United States
Environmental Protection
Agency
Office of Air Quality
Planning and Standards
Research Triangle Park, NC 27711
EMB Report 85-FPE-04
July 1986
Air
Hazardous Waste
Treatment, Storage, and
Disposal Facilities

Site-Specific Test Report
Texaco Refining
and Marketing Company
Delaware City, Delaware

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           SITE-SPECIFIC TEST REPORT

      TEXACO REFINING AND MARKETING, INC.
            DELAWARE CITY, DELAWARE

                  ESED 85/12
                  EMB 85FPE04
                 Prepared by:

        Entropy Environmentalists, Inc.
             Post Office Box 12291
Research Triangle Park, North Carolina   27709

    Contract No. 68-02-3852 and 68-02-4336
     Work Assignment No. 3024 and No. 3501
               EPA Task Manager
                Clyde E. Riley
     U. S.  ENVIRONMENTAL PROTECTION AGENCY
          EMISSION MEASUREMENT BRANCH
 EMISSIONS STANDARDS AND ENGINEERING DIVISION
 RESEARCH TRIANGLE PARK, NORTH CAROLINA  27711
                   July 1986

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                                   DISCLAIMER
    This document has been reviewed by the Emission Standards and Engineering
Division, Office of Air Quality Planning and Standards, Office of Air, Noise
and Radiation, Environmental Protection Agency, and approved for publication.
Mention of company or product names does not constitute endorsement by EPA.
Copies are available free of charge to Federal employees, current contractors
and grantees, and nonprofit organizations - as supplies permit - from the
Library Services Office, MD-35. Environmental Protection Agency, Research
Triangle Park, NC 27711.

Order:  EMB Report 85-FPE-04
                                       11

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                                   CONTENTS

                                                                       Page

 Figures                                                                 v

 Tables                                                                 vi

 1.0  INTRODUCTION                                                      1-1

 2.0  SUMMARY AND DISCUSSION OF RESULTS                                 2-1
      2.1  Background Samples                                           2-4
      2.2  Land Treatment Unit, Cell #4 (Process L)                      2-10
      2.3  Land Treatment Unit, Cell #8 (Process N)                      2-12
      2.4  Land Treatment Unit, Cell #3 (Process 0)                      2-13
      2.5  Unpaved Roads in Land Treatment Unit (Process M)              2-14
      2.6  Repeatability and Reproducibility                            2-16
      2.7  Conclusions                                                  2-18

 3.0  PROCESS DESCRIPTION                                               3-1
      3.1  Land Treatment Cells                                         3-1
      3-2  Unpaved Roadways                                             3~3

 4.0  SAMPLING AND ANALYSIS                                             4-1
      4.1  Site Plot Plan                                               4-1
      4.2  Land Treatment Unit, Cell #4 (Process L)                      4-2
      4.3  Land Treatment Unit, Cell #8 (Process N)                      4-11
      4.4  Land Treatment Unit, Cell #3 (Process 0)                      4-15
      4.5  Unpaved Roads in Land Treatment Unit (Process M)              4-18
      4.6  Repeatability, Reproducibility, and Performance
            Audit Samples                                               4-20
      4.7  Background Samples                                           4-21

5.0  QUALITY ASSURANCE                                                  5-1
                                     111

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                             CONTENTS (continued)

APPENDICES                                                             Page
  A  RAW FIELD DATA AND SAMPLING LOGS                                   A-l
      Process Data Sheets and Sampling Grid Sketches                    A-3
      Repeatability, Reproducibility, and Quality Assurance Samples     A-9
      Chain of Custody Forms                                            A-10
  B  ANALYTICAL DATA                                                    B-l
      EMB Split Sample Inventory                                        B-3
      Moisture Determination Data Sheets                                B-6
      Screening Data Sheets                                             B-43
      Percent PM1(-, Determination Data Sheets                            6-98
      Metals Analysis Results                                           B-110
      Organic Cleanup Data Sheet                                        B-118
      Organics Analysis Results                                         B-119
      Quality Assurance Data                                            B-135
      Oil and Grease Analysis Results                                   B-137
     SAMPLING AND ANALYTICAL PROCEDURES                                 C-l
      Sampling Apparatus                                                C-3
      Sampling Location Selection and Documentation                     C-8
      Sample Collection                                                 C-ll
      Sample Handling and Transport                                     C-14
      Drying and Sieving Procedures                                     C-16
      Chemical Analyses                                                 C-19
      Quality Assurance (QA) Procedures                                 C-25
  D  SAMPLING PROGRAM PARTICIPANTS AND OBSERVERS                        D-l
     PROCESS OPERATIONS DATA                                            E-l
      Summary of Processes Sampled During Site Survey                   E-3
      Summary of Equipment for Processes Sampled During Site Survey     E-4
                                       IV

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                                   FIGURES

Number                                                               Page

 4.la  Site plot plan of Texaco in Delaware City.                     4-3

 4.Ib  Enlargement of site plot plan showing locations of land
       treatment cells and sampling locations for background
       and unpaved road samples.                                      4-5

 4.2   Sampling grid, process dimensions, and sample numbers
       for land treatment unit, Cell #4 at Texaco, Delaware City
       (Process L).                                                    4-6
                                                 i     }
 4.3   Sampling grid, process dimensions, and sample numbers
       for land treatment unit, Cell #8 at Texaco, Delaware City
       (Process N).                                                    4-13

 4.4   Sampling grid, process dimensions, and sample numbers for
       land treatment unit, Cell #3 at Texaco, Delaware City
       (Process 0).                                                    4-16

 4.5   Dimensions and sample numbers for the segments of unpaved
       roads sampled in the land treatment unit at Texaco
       (Process M).                                                    4-19

 C.I   Example process grid.                                          C-10

 C.2   Label used for sample jars.                                    C-12

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                                  TABLES

Number                                                               Page

 2.1    Sampling Plan for Texaco                                      2-3

 2.2    Analytical Results of Silt Screening, Weight Loss on
          Drying, and PMin Sieving, Fugitive Particulate from
          TSDF (85/12), Texaco, Delaware City, DE                     2-5

 2.3    Analytical Results for Metals and Semivolatile Organics,
          Fugitive Particulate from TSDF (85/12)                      2-8

 2.4    Summary of Oil and Grease Analysis, Fugitive Particulate
          from TSDF (85/12)                                           2-11

 2.5    Analytical Results for Repeatability and Reproducibility
          Samples, Metals, Fugitive Particulate from TSDF (85/12)     2-17

 4.1    Sample Drying Procedure Summary                               4-9

 4.2    Metals, Measurement Methods, and Detection Limits             4-10

 4.3    Semivolatile Organics Analyzed For and Their Quantifiable
          Detection Limits at Medium Concentration Levels             4-12

 5.1    Quality Assurance Results for Metals Analysis                 5~2

 5-2    Quality Assurance Results for Semivolatile Organics Analysis  5~3

 C.I    Sampling Equipment Specifications                             C-5

 C.2    Sampling Equipment Preparation and Clean-Up                   C-7

 C.3    Metals and Measurement Methods                                C-20

 C.4    Semivolatile Organic Compounds Measured                       C-22

 C.5    Pesticides Analyzed For and Their Quantifiable
          Dectection Limits                                           C-24

 C.6    Spiking Compounds: Acid Extractables II                       C-27

 C.7    Spiking Compounds: Neutral Extractables V                     C-28

 C.8    Spiking Compounds: Neutral Extractables VI                    C-29

 C.9    Spiking Compounds: Pesticides II                              C-30

 C.10   Spiking Compounds: Metals                                     C-31
                                    VI

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                              1.0  INTRODUCTION



    On October 1? and 18, 1985, Entropy Environmentalists, Inc. collected

soil samples from four treatment, storage, and disposal related processes at

Texaco Refining and Marketing, Inc. (Texaco) located in Delaware City,

Delaware.  The purpose of this sampling program was to provide preliminary

data on the magnitude of fugitive particulate emissions from various

processes at treatment, storage, and disposal facilities  (TSDF's) and the

degree to which these emissions are contaminated.  The U. S. Environmental

Protection Agency (EPA) anticipates utilizing the analytical data from this

program with emission models  to estimate fugitive particulate emissions from

TSDF's.  The information generated by this study may ultimately be used by

the Office of Air Quality Planning and Standards (OAQPS)  of EPA to assess the

adequacy of regulations governing fugitive particulate emissions from TSDF's.

    To accomplish the overall goals of this study, soil samples were

collected from representative processes at this plant and were submitted for

the appropriate analyses in order to determine the following:
       The percent by weight of silt in the soil  (i.e., material that
       passes through a 200 mesh screen and has a nominal diameter
       less than 75 urn) and the percent by weight of moisture in the
       soil.

       The degree of contamination in the soil silt fraction of
       metals, semivolatile organics, and pesticides.

       The percent by weight of soil silt that is less than 20 urn in
       diameter based on a sonic sieving technique.
                                      1-1

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    o  The particle size dependency of the degree of contamination
       (i.e., greater or lesser degree of contamination in particles
       with diameters not in excess of 20 urn) by conducting separate
       analyses of different soil particle size fractions.

    o  The repeatability and reproducibility of the sampling and
       analytical procedures for the entire sampling program (only
       raw data are included in this report; a statistical summary
       will be presented for all sampling sites in a later report).

    At Texaco, the four processes sampled were three different cells within the

land treatment unit and unpaved road segments (3) within the land treatment

site.  A pair of background samples along with samples to assess the

repeatability and reproducibility of the method were also taken.

    Samples taken were analyzed for silt content, PMin content, metals,

cyanide,  and semivolatile organics as described in Chapter 4.  Research

Triangle Institute (RTI) conducted the analyses for metals and PEI and

Associates performed the analyses for the semivolatile organics.  Additional

cleanup of the semivolatile organic extracts was performed by Triangle Labor-

atories,  Inc.  The outside laboratory that performed the metals analysis on the

reproducibility samples was PEI and Associates.   For a cost benefit, all the

reproducibility samples for the entire study were analyzed at the same time.

EPA decided not to have the repeatability and reproducibility samples analyzed

for semivolatile organics because of their high oil and grease content.

    Field sampling was performed by Mr. Steve Plaisance and Mr. Bernie von

Lehmden of Entropy Environmentalists.  Mr. Phillip Englehart and Dr. Tom Lapp

of Midwest Research Institute (MRI) directed Entropy personnel regarding

specific processes to be sampled, the boundaries of the processes, and recorded

the pertinent process and operating characteristics.  Mr. Gene Riley (EPA Task

Manager)  of the Emission Measurement Branch  (EMB) observed the sampling
               <4

program.   Mr. Bob Wojewodski, Senior Environmental Engineer, served as the

principal contact for Texaco.
                                      1-2

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    This report is organized into several chapters that address various aspects




of the sampling and analysis program.  Immediately following this chapter is




the "Summary and Discussion of Results" chapter which presents table summaries




of data on silt and PMir) content and degree of contamination for each sample




fraction analyzed.  Following the "Summary and Discussion of Results" Chapter




is the "Process Description" chapter (supplied by MRI) which includes



descriptions of each process sampled.  The next chapter, "Sampling and




Analysis," presents the plot plan and sampling grid for each process.  The



method of selecting the sampling grid and the sample collection procedures are




outlined, including any deviations and problems encountered.  This chapter also




describes the sample preparation and analytical procedures used for each




sample; any deviations from the normal procedures are addressed.  The




appendices present the Raw Field Data and Sampling Logs (Appendix A);




Analytical Data (Appendix B); detailed Sampling and Analytical Procedures




(Appendix C); Sampling Program Participants and Observers (Appendix D); and




Process Operations Data (Appendix E).
                                      1-3

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                     2.0  SUMMARY AND DISCUSSION OF RESULTS




    This chapter presents a summary of the sampling and analysis results and a




brief discussion of significant deviations from the proposed sampling and anal-




ysis protocol for this program.  Since the standard sampling and analytical




procedures are not addressed in this chapter, it is recommended that those




individuals who are not familiar with the sampling and analytical procedures



used in this study review Chapter 4, "Sampling and Analysis," prior to reading




this chapter.



    Soil samples were collected from four processes at Texaco's refining and




marketing facility located in Delaware City, Delaware.  The processes included:




(1) the land treatment unit, Cell #4, (2) the land treatment unit, Cell #3;




(3) the land treatment unit. Cell #8; and (4) three segments of unpaved roads




within the land treatment unit.  Sampling and analysis were conducted using the




procedures described in the Sampling and Analysis Protocol which was written




specifically for this sampling program.  The protocol was provided to the




facility prior to the sample collection.  The procedures described in this




protocol are described again in detail in Chapter k and Appendix C of this




report.




    As described in the Sampling and Analysis Protocol, this site-specific




report is intended to present the data relevant to the samples obtained at one




site in this study and the procedures used to obtain  these samples.  Some




statistical analyses will be performed on the data concerning this site;



however, the majority of statistical analyses will involve the data collected




over the entire study, including the repeatability and reproducibility and




quality assurance data, and will be included in the summary report to be
                                      2-1

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completed at the conclusion of the program.  With the exception of the data




from the screening conducted to determine silt contents, there is not




sufficient data to conduct meaningful statistical analyses on a site- or




process-specific basis.




    The sampling plan for Texaco is shown in Table 2.1.  The sampling




procedures were designed to obtain a representative sample of that portion of




the contaminated soil with the potential to become airborne.  The analyses of




the collected samples were designed to measure the concentration of the most




likely compounds or elements that could be soil contaminates (metals, cyanide,




semivolatile organics, and pesticides).  The sample collection techniques were




generally as follows:  (1) for undisturbed hard surfaces a sweeping technique




was used to obtain surface samples only;   (2) for moderately disturbed surfaces




a scooping technique was used to obtain near surface samples; and (3) for




surfaces that were mechanically disturbed to a specific depth, coring was used




to sample to the depth of the disturbance.  The number of samples collected



within each process was a function of the variability expected in the degree of




contamination and/or the amount of sample that was needed for the analyses.




    According to the Sampling and Analysis Protocol, the collected samples were




to be analyzed for metals, cyanide, and the semivolatile organics and




pesticides found on the hazardous substance lists (HSL) in the EPA Contract




Laboratory Program (CLP),  Statement of Work.  If significant quantities of




cyanide, semivolatile organics, or pesticides were not expected to be present




in a particular process,  then analysis for those compounds was not performed.




MRI decided that at this particular site, cyanide and pesticides would not be




present in significant quantities in any process sampled, and therefore,




cyanide and pesticide analyses were deleted.  All samples were analyzed for




metals and semivolatile organics, except the repeatability and reproducibility
                                      2-2

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                      TABLE 2.1.   SAMPLING PLAN FOR TEXACO
Process
Sampled
Land Treatment
Unit, Cell #4

Land Treatment
Unit, Cell #8
Land Treatment
Unit, Cell #3
Unpaved Roads
Within Land
Treatment Unit
Background
Samples
Within Land
Treatment Unit
Process
Designation
L

N
0
M
BCD
Number of
Samples
8*
8*
8
8
3
2
Collection
Method
Modified
coring**
(stainless
tube
Modified
coring**
(plastic
tube)
Scooping
Scooping
Sweeping
Scooping
Analyses
Loss on Drying
Silt and PM1Q Content
Semivolatile Organics
Oil and Grease content
Loss on Drying
Silt and PM Content
Metals
Loss on Drying
Silt and PM Content
Metals
Semivolatile Organics
Oil and Grease Content
Loss on Drying
Silt and PM Content
Metals
Semivolatile Organics
Oil and Grease Content
Loss on Drying
Silt and PM Content
Metals
Semivolatile Organics
Loss on Drying
Silt and PM Content
Metals U
Semivolatile Organics
* One to two cores for metals analysis (plastic core tube) and one to two cores for
   organics analysis (stainless core tube) were taken from each of 8 single grid
   cells.

**For each organic sample and each metal sample, 1 to 2 cores approximately
  two to three inches deep were taken.
                                      2-3

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samples.  They were only analyzed for metals since the presence of oil and grease




was anticipated to interfere with the semivolatile organics analysis.  Complete




lists of compounds or elements for which analyses were conducted and their




detection limits are presented in Chapter 4 (see Tables 4.2 and 4.3).




    The analytical results are discussed in the following subsections.  Complete




sampling data sheets are presented in Appendix A and all analytical data sheets




are presented in Appendix B.








2.1  BACKGROUND SAMPLES




    Background samples were collected at a point not used for TSDF activities and




analyzed, because many compounds and elements are either naturally occuring in




the soil or may be present as a result of factors other than those which may be




attributed to Texaco's activities.  The percent weight loss on drying  (LOD)




measured for BGD-420 was 9-46 percent by weight.  The samples were then




oven-dried at 105 C for 4 hours prior to being screened for silt content. The




silt content of the two background samples  (sample identification numbers BGD-420




and BGD-421) averaged 13-7 percent by weight (see Table 2.2).  The composite silt




material (sample identification number BGD-446) separated from the background




samples was sonic sieved.  Material passing through a 20 urn sieve constituted the




PM n content.  The PM1f, content averaged 30.82 percent by weight of the silt




material.  The silt screening did not produce a sufficient amount of silt to




allow for the production of the "greater than PM10" (>PMlfJ and PM 0 fractions




for chemical analyses.  "Greater than PM  '' refers to the fraction of  the silt




material that does not pass through the 20 urn sieve.




    Results of the analyses for metals and semivolatile organics are shown in




Table 2.3-   The analytical results for the metals and cyanide in the background




silt sample (sample ID BGD-455) are in terms of micrograms of the metal per
                                      2-4

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                                   TABLE 2.2.
  ANALYTICAL RESULTS OF SILT SCREENING, WEIGHT LOSS ON DRYING, AND PM
                     FUGITIVE PARTICULATE FROM TSDF (85/12)
                        TEXACO, DELAWARE CITY, DELAWARE
10
   SIEVING

Site and
Process
Texaco, Delaware City
Land Treatment, Cell #4
(Process L)















Texaco, Delaware City
Land Treatment Roads
(Process M)









Sample
ID
L-401-M
L-402-M
L-403-M
L-404-M
L-405-M
L-406-M
L-407-M
L-408-M
L-401-0
L-402-0
L-403-0
L-404-0
L-405-0
L-406-0
L-407-0
L-408-0
Average
Std. Dev.

M-409




M-410



M-411

Percent
Silt
11.8
6.9
8.2
3-5
6.8
11.3
5-7
6.3
9.1
5.6
8.0
3.0
7.4
7-4
4.2
8.9
7.1
2-5

8.2




19-7



10.4
Percent
Loss on
Drying
28.03
21.85
28.50
28.06
26.78
26.02
25-95
33.82
28.09
22.48
22.97
30.07
27.52
32.03
28.75
29.51
27-53
, 3-24

1.65




1.19



1.73


Sample Percent
ID














L-433
L-437


M-440
M-440

Average
Std. Dev
M-443
M-443
Average
Std. Dev
M-446
M-446
PM10














8.51
12.63
10.57
2.92
1.29
2.76

2.03
. 1.04
29.92
34.94
32.43
. 3.55
20.52
21.12
                                                              Average   20.82
                                                              Std.  Dev.   0.42
(continued)
                                      2-5

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TABLE 2.2. (continued)

Site and
Process
Texaco, Delaware City
Land Treatment, Cell #8
(Process N)







Texaco, Delaware City
Background Samples




Texaco, Delaware City
Land Treatment, Cell #3
(Process 0)







Texaco, Delaware City
Land Treatment, Cell #3
Repeatability and
Reproducibility




Sample
ID
N-412
N-413
N-414
N-415
N-416
N-417
N-418
N-419
Average
Std. Dev.
BGD-420
BGD-420
BGD-421
BGD-421
Average
Std. Dev.
0-422
0-423
0-424
0-425
0-426
0-427
0-428
0-429
Average
Std. Dev.
0-422rrl
0-422rr2
0-422rr3
0-422rr4
0-422rr5
Average
Std. Dev.

Percent
Silt
10.9
12.4
14.5
10.3
13.2
11.5
12.9
10.2
12.0
1-5
16.4
15.4
12.5
10.4
13-7
2.7
5.6
5-9
5-8
5-6
6.9
4.4
7-7
7-0
6.1
1.0
6.3
7.8
6.8
6.5
8.3
7-1
0.9
Percent
Loss on
Drying
21.89









9.46












30.49


28.96
32.71
29.47
30.78
27.91
29-97
1.85

Sample Percent
ID PM1Q






N-453 17.06
N-453 18.65
17.85
1.12


BGD-446 31.92
BGD-446 29.72
30.82
1.56






0-463 5.81
0-463 5.24
5-52
0.40







(continued)
                                      2-6

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TABLE 2.2. (continued)

Site and
Process

Sample
ID

Percent
Silt
Percent
Loss on
Drying

Sample
ID

Percent
PMm
Texaco, Delaware City
Land Treatment, Cell #3
Repeatability and
Reproducibility

0-423rrl
0-423rr2
0-423rr3
0-423rr4
0-423rr5
7.1
8.3
4.5
6.1
11.7
31.70
29.23
35-53
28.56
32.48
                             Average
                             Std. Dev.
7-5
2.7
31.50
 2.79
                             0-425rrl
                             0-425rr2
                             0-425rr3
                             0-425rr5

                             Average
                             Std. Dev.
6.7
1.9
3-7
2.7
7.8

4.6
2.6
27-75
30.41
33-21
31.49
27.98

30.17
 2.33
                                      2-7.

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              TABLE 2.3.  ANALYTICAL RESULTS FOR METALS AND SEMIVOLATILE ORGANICS
                           FUGITIVE PARTICULATE  FROM  TSDF  (85/12)
Metals Analysis
Sample Identity

Eleient
AluninuB (AD
Antinony (Sb)
Arsenic (As)
Bar i us (Ba)
Beryllium (Be)
Cadaiua (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Mercury (Hg)
Holybdenuit (Ho)
Nickel (Ni)
Osiiui (Os)
Seleniui (Se)
Silver (Ag)
Thallium (Tl)
Vanadiui (V)
Zinc (Zn)
Semi volatile Analysis
Saiple Identity


2-Hethylnapthalene
Phenanthrene
Pyrene
Land Treatnent Cell
Silt
N-448
(ug/g)
11,100
1.1
6.7
152
<1
<1
209
16.9
207
18,400
57.0
407
1.3
9.2
98.3
<1
2.3
<2
<2
200
248
Land Treatment
Silt
N-447
(ug/g)
N.D.
N.D.
N.D.
PM10
N-450
(ug/g)
13,200
0.8
6.7
215
<1
<1
255
20.6
219
21,400
81.0
473
1.3
9.5
108
<1
2.5
<2
<2
227
287
Cell IB
PH10
N-449
(ug/g)
N.D.
N.D.
N.D.
18
>PH10
N-452
(ug/g)
940
0.6
6.2
272
<1
1.9
196
14.7
200
17,600
65.0
389
1.5
5.7
94.4
U
3.1
<2
<2
190
232







Cell 14
Silt
L-430
(ug/g)
11,000
<0.5
6.6
106
<1
<1
141
17.9
164
22,400
74.0
358
0.9
9.9
86.8
<1
4.2
<2
<2
267
225
Cell 14
Silt
L-434
(ug/g)
N.D.
N.D.
10.0 J
Cell «3
Silt
0-458
(ug/g)
11,900
0.8
7.4
190
<1
<1
142
17.7
198
21,400
92.0
508
1.6
<2
150
<1
3.2
<2
<2
352
296
Cell 13
Silt
0-457
(ug/g)
45.0 J
22.0 J
9.5 J
Roads
Silt
d-439
(ug/g)
11,400
<0.5
5.9
114
<1
1.4
96.7
16.5
110
19,700
49.0
392
0.9
<2
83.8
<1
2.2
<2
<2
207
225
Roads
Silt
H-438
(ug/g)
15.0 J
36.0 J
11.0 J
Background
Silt
BD6-455
(ug/g)
14,000
2.5
5.2
59.9
<1
1.5
21.3
9.5
31.9
19,400
15.0
206
0.1
<2
13.6

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gram of silt sample (dry basis).   These results reflect the nominal concen-




trations of these materials present in the soil which are not a result of




Texaco's activities.  The results for the background samples have not been




subtracted from the results for the other samples since the risk assessments use




the inclusive value of the degree of contamination.  It should be understood,




however, that the actual outside contribution to the degree of contamination of




the soil is that portion of the contaminate concentration which exceeds the




nominal background level.




    For the analysis of  the semivolatile organic compounds, the background




samples were extracted as low-level samples following the U.S. EPA Contract




Laboratory Program, Statement  of Work for Organic Analysis, 7/85 Revision




(refered to as the CLP in this report).  The extract was concentrated and




subjected to an adsorption chromatography cleanup procedure instead of the CLP




gel permeation chromatography  (GPC) cleanup procedure.  The adsorption




chromatography procedure was developed to remove more aliphatic compounds from




the extract than possible with the GPC procedure.  The presence of excessive




amounts of aliphatic material  would require dilution of the extracts prior to the




gas chromatograph/mass spectrometer (GC/MS) analysis and a corresponding increase




in the sample detection  limit.  The dilution would be necessary to protect the




GC/MS from the large amounts of aliphatic compounds present in some samples




(particularly land treatment samples that contain considerable amounts of oil and




grease).




    For the background sample  a 10-fold dilution, determined by GC/flame




ionization detection (GC/FID), was required prior to the GC/MS analysis.  Two of




the CLP hazardous substance list  (HSL) semivolatile compounds were found, but at




concentrations below the quantifiable detection limit.  The compounds detected




met the mass spectral criteria, but the values reported are estimates only.
                                      2-9

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2.2 LAND TREATMENT UNIT, CELL #4 (PROCESS L)




    Cell #4 in the land treatment unit (Process L) was sampled using a coring




technique to obtain samples to a depth of approximately two to three inches,




depending upon the soil conditions in each cell sampled.  A sampling grid was




laid out and eight randomly selected cells were sampled.  Because of the




potential for contamination from materials used in construction of the core




sampling equipment, the samples taken for metals analysis (sample




identification numbers L-401-M through L-408-M) were sampled with a PVC coring




tube, and the samples taken for semivolatile organics analysis (sample




identification numbers L-401-0 through L-408-0) were sampled with a stainless




steel coring tube.  The oil and grease content was determined on a composite




sample made of aliquots taken from all sixteen samples from Cell #4.  The oil




and grease content of the composite sample was 6.11 percent expressed on a dry




basis (see Table 2.4).  The weight loss on drying averaged 27-53 percent by




weight  (see Table 2.2).  Following oven-drying at 105 C for 6 hours, the



sixteen samples were screened for silt content which averaged 7•1 percent by




weight.




    The silt fractions separated from the samples taken for organics analysis




and those taken for metals analysis were each sonic sieved for PM-o-, content




which averaged 10.57 percent by weight of the silt.  The silt screening did not




produce sufficient silt material to allow the production of >PM10 and PM-.n




material by sonic sieving for chemical analyses.  Aliquots of the silt




fractions (one for metals and one for organics) were taken for semivolatile




organics and metals analysis.  These were analyzed separately to determine the



degree of contamination.  The analytical results for metals and semivolatile




organics are shown in Table 2.3-  Like the background silt sample, the land




treatment Cell #4 silt sample was extracted by the low-level method.  The
                                      2-10

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                TABLE 2.4.  SUMMARY OF OIL AND GREASE ANALYSIS
                          FUGITIVE PARTICUALTE FROM TSDF (85/12)
Process Process
ID Description
L Land Treatment, Cell#4
N Land Treatment, Cell #8
0 Land Treatment, Cell#3
Site
Texaco, Del aware City
Texaco, Delaware City
Texaco , De 1 aware C i ty
Oil and
Grease
6. 11%
8.46%
8.92%
       QUALITY ASSURANCE  SUMMARY FOR OIL AND GREASE ANALYSIS
Process
  ID
  Sample
Description
Site
Oil and
 Grease
  Total Repeatability

   0   Oil&Grease 0-rrl  Comp
   0   Oil&Grease 0-rrl  Comp
  Analytical Repeatability

   0   Oil&Grease 0-rrl  Comp
   0   Oil&Grease 0-rrl  Comp
  Sampling Reproducibility

   0   Oil&Grease 0-rr4  Comp
   0   Mean of 0-rrl  Comp
  Performance Audit
  BGD  Spiked with  34  mg of paraffin oil
                         Texaco,Delaware City
                         Texaco,Delaware City
                                                        Mean
                                                         RPD
                         Texaco,Delaware City
                         Texaco,Delaware City
                         Texaco,Delaware City
                                                         RPD
                                    Expected

                                       0.39%
               RPD



                Found

                0.36%
                           6.94%
                           7.91%
                                                          7.43%
                                                          0.48%
                           7.91%
                           7.30%
                                                          0.30%
                           8.12%
                           7.43%
    0.35%



 Recovery

    92.3%
                                   2-11

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extract was concentrated and cleaned by the adsorption chromatography




procedure.  The sample extract required a 165-fold dilution for the GC/MS




analysis.   One semivolatile organic compound was detected in the sample from




Cell #4.  The contamination of the compound was below the quantifiable




detection limit of 54.4 ug/g.




    With the exception of the use of the adsorption chromatography cleanup




procedure, the dilution of the semivolatile organic sample extracts prior to




analysis,  and the increased quantifiable detection limit, all procedures




followed the Sampling and Analysis Protocol.








2.3  LAND TREATMENT UNIT, CELL #8 (PROCESS N)




    Also in the land treatment unit, Cell #8 (Process N) was sampled using a




grid layout.  Eight samples were collected within this grid in a random manner




as described in Chapter 4.  The scoop sampling technique was employed.  The




determination of oil and grease content and LOD was conducted on sample N-412.




The oil and grease content was 8.46% expressed on a dry weight basis  (see




Table 2.4).  The LOD for sample N-412 was 21.89 percent  (see Table 2.2).  All




eight samples were oven dried at 105 C for 6 hours and desiccated overnight




prior to silt screening.  Each of the eight dried samples (sample identi-




fication numbers N-412 through N-419) was screened for silt content which



averaged 12.0 percent silt by weight (see Table 2.2).  The two jars of silt




(sample identification number N-453)• resulting from screening samples N-412




through N-419, were then sonic sieved for PM-ir, content which averaged 17-85




percent by weight in the silt sample.  Portions of the three fractions  (silt,




>PMin, and PM1n) produced from the combined silt sample from Cell #8 were




analyzed for metals.  All three fractions were analyzed for metals to determine




if the degree of contamination was less or greater in the PMin fraction
                                      2-12

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(particle size dependent).  The results for the metals are expressed in micro-




grams of the metal per gram of sample on a dry basis.   The concentrations




measured for the background sample were not subtracted from the sample results.




    As a cost saving measure, only the silt and PM-.0 fractions were analyzed




for semivolatile organics to determine the particle size dependency of the




degree of contamination.  Like the background silt sample, the land treatment




Cell #8 silt and PM1(-. fractions were extracted by the low-level CLP procedure.



The extracts were concentrated and subjected to the adsorption chromatography




cleanup procedure.  Prior to the GC/MS analysis, the silt extract was diluted




238-fold and the PM Q extract was diluted 150-fold.  None of the semivolatile




HSL compounds were detected in the silt or PM1f) extracts at the quantifiable




detection limits of 78.6  ug/g and 49-5 ug/g, respectively.



    With the exception of using the adsorption chromatography cleanup procedure,




diluting the extracts prior to the GC/MS analysis, and the increased quantifia-




able detection limit, all procedures followed the Sampling and Analysis Protocol,








2.4  LAND TREATMENT UNIT, CELL #3 (PROCESS 0)




    Cell #3 of the land  treatment unit (Process 0) was sampled using the




scooping technique.  A sampling grid was laid out and eight randomly selected




cells were sampled.  The determinations of the oil and grease content and LOD




were conducted on aliquots of sample 0-429 taken from Cell #3-  The oil and




grease content of the sample was 8.92 percent expressed on a dry weight basis




(see Table 2.4).  The LOD for sample 0-422 was 30.49 percent  (see Table 2.2).




All samples  (0-422 through 0-429) were oven-dried at 105 C for 6 hours and




desiccated overnight prior to screening.  The resulting dried samples were




screened for silt content which averaged 6.1 percent by weight.
                                      2-13

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    The silt separated from the samples (sample ID number 0-463) was sonic




sieved from PMin content which averaged 5-52 percent by weight of the silt.




Since the amount of silt composite resulting from the silt screening was low




and the PMin content of the silt was also low, the decision was made not to




produce PMlf) or >PM1(-, for chemical analyses.  The results for the analyses done




on the silt fraction for metals and semivolatile organics are shown in Table




2.3.  Three semivolatile organic compounds were detected in the silt samples




from the Cell #3-  The silt sample was prepared for organic analysis like the




background samples.  The extract was diluted 259-fold prior to the GC/MS




analysis.  All of the compounds were below the quantifiable detection limit of




85.6 ug/g, which means that the reported compounds were identified, but the




magnitude of the results are only an estimate.  The analytical results for the




background sample were not subtracted from the sample results.




    With the exception of using the adsorption chromatography cleanup proce-




dure , diluting the extracts prior to the GC/MS analysis, and the increased



quantifiable detection limit, all procedures followed the Sampling and Analysis




Protocol.








2.5  UNPAVED ROADS IN LAND TREATMENT UNIT (PROCESS M)




    Three segments of unpaved roads within the land treatment unit were



sampled.  These segments were located (1) at the main gate to the unit (sample




M-409),  (2) on the north-south access road at the midpoint of Cell #2 (sample




M-410),  and (3) on the east road between Cells #3 and #4 (see Figure 4.1b).




Each segment was sampled using the sweeping technique.




    A brush was used to sweep loose particulate from an 8-inch wide strip




across the width of each segment.  Two sample jars were filled with each




sample.   After drying, the samples were screened for silt content which
                                      2-14

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averaged 8.2, 19-7. and 10.4 percent by weight, for sample numbers M-409.M-410,




and M-411, respectively (see Table 2.2).  The weight losses on drying were




1.65, 1.19 i  and 1-73 percent by weight, respectively.  The silt samples
obtained from these samples were sieved for PMin content which averaged 2.03,




32.43, and 20.82 percent by weight for silt samples M-440, M-443, and M-446,




respectively.  The low PMin content of road sample M-440 as compared with the




other two road samples (M-443 and M-446) correlated with the relatively low




silt content of the same sample.  This was possibly due to the oil and grease



content of the road sample; however, this cannot be confirmed since the oil and




grease content of this sample was not measured.  Since a sufficient quantity of




silt was not obtained from the silt screening, PMin and >PMin fractions were




not produced for the analysis of the metals and semivolatile organics.  The




silt fractions from these three samples were combined.




    The results of metal and semivolatile organic analyses for the composite




silt sample are presented in Table 2.3«  The concentrations measured for the




background sample were not subtracted from the results for the unpaved road




silt sample.  The silt sample was prepared for organic analysis like the




background sample and diluted 185-fold prior to GC/MS analysis.  Three semi-




volatile organic compounds were found in the silt sample and were below the




quantifiable detection limit of 61.2 ug/g, (i.e., the mass spectral criteria




for these compounds were met for identifying the compounds, but the actual




magnitudes reported are only estimated values) .




    With the exception of using the adsorption chromatography cleanup proce-




dure, diluting the extracts prior to GC/MS analysis, and the increased




quantifiable detection limit, all procedures followed the Sampling and Analysis




Protocol.
                                      2-15

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2.6  REPEATABILITY AND REPRODUCIBILITY




    As discussed in more detail in Chapter 4 and Appendix C, additional samples




were collected in three of the sampled grid cells in Cell #3 of the land




treatment unit (Process 0) for use in measuring the sampling and analysis




repeatability and reproducibility.  The silt content values for these samples




are presented in Table 2.2.  The results for the metals analysis for these




samples are presented in Table 2.5-  Analyses for semivolatile organic




compounds were not conducted on these samples because the detection limits for




the samples were expected to be high due to the presence of oil and grease in




the samples. A summary report presenting the repeatability and reproducibility




results for the entire study will be completed at the end of the study.




    The repeatability and reproducibility samples were also used for the oil




and grease analysis.  For total repeatability, the composite sample (sample ID




0-rrl) made of aliquots from 0-422rrl, 0-423rrl, and 0-425rrl was analyzed in




duplicate (see Table 2.4).  For analytical repeatability (defined here as the



gravimetric determination of the extracted residue), the gravimetric determina-




tion was conducted twice on the sample extract.  Sampling reproducibility was




determined by comparing the oil and grease content of a composite sample




(sample ID 0-rr4) made of aliquots of 0-422rr4, 0-423rr4 and 0-425rr4 to the




oil and grease content of the 0-rrl composite.  The rr4 samples were taken from



the same cells by a secondary sampler.




    A performance audit was also conducted by spiking a background sample (from




another site) with paraffin oil dissolved in Freon TF.  The spiked sample was




carried through the oil and grease analysis procedure.  The recovery of the




paraffin oil was calculated to be 9^ percent  (see Table 2.4).
                                      2-16

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TABLE 2.5.  ANALYTICAL RESULTS FOR REPEATABILITY AND REPRODUCIBILITY METALS SAMPLES
            FUGITIVE PARTICUALTE FROM TSDF (85/12)

Sample Identity
Eleaent
AluBinuffl (AD
Arsenic (As)
Bariua (Ba)
Berylliua (Be)
Cadmiua (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Mn)
Hercury (Hg)
Nickel (Ni)
Selenium (Se)
Silver (Ag)
Vanadium (V)
Zinc (Zn)

Sample Identity

Element
Aluminum (AD
Arsenic (As)
Barium (Ba)
Beryllium (Be)
Bismuth (Bi)
Cadmium (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Hercury (Hg)
Nickel (Ni)
Selenium (Se)
Silver (Ag)
Vanadium (V)
Zinc (Zn)
6rid No. 2
RTI PEI
0-465 0-467
(ug/g) (ug/g)
12,400 7,997
6.9 10.9
109 138
<1 <0.1
<1 68.3
137 181
14.5 20.2
174 346
21,000 32,500
69.0 2,620
425 2,100
l.l 1.2
141 34.4
2.5 2.2
<2 8.3
483 21.0
233 27,280
RTI
0-471
(ug/g)
13,700
7.7
121
 _nni
percent
Recovery

-
72. n
12.11
101. 5Z
-
98.57.
-
-
129. OX
-
1 12.5Z
179. 4Z
-
-
72. 81/.
73. IX
-
-
,500 10,100
6.5 6.4
113 678
<1 <1
<1 <1
116 113
15.0 15.2
168 153
,600 18,300
60.5 66.0
400 401
0.8 0.9
489 485
2.7 2.9
<2 <2
,820 2,810
209 207
PEI RTI
0-483 0-485
(ug/g) (ug/g)
7,630 13,600
5.9 7.9
104 146
0.5 <1
0.8 <1
85.6 145
14.4 18.6
134 199
14,600 22,900
50.0 81.3
330 664
1.0 1.2
403 217
0.6 3.6
<0.7 <2
2,160 440
179 330
Unspiked Sample

0-458
(ug/g)
11,900
7.4
190
(1
<10
<1
142
17.7
198
21,400
92.0
508
1.6
150
3.2
<10
352
296
Oy IRC
Amount
(ug/g)
0
89.4
89.4
89.4
0
89.4
0
0
89.4
0
89.4
89.4
0
0
89.4
89.4
89.4
0
PEI
0-487
(ug/g)
10,050
8.6
155
<0.1
1.5
104
21.1
221
19,010
71.2
840
2.3
269
<0.3
<0.7
392
419
Found

0-497

6,577
74
211
79
0
80
95
13
224
13,069
126
422
0
96
57
60
199
294
Grid No. 16

RTI RTI PEI
0-491 0-492 0-493
(ug/g) (ug/g) (ug/g)
12,500 12,300 10
8.4 7.6
145 228
<1 <1
(1 <1
149 147
21.1 20.7
212 204
22,700 22,500 11
86.4 81.0
671 659
1.3 1.4
211 207
2.9 3.8
<2 <2
414 408
341 332
PEI
Percent
Recovery

-
74. 5X
23. 6X
88. 6Z
-
89. n
-
-
28. n
-
37.7Z
-96. OZ
-
-
60. 71
66. 81
-
-
,970
5.7
70
<0.1
1.1
114
15.0
178
,600
48.4
591
1.7
176
<0.3
<0.7
284
309























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2.7  CONCLUSIONS




    No major problems were encountered during sample collection.  It was felt




that the sampling program was successful in obtaining representative samples.




    In the analyses of the samples, no problems were encountered in obtaining




silt content or determining PM1f) content.  The results of the metals analyses




are also believed to be accurate.




    The only significant problem encountered during the analyses was the fact




that the samples contained a significant amount of organics (oil and grease)




not found on the Hazardous Substances List.  This prevented the semivolatile




organics analyses from being conducted at the level described in the analytical




protocol.  Because of the high concentrations of organics, an alternative




sample cleanup procedure was used on the samples to remove these organics.  The




cleanup procedure used on the semivolatile organic sample extracts appeared to




have little effect on the samples from this site.  However, the detection




limits for these samples were believed to be the lowest levels practical for



the analysis of HSL semivolatile compounds by GC/MS.
                                      2-18

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                         3.0  PROCESS DESCRIPTION
     At this  facility,  sampling  was undertaken for  four processes, where
the term  "process"  refers  to a  likely  source  of  potentially contaminated
fugitive  particulate  emissions.   All of  the process samples were  taken
within  the  facility's  land  treatment  unit; processes  sampled include:

     a.   Three different cells within the land treatment unit; and

     b.   Unpaved road  segments  at  three locations within the land treat-
          ment unit.

The following  process  descriptions  are  based largely upon the information
provided  by the  facility and observations made during  the  course of the
survey/sampling effort.

3.1  LAND TREATMENT CELLS

     The  actual working surface of the land treatment unit is approximately
34 acres, and  is  configured  into  12  discrete cells  (see  facility  map,  Fig-
ure 4.2).  At  the time  of  survey,   11 of  the 12 cells were being  used  on  a
strict, rotation basis.  Average cell size is 2.85 acres; the cells range in
size from 2.36 to 3.40 acres.   The  unit  has  been in operation for about
3 years.

     The  land treatment unit  is used exclusively  to  dispose  of wastes
generated at  the facility.  Principal  wastes  and approximate quantities
treated during the past year are shown below.
EPA Hazardous
  Waste No.

K050 and K051
K048 and K049
Quantity
 (tons)

 2,000
 1,850
Non-RCRA waste   8,000-20,000
                Description

API and CPI oil-water gravity separator
bottoms

Vacuum filter cake (VFC) from oil recovery
unit at facility wastewater treatment
plant (WWTP)

Dual cell  gravity solids (DCG)--biosludge
from WWTP
In addition  to  these waste streams, the  unit  occasionally receives tank
bottoms associated with storage tank  cleanup,  as  well  as  oil-contaminated soil
                                    3-1

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            The  principal  equipment types, functions,  and  approximate level  of
       activity for the treatment unit are summarized below.
   Equipment (commercial
 designation if available)

Farm tractor (Ford 7700)
with implements:
1.   Chisel plow
2.   Disc harrow
3.   Lime bucket
4.   Backdrag
Bulldozer (John Deere 350c)
 Two  vacuum
14 wheels
      trucks--4 axles,
Dump truck--3 axles,
10 wheels
                                Function

                        Chisel plow and disc harrow
                        used for initial incorpora-
                        tion and subsequent soil
                        cultivation, respectively.
                        Lime bucket used to add
                        lime to soil for pH con-
                        trol.  Backdrag used to
                        smooth surface prior to
                        waste application.
                                      Activity Units

                             Chisel plow used minimum 4 to
                             6 times/yr.  Disc harrow used
                             minimum of 8 to 12 times/yr.
                             Lime bucket on as-needed
                             basis.  Backdrag minimum 4 to
                             6 times/yr.
                        Functions include spreading  Based on survey observations
                        of solid material on treat-  activity—4 to 6 hr/day.
                        ment plots, and pulling of
                        backdrag over surface.
Delivery of high liquid
content wastes to treat-
ment plots.

Delivery of solid wastes
to treatment plots
3,000-gal.  capacity; avg.
3 loads/day,  when operating,
                                                     Plant considers "full load"
                                                     ~ 14,500 Ib; 2 loads/day.
       The basic sequence of operations for the unit are as follows:

            a.    Waste application;

            b.    Initial  incorporation (chisel plow);

            c.    Addition of lime as needed (lime bucket);

            d.    Soil cultivation (disc harrow);

            e.    Smooth surface (backdrag); and
            f.    Repeat steps d and e.
                                                                  separator sludges)
                                                                  is the principal
                                                                  is maintained
     High liquid content wastes (predominantly API and CPI
are applied from a vacuum tank with a 4-in.  main.  Gravity
mechanism  for  spreading;  to  facilitate  spreading tillage
perpendicular to the  surface  contour.   To prevent undesirable runoff into
the drainage swale  (see  facility map), (along) contour plowing is used at
the extreme  lower  end of each treatment  cell.   Wastes with  higher  solids
content are  delivered  by dump  truck.   Waste  spreading  is  accomplished by  a
bulldozer fitted with a blade.  Observations during the survey suggest that
                                           3-2

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the solids are  spread  quite uniformly over the cell surface to a depth of
2 to 3 in.; gravity  spreading  of the higher liquid content waste produces
considerably less uniform conditions.   In  the  case  of the  liquid wastes  it
is quite possible that areas closest to the point of application experience
far heavier loadings  than  areas at the opposite end of the treatment cell
(i.e.,  closest to the drainage swale).

     The targeted application rate for the treatment unit is set at 80 bar-
rels of oil per acre per application.   This loading allows reapplications
on the order of 4 to 6 times per year.   The treatment unit foreman indicated
that application frequency shows some sensitivity to seasonal  climate varia-
tions.   For example,  during the winter months,  the trafficability of  the
surface typically decreases making it more difficult to incorporate wastes.
As a result, frequency of reapplication may  decrease during these periods.

     The facility uses lime to  immobilize the metals.
This practice creates  a  favorable environment for precipitation of metals
in the zone of  incorporation  (nominal  8-  to  12-in.  depth).  As  a  "typical"
value,  the cells are limed once per week.

     As noted earlier,  sampling was conducted  for  three  different cells
within the treatment unit.   The samples represent three different points in
time after  application.   Cell 3 samples  were  taken immediately (< 4 hr)
after initial  incorporation  of the waste  streams  (combination  of VFC  and
DCG—biosludges).  Cell 4 samples were taken approximately 1 week after ap-
plication of waste material  (predominantly DCG).   Initial  incorporation  as
well as subsequent cultivation  had  already been  completed.  'Cell  8 samples
represent conditions approximately 40 days after application.

3.2  UNPAVED ROADWAYS

     In addition to samples from the actual treatment surface, samples were
also collected from the unpaved roadways located within the treatment unit.
The treatment unit  is  effectively isolated from the rest of the facility,
and as a result traffic  on  the  roadways is restricted to  activity  directly
associated with  the  land treatment  operation.   Estimated  traffic  volume  on
the roadways is < 25 vehicle passes per day.
                                    3-3

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                           4.0  SAMPLING AND ANALYSIS






    This chapter outlines the procedures used for (1) the sampling conducted at




Texaco Refining and Marketing, Inc. (Texaco) and (2) the analysis of the




samples collected.  Included are descriptions of the location of each process




sampled and the sampling grid for sample collection.  Sample handling,




preparation, and/or analysis specific to this facility or any process therein




are described in detail.  Any deviations from the standard sampling and




analysis procedures (see Appendix C) are discussed.




    Four processes were sampled at Texaco:  (1) the land treatment unit,




Cell #4; (2) the land treatment unit, Cell #8;  (3) the land treatment unit,




Cell #3; and (4) three segments of unpaved roads within the land treatment




unit.  The samples from each of these processes were analyzed for weight loss




on drying  (LOD), silt and PMin content, metals, and semivolatile organics.  The




samples from the land treatment cells were also analyzed for oil and grease




content.  A tabular presentation of the sampling plan for Texaco which




specifies  the number and types of samples and the locations at which they were




collected  can be found in Chapter 2  (see Table  2.1).  The subsections that




follow further  describe the sampling locations, sampling grid schemes,  and




applicable sampling and analytical procedures.








4.1  SITE PLOT  PLAN




    Figures 4.la and 4.1b show the site plot plans for the landfill and land




treatment  facilities.  The scale of Figure 4.la is approximately 1 inch equals




250 feet,  the scale of 4.1b is approximately 1  inch equals 230 feet.  The
                                      4-1

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locations of the land treatment cells and unpaved roads sampled are shown on




these site plot plans.  Pertinent topographical features, both natural and




man-made, are also shown.








4.2  LAND TREATMENT UNIT, CELL #4 (PROCESS L)




    Cell #4 (Process L) is in the center on the western side of the land




treatment unit at the Texaco facility (see Figure 4.1b).  The shape of Cell #4




approximated a rectangle with dimensions of 224, 430, 220, and 434 feet.




    Based on these dimensions,  MRI designated that the sampling grid for




Process 0 be a 200 x 400 foot rectangle centered within the cell having 50-foot




square grid cells.  The sampling grid was then laid out using surveyor's stakes




and tape.  The grid cells were numbered starting in the northeast corner of




Cell #4 as shown in Figure 4.2.




    MRI directed that eight grid cells be sampled; a random number table was




used to select the specific grid cells for sampling (see Appendix C).  One of




the grid cells selected (#1) was rejected by MRI because it was on two of the




process boundaries and adjacent to another cell already selected.  Grid cell #2




was substituted in its place.




    MRI determined that for the sample collection, the coring technique would




be used at this process.  Within each cell, a sampling template was randomly




tossed four times. . The cored sample aliquots were taken from inside the areas




defined by the template.  The application of the basic coring technique (see




Appendix C) proved to be difficult and a modified coring technique was devised




based on discussions between MRI and Entropy personnel.  The modified technique




involved taking one or two 2- to 3~inch cored aliquots from each of the four




template areas using each type of core tube  (stainless steel or plastic).




Because of the potential for sample contamination by the coring tube
                                      4-2

-------
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                                                                                               Figure 4.la.  Site plot plan of Texaco
                                                                                                           in Delaware City, DE.
                                                                                                         & Well • Water Data Table
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                        4-3
                                                                                                     4-4

-------

                              LAND TREATMENT FACBJTY
Figure 4.1b.   Enlargement of  Site Plot Plan Showing Locations of Land Treatment
              Cells  and  Sampling Locations for Background and Unpaved Road Samples,
                                  4-5

-------
SO-
SO1

224
^ 	 fe.
i
434
1
1
©
L-402
9
13
©
L-405
©
L-4^6
L-308
29
L-401
6
10
14
18
22
26
30
3
7
(77)
L-403
(is)
L-404
19
23
27
31
4
8
12
16
20
L-407
28
32
*_ 	 	 	 	 	
* 220'
TYPICAL
CELL
j
4301
1
J
N^ 	 ,.,
SCALE: 0.5" - SO1
FIGURE 4.2. SAMPLING GRID. PROCESS DIMENSIONS. AND SAMPLE NUMBERS FOR LAND
TREATMENT UNIT. CELL *4 AT TEXACO. DELAWARE CITY (PROCESS L).

-------
materials of construction, two samples were taken from each grid cell, one for



metals analysis (using the plastic coring tube) and one for organics analysis



(using the metal coring tube).  The sixteen samples taken from the eight grid



cells sampled in this process were numbered using the following scheme:



L-401-0, L-401-M, L-402-0, M-402-M 	 L-408-0, L-408-M.



    Oil and grease analysis was performed on the land treatment, Cell #4 soil



samples.  An aliquot was taken from each sample and mixed to form a soil sample



composite.  The oil and grease analysis was performed following Method 503 D,



Extraction Method for Sludge Samples, found in Standard Methods for Examination



of Water and Waste Water, 1985, l6th Ed.  The method involved acidifying the



sample with concentrated HC1 followed by drying the acidified sample by mixing



the sample with an equal weight of anhydrous magnesium sulfate.  The soil



mixture was extracted with Freon TF, 1,1,2-Trichloro- 1,2,2-trifluoroethane, in



a Soxhlet extraction apparatus.  The weight of the extracted residue was



determined after distilling the solvent and drying the residue.  The loss-on



drying  (LOD) was determined on the soil composites to calculate the oil and



grease as a percent of dry solids.  The following formula was used for the



calculation:






    „, n,,    , _                 Weight of Residue                x 100 %
    % Oil and Grease =	


                       Corrected Dry Weight of Soil Sample




    The quality assurance  (QA) for the oil and grease analysis used the repeat-



ability and reproducibility  (R&R) samples.  A soil composite was made  from three



R&R samples collected by the primary sampler from the three R&R cells  sampled at



the Texaco site.  Duplicate aliquots of the primary soil composite were separately



analyzed for oil and grease.  By comparison of the results from the duplicate oil
                                      4-7

-------
and grease analysis, the degree of repeatability for the total system was




determined.




    A second soil composite was made from three of the R&R samples collected by




the secondary sampler from the three R&R cells at the Texaco site.  An aliquot of




the secondary soil composite was analyzed for oil and grease.  By comparing the




average oil and grease value for the primary soil composite with the oil and




grease value for the secondary soil composite, a measure of the sampling




reproducibility was made.




    A QA spike was done using the background sample from another site.  A USEPA




quality control sample for oil and grease analysis consisting of paraffin, oil




dissolved in Freon TF was used.  The spike provided a concentration of 0.34$ of




oil and grease to the background sample.  The spiked sample was then extracted and




analyzed for oil and grease.  The percent recovery of the spiked oil and grease




mixture was calculated by the following formula:
    Percent Recovery = Spiked Sample % - Background Sample %



                             Calculated Spiked Sample %
    Portions of each of the samples from this process were first analyzed for




weight loss on drying (LOD) by drying for 12 to 16 hours in a 105 C oven.  All




samples were then oven dried at 105°C for 6 hours (see Table 4.1).  Following




drying, each sample was screened to determine percent silt content and then sonic




sieved to determine percent PMin content (see Appendix C for a complete




explanation of sample handling during these analyses).  Material passing through




the 20 urn sonic sieve constituted the PMin fraction.  The portion of the silt




fraction that did not pass through this sieve was referred to as the "greater than




PM  "  (>PM  ) fraction.  With the low yield of silt from the eight samples and
                                      4-8

-------
                    TABLE 4.1.  SAMPLE DRYING PROCEDURE SUMMARY
    Sample             Process
      ID             Description            Drying Procedure


      L       Land Treatment, Cell #4     Oven Dried at 105°C for 6 hours
      M       Land Treatment Roads        Desiccated for 24 hours
      N       Land Treatment, Cell #8     Oven Dried at 105°C for 6 hours
      0       Land Treatment, Cell #3     Oven Dried at 105°C for 6 hours
    O-R&R     Land Treatment, Cell #3     Oven Dried at 105°C for 6 hours
     BCD       Background Sample          Oven Dried at 105°C for 4 hours
the low PMin content of the silt, the decision was made not to produce PMin and
      fractions for the chemical analyses.

    The set of samples collected for metals analysis and the set of samples

collected for organics analysis were each utilized to make separate composite

samples of the silt.  Portions of the silt composite for metals analysis were

sent to RTI for the analysis .  The procedures used for analysis of the metals

followed the methods outlined in the EPA publication, "Testing Methods for

Evaluating Solid Waste," SW-846.  The metals measured and the detection limits

for the analytical methods used are shown in Table 4.2.  Samples for analysis

of all metals except mercury (Hg) were prepared by acid digestion using EPA

Method 3050 (SW-846) .  Mercury samples were prepared and analyzed by the cold

vapor atomic absorption procedure following EPA Method 7471 (SW-846) .  Two

modifications were used in the final dilutions,.,of . the digestates.  The samples

for inductively-coupled argon plasmography (ICAP) determination by EPA Method

6010 and furnace atomic absorption determination of antimony (Sb) by EPA Method

704l were diluted to achieve a final concentration of 5# HC1.  The sample

digestates for arsenic (As) determination by EPA Method 7060, for selenium  (Se)

determination by EPA Method 7740, and for thallium (Tl) determination were

diluted to achieve a final concentration of 0.5% nitric acid.
                                      4-9

-------
           TABLE 4.2.  METALS, MEASUREMENT METHODS, AND DETECTION LIMITS*
Element
Aluminum (Al)
Antimony (Sb)
Arsenic** (As)
Barium** (Ba)
Beryllium (Be)
Cadmium** (Cd)
Chromium** (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead** (Pb)
Manganese (Mn)
Mercury** (Hg)
Molybdenum (Mo)
Nickel (Ni)
Osmium (Os)
Selenium** (Se)
Silver** (Ag)
Thallium (Tl)
Vanadium (V)
Zinc (Zn)
Detection Limits (ug/g)*
ICAP*** GFAA*** Cold Vapor .
75-0 	
	 0.05
01
. X
0.3 	
0.1 	
0.1 	
0.3 	
0.5 	
2.0 	
75-0 	
	 0.3
O.l 	
Om
. Ul
0.2 	
1 9 _____
1 . £. — — — — —
01 _____
. J- — — — __
	 0.05
0.2 	
	 0.2
n R 	
U . O — — — — —
0.1 	
   Detection limits were calculated as three times the standard deviation of
   the values measured for compounds at or near the suspected detection limit
   in the background sample.  For compounds not detected in the background
   sample, the detection limits were calculated as three times the standard
   deviation of the background noise.  Fe, Mg, and Al detection limits were
   determined using low level standards as three times the standard deviation
   of the values measured.
 **
   Eight RCRA metals
*•**
   ICAP = Inductively-Coupled Argon Plasmography
   GFAA = Graphite Furnace Atomic Absorption
     AA = Atomic Absorption
                                      4-10

-------
    A portion of the silt composite  for organics analysis was sent to PEI for




the analysis for compounds listed in Table 4.3-   The sample was prepared by




sonication extraction (EPA Method 3550, SW-846)  using the procedure specified




in the EPA Contract Laboratory Program (CLP),  Statement of Work for Organic




Analysis, 7/85 Revision.  The extract was prepared at the low concentration




level and screened by gas chromatography with a flame ionization detector




(GC/FID).  It was found to contain over 20 ug/g of organic compounds.  The




extract was then transferred to Triangle Laboratories for cleanup by adsorption




chromatography.  The extract was concentrated and a 200 rag portion was




removed.  The 200 mg portion was redissolved in methanol/methylene chloride




(1:1) and chromatographed on Sephadex LH-20.  The cleanup procedure used only




6.2% of  the original sample which represents a 16-fold dilution.




    The  cleaned extract was returned to PEI and screened again by GC/FID.




Based on the results of the screening, the sample was diluted another 10.3 fold




to protect the gas chromatograph/mass spectrometer  (GC/MS).  The cumulative




dilution of 165-fold raised the sample's quantifiable detection limit to




54.4 ug/g.









4.3  LAND TREATMENT UNIT, CELL #8 (PROCESS N)




    Cell #8 (Process N) was located toward the southwest corner of the land




treatment unit at Texaco  (see Figure 4.1b).  The shape of the process




approximated a trapezoid with two right angles; the dimensions were 490, 254,




430, and 252 feet (see Figure 4.3).




    Based on these dimensions, MRI directed that the sampling grid be laid out




toward the center of the process as a 200 x 400 foot rectangle with a typical




grid cell being a 50 foot square.  The grid cells were numbered from left to




right starting in the northeast corner of the sampling grid  (see Figure 4.3).
                                      4-11

-------
            TABLE 4.3.   SEMIVOLATILE ORGANIC COMPOUNDS FOR ANALYSIS
                          ACENAPHTHENE
                          ACENAPHTHYLENE
                          ANTHRACENE
                          BENZO (a)  ANTHRACENE
                          BENZOIC ACID
                          BENZO (a)  PYRENE
                          BENZO (ghi)  PERYLENE
                          BENZO (b)  FLUORANTHENE
                          BENZO (k)  FLUORANTHENE
                          BENZYL ALCOHOL
                          BIS (2-CHLOROETHOXY) METHANE
                          BIS (2-CHLOROETHYL)  ETHER
                          BIS (2-CHLOROISOPROPYL)  ETHER
                          BIS (2-ETHYHEXYL)  PHTHALATE
                          4-BROMOPHENYL PHENYL ETHER
                          BUTYL BENZYL PHTHALATE
                          4-CHLOROANILINE
                          4-CHLORO-3-METHYLPHENOL
                          2-CHLORONAPHTHALENE
                          2-CHLOROPHENOL
                          4-CHLOROPHENYL PHENYL ETHER
                          CHRYSENE
                          DIBENZO (a,h) ANTHRACENE
                          DIBENZOFURAN
                          1,2 DICHLOROBENZENE
                          1,3 DICHLOROBENZENE
                          1,4 DICHLOROBENZENE
                          3,3'-DICHLOROBENZIDINE
                          2,4-DICHLOROPHENOL
                          DIETHYLPHTHALATE
                          2,4-DIMETHYLPHENOL
                          DIMETHYL PHTHALATE
                          DI-N-BUTYLPHTHALATE
                          2,4-DINITROPHENOL
                          2,4-DINITROTOLUENE
                          2,6-DINITROTOLUENE
                          DI-N-OCTYL PHTHALATE
                          FLUORANTHENE
                          FLUORENE
                          HEXACHLOROBENZENE
                          HEXACHLOROBUTADIENE
                          HEXACHLOROCYCLOPENTADIENE .
                          HEXACHLOROETHANE
                          INDENO(l,2,3-cd) PYRENE
                          ISOPHORONE
                          2-METHYL-4,6-DINITROPHENOL
                          2-METHYLNAPHTHALENE
                          2-METHYLPHENOL
                          4-METHYLPHENOL
                          NAPHTHALENE

(Continued)


                                      4-12

-------
TABLE 4.3. (continued)
                          4-NITROANILINE
                          NITROBENZENE
                          2-NITROANILINE
                          3-NITROANILINE
                          2-NITROPHENOL
                          4-NITROPHENOL
                          N-NITROSO-DI-N-PROPYLAMINE
                          N-NITROSODIPHENYLAMINE
                          PENTACHLOROPHENOL
                          PHENANTHRENE
                          PHENOL
                          PYRENE
                          1,2,4-TRICHLOROBENZENE
                          2,4,5-TRICHLOROPHENOL
                          2,4,6-TRICHLOROPHENOL
    MRI determined  that eight grid cells would be sampled.  A random number

table was used to select the grid cells for sampling  (Appendix C).  At MRI's

direction, grid cell #17 was substituted for grid cell #28, because #28 was

adjacent to two cells which had already been selected.

    Because this process involved a disturbed surface, MRI decided that it

would be sampled using the scooping technique (see Appendix C).   As for

Process L, the sampling template was randomly tossed  four times within each

cell sampled.  The  sample from each cell consisted of four soil aliquots  taken

inside the areas defined by the template.  The eight  samples taken were

numbered N-412 through N-419-  Figure 4.3 shows the grid layout and the cell

from which each sample was taken.

    An aliquot of sample number N-412 from this process was analyzed for  oil

and grease content  by the procedure described for Process L.  A portion of

sample N-412 was also analyzed for weight loss on drying (LOD) by drying  for 12

to 16 hours in an oven at 105 C.  Later, all samples  were dried in an oven at

105 C for 6 hours.  Following drying, the samples were analyzed for
                                      4-13

-------
     50'
50'
   TYPICAL
    CELL
                           490'
                                            254'
1
1
5
9
13
©
N-416
21
25
29
2
©
N-412
10
H
18
22
26
®
N-418
3
7
(TT)
N-413
15
19
23
(2?)
N-417
31
4
8
(l2)
N-414
(Te)
N-415
20
24
28
(32)
N-419
                                            252'
                               430'
,
N
                                                  SCALE: 0.5" = 50'
          FIGURE 4.3. SAMPLING GRID, PRXESS DIMENSIONS, AND SAMPLE NUMBERS FOR LAND
                     TREATMENT UNIT, CELL "8 AT TEXACO, DELAWARE CITY (PROCESS N).

-------
percent silt content and percent PM..,-. content (see Appendix C for specifics of




sample handling during each of these analyses).




    Portions of the silt, PMin> and >PMin fractions from this process were




submitted to RTI for metals analysis and portions of the silt and PM10 fraction




only, were submitted to PEI for analysis of semivolatile organics. As a cost




saving measure, the >PM1f, fraction was not analyzed for semivolatile organics




since the particle size dependency of the degree of contamination will




be determined using only the concentration values for silt and PM-,,-, fractions.




All fractions were analyzed for metals and semivolatile organic compounds as




described previously for the samples from Process L.  As for the Process L sample




extracts, the Process N extracts required dilution prior to GC/MS analysis which




resulted in the higher quantifiable detection limits of ?8.6 ug/g for the silt




extract  (diluted 238-fold) and 49.5 ug/g for the PM _ extract  (diluted 150-fold).








4.4  LAND TREATMENT UNIT, CELL #3  (PROCESS 0)




    Cell #3. designated Process 0, is located next to Cell #4  in  the center of




the east side of the land treatment unit at Texaco  (see Figure 4.1b).  The




process boundaries approximated a  trapezoid with sides of 364, 224, 410, and




218 feet.  Based on the process shape and dimensions, the sampling  grid was




designated and laid out to occupy  a rectangular area 200 by 360 feet; the




typical grid cell was a 40-foot square  (see Figure 4.4).  The  grid  cells were




numbered from left to right starting in the northeast corner of the sampling  grid.




    MRI determined that eight  grid cells would be sampled.  A  random number




table was used to select the grid  cells for sampling  (Appendix C) and no




selected cells were eliminated.
                                      4-15

-------
                                         224'
     40'
40'
  TYPICAL
    CELL
                       364'
1 — — '

6

It
©
0-425
21

26
31
36

41
k. , . ..
@
0-422
©
0-423
12
17
22

27
32
37

42

3

8

13
18
23

28
33
©
0-428
©
0-429
4

®
0-424
14
19
@
0-426
29
34
39

44

. 3

10

15
20
(*V
0-427
30
35
40

43
	 1
                                                                   MATERIAL
410'
                                          218'
                                                                               SCALE: 0.0125"" 1'
               FIOURE 4.4. SAMPLING GRID, PROCESS DIMENSIONS, AND SAMPLE NUMBERS FOR LAND
                          TREATMENT UNIT, CELL »3 AT TEXACO, DELAWARE CITY (PROCESS 0).

-------
    MRI determined that for the sample collection, the scooping technique would




be used at this process (see Appendix C).  Within each cell, the sampling




template was randomly tossed four times.  As for Process N, the sample from each




cell consisted of the four soil aliquots (two scoops each) taken from inside the




areas defined by the template.  The eight samples were numbered 0-422 through




0-429-  Figure 4.4 shows each sample and the corresponding grid cell from which




it was taken.




    An aliquot of sample 0-429 was taken for analysis of oil and grease content




by the procedure described previously for Process L samples.  Sample 0-429 was




also analyzed for weight loss on drying (LOD) by drying for 12 to 16 hours in a




105°C oven.  Later, all the samples from this process were oven-dried at 105°C




for 6 hours.  They were then analyzed for percent silt content and percent PM1f.




content (see Appendix C for a complete explanation of sample handling during




these analyses).




    Using the screening and sieving techniques described in Appendix C, all the




samples from this process were used to make a composite sample of the silt. As




for Process L, the decision was made not to produce PM..... and >PMin material for




chemical analysis.   Portions of the composite samples of the silt were sent to




RTI and PEI for metals and semivolatile organics analysis, respectively.  All




samples were analyzed for metals and semivolatile organic compounds as described




previously for the samples from Process L.  As for the Process L sample




extracts, the Process 0 extracts required dilution prior to the GC/MS analysis




which resulted in the higher quantifiable detection limit of 85.6 ug/g after the




260-fold dilution.
                                      4-1?

-------
4.5  UNPAVED ROADS IN LAND TREATMENT UNIT (PROCESS M)

    Three separate segments of unpaved roads (Process M) within the land

treatment unit were sampled.  As may be seen in Figure 4.1b, the areas sampled

were located:


    (1)  at the main gate to the land treatment unit (sample number M-409),

    (2)  on the north-south access road across from the midpoint of Cell #2
         (sample number M-410), and

    (3)  on the east road of the unit between Cells #3 and #4  (sample number
         M-411).


Each of the samples taken (see sample numbers above) was from  a rectangular

area and spanned the road (centered) for 18 feet and was 8 inches wide  (see

Figure 4.5).

    Because unpaved roads consist of hard-crusted, undisturbed surfaces, MRI

recommended sampling this process using the sweeping technique.  A disposable

brush was used to sweep the loose particulate from the surface of each road

area into a disposable scoop, which was then used to deposit the particulate

into the appropriate sample jars.

    Ten-gram portions of the sample from each road segment were first analyzed

for weight loss on drying (LOD) by drying for 12 to 16 hours in a 105°C oven

and then all the samples were dried for 1 day in a desiccator.  They were

analyzed for percent silt content and percent PM1(-. content (see Appendix C) .

Since a sufficient quantity of silt could not be obtained from the silt

screening, PM1f, and >pMin material was not produced for chemical analysis.

    Portions of the silt fraction of the samples were submitted to RTI and PEI

for metals and semivolatile organics analysis, respectively.   They were

analyzed for metals and semivolatile organic compounds as described previously

for the samples from Process L.  As for the Process L sample extracts, the
                                      4-18

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                                    M-409
                                     18'
                                   M-410
                    8"  '
                                    18'
                                   M-411
                                    18'
FIGURE 4.5. DIMENSIONS AND SAMPLE NUMBERS FOR THE SEGMENTS OF UNPAVED
          ROADS SAMPLED IN THE LAND TREATMENT UNIT AT TEXACO (PROCESS M).

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Process M extracts required dilution that resulted in the higher quantifiable


detection limit of 62.5 ug/g after a 185-fold dilution.




4.6  REPEATABILITY, REPRODUCABILITY, AND PERFORMANCE AUDIT SAMPLES


    As part of the sampling conducted within the Process 0 boundries at Texaco,


samples were taken for measurement of repeatability (within laboratory


precision) and reproducibility (between laboratory precision) and for


performance audits.  Three of the grid cells (numbers 2, 7, and 16) previously


sampled were sampled for these purposes.


    Within each of these cells, the primary sampler (in this case, Mr. Bernie


von Lehmden) took three samples (only two needed) and the secondary sampler  (Mr.


Steve Plaisance) took two samples (only one needed), all from the same template
                                                                           #
area.  Samples taken by the primary sampler were used to measure both total  and


analytical repeatability and analytical reproducibility.  They were also spiked

for the performance audits (see Chapter 5 and Appendix C).  Samples taken by the

secondary sampler were used to measure total reproducibility (see Appendix C).


Sampling was conducted using the scooping technique.


    Weight loss on drying determinations, drying, and silt content determinations


for these samples were done as described for the samples from Process L.  The


analyses for metals were done using the same methods previously discussed.

Research Triangle Institute (RTI) (for within laboratory precision) and PEI  (for

between laboratory precision) conducted the metals analysis.  The decision was

made not to have the repeatability and reproducibility samples analyzed for

semivolatile organics because of the higher detection limits anticipated due to

the presence of oil and grease in the samples.
*Sampling and analytical.
                                      4-20

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4.7  BACKGROUND SAMPLES




    Two background samples were taken at Texaco outside the western boundary of




the land treatment unit.  One sample (BGD-420) was taken approximately 75 feet




west and 25 feet north of ground water sampling well No. 26, and the second




sample (BGD-421) was taken approximately 25 feet north of the first sample (see




Figure 4.1b).  The scooping technique was used for sample collection..




    The background samples were analyzed for weight loss on drying (LOD) and




then dried in an oven at 105 C for 4 hours.  They were also analyzed for




percent silt and percent PM-,,-, content (see Appendix C) .




    Portions of the silt fraction generated by screening were sent to RTI and




PEI for metals and semivolatile organics analysis, respectively.  They were




analyzed for metals and semivolatile organic compounds as described previously




for the samples from Process L.  The low-level extraction and adsorption




chromatography cleanup procedure used resulted in a quantifiable detection




limit of 3-3 ug/g after a 10-fold dilution prior to the GC/MS analysis.
                                      4-21

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                             5.0  QUALITY ASSURANCE









    The quality assurance (QA) measures for the chemical analyses were




conducted internally by each laboratory.  For the metals analysis, RTI used




National Bureau of Standards (NBS) water (1643 B) as check samples for the




accuracy of the instrumentation.  A marine sediment reference material (MESS-1)




acquired from the Marine Analytical Chemistry Standard Program of the National




Research Council of Canada and an NBS fly ash sample (1633 A) were used as QA




samples to check the overall accuracy of the digestion and analysis




procedures.  One process sample was spiked with eight elements and their




percent recoveries calculated to assess matrix effects.  Another sample (N-452)




was analyzed as duplicates to demonstrate analytical precision.  Results of




these checks are presented in Table 5-1-




    For the QA on the analysis of the semivolatile organics and pesticides, PEI




used a sample (0-457) for a matrix spike (MS) and a matrix spike duplicate




(MSD).   The percent recoveries were determined and the relative percent




difference (RPD) for the duplicates calculated (see Table 5.2).  The percent




recoveries for all compounds in both the MS and MSD samples, except pyrene in




the MS sample, were outside the QA limits.  Acenaphthene and 2,4-dinitrotoluene




were recovered at levels above the QA limits for both MS and MSD samples.  In




the MSD sample only, 4-nitrophenol and pyrene were recovered at levels above




the QA limit.  The remaining compounds were not detected at all.  The spike




concentrations were all below the quantifiable detection limit for the MS and




MSD samples because of the dilutions required for the GC/MS analysis.
                                      5-1

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TABLE 5.1.  QUALITY ASSURANCE RESULTS FOR METALS ANALYSIS
Sasple Identity
Elements (ug/g)
Aluainua (AD
Antinony (Sb)
Arsenic (As)
Bariua (Ba)
BerylliuB (Be)
Cadffliua (Cd)
Chromium (Cr)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Manganese (Hn)
Mercury (Hg)
Molybdenua (Ho)
Nickel (Ni)
DsniuB (Os)
Selenium (5e)
Silver (Ag)
Thai liuu (Tl)
Vanadiua (V)
Zinc (Zn)
cyanide
EPA Check
Expected
(ug/g)
-
8.2
43.0
-
29.0
9.1
7.1
43.0
8.9
.
43.0
13.0
-
-
-
•
7.6
-
25.2
130
10.0
-
Sanple
Found
(ug/g)
-
9.0
43.6
-
30.5
7.7
6.8
40.1
12.3
-
43.0
12.9
-
-
-
-
6.9
-
26.7
123
10.0
-
NBS Fly Ash 1633 A
Expected
(ug/g)
140,000
7.0
145
1500
12.0
1.0
196
46.0
118
94,000
72.4
190
-
29
127
-
10.3
-
5.7
300
200
-
Found
(ug/g)
17,000
2.6
129
700
4.2
5.5
35.4
25.0
38.5
22,200
31.8
27.9
-
-
53.3
-
7.7
-
3.3
121
69.2
-
NRC Seditent MESS-1
Expected
(ug/g)
58,000
-
10.6
-
1.9
0.6
71.0
10.8
25.1
36,500
34.0
513
-
-
29.5
-
0.4
-
0.7
72.4
191
-
Found
(ug/g)
18,000
<0.5
7.9
87.3
1.4
0.4
40.1
10.2
22.3
25,000
23. B
344
-
-
33.5
-
<0.5
-
<2
54.0
171
-
Matrix Spike
Added
(ug)
-
-
10.0
100.0
100.0
100.0
100.0
-
100.0
-
10.0
100.0
0.40
100.0
100.0
-
11.0
100.0
10.0
100.0
100.0
-
Recovered
(ug)
-
-
8.9
. 239.0
94.2
90.2
97.1
-
96.5
-
8.6
102.0
0.36
91.5
93.7
-
10.0
81.8
11.0
32.8
94.4
-
Percent

-
-
89. OX
239*
94. 21
90.27.
97. IX
-
96. 5X
-
86. OX
102.0X
90. OX
91. 5X
93. 7X
-
90. 9X
91.81
110. OX
32. 8X
94. 4X
-
Duplicates
N-452
(ug/g)
-
0.6
6.2
272
<1
1.9
196
14.7
200
-
65.0
389
-
5.7
94.4
<1
3.1
-
<2
190.0
232
-
N-452
(ug/g)
-
1.0
7.7
147
<1
<1
189
11.8
196
-
55.0
379
-
<2
89.0
<1
2.9
-
<2
178.0
229
-
                         5-2

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                              TABLE 5.2.  QUALITY ASSURANCE  RESULTS  FOR  SEHIVOLATILE  OR6ANICS  ANALYSIS

                                              SOIL SURROGATE PERCENT RECOVERY  SUMMARY
Sanple Identity
Surrogate Coopounds
Nitrobenzene-d5
2-Fluorobiphenyl
Terphenyl-dl4
Phenol-d5
2-Fluorophenol
2,4,6-Tribronophenol
Silt
L-434

01
667,
164X
01
ox
ox
Silt
11-438

01
01
148X
OX
OX
OX
Silt
N-447

OX
OX
119X
OX
OX
OX
PH-10
N-449

OX
OX
105X
OX
OX
OX
Silt
0-457

OX
207X
259X
OX
OX
OX
Silt
BGD-454

OX
171
B3X
OX
OX
661
Sasple
Blank

OX
OX
120X
OX
OX
54X
Matrix
Spike

OX
821
110X
OX
OX
OX
Matrix Spike
Duplicate

OX
OX
192X
OX
OX
OX
                                        SOIL MATRIX SPIKE/MATRIX  SPIKE DUPLICATE RECOVERY SUMMARY
Sanple Identity
0-457
Compound
1,2,4-Trichlorobenzene
Acenaphthene
2,4-Dinitrotoluene
Pyrene
N-Nitrosodi-n-Propylaaine
1,4-Dichlorobenzene
Pentachlorophenol
Phenol
2-Chlorophenol
4-Chl or o-3-nethyl phenol
4-Nitrophenol
2-Hethylnapthalene
Phenanthracene
Napthalene *
Fluorene *
N-Nitrosodiphenylaffline *
3,3'-Dichlorobenzidine *
Benzo(a) anthracene *
Benzo(g,h,i)perylene *
Spike Unspiked
Cone. Saaple
(ug/g)
3.25
3.25
3.25
3.25
3.25
3.25
6.50
6.50
6.50
6.50
6.50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
(ug/g)
0.0
0.0
0.0
9.5 J
0.0
0.0
0.0
0.0
0.0
0.0
0.0
45.0 J
22.0 J
0.0
0.0
0.0
0.0
0.0
0.0
Matrix Percent
Spike Recovery
(ug/g)
0.0
B.2 J
7.3 J
8.0 J
0.0
0.0
0.0
0.0
0.0
0.0
0.0
64.0 J
58.0 J
B.2 J
9.1 J
22.0 J
24.0 J
14.0 J
14.0 J

OX
253X
225X
-4BX
OX -
OX
OX
07.
OX
OX
OX
142X
264X
-
-
-
-
-
-
Matrix Spike
Duplicate
(ug/g)
0.0
8.5 J
5.3 J
17.0 J
0.0
0.0
0.0
0.0
0.0
0.0
8.5 J
65.0 J
47.0 J
7.40 J
12.00 J
28.00 J
51.00 J
0.00
0.00
Percent
Recovery

OX
262X
164X
232X
OX
OX
OX
OX
OX
OX
131X
144X
214X
-
-
-
-
-
-
RPD

OX
-0.4X
3. 97.
-37. 9X
OX
OX
OX
OX
OX
OX
07.
-0.27.
2.67.
-
-
-
-
-
-
Sasiple Detection Liait (ug/g)
                85.6
90.6
105.4
      = Compound Mas not detected in the unspiked sanple and Has not spiked, but was detected in the aatrix spike sample
        and/or natrix spike duplicate saaple.
      = Estieated value where the compound meets the nass spectral or chroaatographic criteria
        but is below the quantifiable liait

                                      METHOD BLANK SUMMARY FOR SEMIVOLATILE ORBANICS ANALYSIS
      Blank ID
Compound Identity

 None Detected
                          Concentration

                           None Detected
   Saople Blank for
 Seoivolatile Organics
                                                           5-3

-------
    Six compounds were detected below the quantifiable limit in the MS and/or


MSD that were not detected in the unspiked sample.  The cause of the compounds


not being found in the unspiked sample was probably the result of the dilution


of the samples.


    All samples received, including the laboratory blanks, were spiked with


surrogate compounds and the percent recoveries of these compounds were


determined (see Table 5-2).  Nitrobenzene-d... phenol-d.., and 2-fluorophenol
                                           5          5

were not detected in any sample.  Terphenyl-d..^. was detected in all the


samples; the recovery of terphenyl-d^ for samples L-434, M-438, 0-457. and the


0-457 MSD was above the QA limit.  For 2,4,.6-tribromophenol, recoveries for the


method blank and the background sample were within the QA limits; the compound


was not detected in the rest of the samples.  For 2-fluorobiphenyl, sample


L-434 and the 0-457 MS showed recoveries within the QA limits; sample 0-456


showed a recovery above the QA limit and the background sample showed a


recovery below the QA limit.  The surrogate compound was not detected in the


other samples.  Again, the dilution of the sample prior to the GC/MS analysis


was thought to be the cause of not detecting the surrogate compounds.


    Analysis was conducted on a blank sample consisting of a purified solid


matrix spiked with surrogate compounds and carried through extraction and


concentration  (see Table 5-2).  The CLP specifies limits for the blanks on the


levels of common phthalate esters and Hazardous Substances List  (HSL)


compounds.  In the blank sample, no phthalate esters or HSL compounds were


detected at a quantifiable limit of 0.33 ug/g.


    Entropy conducted a independent performance audit by spiking a silt sample


from the repeatability and reproducibility sample set.  Two aliquots of a silt


composite made from sample 0-458 were used for the metals spikes (samples 0-495


and 0-497).  The elements and their concentractions in the spiking solution
                                      5-4

-------
used for the metals spike are listed in Table C.10 of Appendix C.  The metals




spike was added to achieve approximately 100 ug/g concentration with the exact




concentration depending on the actual sample weight.  The exact concentration




of the metals spike, the analysis of the unspiked silt sample and the spiked




sample, and the percent recoveries for each element are presented in Table 5-2.
                                      5-5

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