spike Value (b) =
ANA2537APE509/13/89 F2
•ltoxins
%
%
2,3,7,8-TCDD
0.16
0.16
0.0;
a
2,3,7,8-TCDD
0.14
0.16
Sample
TCDD
0.19
0.22
15!l
a
TCDD
0.15
0.19
No. J4783 Se
PeCDD
0.13
0.13
0.0%
a
FeCDD
. 0.020
0.13
0 2
diment WH1278A
HxCDD
0.14
0.14
O.O?
a
HxCDD
0.027
0.14
?8 2 4
HpCDD
0.23
0.20
-14?
a
HpCDD
0.23
0.23
OCDD
1.9
1.5
-24?
a
OCDD
1.7
1.9
Table E-5. (Continued)
Precision of Duplicates
Spike Level (c) ;
Accuracy = b x 100)( =a+c
EPA Range = 60-110;
2,3,7,8-TCDD TCDD PeCDD HxCDD HpCDD OCDD
0 . 1 0 0 . 1 0 0 . 1 0 0 . 1 0 0 .10 0 . 1 0
67» 76? 108)1 110 )1 10% 106)1
b b b b b b
^No EPA Range has been established for these analytes. IT QA/QC limits ;50;."No EPA Range has been established for these analytes, IT QA/QC limits 60-140%.
ANA2537APE509/13/89 F2
0 2 5 8 2 5
Table E-6. QA/QC Report Vertac Off-Site - December 29 , 1987
Precision of Duplicates
Spike Value (b ) =
Spike Dup. Value (a) =
Precision - a-b x \00% =a+b
2
EPA Range == 4:50)1
Accuracy of Spike
Orig. Value ( a ) =
Observed Spike Value ( b ) =
Spike Level ( c ) ;
Accuracy = b x 100)1 =a+c
EPA Range = 60-140)1
Sample N
TCDD
0.057
0.0111
-33?
a
TCDD
ND
0.057
0.040
142)1
c
o. J4800 Wooc
PeCDD
0.046
0.01)3
-6.7?
a
PeCDD
ND
0.046
0.040
115)1
c
i Duck WH1014R
HxCDD
0.062
0.051
-19?
a
HxCDD
0.0052
0.062
0.040
w
c
HpCDD
0.34
0.043
-155)l@
a
HpCDD
0.0061
0.34
0.040
738?1'
c
OCDD
2.4
• 0.087
-186%
a
OCDD
0.044
2.4
0.040
2860?b
c
''No EPA Range has been established for these analytes. IT QA/QC limits ^50;.See QA/QC section of report for a discussion of these values.
^o EPA Range has been established for these analytes. IT QA/QC limits 60-140)1.
ANA2537APE609/13/89 F2
0 2 5 8 2 6
Table E-7. QA/QC Report Vertac Off-Site - February 24, 1988
Surrogate Percent Accuracy for 2,3,7,8
Number of Data Points = 112
Mean Percent Accuracy = 111)(
Range == 96-133
EPA Range =: 60-140
Precision of Duplicates
Spike Value (b ) =
Spike Diip. Value ( a ) =:
Precision - a-b x 100? =a+b
2
EPA Range = i50%
Accuracy of Spike
Ofig. Value (a) =
Observed Spike Value ( b ) =
ANA2537APE709/13/89 F2
-TCDD
%
%
2,3,7,8-TCDD
0.15
0.14
-6.9?
b
2,3,7,8-TCDD
0.021
0.15
Sample Nc
TCDD
0.12
0.13
8.0?
b
TCDD
0.076
0.12
I, '•
?. J1963 Wh
PeCDD
0.11
0.14
Ml,
b
PeCDD
0.098
0.1 1
0 2
ole Fish WH1154
HxCDD
0.12
0.16
28?
b
HxCDD
0.15
0.12
5 8 2 7
HpCDD
0.15
0.26
54^
b
HpCDD
0.23
0.15
OCDD
0.81
0.84
3.6?
b
OCDD
2.6
0.81
Table E-7. (Continued)
Accuracy of Spike
Spike Level (c) =
Accuracy = b x W0% =a+c
EPA Range := 60-140?
2,3,7,8-TCDD TCDD PeCDD HxCDD HpCDD QCDD
0.10 0.10 0.10 0.10 0.10 0.10
124)1 66% 5651'1 48^ 45^a SO?3
)
C 0 C C C C
outside IT established QA/QC limits. See QA/QC section of report for discussion."No EPA Range has been established for these analytes. IT QA/QC limits i_50%."No EPA Range has been established for these analytes. IT QA/QC limits 60-140;l.
)
ANA2537APE709/13/89 F2
•
0 2 5 8 2 8
Table E-8. QA/QC Report Vertac OfP-Site - February 21, 1988
Precision of Duplicates
Spike Value ( b ) =
Spike Dup. Value (a) =
Precision - a-b x 100; :a+b
2
EPA Range = <;50?
Accuracy of Spike
Orig. Value (a) =
Observed Spike Value (b ) =
Spike Level (c) =
Accuracy = b x 100% =a+c
EPA Range = 60-110?
2,3,7,8-TCDD
0.18
0.18
0%
a
2,3,7,8-TCDD
0.033
0.18
0.10
135?
b
Sample
TCDD
0.15
0.14
-6.9?
a
TCDD
0.031
0.15
0.10
111?
b
No. JW1 Who
PeCDD
0.11
0.12
8.7?
a
PeCDD
ND
0.11
0.10
110?
b
Ie Fish WH118
HxCDD
0.12
0.13
8.0)1
a
HxCDD
ND
0.12
0.10
120?
b
1
HpCDD
0.11
0.11
0?
a
HpCDD
0.012
0.11
0.10
125?
b
OCDD
0.19 ")
0.19
0?
a
OCDD
0.077
0.19 ^
0.10
107?
b
o EPA Range has been established for these analytes."No EPA Range has been established for these analytes.
IT QA/QC limits ±50?.IT QA/QC limits 60-110?.
ANA2537APE809/13/89 F2
0 2 5 8 2 9
Table E-9. OA/QC Report Vertac Off-Site - February 21), 1988
Precision of Duplicates
Spike Value (b) -:
Spike Dup . Value (a) =
Precision - a-b x 100? =a+b
2
EPA Range =: +50)1
Accuracy of Spike
Orig. Value (a) =
Observed Spike Value (b) =
Spike Level (c) =
Accuracy ^ b x 100? =a+c
EPA Range : 60-140?
2,3,7,8-TCDD
0.11
0.11
0%
a
2,3,7,8-TCDD
0.0018
0. 11
0. 10
105?
b
Sample
TCDD
0.11
0.12
8.7?
a
TCDD
0.0043
0.11
0,10
105?
b
No. J4980 Who
PeCDD
0.12
0.13
8.0?
a
PeCDD
ND
0.12
0.10
120?
b
Ie Fish HH119
HxCDD
0.13
0.13
0%
a
HxCDD
ND
0.13
0.10
130?
b
3
HpCDD
0.13
0.14
7.4?
a
HpCDD
ND
0.13
0. 10
130?
b
OCDD
0.14
0. 15
6.9?
a
OCDD
0.039
0.14
0.10
101?
b
No EPA Range has been established for these analytes.No EPA Range has been established for these analytes.
IT QA/QC limits ^50?.IT QA/QC limits 60-140?.
ANA2537APE909/13/89 F2
0 2 5 8 3 0
Table E-10. QA/QC Report Vertac Off-Site - April 4 , 1988
Surrogate Percent Accuracy
Number of Data Points ; 58
Mean Percent Accuracy ^ 116?
Range == 96-139?
EPA Range ; 60-140?
Precision of Duplicates
Spike Value ( b ) =
Spike Dup. Value ( a ) =
Precision - a-b x 100? =a+b
2
EPA Range = ^,0%
Accuracy of Spike
Orig. Value (a) =
Observed Spike Value ( b ) =
ANA2537APE1009/13/89 F2
2,3,7,8-TCDD
0.014
0.041
7.0?
a
2,3,7,8-TCDD
0.0023
0.014
Sample
TCDD
0.018
0.038
23?
a
TCDD
0.0039
0.048
Mo. BB0099 1
PeCDD
0.048
0.040
w
a
PeCDD
0.0018
0.048
0 2
food Duck HH134
HxCDD
0.052
0.041
24?
a
HxCDD
0.0042
0.052
5 8 3 1
8
HpCDD
0.054
0.050
7.7?
a
HpCDD
0.0048
0.054
OCDD
0.081
0.068
17?
a
OCDD
0.029
0.081
Table E-10. (Continued)
Accuracy of Spike
Spike Level (c) =
Accuracy = b x 100? =a+c
EPA Range =: 60-140?
2,3,7,8-TCDD TCDD PeCDD HxCDD HpCDD OCDD
0.040 O.OfO 0.040 0.040 0.040 0.040
96? 109? 115!l 118? 120? 189?
^b b b b b b
^Mo EPA Range has been established for these analytes. IT QA/QC limits -^0%."No EPA Range has been established for these analytes. IT QA/QC limits 60-140?.
ANA2537APE1009/13/89 F2
0 2 5 8 5 2
Table E-11. QA/QC Report Vertac Off-Site - April 1 , 1988
Precision of Duplicates
Spike Value (b) =
Spike Dup. Value (a) ;
Precision - a-b x 100? =a+b
2
EPA Range == ^50?
Accuracy of Spike
Orig. Value (a) =
Observed Spike Value (b) =
Spike Level (c) ;
Accuracy = b x 100)1 =a+c
EPA Range ; 60-110;
ii
2,3,7,8-TCDD
0.82
1.1
29?
a
2,3,7,8-TCDD
0.7fi
0.82
0.10
93!
c
Sample
TCDD
0.80
1.1
32?
a
TCDD
0.73
0.80
0.10
96?
c
No. BB0153 Fi
PeCDD
0.18
0.19
6.1?
a
PeCDD
0.011
0.18
0.10
158?11
c
sh Composite:
HxCDD
0.18
0.18
0%
a
HxCDD
ND
0.18
0.10
180?1'
c
WH1086, WH1
HpCDD
0.18
0.20
10?
a
HpCDD
ND
0.18
0.10
^O?13
c
087, WH1088
OCDD
0.18
0.21
15?
a
OCDD
0.021
0.18
0.10
119?''
c
^o EPA Range has been established for these analytes. IT QA/QC limits ^50?."Outside IT established QA/QC limits. See discussion in QA/QC section of report.''No EPA Range has been established for these analytes. IT QA/OC limits 60-140)1.
ANA2537APE1109/13/89 F2
0 2 5 8 3 5
Table E-12.. QA/QC Report Vertac Off-Site - June 10, 1988
I somerSpecific Totals
Surrogate Percent Accuracy
Number of Data Points =
Mean Percent Accuracy =
Range =
EPA Range = 60-140?
10 2
105? 99»• t"
98-113? 95-103? ^•CO
s-n04
—————————————————— 0
ANA2537APE1209/13/89 F2
APPENDIX F
PRIORITY POLLUTANT ANALYSIS CASE NARRATIVE
ANA2537AFF05/15/90 F3
October 30, 1987
Dana SimerlyIT Corporation9041 Executive Park DriveKnoxville, TN 37923
Case Narrative
ITfiS Project Code: ITFK 40036Purchase Order Number: 480030Case Maine: Hercules/Vertac
Enclosures
Enclosed are the data for ITAS Project Code ITFK 40036. Table 1 lists field ®and ITAS sample numbers, sample matrix, sample concentration (for soil samples ®only), and analysis requested. |Q
COSample Receipt QQ
10The samples were received in one shipment on September 24, 1987. The shipment ^contained 3 water samples, 19 sediment samples, and 38 archived sediment Qsamples in good condition.
GC/MS Analysis
The volatiles analyses were performed on 9/30/87 through 10/5/87 and 11/3/87by purge and trap with packed SP-1000 column on two Finnigan OWA GC/MS/DSsystems.
The semivolatlles analyses were performed on 10/9/87, 10/13/87, 10/14/87,10/15/87, and 11/3/87 by direct injection of sample extract on a J&W DB-5capillary column on a Finnigan 4000 GC/MS/DS.
The analyses followed EPA Contract Laboratory Program (CLP) revision 7/87protocol. Please note that all CLP Target Compound List (TCL) parameters arereported since the raw data for such are provided in the data package. In thevolatiles analyses, the following problems and situations occurred. The watersamples were originally run on a short program that omitted styrene andxylene. Reruns for these compounds were made on 10/5/87, one day beyond theprotocol holding time. There is little technical rationale to believe thisdelay would have any impact on the results for these higher boiling species.Both sets of run data are submitted. The soil samples offered difficultiesthrough evident matrix effects, probably related to the high hydrocarbon
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Page 2October 20, 1987
background. It became apparent that direct 5 gram/5 ml purging would resultin anaiytes exceeding the calibration range, nonconformant surrogaterecoveries, and chromatographic distortion in some cases. Therefore, afterseveral test runs, some reasonable low level dilutions (as much as five-fold)were submitted as primary sample runs. Secondary dilutions by medium levelprep were required for some samples, and in accordance with CLP protocol, aseparate specific initial standard calibration, daily standard, and blank wererun for these samples. Due to the number of runs required and the nearness ofthe holding time, the sample extract for the matrix spike and duplicate(medium level) was set aside and refrigerated for analysis at a later date(11/3/87) at which time it was shaken to homogenize and rapidly split intoaliquots for spiking. To indicate the validity of the sample storage, theunspiked sample extract was also rerun at this time to compare with theoriginal run on 10/4/87. The matrix spike and duplicate demonstrated analyterecoveries within Units; however, some surrogate recoveries were slightlylow. We immediately point out that this was most probably due to the(effective) dilution of the extract at the homogenization stage, where a smallvolume of the extract was replaced by soil particles. The sample runs on11/3/87 were based on a specific medium level standard; the initialcalibration and blank were not specific as such. Specific medium level runscontain 100 pi of methanol, other varying amounts. In the experience of thislab, there is no discernable difference in response between the two.
The semivolatiles analyses proceeded with few problems. It was noted thatsome internal standard areas fell below 50 percent of the daily standard insome samples. This was recognized as not due to any instrumental malfunction,but to injection technique. This occurrence, in our experience, would havenegligible effect on data validity, as all peaks, internal standard orotherwise, would be affected similarly. Nevertheless, certain samples wereselected for rerunning on 11/3/87 for comparison. Both sets of data areincluded. We note that especially in the volatiles analyses, there werevarious "test" runs that were marginally noncompliant for reasons indicatedearlier, and these data were not submitted.
Some points on specific samples:
Volatiles:
Sample Situation Effect on Data
WH1252A-P 1 surrogate out, Negligible. He have seen linearityacetone > 200 ppb (230) to 500 ppb. (See 10/29 standards).
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Page 3October 30, 1987
GC/MS Analysis (continued)
Volatiles:
Sample Situation
W1253A-P 2 surrogates out
WH1264A-P 2 surrogates out
Internal standard out,1 surrogate out
WH1267A-P
1 surrogate out
CCC chloroform out
WH1269G-P
11/3/87Standard
Semivolatiles:
Effect on Data
Matrix effect. Sample was rerunwith same results.
Negligible. Sample was rerun, but1 day past holding time. Mediumprep - see above.
Small matrix effect. Sample wasrerun 1 day past holding time.
Matrix effect. Sample was rerun.
Negligible. Analyte not seen.
WH1254A-PWH1254-D-P.MSWH1254D-P,MSDWH1264A-PWH1264E-PSBLK 1965WH1253A-P,MSDWH1269A-P,MSD
11221221
internalinternalinternalinternalinternalinternalinternalinternal
standardstandardstandardsstandardsstandardstandardsstandardsstandard
lowlow
lowlow
lowlowlow
low
Negligible.None. Original sample was O . K .None. Original sample was O . K .None. Sample rerun.Negligible.None. Blank rerun.None. Sample rerun.None. Original samples was O . K .
He have endeavored to point out every noncompliance and/or discrepancyencountered in the analysis. To our knowledge, except where noted above, allCLP criteria were met.
Data were reported with qualifiers as follows:
U - Compound analyzed for but not detected.E - Compound exceeds calibration range of instrument.D - Compound analyzed at a secondary dilution factor.
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Page 4October 30, 1987
J - Compound detected but below the contract required detection limit. Thevalue given was an estimate.
S - Spiked compound.B - Compound was found in method blank.
GC Analysis
CLP protocol does not include criteria for herbicide analysis, so the CLPprotocol for pesticides was approximated for data reporting and packaging.Samples were analyzed for phenoxyacetic acid herbicides in accordance with ITAnalytical Services (ITAS) Standard Operating Procedure No. GC860523RO, withmodifications in the run sequence to more closely approximate the CLPmethod. References for this method are attached. The reporting format was amodification of the 10/86 EPA Contract Laboratory Program Statement of Workfor Organics Analysis.
The designation 0V refers to a column of the type 3 percent OV-1.
The designation Mixed Phase refers to a column type with the packing material1.5 percent SP2250/1.95 percent SP2401.
Both 'retention time windows and detection limits for the compounds of interestwere determined before samples were analyzed. These were analyzed over a 24-hour period with the instrument calibration being repeated every 24-hours.Linearity was determined at the start of each 24-hour period of analysis, withcheck standard analyzed every 10 samples. Solvent checks or blanks were runalternately with the standards, providing a standard or blank run for at leastevery five samples.
The retention time windows determined were extremely tight, so the allowancein the contract for 1 percent window width was used. This window was based onthe first standard which ran each day for the initial series of samples. Itwas found necessary to modify the protocol to allow retention time windows tobe updated as the run progressed. That is, retention time windows for eachgroup of five samples were based on the standard immediately preceding them.
The response factors were not update during the run as were the retentiontimes. The response factors were very stable and when there was a changeduring the run above 15 percent, the run was terminated and a new calibrationwas run.
Samples were analyzed on both a Mixed Phase and an OV-1 column. Reportedpositive values had peaks within the retention time windows and above thedetection limits on both columns.
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Page 5October 30, 1987
Those results with a " U " In the qualifier column are below the reporting limitand can be considered negative for that compound.
Results that have an "S" in the qualifier column are spiked compounds used todetermine the recovery of the analyte from the sample matrix.
Those results which are reported with the qualifier " M " have a high detectionlimit for that compound due to interferences from the sample matrix. Thesesamples required analysis at a dilution to distinguish the compound ofinterest from the background interference.
All results for the soil samples were corrected for percent moisture.
References O———— cr»( 1 ) "Methods for Organochlorine Pesticides and Chlorophenoxy Acid Herbicides ®
in Drinking Water and Raw Source Water", U.S. Environmental Protection lr^Agency, Environmental Monitoring and Support Laboratory, Cincinnati, vt
Ohio, July 1978.
( 2 ) -"Methods for Organic Pesticides in Water and Wastewater", 19 7 1 , U . S .Environmental Protection Agency, National Environmental Research Center,Cincinnati, Ohio 45268.
( 3 ) "Handbook for Analytical Quality Control in Water and HastewaterLaboratories", 1972, U . S . Environmental Protection Agency, NationalEnvironmental Research Center, Analytical Quality Control Laboratory,Cincinnati, Ohio 45268.
( 4 ) Metcalf, L. D. and Schmitz, A . A . , "The Rapid Preparation of Fatty AcidEsters for Gas Chromatographic Analysis", Analytical Chemistry. 33, 363,1 9 6 1 .
( 5 ) Schlenk, H. and Gellerman, J. L . , "Esterification of Fatty Acids withDiazomethane on a Small Scale", Analytical Chemistry, 32, 1412, 1960.
( 6 ) "Pesticide Analytical Manual", U . S . Department of Health, Education andWelfare, Food and Drug Administration, Washington, D . C .
ANA2537APF F-509/13/89 F2