EPA-560/6-76-001
       SAMPLING AND ANALYSIS OF SELECTED TOXIC SUBSTANCES

                       Task IA - Hexachlorobenzene
                      Environmental Protection Agency
                         Office of Toxic Substances
                         Washington, D.C.  20460

                                June 1976

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EPA-560/6-76-001
           SAMPLING AND ANALYSIS  OF SELECTED TOXIC SUBSTANCES

                      Task IA - Hexachlorobenzene
                         Contract No. 68-01-2646
                            Project Officer

                          William A. Coniglio
                      Office of Toxic Substances
                    .Environmental Protection Agency
                        Washington, D.C.. 20460
                             Prepared for

                    Environmental Protection Agency
                      Office of Toxic Substances
                        Washington, D.C.  20460

                               June 1976

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                                 NOTICE

This report has been reviewed by the Office of Toxic  Substances,  Environ-
mental Protection Agency, and approved for publication.  Approval  does not
signify that the contents necessarily reflect  the views  and  policies of
the Environmental Protection Agency. Mention of trade names  or commercial
products is for purposes of clarity only and does not constitute  endorse-
ment or recommendation for use.

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                                CONTENTS
                                                                   Page
Summary .............................     1

Section

  I       Introduction  	     3

  II      Experimental Procedures 	  ........     5

            Sampling Procedures . .  .  .	     5
            Analysis Procedures 	  	  •     5

  III     Selection of Sampling Sites	     9

            Selection Criteria  	  	  ..     9
            Recommended Sampling Sites  •	  .  .  .  .     11

  IV      Presampling Surveys and Field  Sampling  ........     15

            Presampling Surveys	•••	     15
            Field Sampling	     15

  V       Discussion of Results	     20

            Vulcan Materials Company,  Wichita,  Kansas  	     20
            Linden Chlorine Plant, Linden,  New Jersey  	     33
            Stauffer Chemical Company, Louisville, Kentucky  ...     36
            Dow Chemical Company, Pittsburg, California  .....     43
            E. I. du Pont de Nemours and Company,  Inc.,
              Corpus Christi, Texas  	  	     45
            Diamond Shamrock Corporation,  Deer  Park, Texas   ...     50
            Ciba-Geigy Corporation,  St.  Gabriel, Louisiana   ...     53
            Olin Corporation, Mclntosh,  Alabama .	     57
            PPG Industries, Inc., Lake Charles,  Louisiana  ....     61
                                    11

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                           CONTENTS  (concluded)

Section                                                           Page

  VI      Sewage Treatment Facilities 	   69

            Sampling	   69
            Experimental Procedures  ...  	   69
            Results	   70

  VII     Summary and Conclusions  for Program Task  IA	   71

            Summary	   71
            Conclusions 	  ........   74

References	   76

Appendix A - Presampling Survey and  Field  Sampling   .......   77

Appendix B - Analytical Data	130

Appendix C - Method Development for  Sampling  and Analysis  ....  144
                                   111

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                                 FIGURES

No.

 1        Air Sampling Train	•••	     6

 2        Geographic Location of Recommended Sampling Sites  ...    13

 3        Presampling Survey and Field Sampling Schedule   ....    16

 4        Average Concentrations of HCB in Air Per  20-hr Period
            at 18 Sampling Stations at Vulcan Materials Company,
            Wichita, Kansas 	    22

 5        HCB Concentration Per 20-hr Period at Sampling Stations
            Within the Plant Perimeter (Vulcan)  	    23

 6        HCB Concentration Per 20-hr Period, Downwind Stations
            (Vulcan)	    24

 7        HCB Concentration Per 20-hr Period, Upwind Stations
            (Vulcan)	    25

 8        Average Vapor and Particulate Concentrations of HCB in
            Air Per 20-hr Period at 18 Sampling Stations   ....    26

 9        Variation in Vapor and Particulate HCB Levels at
            Station 4 (Vulcan)	    28

10        Variation in Vapor and Particulate HCB Levels at
            Station 18 (Vulcan)	    29

11        Average Concentrations of HCB in Air at Nine Sampling
            Stations at Stauffer Chemical Company,  Louisville,
            Kentucky	    37

12        Average Concentration of  HCB in Vapor and Particulate
            at Nine Sampling Stations  (Stauffer)  	    39
                                   IV

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                           FIGURES (continued)

No.                                                                 Page
 13        HCB Concentration Per 24-hr Period at Sampling
            Stations Around the Plant (Stauffer)	     40

 14        Average Concentrations of HCB in Air at Eight Sampling
            Stations at Dow Chemical Company,  Pittsburg,
            California	     44

 15        Sampling Stations at E. I. du Pont de Nemours and
            Company, Corpus Christi, Texas  	     48

 16        Stations at Diamond Shamrock Corporation,  Deer Park,
            Texas	     51

 17        Average Concentrations of HCB in Air at Eight Sampling
            Stations at Ciba-Geigy Corporation, St.  Gabriel,
            Louisiana	•	••     55

 18        Average Concentrations of HCB in Air at Eight Sampling
            Stations at Olin Corporation,  Mclntosh,  Alabama ...     58

 19        Average Concentrations of HCB in Air at 10 Sampling
            Stations at PPG Industries, Lake Charles,  Louisiana .     64

 20        Average Concentrations of HCB in Vapor and Particulate
            at 10 Sampling Stations Around the Plant (PPG
            Industries)	     65

 21        Summary of HCB Concentrations in Air	     73

 A-l       Presampling Survey and Field Sampling Schedule  ....     79

 A-2       Sampling Locations at Vulcan Materials Company -
            Wichita Plant 	     81

 A-3       Vulcan Materials Company - Wichita Plant,  and Surround-
            ing Areas	     84

 A-4       Sampling Locations at Stauffer Chemical Company -
            Louisville,  Kentucky  	     90

A-5       Sample Locations at Dow Chemical Company,  Pittsburg,
            California	     97
                                    v

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                           FIGURES (concluded)

No.                                                                 Page
A-6       Sample Locations at E. I. du Pont de Nemours and
            Company, Inc., Corpus Christi,  Texas   	  .    102

A-7       Sampling Locations at Diamond Shamrock  Corporation,
            Deer Park, Texas	    109

A-8       Sample Locations at Ciba-Geigy Corporation,  St.  Gabriel,
            Louisiana 	  ..........    113

A-9       Sampling Locations at Olin Corporation,  Mclntosh,
            Alabama	    119

A-10      Sampling Locations at PPG Industries, Lake Charles,
            Louisiana	    126

C-l       Apparatus for Recovery of HCB from Water by  Vaporiza-
            tion at Reduced Pressure  	  ......    148
                                    VI

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                                 TABLES

No.

 1        Estimated Quantities of RGB Present  in  Industrial
            Wastes, By-Products,  and Products  in  1972  	     10

 2        Production Capacity, Process Technology and  Waste Dis-
            posal at Recommended  Sites  .............     14

 3        Field Sampling Summary	•  •     18

 4        Summary of Air Sampling Parameters	     19

 5        Comparison of HCB Levels at 4  and 11 ft for  Five Time
            Periods	     30

 6        HCB Concentrations in Soil and Sediment from Vulcan
            Materials Company, Wichita,  Kansas  	     32

 7        HCB Concentrations in Water from Vulcan Materials
            Company, Wichita, . Kansas	     34

 8        HCB Concentrations in Water and Solids  from  Linden
            Chlorine Company, Linden, New Jersey   	     35

 9        HCB Concentrations in Soil and Sediment from Stauffer
            Chemical Company, Louisville,  Kentucky  	     42

10        HCB Concentration in Water from Stauffer Chemical
            Company, Louisville,  Kentucky 	     42

11        HCB Concentrations in Soil from Dow  Chemical Company,
            Pittsburg,  California	     46

12        HCB Concentrations in Soil and Sediment from E. I. du
            Pont de Nemours and Company,  Corpus Christi, Texas   .     49
                                   VI1

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                           TABLES (continued)

No.

13        HCB Concentrations in Water from E. I. du Pont de
            Nemours and Company, Corpus Christi, Texas  .....    49

14        HCB Concentrations in Soil from Diamond Shamrock
            Corporation, Deer Park, Texas 	    52

15        HCB Concentrations in Water from Diamond Shamrock
            Corporation, Deer Park, Texas	    54

16        HCB Concentrations in Soil from Ciba-Geigy Corporation,
            St. Gabriel, Louisiana	    56

17        HCB Concentrations in Soil and Sediment, Olin Corpora-
            tion, Mclntosh, Alabama ..... 	    60

18        HCB Concentration in Water from Olin Corporation,
            Mclntosh, Alabama ......... 	    62

19        HCB Concentrations in Soil and Sediment from PPG
            Industries, Lake Charles,  Louisiana .... 	    66

20        HCB Concentrations.in Water from PPG Industries,
            Lake Charles, Louisiana	    68

21        Data Summary for Program Task No. 1 . .	    72

A-l       Air Sampling Data at Vulcan Materials Company, Wichita,
            Kansas  ......... 	 • 	    82

A-2       Plant Activities During Sampling at Vulcan Materials
            Company, Wichita, Kansas  ..............    85

A-3       Weather Conditions During Sampling at Vulcan Materials
            Company, Wichita, Kansas	•	    86

A-4       Air Sampling Data at Stauffer Chemical Company,
            Louisville, Kentucky  	    91

A-5       Plant Activities During Sampling at Stauffer Chemical
            Company, Louisville, Kentucky	    93

A-6       Weather Conditions During Sampling at Stauffer Chemical
            Company, Louisville, Kentucky 	    94

                                   viii

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                            TABLES (continued)

No.

A-7       Air Sampling Data at Dow Chemical Company, Pittsburg,
            California	    98

A-8       Weather Conditions and Plant Activities During Sampling
            at Dow Chemical Company, Pittsburg, California  . •  .    99

A-9       Air Sampling Data at E. I. du Pont de Nemours and
            Company, Inc., Corpus Christi, Texas  	 ...   103

A-10      Plant Activities During Sampling at E. I. du Pont de
            Nemours and Company, Inc., Corpus Christi, Texas  .  .   105

A-ll      Weather Conditions During Sampling at E. I. du Pont de
            Nemours and Company, Inc., Corpus Christi, Texas  .  .   106

A-12      Air Sampling Data at Diamond Shamrock Corporation,
            Deer Park, Texas	   110

A-13      Weather Conditions During Sampling at Diamond Shamrock
            Corporation, Deer Park, Texas 	   Ill

A-14      Air Sampling at Ciba-Geigy Corporation, St. Gabriel,
            Louisiana	   114

A-15      Weather Conditions During Sampling at Ciba-Geigy,
            St. Gabriel, Louisiana	   116

A-16      Air Sampling Data at Olin Corporation, Mclntosh,
            Alabama	   120

A-17      Weather Conditions During Sampling at Olin Corporation,
            Mclntosh,  Alabama	   122

A-18      Air Sampling Data at PPG Industries, Lake Charles,
            Louisiana	   127

A-19      Weather Conditions During Sampling at PPG Industries,
            Lake Charles,  Louisiana	   129

B-l       HCB Concentrations in Air Samples  from Vulcan Materials
            Company, Wichita,  Kansas  .... 	   131

B-2       HCB Concentrations in Air Samples  from Stauffer
            Chemical Company,  Louisville,  Kentucky  	   136

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                           TABLES (concluded)

No.

B-3       HCB Concentrations at Air Samples from Dow Chemical
            Company, Pittsburg, California  	  ...    138

B-4       HCB Concentrations in Air Samples from E.  I.  du Pont
            de Nemours and Company, Corpus Christi,  Texas ....    139

B-5       HCB Concentrations in Air Samples from Diamond Shamrock
            Corporation, Deer Park, Texas	•	    140

B-6       HCB Concentrations in Air Samples from Ciba-Geigy
            Corporation, St. Gabriel,  Louisiana 	  ...    141

B-7       HCB Concentrations in Air Samples from Olin Corpora-
            tion, Mclntosh, Alabama	    142

B-8       HCB Concentrations in Air Samples from PPG Industries,
            Lake Charles, Louisiana 	    143

C-l       Recovery Studies of HCB by ri-Hexane Extraction  ....    146

C-2       Recovery of HCB from Water by Concentration on XAD-4   .    146

C-3       Loss of HCB Due to Vaporization	    147

C-4       Recovery of HCB from Water-Saturated Air	    149

C-5       Recovery of HCB from Sediments	  .    150

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                                 SUMMARY

     The purpose of this program is to provide sampling and analysis
capabilities to EPA's Office of Toxic Substances, so that the levels
of suspected toxic substances in air, water, soil,  and sediment at des-
ignated locations throughout the United States may be determined. Four
tasks have been assigned on this program. The first task included the
sampling and analysis for hexachlorobenzene (HCB).

     Methods for sampling and analyzing HCB in air, water,  soil,  and
sediments were evaluated. A protocol was developed and approved.

     Nine industrial plants were selected for sampling. The plants rep-
resent six major industries:  perchloroethylene,  trichloroethylene,  car-
bon tetrachloride, chlorine, triazine herbicides, and pentachloronitro-
benzene.

     Of the six industries sampled, higher concentrations of HCB  were
associated with the production of perchloroethylene,  trichloroethylene,
and carbon tetrachloride. In the one plant that produced only carbon
tetrachloride, HCB levels were quite low. HCB concentrations detected
in samples from the pentachloronitrobenzene plant were relatively high,
i.e., low micrograms per cubic meter range in air and generally over
100 )j,g/g along in-plant roads. The levels of HCB  associated with  plants
producing chlorine and triazine herbicides were very low.

     Several different waste-disposal methods were  used at  the perchloro-
and trichloroethylene plants that were sampled. The highest level of HCB
was detected in air and soil at the plant using on-site landfill  and open
pit storage. High HCB levels were detected in loading and transfer areas
at plants using off-site disposal methods. Lower  levels of  HCB were  found
at plants using on-site incineration but downwind air concentrations were
elevated above background at these plants. The production of perchloro-
and trichloroethylene by low temperature oxychlorination and the  incinera-
tion of liquid bottom wastes resulted in a high HCB level (jig/m ) in the
air but relatively low levels in the effluent water.

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     The highest level of HCB found in the air on plant property was 24
       The HGB level in an open waste treatment pond was 306 |J/g/liter.
The level of HCB in soil within the plant area was over 1,000 |jbg/g at
three plants.

     The maximum concentration of HCB in air sampled off plant property
was 0.36 (ig/nP. A level of 3 ng/m^ was detected at the boundary of another
plant. Soil taken from a cornfield adjacent to one plant contained 1.1
M-g/g, and over 3,000 |J.g/g were detected along a boundary road of another.
HCB levels in water sampled beyond the plant property exceeded 1 ng/liter
at two plants.

     Samples were collected from two sewage treatment plants; negligible
quantities of HCB were detected.

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                              SECTION I

                             INTRODUCTION

     Environmental contamination of hexachlorobenzene  (HCB) has been
reported internationally and nationally.  Detection of  HCB in human adi-
pose tissue has been reported in Australia,  Germany, and Japan.——'  In
the United States, HCB has been detected  in  cattle raised in Louisiana,
and sheep raised in New Mexico, Colorado, and California.—  In addition,
concentrations of HCB at 16 |j,g/m  have been  detected in air samples col-
lected by the Louisiana State Air Control Commission.—

     On July 5, 1973, Midwest Research Institute  (MRl) initiated a study
to estimate the quantities and identify sources of HCB in the environ-
ment. The origin of HCB in the environment in the United States was iden-
tified as the waste materials or by-products from the  production of per-
chloroethylene, trichloroethylene, carbon tetrachloride, chlorine, penta-
chloronitrobenzene and the herbicide Dacthal®. Specific industrial plants
from the above industries were recommended to EPA as potential sampling
sites.

     On June 27, 1974, MRI project (3953-C)  entitled "Sampling and Anal-
ysis of Selected Toxic Substances" was initiated. The  objective of this
program was to provide the EPA with sampling and  analysis capabilities
to determine the levels of toxic substances  in air, water, soil and sedi-
ment from designated sources and ambient  locations throughout the United
States. The first task of this program was the sampling and analysis for
HCB (Task IA) and HCBD (Task IB). Tasks II and III of  this program are
the sampling and analysis for ethylene dibromide, and  evaluation of vinyl
chloride levels in outdoor and indoor air due to  the presence of PVC prod-
ucts, respectively. The ethylene dibromide study  has been completed and
reported to the Office of Toxic Substances in September 1975 under the
title of: "Sampling and Analysis of Selected Toxic Substances: Task II -
Ethylene Dibromide," EPA Report No. 560/6-75-001.

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     This report describes the Task IA of the program, i.e., the sam-
pling and analysis for HCB as follows:  experimental procedures; screen-
ing and selection of sampling sites; presampling surveys and field sam-
pling; discussion of results, sewage treatment facilities; and summary and
conclusions. Site surveys and field sampling data for individual sites,
analytical data, and methods development efforts are appended to the report.

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                               SECTION II

                         EXPERIMENTAL PROCEDURES

SAMPLING PROCEDURES

     Water was sampled by two different methods—grab sampling and porous
polymer extraction. The grab water samples were composited and stored in
glass 1-gal. bottles that had been used for pesticide grade solvents. In
the second technique, water was mechanically pumped through a 30 x 5.2
cm i.d. glass tube packed with 250 g Amberlite XAD-4. The Amberlite resin
removed HCB quantitatively from the water stream flowing at 0.6 to 1.4
liters/min. The composited water samples and the Amberlite resin tubes
were capped and stored in ice chests until ready for analysis.

     Air was sampled through a 37-mm diameter, 0.8 |j,m pore size, milli-
pore filter, followed by a 15-cm, 1.2-cm i.d., glass sampling tube* packed
with 1 g Tenax®-GC. Air was drawn through the filter and Tenax®-GC tube
with the aid of a mechanical pump. The flow rate was regulated with either
an 18-gauge needle («< 3.5 liters/min) or a 26-gauge needle («< 0.4 liters/
min). A schematic of the air sampling train is shown in Figure 1.

     Soil and sediment samples from the top 2 to 5 cm were collected at
designated sites. From 0.5 to 1 kg of sample was composited and stored
in wide-mouth glass bottles with Teflon®-lined caps and kept in an ice
chest until ready for analysis.

ANALYSIS PROCEDURES

Sample Preparation

     The millipore filter and the Tenax®-GC resin for each air sample
was sequentially extracted with 20,  20, and 10 ml of pesticide grade
hexane using an ultrasonic bath. During the extraction,  ice was added
to the ultrasonic water bath to minimize evaporative loss of HCB. The
hexane extracts were combined and diluted to 50.0 ml.
*  In sampling some industrial plants,  two Tenax®-GC tubes were used
     in tandem.

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                                                                       Critical
                                                                       Orifice
                                    \
Millipore
Filter
Tenax-GC
Tubes
                                                                                             Mechanical
                                                                                             Pump
                                   Figure 1.  Air sampling train

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     The  soil samples were first sifted on a U»S» Standard No. 18 sieve
to remove stones and other foreign material. A 100-g sample was then ex-
tracted with 100 ml of n-hexane in a soxhlet apparatus overnight. The
hexane extracts were transferred to 100-ml volume flasks and diluted to
volume. A similar sample preparation procedure was used on the sediment
samples except that the sifting step was omitted.

     A 500 to 1,000-ml portion of each grab water sample was extracted
sequentially with 20, 20, and 10 ml of hexane. The extracts were col-
lected in a 50-ml volumetric flask and diluted to volume. The Amberlite
XAD-4 resin was extracted with 250-ml hexane using a soxhlet apparatus.
The extract was collected in a 250-ml volumetric flask and diluted to
volume.

     All  of the extracted samples were kept in a walk-in cold room main-
tained at 4°C. Prior to analysis, the samples were brought to room tem-
perature  and diluted or concentrated as necessary for analysis.

Instrumentation and Conditions

     A Microtek-2000R gas chromatograph equipped with an electron cap-
ture (tritium) detector was used. The output of the gas chromatograph
was connected to a Hewlett-Packard 3380A integrator-recorder, which
provides  a printout of the chromatogram with integrated areas of in-
dividual  peaks and respective retention times. A 4 ft x 1/4 in. glass
column packed with 1.5% OV-17/1.95% QF-1 coated on 100/120 mesh Supel-
coport® was used as the primary column for analysis. A 6 ft x 1/4 in.
glass column packed with 37o XE-60 on 80/100 mesh chromosorb WHP was
used to verify and differentiate HCB from a-BHC. The chromatographic
operating conditions were:  injector temperature, 200°C; column tem-
perature, 150°C; detector temperature, 180°C; carrier flow rate, 100
ml/min nitrogen; purge flow rate, 90 ml/min nitrogen; and detector
voltage,  10 V DC.

     The  instrumental limit of detection for HCB at the above men-
tioned conditions was 2 pg (10  ^ g). Therefore, as an example, for
any amount of air sampled, the quantity of HCB in the sample required
for detection was greater than 10 ng (based on 10 |j,l injections of a
50-ml solution).

Calibration

     A 10 ng/ml composite standard solution of HCB was used to obtain
the calibration curves. The standard solution was prepared by dilution
of a stock solution made up from EPA reference standards obtained from
Pesticides and Toxic Substances Effects Laboratory,  National Environ-
mental Research Center, Research Triangle Park, North Carolina.  Con-
centration ranges chosen for the calibration curve were from 10 to 60
pg, and linearity was observed.

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     A new calibration curve was obtained daily for the sample  analy-
sis. During the day,  a known amount of the standard was injected peri-
odically into the GC  to check for changes in retention time and peak
intensity.

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                              SECTION III

                      SELECTION OF SAMPLING SITES

     The objective of this task was to determine environmental  levels
of HCB by the sampling and analysis of samples from selected industrial
plants. Therefore, it was important that the selected sampling  locations
be representative of the total industrial locations that  are sources of
HCB.

SELECTION CRITERIA

     Selection criteria were chosen to achieve representative sampling
of sites that are most likely to have detectable quantities  of  HCB
present.

     The criteria used for the selection of industrial plants for sam-
pling are:

     *  Estimated quantity of HCB in industrial wastes, products, and
        by-products.

     *  Methods of production.

     *  Methods of waste disposal.

     *  Geographic location of the industrial plants.

Estimated Quantity of HCB in Industrial Wastes,  Products,  and By-Products

     In 1974, the only active domestic producer of  HCB for sale was
Stauffer Chemical Company. However, industry sources report  that HCB
is contained in the "heavy ends" waste materials (residues)  in  the
production of many chlorinated organic compounds, as well  as in the
electrolytic processes (either diaphragm or mercury cells) for  chlo-
rine gas when graphite anodes are used. An estimation of  the amount
of HCB produced in industrial wastes,  by-products,  and products is
given in Table 1. As indicated in Table 1,  about 90% of the  HCB con-
tamination in the environment was estimated to be from the perchloro-
ethylene, trichloroethylene,  and carbon tetrachloride industries.—

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Table 1.  ESTIMATED QUANTITIES OF RGB PRESENT IN INDUSTRIAL
        WASTES, BY-PRODUCTS, AND PRODUCTS IN 1972I/
                                     U.S.
                                  Production
                                   in 1972
           Product                  (tons)       HCB (tons)

Perchloroethylene                   367,400        1,313
Trichloroethylene                   213,500          171
Carbon tetrachloride                498,500          150
Chlorine                          9,538,000          143
Dacthal®                   .           1,000           45
Vinyl chloride                    2,545,000           13
Atrazine, propazine, simazine        56,000            3.5
Pentachloronitrobenzene               1,500            2.3
Mirex                                   500            0.8
                              10

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Method of Production

     The production method affects the quantity of HCB formed as a by-
product. Therefore, the potential environmental contamination is depen-
dent upon the production method. For example,  carbon tetrachloride,
perchloroethylene, and trichloroethylene are produced in several ways.
If chlorine and the respective aliphatic hydrocarbons are fed into a
high-temperature reactor and the products are collected by distilla-
tion, HCB is discharged as a by-product in the "heavy ends" wastes.
However, if the production of carbon tetrachloride involves the reac-
tion of chlorine with carbon disulfide, coproducts or by-products,
other than reusable sulfur are greatly reduced.

Methods of Waste Disposal

     Disposal methods for "heavy ends" wastes  played a role in the se-
lection of plants for sampling. The selected plants used a variety of
disposal methods including landfill, deep well, sealed lagoons, on-site
incineration, and shipment of wastes to other disposal firms.

Geographic Location of the Industrial Plant

     Industrial plants were selected from across the country to deter-
mine whether the potential for environmental contamination posed a na-
tional problem.

RECOMMENDED SAMPLING SITES

     Using these general criteria as a guide,  10 industrial plants were
selected for inclusion in this study.

     These industrial plants are listed below:

Perchloroethylene

Stauffer Chemical Company                           Louisville, Kentucky
Vulcan Materials Company                            Wichita,  Kansas

Tr i chloroethy1ene

PPG Industry, Inc.                                  Lake Charles,  Louisiana
Diamond Shamrock Corporation                        Deer Park,  Texas
                                   11

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Carbon tetrachloride

E. I. du Pont de Nemours and Company,  Inc.          Corpus  Christ!, Texas
Dow Chemical Company                                Pittsburg,  California

Chlorine

Linden Chlorine                                     Linden, New Jersey
Kaiser Aluminum and Chemical Corporation            Gramercy, Louisiana

Triazine herbicides (atrazine, propazine,  simazine)

Ciba-Geigy Corporation                              St. Gabriel, Louisiana

Pentachloronitrobenzene

Olin Corporation                                    Mclntosh, Alabama

The geographic location and EPA region of  these plants  are  shown in Fig-
ure 2.

     During the process of selecting the sampling sites,  efforts were
made to select industrial plants that  produce a unique product  rather
than a combination of several products. The efforts  were  successful for
the two chlorine plants selected. However, plants producing low mo-
lecular weight chlorinated hydrocarbons do not generally  produce a single
product. All five plants that produce  trichloroethylene also produce per-
chloroethylene. Fortunately, not all the perchloroethylene  production
plants produce trichloroethylene. However, these plants also produce car-
bon tetrachloride. The annual production capacity (1972), process tech-
nology, and latest waste disposal methods  for each of the sampling sites
are presented in Table 2.

     The Dacthal® production facility  (Diamond Shamrock Corporation) in
Greens Bayou, Texas, was not selected  for  sampling because  the  waste hand-.
ling and product contamination were substantially changed from  pre-1972
procedures.

     Vinyl chloride and mirex production facilities  were  omitted from
this survey.
                                   12

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                                SOUTH DAKOTA
• Perch loroethylene
O Trichloroethylene
A Carbon Tetrachloride
^ Chlorine
• Pentachloronitrobenzene
D Atrazine
                                                          o    a.
             Figure 2.  Geographic location of recommended sampling sites

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                             Table  2.  PRODUCTION CAPACITY, PROCESS. TECHNOLOGY AND WASTE DISPOSAL AT RECOMMENDED SITES



Producers
Perchloroethvlene
Stauffer Chemical Company


Vulcan Materials Company
Trichloroethylene
PPG Industry Company

EPA
Production sites region

Louisville, Kentucky IV


Wichita, Kansas VII

Lake Charles, Louisiana VI
Annual
production
capacity
QO-3 tons)

35


25

140


Waste disposal

HCB recovered for sale,
remainder recycled to
chlorinator
Earth-covered groundfill

Incineration, landfill

a/
Process technoloev~





Chlorination with low molecular
weight hydrocarbons, e.g
ane, propane


Ethylene and chlorine as
. , eth-



raw tna-
Diamond Shamrock Corporation    Deer Park,  Texas
                                                          VI
                                                                                                             terials, under catalytic reaction
                                                                                                             at 250 to 300°C
                                         60      Ship to Rollins .Inter-
                                                 national for incineration
Carbon tetrachloride
E. I. du Pont de Nemours and
  Company, Inc.

Dow Chemical Company

Chlorine
Linden Chlorine Company
Kaiser Aluminum and Chemical
  Corporation

Triazine herbicides
Ciba-Geigy Corporation
Corpus Christi,  Texas       VI
Pittsburg, California      IX
Linden, New Jersey         II
Gramercy, Louisiana        VI
St. Gabriel, Louisiana     VI
                                         250
                                          23
66
58
                                       >  75
        Landfill,  ship  to outside
        firm for disposal

        Incineration
Discharge to holding pond
Landfill
                            Chlorination with methane at
                            elevated temperature
Mercury cell; graphite electrode
Diaphragm cell; graphite  electrode
        Still bottoms incinerated   Reaction of cyanuric chloride
        by an outside processor to  with appropriate amino hydrocar-
        extinction                  bons at elevated temperature
Pentach1oroni trobenzene
Olin Corporation
Mclntosh, Alabama
                           IV
 1.5    Stored in "blocks" covered  Nitration of pentachlorobenzene
        with plastic sheet          or chlorination of various chloro-
                                    nitrobenzenes in the presence of
                                    catalyst
j/  Kirk-Othmer, Encyclopedia of Chemical Technology  2nd ed.,  Interscience Publishers, New York, New York (1972).

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                              SECTION IV

                PRESAMPLING SURVEYS AND FIELD SAMPLING

     To plan the strategy for successful field sampling at  the  selected
industrial plants, a presampling survey was conducted at each plant.
Each presampling survey was arranged through telephone  contact  with the
appropriate plant officials whose names were provided by the EPA proj-
ect officer. Figure 3 shows the complete schedule for presampling  sur-
veys and field sampling.

PRESAMPLING SURVEYS

     During the presampling site survey, a plant  map was obtained. In-
formation regarding the possible sources of HCB contamination,  produc-
tion technology and waste disposal techniques were obtained. In addi-
tion, the production and waste disposal sites, as well  as the trans-
portation routes were delineated. Accessible electrical outlets inside
the plant were also located for possible use in air sampling. Meteoro-
logical conditions, such as wind direction and rainfall were investi-
gated. Tentative sampling dates were agreed upon, subject to final con-
firmation by plant officials prior to the departure of  the  sampling
crew from MRI.

FIELD SAMPLING

     Upon the completion of a presampling site survey,  the  sampling
strategy was planned. In general, air sampling stations were positioned
upwind and at several distances downwind from the suspected source(s)
of contamination. The air samplers were usually positioned  4 ft above
ground. When the wind direction was uncertain, stations were positioned
around the entire plant area.

     Water sampling was conducted upstream and downstream of waste ef-
fluent. Storm runoff was collected when appropriate. Water  samples from
equilization ponds or solar ponds were collected  to determine if the
ponds were sources of air contamination through liquid  vapor equilibrium
of HCB.
                                   15

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              May
June
July
August     September
Vulcan Materials
Wichita, Ks.
Linden Chlorine
Linden, N.J.
Stauffer Chemical
Louisville, Ky.
Dow Chemical
Pittsburg, Calif.
du Pont
Corpus Christ! , Tex.
Diamond Shamrock
Deer Park, Tex.
Ciba-Geigy Corp.
St. Gabriel, La.
Olin Corp.
Mclntosh, Ala.
Kaiser Aluminum
Gramercy, La.
PPG Industries
Lake Charles, La.
A —
A
A









—
A










A
A
A '
A





-
-
-
-
-
A
A









-
  A Presampling Visit




 •• Field Sampling




Figure 3.  Presampling  survey and field sampling schedule

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     Soil sampling was generally conducted along the plant boundaries,
transportation routes, and around waste disposal and storage  areas. Sed-
iment samples were collected from streams, equilization  ponds and natu-
ral solar ponds. Solids and liquid were also sampled from open disposal
pits. The preparation for sampling usually was conducted 3 to 5 days
prior to the sampling date. Sampling equipment was  sent  to the plant
scheduled for sampling. Major sampling equipment included vacuum pumps,
poles, rubber hoses, electrical prongs and adapters,  and sampling bot-
tles. To avoid possible breakage and contamination,  the  air sampling
train components, i.e., the filter and the Tenax®-GC tubes, as well as
the Amberlite XAD-4 sampling tubes were all hand carried to the site
by the sampling crew. Generators were rented at local dealers when elec-
trical outlets were not available in the plant.

     Because of the extensive sampling involved in  the first  two sites,
i.e., Vulcan Materials Company and Stauffer Chemical Company,  a four-man
crew was required. The rest of the sampling trips were conducted by two-
or three-man crews. Generally, 3 days were spent on  each sampling site.
The total number of samples analyzed for each sampling site is presented
in Table 3. A summary of air sampling parameters for each site is given
in Table 4. The sites at which HCB particulate was detected are indicated.
Detailed descriptions of the field sampling and presampling surveys con-
ducted at each plant are presented in Appendix A.
                                   17

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                   Table 3.  FIELD SAMPLING SUMMARY
       Site
        Air samples^'
 (stations x train components x
	sampling period)	
Total samples
(number/type)
Vulcan
Linden
Stauffer
Dow
Du Pont
Diamond Shamrock
Ciba-Geigy
01 in
PPG
          18 x 2 x 5
        No air samples
           9x2x6
           8x2x1
           8x2x1
           8x3x1
           8x2x1
           8x3x1
          10 x 3 x 1
 180 air
  10 soil
   4 water
   6 water
   3 solid
   1 soil
 108 air
   5 soil
   6 water
   3 sediment
  16 air
   3 soil
   1 water
  10 air
   3 soil
   7 water
   3 sediment
  24 air
   3 soil
   2 water
  16 air
   4 soil
   2 water
  24 air
  11 soil
  10 water
   1 sediment
  30 air
   4 soil
   7 water
   3 sediment
_a/  The total number of air samples consist of the number of air sampling
      stations times the components of the train, i.e., filter and Tenax®-GC
      resin times the number of sampling periods.
                                    18

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         Table 4.  SUMMARY OF AIR SAMPLING PARAMETERS

Plant
Vulcan^
Stauffer^
Dow
Du Pont
Ciba-Geigy-/
Diamond
Shamrock
OlinS/
PPG
Average
sampling
vol. (j£)
(1) 150-200
(2) 800-1,000
(3) 4,000
450
4,100
4,200
1,200-2,100
550

1,500-2,000
1,200
Average
sampling
time
(hr)
(1) 1
(2) 4
2
20
21
6-8
24

9
24
Rate
(jg/min)
0.5
0.5
3.5
3.5
3.5
3.5
0.4

3.5
0.4
Particulate
(HCB)
Yes
Yes
Limited
No
No
No
No

No
Yes
a]  Five 4-hr periods.
b_/  Six 4-hr periods (2 hr on, 2 hr off).
£/  Three 8-hr periods (each 2 to 3 hr sampling),
                                19

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                               SECTION V

                         DISCUSSION OF RESULTS

     Air, soil, water, and sediment samples were collected from nine
recommended industrial plants whose products included perchloroethyl-
ene, trichloroethylene, carbon tetrachloride,  triazine herbicides,
pentachloronitrobenzene and chlorine. In general,  HCB concentrations
varied from a maximum, near the production and waste disposal  areas,
to a minimum, in the samples taken upwind of a recognizable source.
However, in a few instances, HCB contamination was observed over  the
general plant area and a specific emission source was difficult to
determine. HCB was detected as both a vapor and a particulate;  the
predominate form was dependent upon the production and waste dispo-
sal methods of each plant. The results from each sampling site are
discussed below.

VULCAN MATERIALS COMPANY, WICHITA, KANSAS

     Field sampling at Vulcan Materials Company's  perchloroethylene
plant at Wichita, Kansas, was conducted on May 20, 1975.  Other com-
pounds of interest produced at this plant include carbon  tetrachlo-
ride and chlorine. The samples collected were:   180 air (90 filters
and 90 Tenax®-GC columns), 10 solid, and 4 water.

Air Samples

     The 180 air samples were collected from three samplers which were
positioned upwind, nine samplers immediately downwind of  the general
production and waste storage areas, and six sampling devices positioned
further downwind beyond the northern plant boundary. The  samplers be-
yond the northern plant boundary were positioned at three locations
with two samplers per location at 4 and 11 ft  above ground,  respec-
tively. The upwind and farthest downwind samplers  were operated con-
tinuously for a 4-hr period while those closer to  the general  produc-
tion and waste storage area were operated only  for the first hour of
each 4-hr period. After each 4-hr period, the  filter and  the Tenax®-GC
column in each sampler were replaced by fresh  components. The  sampling
                                   20

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strategy was designed so that results of the analysis  would  elucidate:
(a) the major sources and level of HCB emission,  (b) the  diurnal and
operation-related effects of HCB emission,  (c)  the physical  form,  i.e.,
particulate or vapor of HCB in the plant air, and (d)  the variation of
HCB concentrations with respect to sampler  distance above ground.

Sources and Levels of HCB Emission - The analytical data  for the 180  air
samples are tabulated in Table B-l of Appendix  B. Figure  4 shows the  av-
erage concentrations of HCB during the 20-hr sampling  period at the 18
sampling stations. It is obvious that major sources of HCB in the  air
are the production and waste storage ("Hex  Pit")  areas. In addition,
other sources of HCB are indicated by the upwind  air concentrations.

     The HCB levels in samples immediately  downwind of the production
and storage areas ranged from 0.1 to 24 |J,g/m3.  The levels of  HCB in the
upwind samples and samples taken downwind beyond  the northern plant bound-
ary were similar and in the range of 0,1 to 2.1
Variation of HCB Emission with Time - The variation of HCB  levels  over
the '20-hr sampling period is shown in Figures 5  through 7.

     Figure 5 shows that the HCB levels in air samples immediately
downwind of the production and waste storage area did  not increase
following the dumping of the "hex residue" at the "Perc Plant"  or  the
"Hex Pit." The increase in HCB at Stations 4 and 6 occurred either
prior to or significantly after dumping.
     The variation of HCB levels in samples beyond the northern  boundary
of the plant is shown in Figure 6. Each point  is the average  of  two  sam-
plers positioned at different heights (4 and 11 ft).

     Figure 7 shows that during the entire sampling period, HCB  lev-
els were relatively high in upwind Stations 16 through 18;  in fact,
the 20-hr average values were greater than some of the downwind  sta-
tions. Among the three stations, higher concentrations were detected
at Stations 17 and 18 which were closer to the landfill than  Station  16.

Physical Form of HCB - The average vapor and particulate concentrations
of HCB over the 20-hr sampling period at each  station are shown  in Fig-
ure 8. The physical state of the HCB detected  was dependent upon the  sam-
pling location. Particulate HCB was not detected in samples taken near
the solar pond (Stations 1 through 9) and at the northeast  corner (Sta-
tions 14 and 15),  northwest corner (Stations 10 and 11) and southwest
corner (Station 16) of the sampling area. At all other sampling  stations,
particulate HCB was approximately equal to or  much greater  than  (Sta-
tions 4 through 6) the HCB detected as a vapor.

                                   21

-------
  14 (O.U)
 ' 15 (0.10)
                  (0.36)8'


                   (I.I8>'7.
                  (5.72)6-
                  (1.56)5.
                  (5.52)4.
          Meteorologica
         rl    v. Station
               \
          I       \
          T
        QHex Pit   I
                                                       NORTH
    12 (0.88)
   '13 (1.16)
            (0.55) 3.
            (2.96)2.
            (0.34) 1«
§ Perc Plant
    10 (0.20)
   ' 11 (0.44)
                                      LEGEND
                                         Numbers 1 to 18 Air Sampling Sites
                                         Numbers in Parentheses  Represent
                                           Average Concentration of HCB
                                           Per 20 Hour  Period
                                                                     Scale 1/2" = 150'
                                                                                                      (0.82) 18«
                                                                                (1.08) 17«
                                                                                (0.38)16.
     South Ridge Road
Figure  4.   Average concentrations  (|Jig/m )  of HCB  in air  per  20-hr period at 18
                      stations at  Vulcan  Materials  Company, Wichita,  Kansas
                                                                                sampling

-------
to
u>
                       Perc Plant
                       Dumped Hex
Perc  Plant
and Hex Pit
Dumped  Hex
                                                                                                                 O Station
                                                                                                                 A Station
                                                                                                                 D Station
                                                                                                                 • Station
                                                                                                                 © Station
                                                                                                                   Station 6
                                                                                                                 A Station
                                                                                                                 A Station
                                                                                                                 O Station
                        Figure 5.   HCB concentration per 20-hr period at sampling stations within
                                       the  plant perimeter  (Vulcan)

-------
1.5

1.4

1.3

1.2

1.1
        Perc Plant
        Dumped Hex
                    Hex Pit
                    Dumped Hex
                                                                                       Perc Plant
                                                                                       and  Hex Pit
                                                                                       Dumped Hex
                                                                                                   • Stations  10&11
                                                                                                   A Stations  12&13
                                                                                                   D Stations  14&15
                 Figure 6.  HCB concentration per 20-hr period,  downwind  stations  (Vulcan)

-------
N)
Ul
             2.0
             1.5
         try
         i
             1.0
               2005
               0010
Perc Plant
Dumped Hex
           Hex Pit
           Dumped Hex
              0025
              0345
0355
0744
                                                                                    I
0752
1154
                                                                               Perc Plant
                                                                               and Hex Pit
                                                                               Dumped Hex
                                                                                                             • Station  16
                                                                                                             A Station  17
                                                                                                             O Station  18
1200
1430
                              Figure 7.   HCB concentration per 20-hr period, upwind stations (Vulcan)

-------
CO
            	 Tenax
            	 Filter
            J	I	I.     I
1      2     3
56     7     8     9    10

                    STATIONS
                                                                 11     12     13    14    15     16     17     18
                      Figure 8.   Average vapor and particulate concentrations of HCB in air
                               per 20-hr period at 18 sampling stations (Vulcan)

-------
     The variation of HCB levels over the 20-hr period in samples taken
near the "Hex Pit" was due almost entirely to variation in particulate
levels. Figure 9 shows the HCB vapor concentration at Station 4 was rel-
atively constant, near the 1 |j,g/m  level, whereas the particulate level
fluctuated from 0 to 10 |j,g/m . Particulate HCB was not observed during
the 0110 to 0220 and 0450 to 0550 sampling periods when vehicular ac-
tivity was probably low; particulate levels were 5 )j,g/m^ or higher dur-
ing the periods of 1945 to 2045, 0902 to 1010, and 1307 to 1425. Figure
10 shows a similar, but less pronounced pattern for upwind Station 18;
the HCB vapor concentration ranged from approximately 0.3 to 0.7 (ig/irP
while the particulate HCB varied from 0 to 1.2 (j,g/m .

     All samples showed a relatively constant HCB vapor concentration
during the entire sampling and fluctuating HCB particulate concentra-
tion (when detected) that probably reflects the activity in the immedi-
ate area of the sampling stations. A slight increase in HCB vapor con-
centration during the'warmer sampling periods was observed at some
sampling stations (Figure 10). This increase was not apparent until
the particulate and vapor concentrations were considered separately.

HCB Concentration Versus Sampler Height - A comparison of HCB concen-
trations at 4 and 11 ft for five time periods is shown in Table 5. The
results indicate that the differences in levels at the two heights were
not significant.

Precision of Sampling and Analysis - If it is assumed that the HCB lev-
els were the same at the two sampler heights (4 and 11 ft), the results
from each paired station, i.e., 10 and 11, 12 and 13, and 14 and 15, at
each of the five sampling periods can be considered as duplicates and a
pooled relative standard deviation (PRSD)* determined. The PRSD calcu-
lated from these data indicates the overall precision of the air sam-
pling and analysis methods including sample collection, storage, recov-
ery, and analysis. The PRSD is 17%. The PRSD is based on 13 duplicates.
Two duplicate measurements were not included in the calculations:  one
pair was near the detection limit (< 0.1 pog/m^) and the other station
had a high particulate level and was considered an outlier. The quanti-
ties of vaporous HCB detected in this station pair (Stations 12 and 13)
were approximately equal.
*  The PRSD was calculated as follows:
           S =  V  2  (X-!02/0.889


         RSD =  S/X x 100


        PRSD = V S  RSDi2/n

                                   27

-------
to
c»
10



 9



 8



 7



 6
           D);
              4



              3



              2
              0
                                            HCB Station 4 (Downwind Hex Pit)
                                         Filter

                                         Tenax-GC
                      I
                  1945-2045
                      0110-0220         0450-0550


                                   SAMPLING TIME
0902-1010
1307-1425
                       Figure 9.  Variation in vapor and particulate HCB levels at Station 4 (Vulcan)

-------
   1.2
    1.0
i
 =L
   0.5
     O1 u
                    HCB Station 18 
-------
 Table 5.  COMPARISON OF HCB
  LEVELS AT 4 AND 11 FT FOR
      FIVE TIME PERIODS
                  HCB,
Station pairs    4 ft   11 ft

  10 and 11      0.3     0.3
                 0.2     0.2
                 0.2     0.2
                 0.1     0.1
                 0.2     0.2

  12 and 13      1.0     1.0
                 0.4     0.5
                 1.2     1.3
                 1.4     1.3
                 0.4     1.7

  14 and 15      0.1     0.03
                 0.1     0.1
                 0.1     0.1
                 0.1     0.1
                 0.3     0.2
               30

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Soil Samples

     The nine soil samples and one "Hex Pit" solid sample were collected
at the following locations:  along the plant boundaries,  transportation
routes, landfill, the "Hex Pit" area and the production area. These sites
were selected to determine HCB soil levels associated with production,
waste disposal and transportation of wastes for disposal. Samples were
also taken upwind and in adjacent agricultural fields to  determine back-
ground concentrations in areas in the vicinity of the plant.

     The results of the analysis of the nine soil and one solid samples,
listed in Table 6, indicate that HCB soil concentrations  were in the 1
to 1,500 ppm range, with the exception of the "Hex Pit" soil and the "Hex
Pit" solids. HCB was 5% in the "Hex Pit" soil* and 21% in the "Hex Pit"
solids.

     Of the four plant boundaries, the highest level of HCB, 126 ppm,
was observed in soil from the southern boundary (S-8). HCB levels ranged
from 1.1 to 1.3 ppm in samples taken along the other boundaries.

     The observation of relatively high concentrations of HCB in the
southern boundary soil sample (S-8) could very well be the source of
high concentrations of HCB in the air samples collected at Air Sampling
Stations 16 through 18. The high concentration in the soil samples up-
wind of the production area could be due to the nearby landfill. This
rationale is supported by the presence of over 1,000 ppm  HCB in the S-5
sample, which indicates the landfill is a source of surface contamina-
tion in the immediate area.

     The soil on the route to the "Hex Pit" (S-2) and the soil from the
"Hex Pit" to the landfill (S-4) contained over 100 ppm HCB. HCB concen-
trations found in the water layer covering the "Hex Pit"  were also rela-
tively high. The results of the water analysis are presented below.

Water Samples

     Two samples were taken from Cowskin Creek (Figure A-3) which re-
ceives water from the sanitary sewer system and plant heat exchangers.
Samples were taken from the "Hex Pit" and solar pond to determine
their contribution to HCB levels in air and into the deep well which
receives water from the solar pond.
   Taken from a 10-ft radius of the "Hex Pit."
                                   31

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              Table 6.   HCB CONCENTRATIONS IN SOIL AND SEDIMENT
              FROM VULCAN MATERIALS  COMPANY, WICHITA, KANSAS
Samples-'
  S-2
  S-3
  S-4
  S-5
  S-6
  S-7
  S-8
  S-9
  S-10
"Hex pit"
  solids
Control
  Sample
weight (g)

  42.8
   2.5
  48.4
  38.
  40.
  29.
  35.
  43.
,7
.5
,6
,6
.5
  34.2
   0.95
Concentration
        HCB

        109
          57,
        157
      1,453
          5.6
          1.3
        126
          1.2
          1.1
         21%
         ND
a/  S-2 - Route from 'Terc Plant" to "Hex Pit."
    S-3 - "Hex Pit."
    S-4 - Route from "Hex Pit" to landfill.
    S-5 - Landfill (60 yards north of 63rd Street and 0.4 miles east of
            Ridge Road.
    S-6 - Landfill (180 yards north of 63rd Street and 0.4 miles east of
            Ridge Road.
    S-7 - Landfill (Ridge Road to telephone pole).
    S-8 - Upwind.
    S-9 - Downwind.
    S-10 - Western boundary (cornfield).
    Control - Soxhlet apparatus.
                                    32

-------
     The results of the water analyses are shown in Table 7. The HCB lev-
els were relatively low—parts per trillion in the Cowskin Creek water.

     A high concentration (306 ppb) in the "Hex Pit" water was expected
since this water covers the "hex residues" dumped in the pit. This water
is likely to be saturated with HCB. The concentration in the solar pond
was over two orders of magnitude lower than that in the "Hex Pit" water.
The source of HCB in the solar pond water could be from leaching of the
soil in the plant area or from vapor or airborne particulate from the
neighboring "Hex Pit."

Plant Summary

     The results of the analysis of all air,  soil, and water samples in-
dicate that the "Hex Pit" is the source of the highest levels of HCB. HCB
is present in particulate and vapor form in air samples taken from within
the plant area. The HCB detected in the downwind air samples beyond the
plant perimeter was present mainly as a vapor. There appears to be a rel-
atively constant air concentration of HCB vapor of approximately 0.1 to
1.0 ng/nr even in the upwind air samples. This background level of HCB
in air may be due to the HCB present in the general plant area soil and
landfill. The variation in HCB levels over the sampling period was due
primarily to variations in HCB detected in particulates. HCB concentra-
tions in soil (excluding the "Hex Pit" area)  ranged from 1 to 1,500 ppm.
The water samples taken beyond the plant area from Cowskin Creek contained
very low levels of HCB (parts per trillion range). Downstream levels of
HCB were twice as high as upstream levels.

LINDEN CHLORINE PLANT, LINDEN, NEW JERSEY

     The survey of Linden Chlorine Plant was  conducted on May 29,  1975.
During the intended presampling survey, it was apparent that an extended
air sampling plan was not warranted. Therefore,  sediment, water,  and soil
samples were taken during the survey.

     The Linden Plant was selected as a tentative sampling site because
graphite electrodes were used in the production  of chlorine and the plant
produced a single product. During our visit we learned that graphite elec-
trodes had been phased out at the end of March 1975.

     Seven water and four solid samples were  analyzed for HCB.  The results
are listed in Table 8. HCB was detected in the spent brine at 0.34 |j,g/liter.
Based on the instrumental detection limit for HCB, 2 pg (2 x 10    g)j  the
volume of water extracted, 1 liter; and the final extract volume,  50 ml;
the minimum detectable concentration of HCB in water was 10 parts  per
trillion.
                                   33

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            Table 7.   HCB CONCENTRATIONS IN WATER FROM VULCAN
                  MATERIALS  COMPANY, WICHITA, KANSAS
                         Volume sampled             Concentration
     Samples                 (liter)
ND - None detected.
"Hex Pit" water              0.315                        306

Solar Pond                   0.335                          0.7

Upstream
  (Cowskin Creek)          323                              0.009

Downstream
  (Cowskin Creek)          365                              0.018
                                   34

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           Table.8.   HCB CONCENTRATIONS IN WATER AND SOLIDS FROM
                LINDEN CHLORINE COMPANY, LINDEN, NEW JERSEY
                                                      Concentration (us/I)
              Sample                                          HCB
Water
  Holding pond, inlet                                          ND
  Holding pond, outlet                                         ND
  GAF weir, upstream of Cl£ plant                              ND
  Waste stream, downstream of Cl£ plant                   •     ND
  Process water                                                ND
  Tap water                                                    ND
  Spent brine water                                           0.34


Solid                                                 Concentration (ug/g)

  Holding pond, settled and suspended                          0.1
  Dredged solids adjacent to holding pond                      0.6
  Waste stream, downstream of Clo plant                        7.6
  Soil, around one of the cell buildings                       1.7
                                    35

-------
     All four solid samples contained HCB (from 0.1 to 7.6 |j,g/g)« The
highest level was observed in the waste stream sludge, downstream of
the plant. The HCB level in soil outside a cell building was 1.7 |j,g/g.

     Due to the complexity, i.e., large number of peaks, of these chro-
matograms, selected samples were fortified with standards to confirm the
presence of RGB. In addition, the samples were prepared and analyzed in
duplicate or in triplicate.

Plant Summary

     Air samples were not taken at the Linden Chlorine Plant because
graphite electrodes had been phased out prior to our sampling. HCB was
detected in spent brine. The highest concentration of HCB (7.6 |-ig/g)
was found in the sludge taken from the waste downstream of the plant.
The levels detected in the water and solid samples indicate this plant
is not a current source of significant quantities of HCB.

STAUFFER CHEMICAL COMPANY, LOUISVILLE, KENTUCKY

     Field sampling at Stauffer Chemical Company's perchloroethylene
plant at Louisville, Kentucky, was conducted on June 12, 1975. A total
of 108 air, (54 filters and 54 Tenax®-GC columns) 5 soil, 3 sediment,
and 6 water samples was collected. The results of the analysis of these
samples are discussed below.

Air Samples

     The 108 air samples were collected from nine samplers which were
positioned at nine locations surrounding the plant. The positioning of
downwind samplers was limited by a flood wall along the Ohio River.

     Sampling at these nine locations was divided into six 4-hr periods
and all samplers were operated 2 hr of each 4-hr period. After each 4-hr
period, the filters and the Tenax®-GC columns in the samplers were re-
placed. The sampling was conducted so that the analytical results would
indicate (a) the sources and levels of HCB,  (b) the diurnal and plant
operational effects, if any,  and (c) the physical form of HCB in the air.

Sources and Levels of HCB Emission - The results of the analyses are
listed in Table B-2 of Appendix B. The filters collected at the same
sampling station at various sampling times were combined to form one
sample to reduce the analysis time.  The combined filter analysis is
still indicative of the specific form of the two substances present
in the plant air. The average HCB concentration per 24-hr period at
each sampling station is shown in Figure 11.
                                   36

-------
u>
                                                                                                     150   200
                                                                                                    Immediate Plant
                                                                                                    Boundary
                                                                          Numbers in Parentheses Represent
                                                                          Average Concentration
                                                                          of HCB per 24 hr Period
                       Figure 11. Average concentrations  of  HCB in air at nine sampling stations
                                  at Stauffer Chemical  Company,  Louisville, Kentucky

-------
     The 24-hr average concentrations on the filter and in Tenax®-GC
resin at each sampling station are shown in Figure 12. The average HCB
concentration in upwind samples (Stations 1 and 2) were 0.07 and 0.05
fig/m , respectively, while downwind samples ranged from 0.04 to 1.2
|j,g/m . Of the downwind stations, the highest level of HCB was observed
at Station 4 which was located downwind from the perchloroethylene-
carbon tetrachloride plant. The level of HCB was somewhat lower at Sta-
tion 6, which was further downwind from the perchloroethylene-carbon
tetrachloride plant. Stations 3 and 7 also show significant levels of
HCB.

Variation of HCB Emission with Time - HCB levels detected during the
24-hr sampling period are plotted versus sampling time for each of the
nine sampling stations in Figure 13.

     Higher levels of HCB were observed during the first two sampling
periods (1000 to 1800 hr) which may be indicative of a diurnal effect.

     The removal of the solid waste drums from the plant area occurred
during the latter part of the first sampling period and early part of
the second (1400 to 1500 hr). HCB levels were uniformly high during
this period. The exact time when the drums were removed from the drum
loading area and transported off-site was not known.

Physical Form of HCB - There is some contribution to the total HCB lev-
els from particulates collected on the filters at Stations 3 through 6,
Surprisingly, HCB was not detected on the filters at Station 7, which
was near the drum loading area. Although particulate HCB was not de-
tected, settled particulates could contribute to the HCB level through
the solid-vapor equilibrium of HCB-contaminated particulates. HCB has
a boiling point of 230°C, but it co-distills with water vapor at low
temperature and readily sublimes. It is apparent from Figure 12 that
the major portion of HCB in the air was in the vapor state, since all
the stations showed higher levels in the Tenax®-GC resin than on the
filters.

Soil and Sediment Samples

     Two soil samples were collected along the plant boundaries, one
along the waste transportation route, and two from near waste handling
areas; three sediment samples were taken, two from the Ohio River and
one from the holding pond.
                                    38

-------
CO
 E
\
 O)
                                                                                 HCB
                                                                                    ——  Tenax
                                                                                    	  Filter
                     Figure  12.  Average  concentration of HCB in vapor and particulate
                                  at  nine sampling  stations (Stauffer)

-------
           3.0-1
                                                     KCB
           2.0-
-P-
o
        ^
        o>
           i.o-
           0.5-
                                                     Stations
                                                      • 1
                                                      x 2
                                                      O 3
                                                      A 4
                                                      a 5
                                                      e 6
                                                      A 7
                                                      0 8
                                                      • 9
           1000-1400
1400-1800
                                                  1800-2200
2200-0200
0200-0600
0600-1000
                          Figure  13.   HCB concentration per 24-hr period  at  sampling
                                           stations around the plant  (Stauffer)

-------
     The results, shown in Table 9, indicate that HCB soil concentrations
were generally in the low parts per million range with the exception of
the soil sample around the drum loading area (S-3), which contained 5,700
ppm HCB.

     The soil concentrations followed the same general pattern as the air
concentrations, i.e., the upwind sample had the least amount of HCB, 0.25
|j,g/g; the downwind sample (northern plant boundary) contained 4.75 |j,g/g.
Other soil samples—the settling pond, main road, and northern plant
boundary—show HCB levels from 5 to 20 times greater than levels found in
the upwind samples.

     Of the three sediment samples analyzed, the settling pond sample con-
tained the highest level of HCB, 284 ^g/g. The downstream HCB .concentra-
tion was higher (0.05 |j,g/g) than the upstream concentration (0.008 |J,g/g).
However, both concentrations are near the detection limit where the rela-
tive error in analysis is high.

Water Samples

     Six water samples were collected—one from the plant well and five
from the settling pond. The results are listed in Table 10. HCB was pres-
ent in the plant well water below the parts per billion level, i.e., 0.2
jj,g/liter. The HCB concentration in the settling pond (grab) after treat-
ment, i.e., the sample collected at the outlet, was half the HCB concen-
tration in the sample taken from the inlet (grab). However, data from
the 24-hr composite sample (collected by Stauffer) indicate that almost
all HCB was eliminated after treatment. The XAD-4 results agree quite
closely with the results obtained for the outlet grab sample.

     Generally, the 24-hr composite sample is more representative. How-
ever, in the samples analyzed here, it is very likely that some HCB was
lost during sampling for the 24-hr composite. The agreement between re-
sults obtained for the Amberlite XAD-4 resin and the grab sample substan-
tiate their validity.

Plant Summary

     The results of the analyses of all air samples indicate that the
carbon tetrachloride-perchloroethylene plant is the major source of HCB
in the general plant area.  Slightly elevated levels of HCB were also ob-
served on the eastern and western boundaries of the plant. The source of
this contamination is very likely from vapor-solid equilibrium of the
particulate "fall out" accumulated on the soil. The background level of
                                   41

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         Table 9.  HCB CONCENTRATIONS IN SOIL AND SEDIMENT FROM
            STAUFFER CHEMICAL COMPANY, LOUISVILLE,  KENTUCKY
                                             Concentration (ug/g)
                 Samples                               HCB

                  Soil

S-l - Upwind (southern plant boundary)                  0.25
S-2 - Plant road                                        2.25
S-3 - Drum loading area                             5,700
S-4 - Downwind (northern plant boundary)                4.75
S-5 - Settling pond area                                1.3

                Sediment

R-l - Settling pond                                   284
R-2 - Ohio River (upstream)                             0.008
R-3 - Ohio River (downstream)                           0.055
         Table 10.  HCB CONCENTRATION IN WATER FROM STAUFFER
                CHEMICAL COMPANY, LOUISVILLE, KENTUCKY
                                                Concentration (ug/l)
                   Samples                               HCB

   Plant well water                                      0.2
   Settling  pond  inlet  (grab)                            15
   Settling  pond  outlet  (grab)                            7
   Settling  pond  inlet  (24-hr composite)                 35
   Settling  pound outlet  (24-hr  composite)                0.7
   Settling  pond  outlet  (Amberlite  XAD-4)                 7
                                  42

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                            o
HCB in the air was 0.06 |j,g/m  . Average concentrations of HCB on the mil-
lipore filter versus the Tenax®-GC resin indicate that the major portion
of HCB in air was in the form of vapor rather than particulate. The HCB
concentration was highest in soil near the "drum loading area"--5,700
|ig/g« This level indicates a localized contamination from solid waste
handling. Otherwise, HCB concentrations from 0.25 to < 5 (ig/g were ob-
served in other soil samples around the plant. A slight buildup of HCB
levels was observed in samples taken along the waste transportation
route. Sediment samples from the settling pond showed high levels of
HCB, 284 M^g/g, but levels observed in samples taken from the Ohio River
were insignificant. Results for grab samples collected at the settling
pond outlet show excellent agreement with samples collected through
Amberlite XAD-4 resin; 7 p,g/liter of HCB for both.

DOW CHEMICAL COMPANY, PITTSBURG, CALIFORNIA

     Field sampling at Dow Chemical Company's carbon tetrachloride-
perchloroethylene plant at Pittsburg, California, was conducted on
August 7, 1975. A total of 24 air, including 8 filters and 16 Tenax®-GC
columns, 3 soil, and 1 water sample was collected.

Air Samples

     The 24 air samples were collected from 8 samplers, 2 of which were
placed upwind at the western plant boundary, 3 at the midplant area, im-
mediately downwind from the production and incinerator areas, and 3 far-
ther downwind at the eastern plant boundary. Because no significant di-
urnal effects were observed at the Vulcan and Stauffer plants where air
sampling was conducted in discrete 4-hr periods,  the sampling at Dow was
conducted for an integrated 24-hr period. Each sampling train was set up
with two Tenax®-GC columns in tanden to check for possible breakthrough
of HCB. The samplers were positioned so that results of the analysis
would indicate (a) the sources and levels of HCB emission, (b) the phys-
ical form of HCB, and (c) the efficiency of HCB collection.

Sources and Levels of HCB Emission - The results are presented in Table
B-3 of Appendix B. The average HCB concentration at each station is shown
in Figure 14. The upwind (Stations 1 and 2) concentration was 0.02 |j,g/m ,
while downwind concentrations ranged from 0.02 to 0.08 [j,g/m . The recorded
wind direction during the sampling was primarily from the west.

     The increase in HCB concentration observed for Stations 3 and 4 in-
dicates the production area which includes the thermal oxidizer (inciner-
ator) is a source of HCB emission. Elevated HCB levels did not extend be-
yond the plant boundary. HCB levels for the upwind Stations 1 and 2 are
about the same as those at downwind Stations 6 through 8. The results in-
dicate there is no widespread contamination of the plant area.
                                   43

-------
Numbers in Parentheses Represent
Concentration (fj.g/m^) of
HCB per 24 hr Period
                                                              6) (0.02)
                                                              7) (0.02)
                                                                                   N
                                                                                   t
0    500   1000
I	|	|
Scale  in Feet
                                                            ©(0.02)
                                                                               Immediate Plant
                                                                               Boundary
      Figure 14.  Average concentrations of HCB  in  air  at eight sampling stations
                     at Dow Chemical Company, Pittsburg,  California

-------
Physical Form of HCB - HCB was not detected on any of'the filter samples.
Since the instrumental limit of detection was 2 pg (2 x 10    g) for HCB,
for an average of 4,000 liters of air sampled, the quantity of RGB col-
lected in the form of particulates on each millipore filter was less than
10 ng. Therefore, HCB was present in the vapor form only.

     HCB was not found in the back-up Tenax®-GC tube, indicating that it
does not migrate through the Tenax®-GC resin.

Soil Samples

     Three soil samples were collected along the eastern, western, and
southern plant boundaries. The highest level (2.6 ^.g/g) was observed in
soil from the southern boundary (Table 11). Without additional informa-
tion on plant activities that might involve transportation of chlorinated
hydrocarbons, we cannot explain the distribution of HCB in the soil sam-
ples. The relative concentrations do not coincide with wind direction.

Water Sample

     One water sample was collected from the New York slough at the north-
west corner of the plant. However, the sample was lost when the bottle
containing the water was broken during shipping.

Plant Summary

     The results of the analysis of air samples from the Dow plant in-
dicate that the chlorinated hydrocarbon plant area which includes the
carbon tetrachloride, tri- and perchloroethylene plants is a source of
HCB. Relatively low levels of HCB, 0.02 |j,g/m^, were detected in air at
the eastern and western boundaries of the plant. Midplant HCB levels
were slightly elevated over background. The absence of HCB on the mil-
lipore filter indicates that HCB was in the form of vapor rather than
particulate in the plant air. The concentration of HCB was highest in
the soil collected along the southern plant boundary. HCB concentrations
of 0.22 |ig/g or less were observed in the soils collected from the west-
ern and eastern plant boundaries.

E. I. DU PONT DE NEMOURS AND COMPANY, INC., CORPUS CHRISTI,  TEXAS

     Field sampling of Du Font's carbon tetrachloride plant  at Corpus
Christi,  Texas,  was conducted on August 3,  1975. Because of  generator
failure,  only five air sampling stations were in operation,  which re-
sulted in the collection of a total of 15 air samples. The generator
failure limited the location as well as the number of samples taken.
In addition to the air samples, 6 soil and  sediment,  and 7 water sam-
ples were collected.


                                   45

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   Table 11.  HCB CONCENTRATIONS IN SOIL FROM DOW
       CHEMICAL COMPANY, PITTSBURG, CALIFORNIA
                                 Concentration (p»g/g)
       Samples                           HCB

Western plant boundary                  0.22

Eastern plant boundary                  0.014

Southern plant boundary                 2.6
                         46

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Air Samples

     The 15 air samples were collected from five samplers which were
positioned at two upwind, and three downwind locations from the gen-
eral production area. The samplers were operated continuously for a
period of 24 hr, with two Tenax®-GC columns in tandem.

Levels of RGB - The results of the analysis are listed in Table B-4
of Appendix B. HCB was not detected in either the upwind or the down-
wind samples. Sampling locations are shown in Figure 15. Based on the
instrumental limit of detection for HCB, 2 pg (2 x 10   g), and a 50-
ml solution with a 10-^,1 injection for gas chromatographic analysis,
the amount of HCB collected in a 4,000-liter sample was less than 10
ng.

Soil and Sediment Samples

     The three soil samples were collected along the southern and north-
ern plant boundaries, and near the landfill site. The sediment samples
were collected at the storm runoff outfall, settling pond inlet and out-
let. The HCB level observed in the landfill sample, 0.39 fig/m^, was higher
than the level in the upwind or downwind soil samples (Table 12).

     In the sediment, the highest level of HCB was detected in the storm
runoff outfall sample, 0.11 p,g/g. HCB (0.01 |o,g/g) was detected in the set-
tling pond outlet.

Water Samples

     The seven water samples were collected from plant facilities where
water was used either during the production process or for cleanup fol-
lowing production. Two types of sampling were conducted at the settling
pond, grab sampling and sampling through an Amberlite XAD-4 column.

     The results of the analysis of the seven samples are listed in
Table 13. HCB was not detected in the raw plant water. The highest con-
centration was detected in the water standing in the landfill, 2.8 p,g/
liter. HCB was detected in the settling pond water, 0.037 |j,g/liter in
the inlet and 0.015 p,g/liter in the outlet. However, HCB was not de-
tected in the grab samples taken at the inlet and outlet of the set-
tling pond because only 1 liter of water was sampled versus 125 liters
sampled through the Amberlite XAD-4 column.
                                    47

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00
                                           Landfill  Soil
                                           Composite
                                                                    Equalization  Pond
O                                                                    Production
                                                                    Area
             3)(ND)
        ND
Scale  in Feet


   Immediate Plant
   Boundary
               Figure  15.   Sampling stations  at  E.  I.  du Pont de Nemours and Company, Corpus  Christi, Texas

-------
     Table 12.  RGB CONCENTRATIONS IN SOIL AND SEDIMENT FROM E. I. DU
            PONT DE NEMOURS AND COMPANY,  CORPUS CHRISTI, TEXAS
                                                   Concentration  (ug/g)
       Soil samples                                          RGB

Upwind (southern boundary)                                  0.16
Downwind (northern boundary)                                (h015
Landfill area                                               0.39

        Sediment

Settling pond inlet                                          ND
Settling pond outlet                                        0.01
Storm runoff outfall                                        0.11
        Table 13.  RGB CONCENTRATIONS IN WATER FROM E.  I. DU PONT
               DE NEMOURS AND COMPANY, CORPUS CHRISTI,  TEXAS
                                                       Concentration
             Samples                                         HCB

W-l   Raw plant water before  use                             ND
W-2   Settling pond inlet  (amberlite)                        0.037
W-3   Settling pond inlet  (grab)                             ND
W-4   Settling pond outlet  (amberlite)                       0.015
W-5   Settling pond outlet  (grab)                            ND
W-6   Storm runoff outfall  (grab)                            ND
W-7   Water standing in  landfill                             2.8
                                    49

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 Plant  Summary

     HCB  was not  detected  in any of the air samples. The concentration
 of RGB was highest  in the  soil collected around the landfill area. Of
 the  water samples,  the highest concentration of HCB was detected in the
 landfill  standing water. The landfill area is a source of elevated soil
 and  groundwater HCB levels. In general, the levels of HCB in this plant
 were very low. The  plant began operations as recently as 1973 and ap-
 pears  to  be successful in minimizing HCB emissions.

 DIAMOND SHAMROCK  CORPORATION, DEER PARK, TEXAS

     Field sampling at Diamond Shamrock Corporation's trichloroethylene
 plant  at  Deer Park,  Texas, was conducted on August 20, 1975. A total of
 24 air, including 8 filters and 16 Tenax®-GC columns, 3 soil, and 2 wa-
 ter  samples was collected.

 Air  Samples

     The  24 air samples were collected from eight sampling stations,
 five of which were  positioned in a circle around the production area;
 two  locations were  along the north boundary and one at the south bound-
 ary  of the plant  area. Changing wind directions (TAble A-13) during sam-
 pling  prevented the samplers from being positioned in upwind and downwind
 locations. The sampling was conducted over three 8-hr sampling periods
 covering  3 days.  Rain interrupted the second sampling period and pre-
 vented sampling during 1200-1700 hr on any of the 3 days. The samplers
 were operated at  0.4 liters/min, resulting 600 liters or less of air
 sampled.  Two Tena:x®-GC columns were used in tandem.

 Sources and Levels  of HCB Emission - A simplified plant map with the
 sampling  locations  is shown in Figure 16. HCB was not detected in any
 of the samples.

 Soil Samples

     Three soil samples were collected from (a) along the northern .
 plant  boundary, (b)  along the southern plant boundary, and (c) the
 production area.

     The  results  of  the analysis of the three soil samples are shown
 in Table  14. The  highest concentration of HCB was detected in the pro-
 duction area,  i.e.,  24 |ig/g. A higher level of HCB was detected in the
 soil sample collected near air sampling Station 1 (0.68 (j,g/g) than in
.the  samples collected near Stations 7 and 8  (O.OlT~|j,g/g).
                                   50

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                                                           N
                                                     0 -  • 300   600
                                                      Scale  in  Feet
                                                          Immediate  Plant
                                                          Boundary
Figure 16.  Stations at Diamond Shamrock Corporation, Deer Park, Texas
                                 51

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        Table 14.   HCB CONCENTRATIONS IN SOIL FROM DIAMOND SHAMROCK
                       CORPORATION, DEER PARK, TEXAS
                                                     Concentration (ug/g)
        Soil samples                                         HCB

Upwind  (southern boundary)                                  0.68

Downwind  (northern boundary)                                0.08

Production area                                            24.0
                                    52

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Water Samples

     The two water samples collected for the analysis of HCB were the
raw plant water and plant effluent. The results shown in Table 15 in-
dicate that HCB was not detected in the raw water. However, 0.1 (o,g/
liter of HCB was detected in the plant effluent. This effluent is dis-
charged into nearby Pattrick Bayou.

Plant Summary

     HCB was not detected in the air samples from any of the sampling
stations. HCB was detected in soil samples collected along the northern
and southern plant boundaries at parts per billion levels. The concen-
tration of HCB in production area soil was 24 |J,g/g« The inlet plant wa-
ter did not contain detectable quantities of HCB while the process plant
effluent showed an HCB level of 0.1 |j,g/liter.

CIBA-GEIGY CORPORATION, ST. GABRIEL, LOUISIANA

     Field sampling at Ciba-Geigy Corporation's triazine herbicide plant
in St. Gabriel, Louisiana, was conducted on August 13, 1975. A total of
16 air, 4 soil, and 2 water samples was collected.

Air Samples

     The 16 air samples were collected from eight samplers which sur-
rounded the entire production area. Stations 2, 4, 6, and 8 were posi-
tioned about 400 ft,  and Stations 1, 3, 5, and 7 were approximately
1,000 ft from the production area. One Tenax®-GC column was used in
the sampling train. The sampling was conducted 2 hr of every 8-hr pe-
riod, over a 24-hr period.

Sources and Levels of HCB Emission - The results of the analyses are
listed in Table B-16 of Appendix B. The average concentrations of HCB
are shown for each sampling station in Figure 17. HCB concentrations
were from nondetectable to 0.02 fig/m . The wind directions were quite
erratic during sampling, and upwind-downwind patterns were not observed.
HCB in the plant air was in the form of vapor rather than particulate.

Soil Samples

     Four soil samples were collected from the general areas of Air
Sampling Stations 1,  3, 5, and 7, respectively. The results of the
analysis are listed in Table 16. HCB was found in only two samples—
around Air Sampling Stations 3 and 5,  at 0.003 and 0.011 |j,g/g, respec-
tively. The analysis of the soil samples collected near Station 7 was
negative.
                                   53

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          Table 15.  HCB CONCENTRATIONS IN WATER FROM DIAMOND
                  SHAMROCK CORPORATION, DEER PARK, TEXAS
                                                       Concentration
             Samples                                           HCB

W-l     Raw unused plant water                                 ND

W-2     Plant effluent                                         0.1
                                 54

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                                             Numbers in Parentheses Represent
                                             Average Concentration
                                             of HCB per 24 hr Period
                            (0.02) (3
                2)(O.OI)
(ND)    (8
Production
Area
                                   (0.01)
                                 Effluent Pond
0
I
 400
	I	
 800
	I
                                                                    Scale  in  Feet
                                                                                               Immediate  Plant
                                                                                               Boundary
       Figure 17.  Average concentrations of  HCB in air at eight sampling  stations
                     at Ciba-Geigy Corporation,  St.  Gabriel, Louisiana

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    Table 16.  HCB CONCENTRATIONS IN SOIL  FROM CIBA-GEIGY CORPORATION,
                          ST. GABRIEL,  LOUISIANA
                                                     Concentration (ug/g)
             Soil samples                                    HCB

S-l   Northwest of plant at Air Sampling                     ND
        Site No. 1
S-2   Northeast of plant at Air Sampling                    0.003
        Site No. 3
S-3   Southeast of plant at Air Sampling                    0.011
        Site No. 5
S-4   Southwest of plant at Air Sampling                     ND
        Site No. 7                                     .      ,
                                  56

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Water Samples

     Two grab samples were collected, raw plant water and process efflu-
ent. HCB was not detected in either sample.

Plant Summary

     The concentrations of HCB in the plant air were very low--from 0.01
to 0.02 |j,g/m . In the soil, HCB was detected in the low parts per billion
range. Since HCB was not detected in the process effluent, the water dis-
charged into the Mississippi River contains less than 10 ng/liter of HCB.

OLIN CORPORATION, MCINTOSH, ALABAMA

     Field sampling at Olin Corporation's pentachloronitrobenzene (PCNB)
plant at Mclntosh, Alabama, was conducted on August 18,  1975. A total of
24 air, including 8 filters and 16 Tenax®-GC columns, 12 soil and sedi-
ment, and 10 water samples was collected. In addition to the PCNB plant,
this facility included a chlorine production plant which used graphite
electrodes in the production process.

Air Samples

     The 24 air samples were collected from two samplers positioned at
the southern boundary, three at the mid-plant area, three north of the
PCNB production plant, and three at the northern boundary. Each sampling
train consisted of a millipore filter and two Tenax®-GC  columns. Essen-
tially no breakthrough of HCB through the first column was observed. The
samplers were operated 3 hr of each 8-hr period for three 8-hr periods.
The wind direction during the sampling varied. Therefore, upwind-downwind
stations could not be designated.

Sources and Levels of HCB Emission - The results of the  air sample anal-
ysis are listed in Table B-7 of Appendix B. The sampling locations and
average 24-hr HCB concentrations are shown in Figure 18; HCB concentra-
tions ranged from 0.04 to 2.2 |j,g/m . From the map of the plant area shown
in Figure 18, three possible sources of HCB are apparent:  the PCNB pro-
duction area, the "hex" storage area, and the chlorine production area.
The highest concentrations of HCB were observed in the samples collected
along the southern boundary. These samples were south-southwest of the
"hex" storage area, which, is in the southeast corner of  the plant. The
wind was recorded from almost all directions during the  sampling, but
the highest wind speed was observed when the direction was from the
north-northeast and the north. Neglecting direction and  notwithstanding
Station 1,  the closer the sampler was to the "hex" storage area,  the
greater the HCB concentration. These results indicate that the "hex"
storage area is the primary source of HCB. Because of the varied wind
                                   57

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(0.04)
                            2
                           V_x
                          (0.06)
                        (0.26)
                                Chlorine
                                Production
                                Area
                 (0.03)     (0.24)     (0.48)
                    Strong
                    Brine
                    Pond
                   Weak
                   Brine
                   Pond
                 O
                                     Production
                                     Area
Numbers in Parentheses Represent
Average Concentration
of HCB per 24 hr Period
(i.ID®
                        Hex
                        Storage
                        Area
                                   (2.22)
                                                                     N
                                                                     1
                                           0     160    320
                                            I	i	i
                                            Scale in  Feet
                                                                   Immediate Plant
                                                                   Boundary
            Figure 18.  Average concentrations of HCB in air at
                 eight sampling stations  at  Olin Corporation,
                               Mclntosh,  Alabama
                                     58

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conditions, it is difficult to quantitatively determine the contribu-
tion of the PCNB production plant to HCB emissions but it appears to
be much less than the "hex" storage area. The HCB emission from the
chlorine production plant is negligible since the air concentrations
at stations closest to the chlorine production area were from 0.03 to
0.06 |j,g/m3.

Physical Form of HCB

     HCB was not detected in any of the filters indicating that it was
present as a vapor rather than in particulate form. The absence of par-
ticulate HCB is somewhat surprising since the heavy wastes from PCNB pro-
duction are stored in solid blocks in the storage area. The blocks are
covered with plastic sheets which appear to be effective in eliminating
particulate HCB in the air but not HCB vapor. Sporadic rain and low wind
speed during the sampling also may have reduced the particulate HCB.

Soil and Sediment Samples

     The 12 soil and sediment samples were collected from plant bound-
aries, transportation routes, landfill and storage areas.

     The results of the analysis of these samples are shown in Table 17.
The concentration levels were from a low of 0.98 fj,g/g (soil from the
brine pond area) to a high of 13% (soil from the "hex" storage area).
The blocks of "hex" wastes stored in this area contain up to 80 to 90%
HCB. The soil sampled along the transportation route of the "hex" blocks
showed an HCB concentration of 4,100 pg/g. HCB concentrations over 100
ppm were detected in samples collected along the road to the old land-
fill, and from within the old landfill. It was learned that prior to
the practice of casting the "hex" wastes into blocks, the old landfill
was used for the "hex" disposal.

     Soil samples from the east road, as well as the "hex" storage area,
old landfill and the current landfill area all show much higher levels
of HCB than those detected on the west road. The relative concentrations
of the air samples followed the same pattern.

Water Samples

     Ten water samples were collected:  two from ditches within the plant
area, three from the nearby creek,  one from the settling pond, two from
the solar pond, and two from the two brine ponds (strong and weak).
                                    59

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             Table 17.   HCB CONCENTRATIONS IN SOIL AND SEDIMENT
                    OLIN CORPORATION, MCINTOSH, ALABAMA
                                                      Concentration (ug/g)
                  Samples                                    HCB
Soil
S-l   Northern boundary road                                3,200
S-2   Old landfill (northeastern boundary)                    480
S-3   Brine pond area                                           0.98
S-4   Center road (running north/south)                        72  •
S-5   High-lift route (organic plant to storage
        area)                                               4,100
S-6   Southeast landfill                                       53
S-7   "Hex" storage area                                       13%
S-8^.' Old "Hex" dump area                                   Not analyzed
S-9   East road                                               400
S-10  West road                                                 1.1
S-ll  South road                                              350

Sediments

Strong brine pond sediment                                     12
a/  This sample is mostly tar which is used to cover the general old "Hex"
      area; the extracted solution was so dirty that analysis was not pos-
      sible even after cleanup.
                                   60

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     The results are shown in Table 18. The highest level of HCB, 159
|j,g/liter, was detected in the spent brine pond. Concentrations ranged
from nondetectable to less than 10 |j,g/liter in the other samples.

     The relatively close agreement of the HCB concentrations deter-
mined in the single grab sample (5.0 |j,g/liter) versus the 24-hr com-
posite sample (2.5 p,g/liter) of the creek water collected 200 yd up-
stream of the basin indicates the instantaneous HCB concentration
did not vary significantly from the 24-hr average. HCB was not de-
tected in the basin water indicating that detectable amounts of HCB
were not discharged into the Tombigbee River.

Plant Summary

     The results of the analysis of air, soil, sediment, and water
samples indicated that the "hex" storage area is the primary source
of HCB contamination, whereas the PCNB production area, old landfill
site, and weak brine pond are secondary sources. The chlorine produc-
tion plant is not a source of HCBD. Soil and sediment samples showed
relatively high levels of HCB—from 0.98 to 1.3 x 105 |j,g/g. All the
plant road samples contained HCB:  the lowest was on the west road
(1.12 (J,g/g), the highest on the "high-lift road" (organic plant to
storage area, 4.1 x 10  (J,g/g)» Detectable quantities of HCB were not
discharged into the Tombigbee River.

PPG INDUSTRIES, INC., LAKE CHARLES, LOUISIANA

     Field sampling at PPG Industries' trichloroethylene and perchloro-
ethylene plant at Lake Charles, Louisiana, was conducted on September 4,
1975. A total of 30 air, including 10 filter, 20 Tenax®-GC columns, 7
soil and sediment, and 7 water samples was collected.

Air Samples

     The 30 air samples were collected from 10 samplers which circled
the plant. The samplers were not positioned in an upwind-downwind ar-
ray because varied wind direction was expected from information ob-
tained during the presampling site visit. However, the wind was pre-
dominately from the east and east-southeast during sampling. Samplers
were positioned to take advantage of existing electrical outlets, also.
The sampling was conducted for an integrated 24-hr period; two Tenax®-GC
columns in tandem were used.
                                   61

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      Table  18.    HCB CONCENTRATION IN WATER .FROM OLIN CORPORATION,
                            MCINTOSH, ALABAMA
                 Samples                            HCB concentration (ug/l)

W-l     Weak brine pond                                       160
W-2     Strong brine pond                                       1.4
W-3     Settling pond                                         ND
W-4     North/south running ditch                               1.0
W-5     Southern ditch area (upper drop)                        7.5
W-6^'   Combined creek (200 yard before basin)                  5.0
W-7-'   Basin (at mouth of creek)                '             ND
W-8     24-Hr composite of plant effluent                       2.5
     ,     (combined creek)
W-9^    Solar pond, west                                        3.8
W-10^-   Solar pond, east                                      ND
B-l     Sampling bottle blank
B-2     Sampling bottle blank                   Average
B-3     Sampling bottle blank
0.4
a/  All water samples using Olin's sample bottles are reported after sub-
      tracting blank bottle value.
                                    62

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Sources and Levels of HCB Emission - The results are shown in Table B-8
in Appendix B. A simplified plant map with the sampling locations and the
24-hr average concentrations (Tenax®-GC plus filter) of HCB is shown in
Figure 19. HCB concentrations were from nondetectable,  at Stations 8 and
9, to 1.7 |o,g/nr at Station 7. Relatively higher concentrations of HCB
were detected at Stations 4 through 7, which were located downwind of
the incinerator-production area. The presence of low concentrations of
HCB at Stations 2, 3, 9, and 10 could be due to other sources, e.g., the
old landfill site and the barges which were located upwind.

     The presence of HCB beyond the northern plant boundary is probably
due to the incinerator since Station 6 is somewhat downwind. However, a
relatively high level of HCB was detected at Station 1 which is upwind
of the incinerator and plant area. The HCB level in this sample may in-
dicate a general contamination of the area south of the plant. Sampling
Station 6 was located in a sparsely populated residential area.

Physical Form of HCB - Figure 20 shows that HCB was predominantly in the
form of particulate rather than vapor (majority detected on the filter).

     The occurrence of HCB in particulate form could be the results of
(a) particulates from the incinerator or (b) the production process em-
ployed by PPG for perchloroethylene and trichloroethylene. PPG uses a
catalytic oxychlorination technique, resulting in a lower reaction tem-
perature than that generated by the thermal chlorination of hydrocarbons.—

Soil Samples

     Four soil samples were collected:  two at the plant boundaries, one
along Mobil South Road, and one from the landfill. The results are shown
in Table 19. The levels of HCB in the soil ranged from 0.015 (J,g/g, around
Air Sampling Stations 8 through 10, to 0.10 |j,g/g, along Mobil South Road
and around Air Sampling Stations 4, 5, and 7.

     The elevated levels of HCB at Stations 4, 5, and 7 are consistent
with a prevailing east and east-southeast wind resulting in particulate
fallout and vapor condensation from the incinerator and production plant.
The concentration detected in the Mobil South Road composite sample in-
dicates the PPG canal is a possible source of HCB. The results of sedi-
ment and water analyses discussed below support this possibility.

Sediment Samples

     The three sediment samples were taken one each from the PPG canal
(near Air Sampling Station 1), the ship channel, and the main effluent
from the organic plant. HCB was detected in all three sediment samples;
the lowest level (0.01 |j,g/g) was in the ship channel, and the highest
in the sediment at the organic plant effluent (0.87 |o,g/g). The presence
of HCB in the ship channel sediment may be associated with waste load-
ing into the barges.
                                   63

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   Numbers in Parentheses Represent
   Concentration (^i.g/m^) of
   HCB per 24 hr Period
                                                                              Immediate Plant
                                                                              Boundary
Figure 19.
Average concentrations  of  HGB in air at 10 sampling stations
   at PPG Industries, Lake Charles,  Louisiana

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CO
    O1
                                                                                                      HCB

                                                                                              	  Tenax
                                                                                              	  Pilfer
                                                     5.           6
                                                        Station
8
10
            Figure 20.    Average concentrations  of HCB in vapor and particulate at 10 sampling stations
                                       around the plant (PPG Industries)

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            Table 19.   HCB  CONCENTRATIONS IN SOIL AND SEDIMENT
               FROM PPG INDUSTRIES, LAKE CHARLES, LOUISIANA
                                                    Concentration  (ug/g)
              Samples                                          HCB

Air Stations 4, 5, 7 soil composite                           0.10
Air Stations 8, 9, 10 soil composite                          0.015
Mobil south road                                              0.10
Landfill                                                      0.025

              PPG sediments

Sediment 1 (downstream PPG canal)                             4.4
Sediment 2 (main organic plant effluent)                      6.9
Ship channel sediment                                         0.01
                                    66

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     The presence of significant amounts of HCB (4.4 |j,g/g) in the down-
stream PPG canal sediment indicates accumulation of deposits from the
organic plant effluent. This sediment was collected 1,000 ft beyond Air
Sampling Station 1, i.e., at least 4,000 ft from the organic plant.

Water Samples

     Seven water samples were collected:  one from the lake (incinerator
feed), one incinerator scrubber, two from the treatment canal,  one from
the landfill (standing water), one from the PPG canal, and one from the
ship channel.

     The results are shown in Table 20. The highest concentration of HCB
(7.1 fig/liter) was detected in the treatment canal inlet sample, and the
landfill surface water. The treatment canal outlet contained 4.1 fig/liter
HCB, indicating that the treatment removed about 40% of the HCB. The sam-
ple collected downstream of the PPG canal near Air Sampling Station 1 con-
tained 1.1 |j,g/liter HCB. This concentration in the canal water at more
than 3,000 ft downstream from the effluent point is consistent with the
levels detected in sediment collected 1,000 ft further downstream.

     The lake water (incinerator feed water) contained 0.22 [j,g/liter HCB.
This level of HCB could, depending on the amount of feed water versus
"liquid bottoms" that passes through the incinerator, contribute signi-
ficantly to the HCB emission from the incinerator.

     The. scrubber water from the incinerator contained a lower level of
HCB (0.09 |j,g/liter) than the feed water and the treatment canal inlet.

Plant Summary

     The primary source of HCB in air is the incinerator and organic plant.
The HCB present in the incinerator feed water (0.22 ng/liter) may be a fac-
tor in HCB concentrations in air. The HCB was present predominantly as par-
ticulate in air. This plant was unique in the relative distribution of HCB
in air versus soil, sediment and water. The air concentrations were rela-
tively high at this plant when considering the relatively low concentra-
tions in the other types of samples. The distribution of HCB may be ac-
counted for by the plant production and waste disposal methods. Solid wastes
are not formed in the low temperature catalytic oxychlorination production
process. "Liquid bottoms," which contain HCB,  are incinerated;  process
water, which contains lighter chlorinated hydrocarbons, e.g., HCBD,  is
treated and flows into the PPG channel and eventually the Calcasieu River.
Water sampled in the PPG canal at a point approximately 3,000 ft from the
organic plant effluent contained 1 ppm HCB. The HCB concentration in a
sparsely populated residential area downwind of the incinerator was 0.36
                                    67

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             Table 20.  RGB CONCENTRATIONS IN WATER FROM PPG
                   INDUSTRIES, LAKE CHARLES, LOUISIANA
                                                    Concentration
              Sample                                       HCB

Incinerator feed water (lake water)                       0.22
Scrubber water                                            0.09
Inlet (treatment canal)                                   7.1
Outlet (treatment canal)                                  4.12
Surface water (landfill)                                  7.1
Downstream PPG canal  (Mobil Bridge No. 1)                 1.1
Ship channel (next to Air Station No. 10)                  ND
Note:  ND = none detected.
                                   68

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                               SECTION VI

                       SEWAGE TREATMENT FACILITIES

     Chlorination as a means of disinfecting treated sewage has been
known to result in the "in situ" synthesis of numerous halogenated hy-
drocarbons. It was not known whether HCB is produced in significant
concentrations by this process. For this reason, samples were collected
from two sewage treatment plants utilizing chlorination and analyzed for
HCB.

SAMPLING

     Samples were collected from two sewage treatment facilities in the
Kansas City area. Both facilities utilize chlorination for disinfecting
the treated sewage. One-gallon samples were collected from the sewage
treatment stream immediately before and after the chlorination step. The
samples were returned to MRI and stored at 4°C until analyzed.

EXPERIMENTAL PROCEDURES

     A 1-liter sample of the sewage treatment effluent was extracted
twice with 100 ml of 157» (v/v) ethylether in hexane and once with 100
ml of hexane. The extracts were combined and dried by passage through
Na2SOA. The sample volume was reduced to 5 ml by means of a Kuderna-
Danish evaporator. One milliliter was reserved and the remaining 4 ml
were reduced to 1 ml using a slow stream of N2 to evaporate the solvent.
The samples were analyzed using electron capture gas chromatography. The
column was 6 ft x 1/4 in. o.d. packed with 4.0% SE-30 and 6.0% OV-210 on
ChromosorbW HP. The operating conditions were as follows:  injector tem-
perature, 220°C; column temperature, 200°C; detector temperature, 250°C;
and carrier gas, 17 ml/min.
                                  69

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RESULTS

     Analysis of both sewage samples collected ahead of the chlorination
facilities showed no significant peaks at the retention time of HCB.  Based
upon the instrumental sensitivity toward HCB and the concentration  enhance-
ment by extraction and evaporation,  the sewage samples contained less than
1 part per trillion HCB.

     The samples collected after the chlorination facility gave highly com-
plex gas chromatograms. Numerous peaks were present  at and near the reten-
tion time of HCB. Assuming that the  observed peak at the retention  time of
HCB was due solely to HCB, the sewage samples contained a maximum of  4 to
8 ppt HCB. As this was undiluted sewage, it appears  that chlorination of
raw sewage produces a negligible quantity of HCB.
                                    70

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                               SECTION VII

               SUMMARY AND CONCLUSIONS FOR PROGRAM TASK IA

SUMMARY

     A summary of results is listed in Table 21. The high and low con-
centrations of HCB are listed for each type of sample,  along with the
products and waste-disposal methods for each site.

     Figure 21 shows the highest levels of HCB in air and the levels
detected in the samples taken the greatest distance downwind from the
suspected source(s) at each plant. Sampling distances from each source
are shown in parentheses. The concentrations shown in Figure 21 should
not be compared directly because of differences in sampling distances,
meteorological conditions, etc., during sampling.

     In general, higher concentrations of HCB were associated with the
production of perchloroethylene and trichloroethylene than with other
industries. However, most of the chlorinated hydrocarbon plants produced
a combination (perchloroethylene, trichloroethylene, carbon tetrachlo-
ride,  etc.) of products which makes it difficult to extrapolate the re-
sults obtained at a particular plant to a single product. In the one
plant that produced only carbon tetrachloride, the HCB levels were
quite low. The HCB concentrations detected in samples from the penta-
chloronitrobenzene production plant were relatively high, i.e., |j,g/m
range in air. The levels of HCB associated with plants  producing chlor-
ine and triazine herbicides were very low.

     Several different waste-disposal methods were used at the perchloro-
and trichloroethylene plants that were sampled. They included off-site
and on-site landfill combined with open pit or pond storage and off-site
and on-site incineration. Higher levels of HCB were detected in air and
soil at the plant using on-site landfill and open pit storage. The levels
of HCB detected in soil and samples taken upwind of suspected point sources
indicated a wide area of HCB contamination at this plant. Elevated HCB lev-
els were detected in loading and transfer areas at plants using off-site
                                   71

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                                                  Table  21.   DATA SUMMARY FOR  PROGRAM  TASK  NO. 1
NJ
Cone any
Vulcan Hater la li Company
Wichita. Kansas
Stauffer Chemical Coopany
Louisville, Kentucky
Dow Chemical Company
Pittsburg, California
E. I. du Pont de Meraour*
Corpus Chrlstl, Texas
Diamond Shanrock
Deer Park, Texas
Olln Corporation
Kclntosh, Alabama
Clba-Ceigy Corporation
St. Gabriel, Louisiana
Products Substance
Perchloroethylene HCB
Carbon tetrachlorlde
Chlorine
Perchloroethylene HCB
Carbon tetrachlorlde
Methylen chloride
Chloroform, chlorine
Perchloroethylene HCB
Carbon tetrachlorlde
Chlorine
Carbon tetrachlorlde HCB
Trlchloroethylene HCB
Perchloroethylene
Chlorine
Pentachloronltrobencene HCB
Chlorine
Atrazlne HCB
Propazlne
Slmazine
Air (HR/m3) Water (ng/ t) Soil(ua/g> Sediment (ug/g.)
High Low High Lew High Low High Lev
24 0.53 300 0.009 5% 1.1 „
no
sample
7.0 0.24 35 0.2 3,700 0.23 280 0.008
0.08 < 0.02 Ho 2.61 0.014 H<)
': sample sample
ND ND 2.8 «D 0.39 0.013 0.11 ND
ND ND 0.1 ND 24 0.08 u
wo
sample
2.2 0.03 160 ND 13X 0.98 12.4 Only
one
sample
0.02 ND ND ND 0.01 ND
NO
sample
Vaste disposal
On-site landfill,
and deep well
Off-site landfill
Incineration
Co- site landfill
and off-site
disposal
Off-site
incineration
Solid wastes (in
blocks) stored in
open field covered
with plastic
Off-site
incineration
          PPG Industries
          Lake Charles, Louisiana
          Linden Chlorine
          Linden, New Jersey
Trlchloroethylene         HCB
Perchloroethylene
Vinyl chloride
Vlnylldene chloride
Chlorine, etc.

Chlorine                 RGB
                                                                       1.7       ND     7.1    ND
                                                     0.34   ND
                                       sample
0.10    0.013    69
                        0.01     Incineration, land*
                                 fill, and treatment
                                 canal
1.7     Only      7.6    0.10     Holding pond
        one
        sample

-------
    7r
    6 -
    5 -
    4 -
CO



 TO
    3 -
    2 -
(90')
2
.

-

-



-


-




9
















(2







(725')
















50
















')






UOO1)
















1


















.



LEGEND
HIGHEST LEVELS OF HCB OBSERVED
IN AIR AT 8 INDUSTRIAL PLANTS
HCB CONCENTRATIONS IN AIR
AT DOWNWIND STATIONS



(16001)




(1000') (19001)
\ / (1800')
\ / /nnAi\ N.D.
(752%\_ N.D. N.D. \ / N.D. /









(1





(1600')











ooc

















>')

-
„

-

-



-

(23001)





-




7
6

5

4
3


2


1



0
          VULCAN   STAUFFER
DOW    DUPONT  CIBY-GEIGY DIAMOND
                            SHAMROCK
         PRODUCTION PLANT
OLIN
PPG
                         Figure 21.  Summary of HCB  concentrations in air

-------
disposal methods. Lower HCB levels were detected at plants using on-site
incineration, but downwind air concentrations were elevated above back-
ground at both plants; for example, an HCB concentration of 1 (j,g/m  was
detected 2,300 ft downwind of the incinerator at one site. The lowest
levels of HCB for perchloro- and trichloroethylene production plants
were detected at the plant which used off-site incineration. Waste treat-
ment at the PCNB production plant involved casting the solids into blocks
which are stored under plastic. HCB vapor was detected in the low micro-
grams per cubic meter range near the storage area.

     HCB was detected as vapor and particulate in three plants. In two of
the three, the particulate HCB in air coincided with relatively high soil
concentrations in the vicinity of the air sampling stations. At the third
plant, which used a low temperature reaction process, analysis of the
incinerator scrubber water showed 0.2 ng/liter HCB. Negligible levels of
HCB were detected in samples from two sewage treatment facilities.

     The overall relative standard deviation of the air sampling and
analysis procedure, i.e., sample collection, storage, extraction, and
analysis, was calculated to be less than 20%, based on determinations
of HCB levels from sample pairs positioned at the same distances, but
at different heights from the emission source. Good agreement was ob-
tained from the analysis of water samples collected by "grab" sampling
and by concentration of HCB on XAD-4 resin.

CONCLUSIONS

Industrial Sources of HCB

     Considering the estimated production volumes of each of the six
industries and the concentrations detected in this study, perchloro-
ethylene and trichloroethylene production was easily the most signifi-
cant source of HCB for the industries' sampled. Although the total vol-
ume of chlorine produced was estimated to be 20 times that of perchloro-
ethylene and trichloroethylene combined, the production of chlorine did
not appear to be a significant source of HCB. Carbon tetrachloride pro-
duction alone did not appear to be a significant source of HCB but this
conclusion could be biased by the fact that the single-product carbon
tetrachloride plant was the newest facility that was sampled (on-line
in 1973). The production of PCNB resulted in the detection of moderately
high levels of HCB but the total quantity of HCB released to the air was
not significant because of the relatively low estimated production vol-
ume of PCNB. Estimated triazine herbicide production volumes and the as-
sociated HCB levels determined in this study were very low; therefore,
the production of these compounds is not a significant source of HCB.
                                   74

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Effects of Waste Disposal Methods

     In general, methods that involve open storage (pits,  lagoons,  etc.)
resulted in elevated levels of HCB in air and surrounding  soil.  Waste
holding areas were often the most significant emission source within the
plant area. Contaminated soil appeared to be a secondary source  of  both
particulate and vaporous HCB in air at two sites. Transportation of wastes
resulted in at least part per million levels of HCB in roadside  soil within
plant areas. On-site incineration resulted in elevated air HCB levels for
750 ft and 2,300 ft, respectively, at two sites. Plastic sheets  that were
used to cover solids from PCNB production were effective in reducing par-
ticulate HCB but the storage area was the major source of  HCB vapor at  the
plant. The HCB levels in water were reduced by approximately 50% at two
plants that passed liquid wastes through holding ponds or  treatment canals.
                                                                 i
Physical Form of HCB

     HCB was detected in particulate and vapor form. The detection  of
particulate HCB in air can be attributed to contaminated soil or blowing
waste solids in the vicinity of air sampling stations. An  exception was
the incineration of wastes at the low temperature oxychlorination plant.
The particulate HCB observed at this plant was due to either the produc-
tion process or the incineration of li'quid "bottoms." The  latter conclu-
sion is supported by the detection of a significant concentration of HCB
in the incinerator scrubber water.
                                   75

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                                REFERENCES

1.  Brady, M. N., and D. S. Siyali, Med. J. Aust.. _!, 158 (1972).

2.  Acker, L., and E. Schulte, Naturwissenshaften. 57/10), 497 (1970).

3.  Curley, A., V. W. Burse, R. W. Jennings, E. G. Villaneuva, L. Tomatis,
      and K. Akazake, Nature. 242, 333 (1973).

4.  EPA Report, "Environmental Contamination from Hexachlorobenzene," Of-
      fice of Toxic Substances, Environmental Protection Agency, July 20,
      1973.

5.  Mumma, C» E., and E. W. Lawless, "Survey of Industrial Processing Data:
      Task I - Hexachlorobenzene and Hexachlorobutadiene Pollution From
      Chlorocarbon Processes," Final Report by Midwest Research Institute
      on Contract No. 68-01-2105 for the Environmental Protection Agency,
      June 1975.

6.  Personal communication with Mr. G. A. Burns, Environmental Control
      Specialist, PPG Industries, Lake Charles, Louisiana, November 1975.
                                    76

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             APPENDIX A
PRESAMPLING SURVEY AND FIELD SAMPLING
                 77

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     Presarapling surveys and field sampling were conducted on the recom-
mended industrial plants according to the schedule shown in Figure A-l.
Essentially, during the presampling survey, information such as the sur-
rounding terrain, meteorological conditions, production technology, and
waste disposal technique was gathered.  Following each site visit, a de-
tailed field sampling strategy was devised and carried out approximately
2 to 4 weeks after the presampling survey date.  Presented below are de-
tailed descriptions of the presampling survey and field sampling conducted
at each plant.

                VULCAN MATERIAL COMPANY, WICHITA, KANSAS

PRESAMPLING SITE SURVEY

     The presampling site survey at Vulcan Materials Company's Wichita,
Kansas, plant was conducted on May 6, 1975.  The following personnel were
present:

     Mr. J. I. Jordan, Jr.          Manager, Research and Development,
                                      Vulcan Materials Company

     Mr. R. A. Bondurant, Jr.       Director, Environmental Control
                                      Safety, Vulcan Materials Company

     Mr. Dave Harrison              Acting Technical Manager, Wichita
                                      Plant, Vulcan Materials Company

     Mr. P. Constant                Midwest Research Institute

     Mr. P. Kuykendall              Midwest Research Institute

     Dr. J. Spigarelli              Midwest Research Institute

     Vulcan Materials Company is located approximately 7 miles southwest
of downtown Wichita and approximately 4 miles from any major residential
area.  The surrounding terrain is level with only one nearby water source,
Cowskin Creek.  The prevailing wind in May is generally from the south,
southeast or southwest.

     Perchloroethylene is produced by the reaction of hydrocarbons and
chlorine.  The hydrocarbons are generally of a widely variable composition
and are obtained from many sources.  The chlorine is produced by Vulcan
and piped directly from their liquification station to the perchloroethylene
reaction pot.  Their chlorine production utilizes diaphragm cells and ap-
proximately 25% of their anodes are graphite, the remainder being dimensionally
stabilized anodes.
                                   78

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                                            May
June
July
August     September
VD
Vulcan Materials
Wichita, Ks.
Linden Chlorine
' Linden, N. J.
Stauffer Chemical
Louisville, Ky.
Dow Chemical
Pittsburg, Calif.
du Pont
Corpus Christi, Tex.
Diamond Shamrock
Deer Park, Tex.
Ciba-Geigy Corp.
St. Gabriel, La.
Olin Corp.
Mclntosh, Ala.
Kaiser Aluminum
Gramercy, La.
PPG Industries
Lake Charles, La.
A _
A
A









—
A










A
A
A
A





-
-
-
-
-
A
A









-
                                A Presampling Visit
                               •• Field Sampling
                             Figure A-l.   Presampling survey and field sampling schedule

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     Vulcan uses two types of waste disposal, deep wells and landfills.
The deep wells are used for the disposal of storm runoff, while the land-
fills are used for the disposal of "heavy ends" waste from perchloro-
ethylene production.  The residues are collected in a sealed vessel, trans-
ferred to another sealed vessel mounted on a trailer, and transported to
an open pit where they are stored under water.  When the residue level in
the pit reaches a certain level, it is transferred by means of a backhoe
to a dump truck and transported to the landfill, which is located south-
east of the plant.  There it is dumped, covered with polyethylene sheeting,
then covered with dirt.

     At the conclusion of the presampling survey, it was agreed upon that
field sampling would be tentatively scheduled in the week of May 19, 1975.

FIELD SAMPLING

     Field sampling at the Vulcan plant was conducted on May 20, 1975.
Air, soil, and water samples were collected as planned.  Detailed descrip-
tion of the sampling, plant activities, and weather conditions, are dis-
cussed below.

Air Sampling

     Five general areas were chosen for air sampling:  (a) perchloroethylene
plant; (b) "Hex Pit;" (c) solar pond - landfill; (d) downwind of these loca-
tions; and (e) upwind of these locations.  The total sampling time was
divided into 4-hr periods.  The upwind and downwind samplers were operated
continuously during each 4-hr period,  whereas all other samplers were
operated only for the 1st hr of each 4-hr period.  Each sampling location
is shown in Figure A-2.  Exact location was measured with respect to the
suspected emission source and was reported along with other sampling data
in Table A-l.

Soil Sampling

     Soil sampling covered eight general areas:

     S-l     Around the perchloroethylene plant

     S-2     Route from perchloroethylene plant to "Hex Pit"

     S-3     Around the "Hex Pit"

     S-4     Route from "Hex Pit" to landfill

     S-5     Between old and current landfill sites
                                   80

-------
CO
           S
            §
            u
           S
               g.
              1
                  12
                  13
                  10
                  11
                                          S-3 T
                                            QHex Pit
         , /

        oT
         x
                                            S-l
                                    g Perc Plant
il
                                       LEGEND:
                                          Numbers 1 to 18 Air Sampling Sites
                                          S-l Perc Pjgnt
                                          S-2 Route from Perc  Plant to Hex Pit
                                          S-3 Hex Pit
                                          S-4 Route from Hex Pit to Landfill
                                          S-5,S-6,S-7  Landfill
                                          S-8 Upwind
                                          S-9 Downwind
                                          S-10 Western Boundary  (Cornfield)
                                                  Scale 1/2" =150'
                                                                                                                           18
                                                                                        17 .
                                                                                        16 •
°P
in
                                                                                                                                            S
                                                                                                                                            a.
                                                                                                                                            §
                                                                                                                                            U
                   South Ridge Road
                                                          West Soil Composite S-10
                        Figure  A-2.   Sampling  locations  at  Vulcan Materials  Company  - Wichita  plant

-------
                                    Table A-l.  AIR SAMPLING DATA AT VULCAN MATERIALS COMPANY, WICHITA,  KANSAS
00
ho

General Sample
area no.
1

"Perc Plant"
2
3


4

"Hex Pit"
5
6


7

Solar pond-
landfill 8

9


10 and 11

Downwind 12 and 13

14 and 15

16

17

18


Exact location
250 ft north of "Perc Plant"- 1st
250 ft west of Sample No.
2
250 ft north of "Perc Plant" 1st
250 ft north of "Perc Plant"- 1st
50 ft east of Sample No.
2
150 ft north of "Hex Pit" 1st
75 ft west of Sample No.
2
150 ft north of "Hex Pit" 1st
150 ft north of "Hex pit"- 1st
75 ft east of Sample No.
2
1,500 ft north of landfill- 1st
225 ft northwest of solar
pond
1,500 ft north of landfill- 1st
225 ft north of solar pond

Sampling
period
hr of 4 hr


hr of 4 hr
hr of 4 hr


hr of 4 hr


hr of 4 hr
hr of 4 hr


hr of 4 hr


hr of 4 hr

1,500 ft north of landfill- 1st hr of 4 hr
440 ft northeast of solar
pond
525 ft north of plant boundary-
340 ft east of Ridge Road
525 ft north of plant boundary-
850 ft east of Ridge Road
525 ft north of plant boundary-
2,100 ft north of Ridge Road
On southern plant boundary-
225 ft east of Ridge Road
On southern plant boundary-
300 ft east of Ridge Road
On southern plant boundary-


4 hr
4 hr
4 hr
4 hr
4 hr
4 hr
4 hr

4 hr

4 hr
Total
sampling
time (hr)
19.5


19.5
19.5


19.5


19.5
19.5


19.5


19.5

19.5


19.5
19.5
19.5
19.5
19.5
19.5
19.5

19.5

19.5

Sampling rate
( £/min)
0.5


0.5
0.5


0.5


0.5
0.5


3.5


3.5

3.5


3-5
3.5
3.5
3.5
3.5
3.5
3.5

3.5

3.5
Total
sample
vol. U)
178


149
207


156


232
195


813


1,123

1,198


3,646
3,862
3,930
4,172
4,291
4,272
3,744

3,176

3,353

Sampler
height (ft)
11


11
11


4


4
4


4


4

4


10-4
11-11
12-4
13- 11
14-4
15-11
4

4

4
                                      700  ft east of Ridge Road

-------
     S-6     North of current landfill site

     S-7     Along the eastern plant boundary

     S-8     Along the southern plant boundary, passed 63rd Street

     S-9     Beyond the northern plant boundary, along Racon Road

     S-10    Along the western plant boundary, along the cornfield

All the samples were composites except the landfill samples.  In addition,
a sample of the "Hex Pit" solids was also collected.

Water Sampling

     Water samples were taken from four general areas:

     1.  Upstream from waste inflow - Cowskin Creek

     2.  Downstream from waste inflow - Cowskin creek

     3.  Solar pond water

     4.  "Hex Pit" water

The location of the solar pond and "hex" pit is shown in Figure A-2;  the
sampling locations in Cowskin Creek are shown in Figure A-3.

     Samples from Cowskin Creek were collected on Amberlite XAD-4 resin
via a battery-operated pump.  Grab samples were taken from the solar
pond and "Hex Pit."

Plant Activities and Weather Conditions

     Plant activities were observed during the sampling period and are
tabulated in Table A-2.

     The weather conditions during the sampling period are summarized in
Table A-3.  Fortunately, the wind was from the south or southeast during
the entire sampling period except for the last 4-hr interval.   The change
in wind direction coincided with a thunderstorm which forced a termination
of sampling during the final 4-hr period.
                                  83

-------
        Upwind Air Samples
Figure A-3.  Vulcan Materials Company - Wichita plant, and
            surrounding areas (2.6 in. = 1 mile)
                             84

-------
Table A-2.  PLANT ACTIVITIES DURING SAMPLING AT VULCAN MATERIALS COMPANY,
                               WICHITA, KANSAS


Time
May 21
1900
2000
2100
2200
2300
2400
May 22
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400
1500

"Perc plant"

Normal
Normal
Normal
Normal
Normal
Dumped "Hex"

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Pumped "Hex"
Normal
Rain

"Hex pit"

Fuller than usual
Fuller than usual
Fuller than usual
Fuller than usual
Fuller than usual
Fuller than usual

Dumped "Hex"
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Dumped "Hex"
Rain
Solar pond
landfill

Normal
Normal
Normal
Normal
Normal
Normal

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Rain

Downwind

Normal
Normal
Normal
Normal
Normal
Dumped "Hex"

Dumped "Hex"
Normal
Normal
Normal
Norma 1
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Dumped "Hex"
Dumped "Hex"
Rain

Upwind

Normal
Normal
Normal
Normal
Normal
Normal

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Rain
                                     85

-------
            Table A-3.   WEATHER CONDITIONS DURING SAMPLING AT VULCAN MATERIALS COMPANY, WICHITA, KANSAS
00


Time
May 21
1900
2000
2100
2200
2300
2400
May 22
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
1400
1500
Temperature
(°C)

27
27
24
23
23
23

23
23
23
23
21
21
23
25
25
26
26
27
29
29
29
Barometric
pressure
(mm Hg)

722
722
723
724
724
724

724
724
724
724
723
723
723
725
725
725
725
725
725
725
725

Precipitation

None
None
None
None
None
None

None
None
None
None
None
None
None
None
None
None
None
None
None
None
Rain

Speed

15
12
11
12
13
12

11
12
13
10
9
9
9
9
11
10
12
15
15
12
10
Wind
Direction

South southeast
South southeast
Southeast
Southeast
South southeast
South

South southeast
Southeast
South southeast
South southeast
South
South southeast
South southeast
South southeast
South southeast
South
South
South
South
South
Northwest

-------
               LINDEN CHLORINE COMPANY, LINDEN, NEW JERSEY

     Presampling site survey at Linden Chlorine Company was conducted on
May 29, 1975.  The following personnel were present:
     Mr. Ronald Burkett
     Mr. Bill Heineman
     Mr. Edward J. Finfer
Linden Chlorine Plant

Linden Chlorine Plant

Environmental Protection Agency,
  Region II
     Mr. Martin L. Sanvito       DEP, BAPC

     Mr. William J. 0"Sullivan   DEP, Springfield office
     Mr. William A. McGough
     Mr. Richard pills
     Dr. George Scheil
     Dr. J. Spigarelli
Central Jersey Regional Air Pollution
  Control Agency

Central Jersey Regional Air Pollution
  Control Agency

Midwest Research Institute

Midwest Research Institute
     Linden Chlorine Company is located in the middle of a heavy industrial
area.  The closest residential areas are greater than 1 mile away, and
nearby water source is the Arther Kill River.      '

     During the visit, it was learned that graphite electrodes are no longer
used in production of chlorine, instead platinum-coated titanium electrodes
(dimensionally stabilized anodes) have been used since the end of March 1975.
Because the potential for producing HCB and HCBD is much less for this type
of electrode, it was decided that air sampling was not necessary.  However,
the holding pond that contains brine sludge and eroded graphite from previ-
ously used electrodes may contain significant quantities of chlorinated
organics.  In addition to carbon from eroded electrodes, the pond also con-
tains spent carbon filters that were used to remove organics from process
and surface water which flows through an open ditch to the Arthur Kill River.
By far the largest portion of this water is made up of wastes from the nearby
Gaf dye plant.  The Gaf flume appeared to have a high organic content before
the wastes from the chlorine plant  enter the stream.  Because of possible
past HCB and HCBD contamination in the holding pond,  samples were taken from
the pond and wastewater stream.  The samples are described below:
                                    87

-------
          Sample  type                     Sample location

              Water                  Holding pond, inlet
              Water                  Holding pond, outlet
              Water                  Gaf weir, upstream of Cl2 plant
              Water                  Waste stream, downstream of Cl2 plant
              Water                  Tap water (control)
              Solids                 From holding pond, settled and suspended
              Solids                 Dredged solids adjacent to holding pond
              Sludge                 Waste stream, downstream of C^ plant

     The following samples were sent to Midwest Research Institute, on a
later date by the Linden Chlorine Plant:  process water, circulating brine,
and uncontaminated soil.

             STAUFFER CHEMICAL COMPANY, LOUISVILLE, KENTUCKY

PRESAMPLING SITE SURVEY

     The ^resampling site survey at Stauffer Chemical Company's Louisville,
Kentucky, plant was conducted on May 30, 1975.  The following personnel were
present:

     Mr. Arthur Wood               Manufacturing Manager,  Stauffer Chemical
                                     Company

     Mr. Harry Kutz                Plant Manager, Louisville plant

     Mr. Kenneth G. Hebel          EPA/OSHA Testing Coordinator, Eastern
                                     Research Center, Dobbs Ferry, New
                                     York

     Mr. Arthur E. Dungan          Assistant Plant Manager, Louisville plant

     Mr. John R. Blunk             Process Superintendent,  Louisville plant

     Dr. George Scheil             Midwest Research Institute

     Dr. J. Spigarelli             Midwest Research Institute

     Stauffer Chemical Company is located on the east bank  of the Ohio
River approximately 6 miles southwest of downtown Louisville, Residential
areas surround the plant, the closest being about 1 mile northeast of the
plant.  The wind direction, according to the weather bureau records (10-
year average) at the Louisville airport indicated that during the month
of June there is a 5070 probability of a south wind (from one of the four
southern quadrants) and a much lower probability from any other direction.

                                   88

-------
     The "hex" solids from the perchloroethylene production plant are
gravity fed into drums  (batch-wise).  After several drums (unsealed, pos-
sibly covered with a pleastic sheet) accumulate, they are removed from
the plant area.  Company officials said that the drums are usually re-
moved once a day at 8:00 a.m.  The plant operated 24 hr a day, 7 days a
week.

     The drums are transported to an area just west of the surplus storage
building where they are loaded onto trucks and taken to an approved land-
fill site approximately 15 miles from the plant.  Cooling water and sur-
face runoff from the plant area are fed to a sump where the pH is adjusted
to 6 to 9, the liquid is pumped to a concrete settling pond, and gravity
fed through a pipe into the Ohio River.

     Based on the plant operation described above, three possible sources
of RGB and HCBD contamination were considered, namely:  (a) the production
area, especially at the location of the open barrels, (b) the settling
pond and (c) the "hex" loading area and the transportation route to the
landfill.

FIELD SAMPLING

     Field sampling at the Stauffer plant was conducted on June 12, 1975.
Air, water, soil, and sediment samples in and around the plant were col-
lected.  Detailed descriptions of the sampling and plant activities during
sampling are discussed below.

Air Sampling

     Eight sampling stations encircling the immediate plant area, and one
downwind station were set up.  The total sampling period was divided into
six 4-hr periods and samplers were operated 2 hr of each 4-hr period.  Each
sampling location is shown in Figure A-4.  Exact locations with respect to
the perchloroethylene plant area, are listed along with other sampling data
in Table A-4.

Soil Sampling

     Soil sampling was conducted in five general areas:

     S-l     Upwind (along the southern plant boundary)

     S-2     Plant road (along the main road)

     S-3     Drum loading area
                                    89

-------
\D
O I
                                  L
                 4  R-2 Sediment Sample
                  I  (700 Meters Upstream)
                                                                         Solvent
                                                                 Chlorine Stora9e
                                                                  uilding
Settling
 Pond
Outflow
 R-3
 Sediment
 Sample
Main Rood
                                                                                                         S-2 Soil Composite
                                                                S-l Soil Composite
                       Figure A-4.   Sampling  locations at Stauffer  Chemical Company - Louisville,  Kentucky

-------
                     Table A-4.   AIR SAMPLING DATA AT STAUFFER CHEMICAL COMPANY,  LOUISVILLE,  KENTUCKY
General area
Upwind
Upwind
East of "Perc Plant"
Northeast of "Perc
Plant"
Downwind
Downwind
Northwest of "Perc
Total
Sample Sampling sampling
No. Exact location period time (hr)
1
2
3
4
5
6
7
450 ft south southwest of T'Perc 1st 2 hr of 4 hr 12.3
Plant" area
500 ft south southeast of "Perc 1st 2 hr of 4 hr 11.8
Plant" area
340 ft east of "Perc Plant" area 1st 2 hr of 4 hr 10.6
250 ft northeast of "Perc Plant" 1st 2 hr of 4 hr 12.5
area
300 ft north of "Perc Plant" area 1st 2 hr of 4 hr 12.9
400 ft north of "Perc Plant" area 1st 2 hr of 4 hr 13.1
330 ft northwest of "Perc Plant" 1st 2 hr of 4 hr 13.2
Total
Sampling Sample Sampler
rate vol. height
U/min) (H) (ft)
3.5 2,588 4
3.5 2,626 4
3.5 2,221 4
3.5 2,768 4
3.5 2,787 4
3.5 2,662 4
3.5 2,850 4
  Plant"

West of "Perc Plant"
  north of settling
  pond

Southwest of "Perc
  Plant," northwest
  of settling pond
       area
     420 ft west of "Perc Plant" area    1st  2  hr  of 4 hr      13.3         3.5       2,872
9    540 ft southwest of "Perc Plant"   1st  2  hr  of  4  hr      13.5
       area
3.5
2.926

-------
     S-4     Downwind  (along the northern plant boundary)

     S-5     Settling  pond area

     All samples were  composites.

Water Sampling

     Water sampling was limited to the plant well water and the settling
pond.

     W-l     Plant well water

     W-2     Settling  pond inlet (24 hr composite)

     W-3     Settling  pond inlet (grab sample)

     W-4     Settling  pond outlet (24 hr composite)

     W-5     Settling  pond outlet (grab sample)

     W-6     Settling  pond outlet (through Amberlite XAD-4)

Sediment Sampling

     Sediment sampling was conducted at three locations:

     R-l     Settling pond sediment

     R-2     Ohio River, 700 m upstream of Stauffer outflow

     R-3     Ohio River, 250 m downstream of Stauffer outflow

Plant Activities and Weather Conditions

     Plant activities were observed during the sampling period and are shown
in Table A-5.

     The weather conditions during the sampling period are summarized in
Table A-6.
                                     92

-------
Table A-5.   PLANT ACTIVITIES DURING SAMPLING AT STAUFFER CHEMICAL COMPANY,
                          LOUISVILLE,  KENTUCKY
Time
12 June
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
13 June
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
"Perc plant"!/

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Drum loading area

Normal
Normal
Normal
Normal
"Hex" drums removed
"Hex" drums removed
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Settling pond

Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow

Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
Normal flow
a/  Normal operation utilizing HCBD recovery.
                                  93

-------
Table A-6.   WEATHER CONDITIONS DURING SAMPLING AT STAUFFER CHEMICAL
                   COMPANY,  LOUISVILLE,  KENTUCKY



Time
12 June
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
13 June
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000

Temperature
(°C)

26
28
29
29
29
29
29
27
25
24
25
23
21
20
20

19
18
17
16
16
17
17
19
22
25
Barometric
pressure
(mm Hg)

757
757
757
757
757
757
758
758
758
758
759
759
759
759
759

760
760
760
760
760
760
760
760
760
760
Wind
Precipi-
tation

None
None
None
None
None
None
None
None
None
None
None
None
None
10 min rain
None

None
None
None
None
None
None
None
None
None
None

Speed

4
4
4
6
8
7
6
7
6
6
5
2
5
5
4

4
2
2
0
0
0
0
0
0
0
Direc-
tion

S
S
S
S
S
S
S
S
S
S
S
S
S
E
S

S
S
S
S
S
S
S
S
S
S
                               94

-------
                DOW CHEMICAL COMPANY, PITTSBURG, CALIFORNIA

PRESAMPLING SITE SURVEY

     Presampling site survey at Dow Chemical Company's Pittsubrg, California,
plant was conducted on June 30, 1975.  The following personnel were present:

     Mr. Ed Elkins            Manager, Environmental and operational
                                Services, Dow Chemical Company

     Mr. David Baur           Dow Chemical Company

     Mr. Mike Thomas          Dow Chemical Company

     Mr. Paul Constant        Midwest Research Institute

     Mr. Jim Spigarelli       Midwest Research Institute

     Dow Chemical Company is located approximately 2 miles northeast of
Pittsburg, California, and 4 miles west of Antioch, California, and is
situated on the southern bank of the New York slough of the San Joaquin
River.  The immediate vicinity is flat, but mountains lie approximately
5 miles south of the plant.  Approximately 70% of the time during July
the wind is from west or west-northwest.  Residential areas are in
Pittsburg and Antioch.

     Chemicals produced at this Dow facility include chlorine, carbon tetra-
chloride, and perchloroethylene.  According to Mr. Elkins, all wastes from
the chlorinated hydrocarbon production flow to a thermal oxidizer, are con-
verted to hydrochloric acid and are recycled.  In most instances, surface
runoff from the plant areas flow into a solar pond.  However, inspection
on the plant and the solar pond area were not allowed.  Only the plant
perimeter and beyond were surveyed.

     Air sampling locations were planned based on the thermal oxidizer
parameters such as stack gas temperature, gas flow rate, aid stack height
and diameter.

FIELD SAMPLING

     Field sampling at the Dow plant was conducted on August 7, 1975,  after
several postponements.  Air,  soil,  and water samples were collected.   De-
tailed descriptions of the sampling, plant activities,  and weather condi-
tions are discussed below.
                                    95

-------
Air Sampling

     Eight sampling stations were located so that two upwind,  three near
downwind, and three far downwind samples were obtained.  Air was sampled over
a 24-hr period with the exception of Stations 2 (upwind)  and 7 (far down-
wind) .  Two air sampling tubes were operated in series at each station.
Each sampling location is shown in Figure A-5.  The exact location was mea-
sured with respect to the production plant area and is listed along with
other sampling data in Table A-7.

Soil Sampling

     Soil sampling was conducted in three general areas:

     S-l     Upwind (western plant boundary)

     S-2     Southern property boundary

     S-3     Downwind (eastern plant boundary)

All samples were composites.

Water Sampling

     One grab water sample of the New York Slough was obtained at the north-
east corner of Dow's property.  Water sampling at the solar pond was not
permitted by the Dow officials.

Plant Activities and Weather Conditions

     Plant activities and weather conditions during sampling are shown in
Table A-8.
                                    96

-------
vO
                 «;ok
                      H*f 4^
                                BROWNS
                                ISLAND
                                ^Ofijf     SLOUGH
                                                                                    \

                                                                                                   \

                                                    Pittstaurg
                                               --f-e   Poi"»-....>?tPer'c
  ,.rf<
Plont Area
gv:
^j/ ""! .7,
Y //
} s *
^ ..
Solar Pond
f;>:.:.xf
( : ^
\Jtfte.
® 	 	
/
7^;
.A
Plant

.N^^
*. .
Soundary oeh
'•"•"ev'eE -.
TOPEK A/. / '
"«
Point

' 	 N
n \s
9&S
"\ X
']--.. ^^
' '"'-:
\ A
i / ' 'N
AHD , /
'\

\
"\.
\
                                                                                           ur<(<~- J
                     yo-
                                                                                                        ^
                                                                                               r^
                                                                                                                JM/-VT
                                                                                                                       ^r=4
                                                                                                            '0	^
                                                                                                                L  £_j=i
                                          = =J.. ^^r^- —*»-• - ;.
                                          .  ,• CiK i*..    '
                                          *r~ ==•- --=
                                          JlJ'phn'pSr-^^
                                         l(Z]""9<;hi
-------
                      Table A-7.   AIR SAMPLING DATA AT DOW CHEMICAL COMPANY,  PITTS BURG,  CALIFORNIA
00
General area

Upwind


Upwind

Near downwind


Near downwind


Near downwind


Far downwind

Far downwind


Far downwind
                          Sample
                           No.
        Exact location

2,630 ft west-northwest of
  "Perc Plant"

2,780 ft west of  "Perc Plant"

900 ft east-northeast  of
  "Perc Plant"

830 ft southeast  of  "Perc
  Plant"

1,280 ft south-southeast of
  "Perc Plant"

2,550 ft east of  "Perc Plant"

3,600 ft southeast of  "Perc
  Plant"

5,100 ft south-southeast of
  "Perc Plant"
                     Total       Sampling    Sample    Sampler
                    sampling       rate       vol.     height
Sampling period     time  (hr)      (l/min)     (j)        (ft)
24 hr continuous       20.7


24 hr continuous        2.0-

24 hr continuous       19.8


24 hr continuous       18.4


24 hr continuous       17.7


24 hr continuous       20.5

24 hr continuous        4.6-


24 hr continuous       18.9
3.5       4,336       4


3.5         427       4

3.5       4,166       4


3.5       3,870       4


3.5       3,713       4


3.5       4,314       4

3.5         962       4
                                                                                                        3.5
                                                                                                        3.963
         a/  Generator failure.

-------
    Table A-8.  WEATHER CONDITIONS AND PLANT ACTIVITIES DURING
    SAMPLING AT DOW CHEMICAL COMPANY, PITTSBURG, CALIFORNIA*/



Time
August 7
1700
1800
1900
2000
2100
2200
2300
2400
August 8
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000

1100
1200
1300
1400
1500
1600
1700
1800
Temper-
ature
(°F)

97
96
92
87
84
82
79
80

74
74
74
73
71
69
67
73
83
87

91
96
98
101
101
103
102
99
Barometric
pressure
(mm Hg) Speed

760 8
12
10
10
760 8
8
6
2

760 0
6
8
6
760 4
0
0
0
760 0
2

6
2
760 4
4
10
12
759 12
13

Wind
Direction

West
West
West
West
West
West
West
West


West
West
West
West
-
-
•
-
West

West
Northwest
Northwest
West
West
West
West
West

Plant
activities

Normal
Normal
Normal
Normal
Normal
Norma 1
Normal
Normal

Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Normal
Incinerator feed
rate reduced
Normal
Normal
Normal
Normal
Possible event
Normal
Normal
Normal
aj  No precipitation during sampling period.
                                 99

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    E. I. du PONT de NEMOURS AND COMPANY, INC., CORPUS CHRISTI, TEXAS

PRESAMPLING SITE SURVEY

     The presampling site survey at du Font's Corpus Christi, Texas, plant
was conducted on July 11, 1975.  The following personnel were present:

     Mr. Charles Evans          Plant Manager, du Pont

     Mr. Dave Brooks            Assistant Plant Manager, du Pont

     Mr. Phil Kuykendall        Midwest Research Institute

     This du Pont plant is located on Corpus Christi Bay approximately 3
miles northeast of downtown Corpus Christi.  The immediate area surrounding
the plant contains several industries, but the small town of Ingleside is
about 1 mile east of the plant.  Wind direction in the summer is generally
from the south, south southeast, and south southwest.

     Carbon tetrachloride is produced by chlorination of methane or ethylene
at elevated temperatures.  All by-products are continuously recycled to in-
sure total chlorination.  Chlorine is obtained from an outside source.  Solid
wastes from the process are minimal and are not frequently removed from the
reaction vessel.

     Solid wastes are generally drummed and shipped to an outside firm for
disposal although some wastes are dumped into du Font's two landfills.  One
landfill is dedicated to the disposal of a mixture of cement, lime, and
catalyst from Freon production.  The other landfill normally receives such
wastes as contaminated containers, spills, or "heavy ends" waste from the
carbon tetrachloride production.

     Wastewater is handled separately as process waste and storm runoff.
Process wastes are channeled via open concrete ditches, to an equalization
pond where the residence time is 3 to 6 days.  Underground pipes discharge
the wastewater into Lacita Channel at a flow rate of approximately 2,000
gal/min.

     Storm runoff is discharged, via open dirt ditches, directly into
Lacita Channel

FIELD SAMPLING

     Field sampling at the du Pont plant was conducted on August 3, 1975.
Air, soil, water, and sediment samples were collected.  Detailed descrip-
tions of the sampling, plant activities, and weather conditions, are dis-
cussed below.

                                    100

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Air Sampling

     Due to equipment failure,only five air sampling stations were operated.
Two were upwind and three were downwind.  All samples were operated for 24
hr utilizing one filter and two Tenax tubes in tandem.  Sampling locations
are shown in Figure A-6.  Exact distance of each station to the production
area was determined and reported along with other sampling data in Table
A-9.

Soil Sampling

     Soil sampling was conducted in three general areas:

     S-l     Upwind (at Stations 1 and 2 on southern boundary)

     S-2     Downwind (at Stations 3, 4, and 5 on northern boundary)

     S-3     Landfill area (20 ft from edge of miscellaneous landfill)

All soil samples were composites.

Water Sampling

     Water sampling was conducted at seven locations:

     W-l     Raw plant water before use

     W-2     Settling pond inlet (amberlite)

     W-3     Settling pond inlet (grab)

     W-4     Settling pond outlet (amberlite)

     W-5     Settling pond outlet (grab)

     W-6     Storm runoff outfall (grab)

     W-7     Water standing in landfill

Sediment Sampling

     Sediment sampling was conducted at four locations:

     R-l     Settling pond inlet

     R-2     Settling pond outlet

     R-3     Storm runoff outfall
                                   101

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O'
                                                                                                                 STORM SEWER
                                                                                                                 PROCESS SEWER
                                                                                                                    I" - 150'
            Figure A-6.  Sample  locations at E.  I.  du Pont de Nemours and Company,  Inc., Corpus  Christi,  Texas

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Table A-9.   AIR SAMPLING DATA AT E.  I.  DU PONT  DE NEMOURS AND COMPANY,  INC., CORPUS CHRISTI, TEXAS


General area
Upwind
Upwind

Downwind

Downwind

Downwind

Sample
Total Sampling
sampling rate
No. Exact location Sampling period time (hr) (£/min)
1 675 ft south
2 700 ft south
tion area
3 640 ft north
tion area
4 64- ft north
tion area
5 640 ft north
tion area
of production area 24 hr continuous 22.8 3.5
southeast of produc- 24 hr continuous 19.5 3.5

northwest of produc- 24 hr continuous 21.2 3.5

northwest of produc- 24 hr continuous 21.2 3.5

northwest of produc- 24 hr continuous 21.3 3.5

Sample Sampler
vol. height
(£) (ft)
4,371 4
3,621 4

4,070 4

4,007 4

3,965 4


-------
Plant Activities

     Plant activities during sampling are shown in Tables A-10 and A-11,
respectively.
                                    104

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Table A-10.  PLANT ACTIVITIES DURING SAMPLING AT E.  I.  DU
PONT DE NEMOURS AND COMPANY,  INC.,  CORPUS CHRISTI,  TEXAS



Time
August 3
0700
0800
0900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000

Chlorocarbon
unit

Normal production
Normal production
Normal production
Down
Down
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production
Normal production


Landfill

No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
No activity
Settling pond
flow
(gal/min)

2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
2,300
                             105

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Table A-11.   WEATHER CONDITIONS DURING SAMPLING AT  E.  I.  DU  PONT DE
         NEMOURS AND COMPANY,  INC.,  CORPUS  CHRISTI,  TEXAS

Temperature
Time
August 3
0700
0800
0900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
August 4
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
(°C)

28
28
28
29
29
29
29
30
29
29
27
28
28
28
28
27
27
27

27
26
28
27
28
29
29
29
30
30
30
Barometric
pressure
(mm Hg)

762
762
762
762
761
761
761
761
761
760
760
760
760
760
760
762
762
762

762
762
761
761
761
761
761
760
760
760
760


Precipitation Speed

none
none
none
none
none
none
none
none
none
rain
rain
none
none
none
none
none
none
none

none
none
none
none
none
none
none
none
none
none
rain

19
17
15
11
11
11
10
10
12
22
9
10
10
9
9
7
10
10

10
18
16
17
17
15
15
18
15
13
12
Wind
Direction

South
South
South
South
South southeast
South southeast
South southeast
South southeast
South southeast
North northwest
East
East southeast
Southeast
Southeast
Southeast
Southeast
Southeast
South southeast

South southwest
South
South
South
South
South
South southwest
South southwest
South southwest
South southwest
Southwest
                                 106

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             DIAMOND SHAMROCK CORPORATION, DEERK PARK, TEXAS

PRESAMPLING SITE SURVEY

     The presampling site survey at Diamond Shamrock's, Deer Park, Texas,
plant was conducted on July 10, 1975.  The following personnel were present:

     Mr. Lavern R. Heble          Environment Control Manager, Gulf Coast
                                    Area, Diamond Shamrock Corporation

     Mr. William C. Hutton        Senior Environmental Control Engineer,
                                    Diamond Shamrock Corporation

     Mr. Bob Baxter               Perchloroethylene Unit Manager,
                                    Diamond Shamrock Corporation

     Ms. Sandra Quinlivan         TRW, Rodondo Beach, California

     Mr. Phil Kuykendall          Midwest Research Institute

     This Diamond Shamrock plant is located in the heart of a huge industrial
area along the Honston ship channel.  The nearest residential area is Deer
Park, located approximately 5 miles south of the plant.  Wind direction in
the summer months is mostly from the south.

     Perchloroethylene and trichloroethylene are produced in this plant by
the reaction of chlorine and hydrocarbons.  The chlorine used is produced at
a nearby Diamond Shamrock plant and is piped to the production area.   "Hex"
solids resulting from the process are stored in large tanks awaiting  disposal.

     The major possible sources of HCB and HCBD are (a) the production area
and  (b) the "Hex" solids storage area.

     Diamond Shamrock uses two types of waste disposal; contracted solid
waste disposal and channeling of wastewater into Patrick Bayou.  The solid
wastes  are transferred from the holding tank to a tank truck which trans-
ports the waste to an outside firm for incineration or landfill disposal.
Solid waste removal does not occur daily.  A solvent flush of the lines into
the  tank truck follows each dumping of "Hex" solids.  Wastewater is steam-
stripped in the production area then piped to a waste treatment plant prior
to discharge into Patrick Bayou.
                                    107

-------
FIELD SAMPLING

     Field sampling at the Diamond Shamrock plant was conducted on August
20, 1975 after several postponements due to plant down time.  Air, soil,
and water samples were collected.  Detailed description of the sampling,
plant activities, and weather conditions, are discussed below.

Air Sampling

     Eight air sampling stations were used—three upwind and five downwind.
To avoid possible breakthrough of the Tenax^-GC,  smaller critical orifices
were used.  All samples were operated for three 8-hr periods, resulting in a
24-hr sampling time.  Sampling locations are shown in Figure A-7.  The exact
distance of each station to the production area was determined and reported
along with other sampling data in Table A-12.

Soil Sampling

     Soil sampling was conducted at three areas:

     S-l     Upwind (along southern boundary)

     S-2     Downwind (along northern boundary)

     S-3     Production area

All soil samples were composites.

Water Sampling

     Water sampling was conducted at two points:

     W-l     Incoming channel water

     W-2     Process water outfall

All samples were grab samples.

     No sediment sampling was conducted because of no existing sampling
site.

Plant Activities and Weather Conditions

     The weather conditions during sampling are shown in Table A-13.
Plant activities were normal during the entire sampling period.
                                     108

-------
                                                     '•-..    c
N
          PRODUCTION
              AREA
                I
Figure A-7.   Sampling locations  at Diamond Shamrock Corporation,

                       Deer  Park, Texas
                             109

-------
Table A-12.   AIR SAMPLING DATA AT DIAMOND SHAMROCK  CORPORATION,  DEER PARK,  TEXAS


General area
Far upwind
Near upwind

Near. upwind

Near downwind

Near downwind

Near downwind

Far downwind

Far downwind

Sample
No. Exact location Sampling period
1 1,300 ft south of "Perc Plant" area 24 hr continuous
2 510 ft southwest of "Perc Plant" 24 hr continuous
area
3 420 ft southeast of "Perc Plant" 24 hr continuous
area
4 1,200 ft northeast of "Perc 24 hr continuous
Plant" area
5 1,300 ft northwest of "Perc 24 hr continuous
Plant" area
6 1,860 ft north northeast of 24 hr continuous
"Perc Plant" area
7 2,850 ft north northwest of 24 hr continuous
"Perc Plant" area
8 2,900 ft north of "Perc Plant" 24 hr continuous
Total
sampling
time (hr)
24.2
24.9

20.2

22.5

22.6

25.3

23.3

23.1
Sampling
rate
U/min)
0.4
0.4

0.4

0.4

0.4

0.4

0.4

0.4
Sample
vol.
(I)
580
598

485

540

542

608

559

555
Sampler
height
(ft)
4
4

4

4

4

4

4

4
   area

-------
Table A-13.   WEATHER CONDITIONS DURING SAMPLING AT
  DIAMOND SHAMROCK CORPORATION, DEER PARK,  TEXAS


Time
August 20
1600
1700
1800
1900
2000
2100
2200
2300
2400
August 21
0100
0200
0300
0400
0500
0600
0700
0800
2100
2200
2300
2400
August 22
0100
0200
0300
0400
0500
0600
0700
0800
0900
Tempera-
ature
(°C)

34
34
33
33
31
31
29
29
27

26
26
28
28
30
30
30
30
28
28
27
25

25
28
29
29
31
31
31
30
31
Barometric Precipi-
pressure tat ion Speed

7 66 None 4
766
766
766
767
767
767
767
767

766
766
766
766
765
765
5
4
3
2
1
1
1
1

1
1
1
1
2
6
765 * 5
765 Rain 3
765 Rain 1
765 None 1
765 l
765

765
765
766
766
766
766
766
766
\
1
1

1
1
1
1
1
1
1
1
766 > 2
Wind
Direction

Southeast
South southeast
South
South southeast
South southeast
South
South
South
South

South
South
North northwest
North
North northwest
Southeast
South
North northwest
East northeast
East
North northeast
North

North northeast
North
West northwest
East
East
East
North northeast
East northeast
North northeast
                     111

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             CIBA-GEIGY CORPORATION, ST. GABRIEL, LOUISIANA

PRESAMPLING SITE SURVEY

     The presampling site survey at Ciba-Geigy Corporation, St. Gabriel,
Louisiana, plant was conducted on July 15, 1975.  The following personnel
were present:

     Mr. William F. Snyder          Staff Engineer, Environmental
                                      Engineering, Ciba-Geigy

     Mr. Phil Kuykendall            Midwest Research Institute

     Ciba-Geigy Corporation is located in a large industrial area which is
approximately 20 miles south of Baton Rouge.  The plant is on the east bank
of the Mississippi River in a predominantly swampy area with minimal residences,
Wind direction during the summer months are generally from the south and
west.

     Triazine herbicides are produced by the amination of cyanuric chloride.
The production processes result in the accumulation of "still bottoms" with
an approximate concentration of 2,000 ug/g.

     Solid wastes are drummed and shipped to an outside firm for incinera-
tion.  A vent scrubber is used for vapor emissions.  Wastewater is dis-
charged via open ditches to a holding pond, then discharged into the
Mississippi River at an average flow rate of 2,000 gal/min.  An emergency
wastewater outfall into Bayou Braud is occasionally used.

FIELD SAMPLING

     Field sampling at the Ciba-Geigy plant was conducted on August 13,
1975.  Air, soil, and water samples were collected.  Detailed description
of the sampling, plant activities, and weather conditions, are discussed
below,

Air Sampling

     Eight air sampling stations were positioned around the plant because
of the erratic wind direction.  Only one Tenax®-GC tube was used.  To avoid
possible breakthrough of the Tenax®-GC, sampling was operated 2 hr out of
every 8-hr period.   The sampling locations are shown in Figure A-8.  Exact
distance of each station to the production areas was determined and reported
along with other sampling data in Table A-14.
                                    112

-------
u>
                   . r~-\
   I 3j.
                         4200
':!! — | i MJ  ill i  ««,  jjjjte^^
i L^ ii	111	Jji—J


iii woo i II=^F—^"-^jir^i
 I    I ! 7100   7200   7300 I j I
      : i	1 ,	1 r	ill
    ,1+SON s
   _,  i  l3  ; 4: ™ U i  260° 'fi< *°° ! l^^p-^'^^l!   n|iL_zii!r_--jjp_z]ji
  f 1  !  ; '    i  800 e=±=}!=ss=5  I i ;    I i    !       !   740°  !    II    I
  \ (l—rf_ !  'Rn^""1   '   I ' PT ^  I '      ! 7K»  i 7200   7300 ||     I 76OO I: 77OO I TWO  \\\





^'^s^M^^^Sy^^ "T """"ir^T'T""!   I


_:     .if L"^°: nil __J~l:£lvjUI»°° 0iL~J .r~"j .-'z:J.ii L=^l.L-i3.^r^.-i^jl -~


      in""r':"i°1[p±s^®i!'; r^n^ !;^ ff^fl f    iii r    iiin^n s r^ ' iii n'^n I
      :l  I 1=3.  . i'  o -o: ' LJ	J- K  •""«-— f1'     i |     ill     I !i I    ;i;i     !i
      I  ,.. zzoo-^  j aoo  •. ._... 2100  !• U  2'100 III ' 9IO°  'Ii  9ZO°  ! I '  93O°  ! ii1 |  9*°°  '!  95O° ! I     /




 PCTOfECTTV (.IME---4-. Q. 00 N—\7 J	.	^ >-		     i                   /f
   ._. ~*T Process Water Outflow into Mississippi River ~   1      7  '"      .,     ,           3    '
	B	uj	ij	i_i i  i	E	F	G	H	I	.J	K. 	

     ZOMXJE      » "" J 3I«»E   37«OOE    42«5OE                              CIBA — GEIGY
           To Stouffer  IbStauffw     '        TOO..i-?  "^  *?                          cow«uw)«
            Figure A-8. Sample locations at Ciba-Geigy Corporation, St. Gabriel, Louisiana

-------
         Table A-14.  AIR SAMPLING AT CIBA-GEIGY CORPORATION, ST. GABRIEL,  LOUISIANA

Sample No
1

2
3

4

5

6
7

Exact location Sampling period
2,200 ft nortWwest of produc- 1st 2 hr of 8 hr
tion area
920 ft north of production area 1st 2 hr of 8 hr
1,600 ft northeast of produc- 1st 2 hr of 8 hr
tion area
800 ft east southeast of produc- 1st 2 hr of 8 hr
tion area
2,200 ft southeast of production 1st 2 hr of 8 hr
area
950 ft south of production area 1st 2 hr of 8 hr
1,600 ft southwest of production 1st 2 hr of 8 hr
Total sampling
time (hr)
7.6

8.8
6.8

6.3

6.4

Lost
6.1
Sampling Sample Sampler
rate (£/min) vol. (4) height (ftl
3.5 1,772 4

3.5 2,164 4
3.5 1,630 4

3.5 1,442 4

3.5 1,561 4

3.5 Lost 4
3.5 1,277 4
1,000 ft west of production  area   1st  2 hr of 8 hr
5.6
3.5
1,298

-------
Soil Sampling

     Soil sampling was conducted at four locations:

     S-l     Northwest of plant at Air Sampling Site No. 1

     S-2     Northeast of plant at Air Sampling Site No. 3

     S-3     Southeast of plant at Air Sampling Site No. 5

     S-4     Southwest of plant at Air Sampling Site No. 7

All soil samples were composites.

Water Sampling

     Water sampling was conducted at two locations:

     W-l     Raw plant water before use

     W-2     Process outflow

All water samples were grab samples.

Sediment Sampling

     No sediment samples were taken.  The process outflow ditch has a
gravel bottom.   The effluent pond was not available for sampling,  per Ciba-
Geigy's request.

Plant Activities and Weather Conditions

     The weather conditions during sampling are shown in Table A-15.
Plant activities were normal.
                                  115

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Table A-15.   WEATHER CONDITIONS DURING SAMPLING AT
        CIBA-GEIGY,  ST.  GABRIEL, LOUISIANA

Temper-
ature Precipi- Wind
Time
August 13
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
August 14
0100
0200
0300
0400
0500
0600
0700
0800
0900
1000
1100
1200
1300
(°C) tation Speed

39 none 3
37
37
36
36
36
34
32
32
29

27
27
27
29
29
30
32
32
33
35
35
36
7
5
5
4
7
5
5
3
5

5
6
8
7
7
5
4
6
5
6
4
4
36 2
Direction

North northwest
Northwest
Northwest
North northwest
Southwest
South
South
South
Southwest
Southwest

West southwest
Southwest
Souwthwest
West
West
West
West northwest
Northwest
Northwest
North northwest
North northwest
North northwest
North northwest
                      116

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                   OLIN CORPORATION, MCINTOSH, ALABAMA

PRESAMPLING SITE SURVEY

     The presampling site survey at Olin Corporation's Mclntosh, Alabama,
plant was conducted on July 23, 1975.  The following personnel were present:

     Mr. J. Oertling                    Works Manager, Olin

     Mr. F. Champion                    Production Manager, Organic
                                          Section, Olin

     Mr. C. Hovater                     Q. C. Manager, Olin

     Mr. R. Reams                       Technical Manager, Olin

     Mr. N. Barone                      Specialist - Environmental Affairs,
                                          Olin

     Mr. D. Sauter                      Midwest Research Institute

     Olin Corporation is located approximately 30 miles north of Mobile,
Alabama.  The area in the immediate vicinity of the plant is flat and
marshy.  Residential areas around the plant are minimal.  Winds are gen-
erally from the south during the summer.

     The production of pentachloronitrobenzene is by chlorination and
nitration of isomeric chlorobenzenes.  The production process results in
                                                             o
the accumulation of "still bottoms" which are cast into 27-ft  blocks
containing 80 to 90% HCB.  The rated capacity of the plant for PCNB is ap-
proximately 7 million pounds per year.  Approximately 2.8 to 3.0 million
pounds per year of HCB is generated in this process.

     Chlorine is also produced by mercury cells using carbon electrodes at
a rate of 130,000 tons/year.

     Solid wastes (HCB blocks) are stored in an open field in the southeast
corner of the plant.  The HCB block pile is covered with plastic.  This pile
represents HCB wastes from the last 2-1/2 years of PCNB production.  Ultimately,
Olin hopes to reclaim the HCB.

     Wastewater is discharged into two open ditches with an average combined
flow of 5 million gallons per day.  The south ditch, which is adjacent to
the PCNB plant and receives runoff from the waste disposal settling pond,
contributes mostly to this flow.  Both ditches combine outside the plant
boundary, and flow into a basin, and ultimately into the Tombigbee River.
                                    117

-------
     At least two landfills were observed.  The first landfill is located
directly outside the northeast corner of the plant boundary.  This land-
fill was used for HCB disposal before 1971.  The second landfill is the
southeastern section of the plant is primarily a garbage dump.  No land-
fills are currently in use for chemical disposal.

     At the conclusion of the presampling survey, it was agreed upon that
field sampling would be tentatively scheduled in the week of August 18,
1975.

FIELD SAMPLING

     Field sampling at the Olin plant was conducted on August 18, 1975.
Air, soil, water, and sediment samples were collected.  Detailed descrip-
tion of the sampling, plant activities, and weather conditions, are dis-
cussed below.

Air Sampling

     Eight sampling stations were positioned to give two upwind,  three mid-
plant, and three downwind sites.  Two Tenax®-GC sampling tubes were operated
in tandem at each site for three, 3-hr periods.  Sampling locations are
shown in Figure A-9.  The exact distance of each station to the production
area was determined and reported along with other sampling data in Table
A-16.

Soil Sampling

     Composite grab samples were taken outside and inside the plant boundary:

     S-l     Downwind (north boundary)

     S-2     Old landfill (northeast boundary)

     S-3     Brine pond area

     S-4     Center road (running north/south)

     S-5     High lift route (organic plant to storage area)

     S-6     Southeast landfill

     S-7     "Hex" storage area

     S-8     Old "Hex" dump area

     S-9     East road

                                   118

-------
                                             Chlorine
                                             Production
                                             Area

                                              H-l
Figure A-9.   Sampling locations  at Olin Corporation,  Mclntosh, Alabama
                                   119

-------
                         Table A-16.  AIR SAMPLING DATA AT OLIN CORPORATION, MCINTOSH, ALABAMA


Sample
General area No. Exact location
Far downwind 1 2,100 ft north northeast of
production area
Far .downwind 2 2,100 ft north of production
area
Far downwind 3 2,200 ft north northwest of
production area
f~~*
N)
° Near downwind 4 720 ft north northeast of
production area
Near downwind 5 700 ft north of production
area
Near downwind 6 800 ft north northwest of
production area
Upwind 7 640 ft south of production
area
Upwind 8 640 ft south of production
area
Total
sampling
Sampling period time (hr)
1st 3 hr of 12 hr 10.0

1st 3 hr of 12 hr 5.2

1st 3 hr of 12 hr 5.7

1st 3 hr of 12 hr 6.9

1st 3 hr of 12 hr 7,0

1st 3 hr of 12 hr 7.0

1st 3 hr of 12 hr 7.8

1st 3 hr of 12 hr 7.3

Sampling Sample
rate ' vol.
(4/min) (i)
3.5 2,103

3.5 1,100

3.5 1,204

3.5 1,445

3.5 1,473

3.5 1,472

3.5 1,630

3.5 1,525

Sampler
height
(ft)
4

4

4

20^

20S/

20*'

4

4

a/  Samplers were positioned on Brine Pond dike.

-------
     S-10     West road

     S-ll     Upwind south road

Water Sampling

     The following grab samples were obtained:

     W-l      Weak brine pond

     W-2      Strong brine pond

     W-3      Settling pond

     W-4      North/south running ditch

     W-5      Southern ditch area (upper drop)

     W-6      Combined creek (200 yard before basin)

     W-7      Basin (at mouth of creek)

     W-8      24-Hr composite of plant effluent (combined creek)

     W-9      Solar pond, west

     W-10     Solar pond, east

Sediment Sampling

     One sediment sample was collected at the strong brine pond.

Plant Activities and Weather Conditions

     The weather conditions during sampling are shown in Table A-17,
Plant activities were normal.
                                   121

-------
         Table A-17.   WEATHER CONDITIONS DURING SAMPLING AT
                 OLIN CORPORATION, MCINTOSH, ALABAMA

Time
August 18
1500s/
1600s-/
1700s/
1800
1900
2000
2100
2200
2300
24002/
August 19
0100—'
0200S/
O300i/
0400
0500
0600
0700
OSOO3-/
09002/
1000s/
1200S/
Tempera-
ture
37
37
36





26
23
23
23



25
27
29
32
35
Barometric
pressure
(mm Hg)
738
738
738





756
741
740
740



740
740
739
739
738

Speed
2-4
2-4
4-10
6-13
4-6
2-6
2-4
. 2-4
2-4
2-4
-
-
-
2-4
2-6
Wind ;
Direction
South
Southeast
North northeast
North
Southeast
East
Northwest
West
No wind
South
Southwest
No wind
No wind
No wind
No wind
No wind
North northeast
No wind
No wind
No wind
No wind
North
Precipi-
tation
None
None
None
Rain
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
None
a/  Indicates air sampling.
                                122

-------
      KAISER ALUMINUM AND CHEMICAL CORPORATION, GRAMERCY, LOUISIANA

     The presampling site survey at Kaiser Aluminum was conducted on
August 14, 1975.  The following personnel were present:

     Dr. Robert M. Hansen               Research and Development, Kaiser

     Mr. Phil Fourmet                   Environmental Manager, Kaiser

     Mr. Bob Curtis                     Environmental Control Specialist,
                                          Kaiser

     Mr. Phil Kuykendall                Midwest Research Institute

     Upon discussion with the plant officials, it was learned that chlorine
production utilizing graphite anodes had been terminated in 1973, and was
replaced by dimensionally stabilized anodes.  For waste disposal, prior to
1973, solid wastes were dispoded by landfill.  These residues have since
been covered by aluminum production wastes.  Water effluent is channeled
into the Mississippi river following on-line pH adjustment.

     As a result of the change in production technology and the solid wastes
disposed since 1973, it was decided that sampling at this plant would yield
no usable data.  Furthermore, samples collected from the Linden Chlorine
Company, at Linden, New Jersey, and the other chlorohydrocarbon plants,
which also produce chlorine, would serve the purpose of monitoring the chlorine
production plant for the HCB and HCBD emission.

                 PPG INDUSTRIES, LAKE CHARLES, LOUISIANA

PRESAMPLING SITE SURVEY

     The presampling site survey at PPG Industries' Lake Charles, Louisiana,
plant was conducted on August 22, 1975.  The following personnel were present:

     Mr. T. G. Taylor                   Technical Plant Manager, PPG

     Mr. Thomas C. Jeffery              Chief Process Engineer, PPG

     Dr. Earl Gorton                    Senior Research Supervisor, Organics,
                                          PPG

     Mr. C. A. Burns                    Environmental Control Specialist, PPG

     Mr. Mark Wood                      Environmental Analysis Coordinator, PPG

     Dr. Raymond Li                     Midwest Research Institute

                                   123~

-------
     PPG Industries is located more than 2 miles west of downtown Lake
Charles, Louisiana.  The surrounding terrain is flat and marshy.  The PPG
canal runs through the plant and into the Calcasieu River which flows to
Lake Charles.  The closest residential area is about 1 mile northwest of
the plant.  The wind, in the summer months, is very variable but most likely
from south southeast and least likely from the west.

     Chemicals produced in this plant include trichloroethylene, perchloro-
ethylene, ethylene dichloride, ethyl chloride, vinylidene chloride, methyl
chloroform, vinyl chloride, chlorine, hydrochloric acid, caustic soda, and
silica pigments.  The current production capacities of trichloro- and per-
chloroethylene are 350 tons/day.  However, the production of 725 tons/day
could be achieved and was produced in the past.  The plant operates 24 hr
a day, 7 days a week.

     Trichloro- and perchloroethylene are produced by a catalytic oxy-
chlorination process rather than the thermal process of chlorine and
hydrocarbons, thus resulting at a lower reaction temperature.  The chlorine
is produced in the plant (DSA has been used since 1969).  The production
wastes are piped into the incinerator and burnt at a residence time from
1/4 to 1/3 sec at 2500°F.  The water effluent is channeled into the PPG
canal which flows into the Calcasieu River.  The PPG canal also received
runoffs from the organochlorine production as well as effluents from the
power plant.

     Prior to the operation of the incinerator, landfill was used for waste
disposal.  The bid landfill site was covered with water.  It is still being
used for wastes than cannot be burnt in the incinerator or when incinerator
breakdown occurs.

     At the conclusion of the presampling survey, it was agreed upon that
field sampling would be tentatively scheduled in the week of September 2,
1975.

FIELD SAMPLING

     Field sampling at the PPG plant was conducted on September 4, 1975.
Air, soil, water, and sediment samples were collected.   Detailed descrip-
tion of the sampling, plant activities, and weather conditions, are dis-
cussed below.

Air Sampling

     Ten sampling stations were positioned to encircle the plant's in-
cinerator and organochlorine production area.  Two Tenax-GC®sampling tubes
were operated in tandem with 24-hr continuous sampling time.  Sampling

                                   ~ 124

-------
locations are shown in Figure A-10.  The exact distance of each station to
the incinerator/production area is listed along with other sampling data in
Table A-18.

Soil Sampling

     Composite grab samples were taken outside and inside the plant area.

     S-l      Landfill composite

     S-2      Composite at Air Stations 7, 5, and 4

     S-3      Composite at Air Stations 8, 9, and 10

     S-4      Composite near Air Station 1 on Columbia Southern Road

Water Sampling

     Grab samples were obtained at the following locations:

     W-l      Incinerator feed water, lake water

     W-2      Scrubber water

     W-3      Inlet treatment canal organic effluent before  scimmer

     W-4      Outlet treatment canal organic effluent after  scimmer.

     W-5      Surface water, landfill

     W-6      Downstream PPG canal, at Mobile Bridge No.  1,  1 gal.  taken

     W-7      Ship channel, adjacent to Air Station No.  10

Sediment Sampling

     Sediment samples were collected at three general areas.

     R-l      Downstream PPG canal near Air Sampling Station No.  1

     R-2      Main organic plant effluent, near Air Sampling Station No.  2

     R-3      PPG ship channel, near Air Sampling Station No.  10
                                   125

-------
Figure A-10.  Sampling locations at PPG Industries, Lake Charles, Louisiana

-------
                       Table A-18.  AIR SAMPLING DATA AT PPG INDUSTRIES, LAKE CHARLES, LOUISIANA
Sample
No.a/
1

2

3

4

5

6

7

8

9

10

Total
Location Sampling period sampling time (hr)
4,700 ft south of production 24 hr continuous 21.6
area
2,500 ft south southeast of 24 hr continuous . 21.4
production area
1,550 ft south of production 24 hr continuous 21.3
area *•
2,300 ft west northwest of 24"'hr continuous 21.0
production area
2,000 ft northwest of produc- 24 hr continuous 19.0-'
tion area
3,500 ft north northwest of 24 hr continuous 22.0
production area
1,250 ft north of production 24 hr continuous 20.7
area
1,250 ft northeast of production 24 hr continuous 21.8
area
2,250 ft east of production 24 hr continuous 21.9
area
2,700 ft east southeast of 24 hr continuous 21.9
production area
Sampling
rate (A/min)
0.9

0.9

0.9

0.9

0.9

0.9

0.9

0.9

0.9

0.9

Sample Sampler
vol. (A) height (ft)
1,180 4

1,170 4

1,210 4

1,170 4

950^ 4

1,250 4

1,180 4

1,190 4

1,250 4

1,130 4

a/  Stations were positioned surrounding the production area.
b/  Approximate value due to pump failure, indicates minimum volume.

-------
Plant Activities and Weather Conditions

     The weather conditions during sampling are shown in Table A-19.  Plant
activities were normal.
                                   128

-------
    Table A-19.  WEATHER CONDITIONS DURING SAMPLING AT PPG INDUSTRIES,
                        LAKE CHARLES, LOUISIANA



Temperature
Time ( °F)
Spetember 4
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
September 5
0100
0200
0300
0400
0500
0600
0700
0800

0900

85
86
88
85
85
85
82
80
78
77
76
75
76
75

75
75
75
75
75
75
74
73

72
Barometeric
pressure
(mm Hg)

763
762
762
762
762
762
762
762
763
763
763
763
762
762

762
762
762
762
762
763
763
763

763

Speed
(mph)

7
7
7
7
7
7
8
7
5
4
3
2
-
-

3
6
5
3
2
3
2
3

3
Wind
Direction

East
East
East
East
East
East southeast
East southeast
East
East
East
East
West
-
-

East
East
East
East
East
East
East
East ,
a 1
East-7
a/  Rain.
                                   129

-------
  APPENDIX B
ANALYTICAL DATA
      130

-------
Table B-l.  HCB CONCENTRATIONS IN AIR SAMPLES FROM VULCAN
           MATERIALS COMPANY, WICHITA, KANSAS

Sampling
station
1









2









3









4









Sampling
time
1935-2035

0120-0227

0430-0523

0841-0941

1320-1424

1935-2035

0120-0227

0430-0523

0841-0941

1320-1424

1935r

0120-0227

0430-0523

0841-0941

1320-1424

1945-2045

0110-0220

0450-0555

0902-1010

1307-1425

Volume sampled
(liter)
26

42

33

37

40

17

36

29

32

35

Lost

57

45

51

54

27

32

30

31

36

Type of
sample
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
HCB
Total ng pg/m3g/
5 0.6
10
< 2 0.2
7
< 2 0.2
6
< 2 0.3
10
4 0.4
10
167 11.3
25
< 2 0.6
18
< 2 1.6
45
< 2 0.3
7
< 2 1.0
32


< 2 0.1
5
< 2 0.2
6
< 2 0.2
8
65 1.7
25
275 11.5
35
2.5 0.6
18
< 2 0.8
20
270 9.7
30
144 5.0
36
                              131

-------
Table B-l.  (continued)

Samp 1 log
gtation
5









6









7









8









Sampling
time
1945-2045

0110-0220

0450-0555

0902-1010

1307-1425

1945-2045

0110-0220

0450-0555

0902-1010

1307-1425

1950-2050

0051-0158

0456-0555

0904-1010

1308-1425

1950-2050

0103-0202

0458-0600

0908-1010

1308-1420

Volume sampled
(liter)
41

48

44

46

53

34

40

37

39

45

148

166

146

163

190

212

209

220

227

255

Type of
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
RGB
Total ng
100
40
38
15
2.2
12
50
16
75
3.3
< 2
38
< 2
18
<2
14
900
21
119
20
<2
250
<2
125
<2
142
< 2
150
< 2
275
<2
116
< 2
46
<2
66
< 2
66
<2
88
pg/m3
3.4

1.1

0.4

1.4

1.5

1.1

0.5

0.4

23.6

3.0.

1.7

0.8

1.0

0.9

1.5

0.6

0.2

0.3

0.3

0.4

             132

-------
Table B-l.  (continued)

Sampling
station
9
\



10




11




12




Sampling
time
1950-2050
0103-0202
0458-0600
0908-1010
1308-1420
1910-2310
0005-0330
0340-0728
0737-1117
1124-1433
1910-2310
0005-0330
0340-0728
0737-1117
1124-1433
1919-2315
2350-0315
0325-0712
0721-1101
1113-1433
Volume sampled
(liter)
227
223
234
242
272
809
691
768
741
637
856
732
814
785
675
863
738
817
792
720
Type of
sample
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
HCB
Total ng
7
167
<2
65
< 2
114
< 2
87
7
135
< 2
250
< 2
150
< 2
134
<2
91
< 2
97
< 2
278
< 2
109
< 2
75
< 2
78
Sample lost
106
14
850
< 2
300
815
190
875
210
18
260

0.8
0.3
0.5
0.4
0.5
0.3
0.2
0.2
0.1 .
0.2
0.3
0.2
0.1
0.1
0.2
1.0
0.4
1.2
1.4
0.4
             133

-------
Table B-l.  (continued)

Sampling
station
13




14




15




16




Sampling
time
1915-2315
2350-0315
0325-0712
0721-1101
1113-1433
1920-2259
2335-0258
0310-0640
0650-1046
1057-1435
1920-2259
2335-0258
0310-0640
0650-1046
1057-1435
2005-0010
0025-0345
0355-0744
0752-1154
1200-1430
Volume sampled
(liter)
917
784
867
840
764
806
816
844
949
876
837
805
832
935
863
862
702
804
849
527
Type of
sample
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Filter
Tenax
Filter
Tenax
HCB
Total na
5
950
91
320
950
200
900
180
980
280
< 2
40
< 2
< 2
60
< 2
85
< 2
225
< 2
25
< 2
60
< 2
97
< 2
81
5
200
4
330
< 2
138
< 2
160
21
230
< 2
440

1.0
0.5
1.3
1.3
1.7
0.1
0.1
0.1
0.1
0.3
0.03
0.1
0.1
0.1
0.2
0.4
0.2
0.2
0.3
0.8
              134

-------
                 Table B-l.    (concluded)

Sampling
station
17









18









Tena™GC
blank
Millipore
filter
blank
Sampling
time
2005-0010

0025-0345

0355-0744

0752-1154

1200-1430

2010-

0022-0355

0400-0755

0759-1121

1215-1430






Volume sampled
(liter)
730

596

682

721

447

548

711

785

858

451






Type of
sample
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax
Filter
Tenax





HCB
Total ng
NDb/
420
< 2
200
950
130
21
350
925
330
9
395
< 2
230
935
280
3
490
10
320






Hg/m3
0.6

0.3

1.6

0.8

2.1

0.7

0.3

1.6

0.6

0.7

ND

ND


a/ Concentration based on the sum of ng  found on the filter and Tenax.
bV ND - None detected.
                              135

-------
Table B-2.  RGB CONCENTRATIONS IN AIR SAMPLES FROM STAUFFER
          CHEMICAL COMPANY, LOUISVILLE, KENTUCKY

Concentration
Sampling
station
1






2






3






4






5







Sampling time
1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

Type of
sample
Tena«®-GC
Tena^-GC
Tena^5)-GC
Tenaj^-GC
Tenax®-GC
TenaxSSi-GC
Filters
Tenax®-GC
Tenax@-GC
Tenax@-'GC
Tenaj^-GC
Tena^B^GC
Tenax@-GC
Filters
Tenax®-GC
Tenax®-GC
Tenax<®-GC
Tena*5*-GC
Tenaxl^GC
Tenax@-GC
Filters
Tena^GC
Tenaji®-GC
Tena^GC
TenaxiSi-GC
Tenax@-GC
Tenax@-GC
Filters
Tena^SLGC
Tenax!®-GC
Tenaj<®-GC
Tena^-GC
Tenax®-GC
Tenax®-GC
Filters
Volume sampled
(liter)
415
414
540
390
380
449

455
408
514
463
336
450

384
438
490
448
Lost
461

432
456
454
519
437
470

420
470
540
496
426
435

(U»g/m3)
HCB
0.04
0.07
0.12
0.05
0.05
0.08
< 0.01
0.08
0.04
0.04
0.03
0.07
0.05
< 0.01
1.1
1.4
0.35
0.35
—
0.19
0.07
2.56
2.06
0.62
0.42
0.16
0.13
1.0
0.85
1.03
0.71
0.36
0.20
0.34
0.09
                            136

-------
Table B-2.  (concluded)


Sampling
station
6






7






8






9








Sampling time
1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000

1000-1400
1400-1800
1800-2200
2200-0200
0200-0600
0600-1000


Type of
sample
Tenax®-GC
Tenax®-GC
Tenax®-GC
Tenax®-GC
Tena*®-GC
Tenax®-GC
Filters
Tenax®-GC
Tenax@-GC
Tenax@-GC
Tenax@-GC
TenaxR-GC
Tenax®-GC
Filters
Tenax^-GC
Tenax@-GC
Tenax®-GC
Tenax®-GC
Tenax@-GC
Tenax®-GC
Filters
Tenax^-GC
Tenax®-GC
Tenax®-GC
Tenax@-GC
Tenax®-GC
Tenax®-GC
Filters

Volume sampled
(liter)
408
455
464
442
425
468

450
472
563
469
426
470

450
488
554
476
436
468

455
492
562
483
466
468

Concentration
(Ug/m3)
HCB
0.69
0.71
0.45
0.31
0.11
0.19
0.20
0.57
0.53
. 0.24
0.23
0.12
0.28
<0.01
0.32
0.20
0.07
0.16
0.05
0.06
0.01
0.05
0.06
0.02
0.05
0.02
0.03
< 0.01
           137

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         Table B-3.   RGB CONCENTRATIONS  IN AIR SAMPLES FROM DOW
                  CHEMICAL COMPANY,  PITTSBURG,  CALIFORNIA


Sampling
station
1


2
•

3


4


5


6


7


8



Type of
samp le
Tenax®GC (front)
Tenax®GC (back)
Filter
Tenax®bc (front)
Tenax®GC (back)
Filter
Tenax®GC (front)
Tenax®GC (back)
Filter
Tenax®bc (front)
Tenax®GC (back)
Filter
Tenax®GC (front)
Tenax^GC (back)
Filter
Tenax®GC (front)
Tenax®GC (back)

Tenax®GC (front)
Tenax®GC (back)
Filter
(R)
Tenax^GC (front)
Tenax®GC (back)
Filter
Vo lume
sampled
(liter)
4,336


427


4,166


3,870


3,713


4,314


962


3,963


Concentration
(ug/m3)
HCB
0.02
ND
ND
< 0.02
ND
ND
0.05
ND
ND
0.08
ND
ND
0.02
ND
ND
< 0.02
ND
ND
< 0.02
ND
ND
< 0.02
ND
ND
Note:  ND = none detected.
                                  138

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Table B-4.  HCB CONCENTRATIONS IN AIR SAMPLES FROM E. I. DU PONT
          DE NEMOURS AND COMPANY, CORPUS CHRIST!, TEXAS

Sampling
station Type of
1 Tenax®-GC
Tenax®-GC
Filter
2 TenaxfSLGC
TenaxS^-GC
Filter
3 Tenax^-GC
Tenax1?)-GC
Filter
4 Tenax^-GC
Tenax@-GC
Filter
5 Tenax®-GC
Tenax®-GC
Filter

sample
, front
, back

, front
, back

, front
, back

, front
, back

, front
, back

Volume sampled
U)
4,371
4,371
4,371
3,621
3,621
3,621
4,070
4,070
4,070
4,007
4,007
4,007
3,965
3,965
3,965
Concentration (ug/nr)
HCB
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
                               139

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Table B-5.  RGB CONCENTRATIONS IN AIR SAMPLES FROM DIAMOND
          SHAMROCK CORPORATION, DEER PARK, TEXAS

Sampling
station
I


2


3


4


5


6


7


8




Type of sample
Tenax®-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenaj^-GC,
Filter
Tenax®-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenax®-GC,
Filter
Tenax^-GC,
Tena^-GC,
Filter
Tenax®-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenax®-GC,
Filter
front
back

front
back

front
back

front
back

front
back

front
back

front
back

front
back

Volume sampled
(£)
580
580
580
598
598
598
485
485
485
540
540
540
542
542
542
608
608
608
559
559
559
555
555
555
Concentration (ug/m3)
HCB
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
                            140

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Table B-6.  HCB CONCENTRATIONS IN AIR SAMPLES FROM
  CIBA-GEIGY CORPORATION, ST.' GABRIEL, LOUISIANA

Sampling
station
1
2
3
4
5
6
7
8
Type of sample
Tenax@-GC
Filter
Filter
Tena^-GC
Filter
Filter
Filter
Lost
Filter
Filter
Volume sampled
1,772
1,772
2,164
2,164
1,630
1,630
1,442
1,442
1,561
1,561
Lost
1,277
1,277
1,298
1,298
«%
Concentration (ug/nr)
HCB
0.02
ND
0.01
ND
0.02
ND
0.01
ND
0.01
ND
Lost
ND
ND
ND
ND
                         141

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Table B-7.  RGB CONCENTRATIONS IN AIR SAMPLES FROM
        OLIN CORPORATION, MCINTOSH, ALABAMA

Sampling
station
1


2


3


4


5


6


7


8


Volume sampled
Type of sample
Tenax®-GC,
Tenaxi^GC,
Filter
Tenax@-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenax@-GC,
Filter
Tenax®-GC,
Tenax@-GC,
Filter
Tenas®-GC,
Tenax®-GC,
Filter
Tenax®-GC,
Tenax@-GC,
Filter
Tenax®-GC,
TenaxS®-GC,
Filter
front
back

front
back

front
back

front
back

front
back

front
back

front
back

front
back

U)
2,103
2,103
2,103
1,100
1,100
1,100
1,204
1,204
1,204
1,445
1,445
1,445
1,473
1,473
1,473
1,472
1,472
1,472
1,630
1,630
1,630
1,525
1,525
1,525
Concentration (ug/m3l
HCB
0.26
ND
ND
0.06
ND
ND
0.04
ND
ND
0.48
0.08
ND
0.24
ND
ND
0.03
ND
ND
2.22
ND
ND
1.11
ND
ND
                        142

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Table B-8.  HCB CONCENTRATIONS IN AIR SAMPLES FROM PPG
          INDUSTRIES, LAKE CHARLES, LOUISIANA

Sampling
station
1 .


2


3


4


5


6


7


8


9


10


Volume sampled
Type of sample
Tenaj^-GC, front
Tenaa@-GC, back
Filter
Tenaj@-GC, front
Tenaji®-GC, back
Filter
Tenax®-GC, front
Tena3@-GC, back
Filter
Tenax®-GC, front
Tenax®-GC, back
Filter
Tena^§X-GC, front
Tena*®-GC, back
Filter
Tenaj@-GC, front
Tena^5)-GC, back
Filter
Tena2$-GC, front
Tena3®-GC, back
Filter
Tenaj@-GC, front
Tena3®-GC, back
Filter
Tena^-GC, front
Tena^-GC, back
Filter
Tena^-GC, front
Tena^-GC, back
Filter
U)
1,180
1,180
1,180
1,170
1,170
1,170
1,210
1,210
1,210
1,170
1,170
1,170
950
950
950
1,250
1,250
1,250
1,180
1,180
1,180
1,190
1,190
1,190
1,250
1,250
1,250
1,130
1,130
1,130
Concentration (ug/nr)
' HCB
0.02
ND
0.42
0.02
ND
0.07
0.03
ND
0.13
ND
ND
1.30
ND
ND
1.47
0.03
ND
0.33
0.03
ND
1.63
ND
ND
ND
ND
ND
ND
ND
ND
0.02
                           143

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                APPENDIX C
METHOD DEVELOPMENT FOR SAMPLING AND ANALYSIS
                    144

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 LITERATURE SEARCH

      A search of the literature to  1967  revealed  that  there was  no  specific
 method for sampling RGB in water. The method  used most often  for sampling
 pollutants in water was the  "grab   technique." Detailed procedures  of  the
 grab technique can be found  in many of the  standard method texts.JLli'  HCB
 in water samples is concentrated by extraction with appropriate  organic
 solvents.  In some cases,  HCB is concentrated  by passing the water sample
 through a  column filled with an appropriate trapping medium.  Gesser et al.ft/
 used a glass column with two polyurethane plugs,  and found that  HCB, along
 with a number of polychlorinated biphenyls, could be absorbed on the column.
 These compounds were then extracted by treating with acetone  and hexane.
 This kind  of concentration technique, with  other  trapping media  such as
 activated  charcoal, and polystyrene copolymer, Amberlite XAD-2 and  XAD-4,
 has been successfully applied in trapping other chlorinated pesticides,    '

      Sampling of HCB in air  is generally carried  out by trapping the com-
 pound either in an appropriate organic solvent or in an appropriate organic
 resin.   Columns of wood-charcoal cigarette-filter in series as well as silica
 gel have been used to trap HCB in air.H-lft/  The  HCB is recovered by appro-
 priate solvent  extraction. Organic  resins such as Chromosorb  A and  Chromosorb
 101 have been used to trap HCB and  other chlorinated pesticides.J^il^./ A
 nylon-chiffon cloth (0.25 or 0.5 wr~) impregnated  with  ethanediol and held
 vertically in a wooden frame and exposed to the atmosphere for 5 days  has
 been reported to trap organochlorine as  well  as organophosphorus compounds.±Z/
 Another organic resin,  Tenax®-GC, has been  reported to be an  efficient trap-
 ping medium for aromatic  hydrocarbon and organochlorine.—'

 WATER SAMPLING  AND RECOVERY  STUDIES

      As  a  result  of the literature  search,  it was decided that for  water
 sampling,  the "grab" method  would be employed as  the primary method. If the
 concentration of  HCB was  suspected to be low, an Amberlite XAD-4 column
 would be used to  concentrate the two substances.  Both  sampling techniques
 were evaluated  prior to actual field sampling.

 Hexane  Extraction

      Table  C-l  shows  the results of recovery  studies for ri-hexane extrac-
 tion of  HCB from water  samples fortified with 1 to 30 p,g/liter.  Each of the
 water samples  (1  liter) was  extracted with three  10-ml aliquots  ii-hexane,
made  up  to  the mark of  a  100-ral  volumetric flask, and analyzed for HCB by
 gas  chromatography.  The average  recovery was over 100% for HCB. The slightly
 positive error  observed in the HCB recovery studies was probably  due to the
 fact  that the fortified HCB  samples and the standard HCB solution used for
 calibration were  prepared from two different stock solutions.
                                    145

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       Table C-l.  RECOVERY STUDIES OF RGB BY n-HEXANE EXTRACTION
Sample

  1
  2
  3
  4
  5
  6
  7
Blank
Amount in 1 liter
  of water

       1
       2
       3
       5
      10
      20
      30
      None
Amount found in
 n-hexane

     1.1
     2.2
     3.4
     5
    11
    22
    32
    None
% Recovery

   110
   110
   113
   100
   110
   110
   106
Elution from Amberlite XAD-4

     Water samples fortified with 1 to 30 Vig/liter of RGB were passed
through Amberlite XAD-4 columns containing 7 g of the trapping material.
Recovery of the two substances was accomplished by eluting, first with a
small amount of acetone, followed by a larger volume of ji-hexane. Table
C-2 shows that the average recovery of HCB was greater than 70% (first
five runs).* Recoveries of HCB with either a closed or open system showed
no significant difference, indicating volatilization of HCB is not a problem
over short time periods.

    Table C-2.  RECOVERY OF HCB FROM WATER BY CONCENTRATION ON XAD-4

Run (U.R/4)
1 (30)
2 (30)
3 (1 )
4 (5 )
5 (30)
6 (30) I/
Flow rate
(ml/min)
2
2
2
2
8
10 1
                             Recovery from
                               ii-hexane
                              elution (%)

                                  65
                                  63
                                  85
                                  73
                                  80
                                  77
                               Recovery from
                                  Soxhlet
                                extraction

                                    0
                                    0
                                    0
                                    0
                                    0
                                    0
                      Recovery from
                          water
                      extraction (%)

                           13
                           17
                            0
                            0
                            3
                           14
a/  Closed elution system.
   When actual environmental samples were analyzed, the amount of Amberlite
     XAD-4 used in sampling (250 g) was so high that recovery by elution was
     very time-consuming. Elution was replaced by overnight Soxhlet extrac-
     tion.
                                   146

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      Evidence of volatilization  loss of RGB was demonstrated by the re-
 sults of  the following  experiment. Five 250 ml water  samples fortified with
 5  y,g/liter  of HCB were  placed  in five  250 ml separatory funnels. Three of
 the  funnels were left uncapped overnight while the remaining two funnels
 were capped. Each water sample was then extracted and analyzed for HCB.
 The  results, shown  in Table C-3,  indicate that measurable amounts of HCB
 were lost due to volatilization  from the open system.
           Table C-3.  LOSS OF HCB DUE TO VAPORIZATION
Run              Separatory funnel              HCB recovery (%)

  1                  Capped                            94
  2                  Capped                            94
  3                  Uncapped                          58
  4                  Uncapped                          55
  5                  Uncapped                          51

AIR SAMPLING AND RECOVERY STUDIES

     Chromosorb 101 and Tenax®-GC were tested for their trapping efficiency
utilizing a device shown in Figure C-l. This device was initially designed
to check the recovery of HCB from water by vaporization at reduced pressure.
The results also indicate efficiency for collecting HCB from water-saturated
air.

     One liter of water, fortified with 1 to 30 jig/liter of HCB, was placed
in a one-neck 24/^0 flask with a thermometer pit so that the water tempera-
ture was monitored. The vapor was drawn through a Tenax®-GC or Chromosorb
101 (approximately 1 g) column with a vacuum pump or water aspirator. The
vapor flow rate through the trapping column was monitored with a calibrated
flowmeter and was maintained at 3 liters/min. After passing a known volume
of vapor through the column, the trapping material was first extracted with
ii-hexane in an ultrasonic bath, then by overnight Soxhlet extraction. The
remaining water was also extracted with ja-hexane. All the extracts were
analyzed for HCB by electron capture gas chromatography.

     Table C-4 shows the results of a set of seven experiments. Runs 1 and
2 were designed to compare the efficiency of Chromosorb 101 and Tenax@-GC,
while Runs 3 through 7 were repeated experiments to evaluate the efficiency
of Tenax®-GC at various HCB concentrations. In general, under these experi-
mental conditions, the trapping and recovery of HCB with Tenax®-GC is more
effective than with Chromosorb 101.
                                   147

-------
00
                           .6 in.
                            Trapping  Column
•18/7
 Ball Joint
                                 Thermometer
                                 Pit
                                   Heating
                                   Mantle
                                                    To Meleod Gauge
                  T Pinch
              Of- v Clamp
                n 1
                                     Cold Trap
                                                                                                    To Water Aspirator
                                                                                                    or Mechanical Pump
                           Figure C-l.  Apparatus for recovery of RGB from water by vaporization
                                                           at reduced pressure

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         Table C-4.  RECOVERY OF HCB FROM WATER-SATURATED AIR
Run        Column

  1     Chromosorb  101

  2     Tenax®-GC
  3     Tenax®-GC
  4     Tena:x®-GC
  5     Tena*®-GC
  6     Tenax®-GC
  7     Tenax®-GC
Total HCB
in sample
  (y.g)

   30

   30
    1
    1
    5
   30
   30
                                      7
                                      10
  Recovery
   from
ultrasonic
extraction
                          7
                          10
  Recovery
   from
  Soxhlet
extraction
None de-
tected
100
94
85
102
90
86
None de-
tected
Trace
Trace
Trace
Trace
2
2
% Recovery
   from
extraction
 of water

    46

     6
     5
     2
     4
     3
     9
SEDIMENT SAMPLING AND RECOVERY STUDIES
     Sediment was taken from two Kansas City area creeks. The samples were
collected from the top 1 to 2 in. of sediment. The samples were fortified
with HCB and recoveries were determined using standard procedures (for
sediments) described in the Manual of Analytical Methods prepared by the
Pesticides and Toxic Substances Effects Laboratory of the National Environ-
                                         TM
mental Research Center, USEPA. A Florisil  column was used for sample
cleanup and 67o ethyl ether in petroleum ether was used for the elution of
HCB.
     Two different procedures were used to prepare fortified sediment sam-
ples. In the first method, HCB was added to known amounts of sediment prior
to evaporation of moisture from the sediment; in the second method, HCB was
added after the moisture in the sediment had evaporated almost to dryness.
Results of the recovery studies of these sediment samples (Runs 1 through 4)
are shown in Table C-5.

     Because of the low recovery of HCB in Runs 1 through 4, direct Soxhlet
extraction (1:1 acetone/hexane) of the fortified sediment samples was tested.
Runs 6 and 7 in Table C-5 show the results of Soxhlet extraction. The re-
covery of HCB improved significantly.  Therefore, direct Soxhlet extraction
of the sediment was chosen as the standard method.  However,  if interferences
from other impurities were present, FlorisilM cleanup would  be used.  The
amount of HCB determined in the sample analysis was reported on dry weight
basis.
                                    149

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               Table C-5.  RECOVERY OF HCB FROM SEDIMENTS
Run      Sample weight (g)      Amount HCB added (p,g)     % Recovery (HCB)

Li/             50                       5                       59
2£/             50                       5                       64
3k/             50                       5                       73
4k/             50                       5                       67
5               50                     Control                   ND
6£/             50                       5                       95
7£/             50                       5                       98
a/  HCB added before moisture in sample was almost evaporated to dryness.
b/  HCB added after moisture in sample was almost evaporated to dryness.
c/  Direct Soxhlet extract of sample.
                                   150

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                        REFERENCES FOR APPENDIX C

 1.  Standard Methods;  Water and Wastewater,  13th Edition, APHA  (1971).

 2.  ASTM Standards, "Water—Atmospheric Analysis," Part 23 (1972).

 3.  Cox, G. V., Amer. Lab., 6(7):36 (1974).

 4.  Gesser, H. D., et al., Anal. Letter, 4_(12):883-886 (1971).

 5.  Hyndshaw, A. Y., J.A.W.W.A., 64j309 (1972).

 6.  Buelow, R. W., J. K. Carswell, and J. M.  Symons, J.A.W.W.A., 65j57 (1973).

 7.  Ibid., 65jl95 (1973).

 8.  Burnham, A. K., G. V. Calder, J. S. Fritz, G. A. Junk, H. J. Svec, and
       R. Willis, Anal. Chem., 44j 139 (1972).

 9.  Kennedy, D. C., Environ. Sci. Technol., 7(2):138 (1973).

10.  Burnham, A. K., G. V. Calder, J. S. Fritz, G. A. Junk, H. J. Svec, and
       R. Vick, J.A.W.W.A., 65j722 (1973).

11.  Lebedeva, T. A., et al., Metody Anal. Pestits.. pp. 57-59 (1970)  in
       Russian.

12.  Dranovskaya, L. M., and A. G. Gul'ko, Ostsillogr. Peremen. Polyarografiya,
       pp. 163-167 (1971).

13.  Gul'ko, A. G., L. M. Dranovskaya, and V. F. Chernokan, Aktual. Vop. Gig.
       Epidemiol.. pp. 71-73 (1972).

14.  Grob, K., and G. Grob, J. Chromatogr., 62(1):1-13 (1971).

15.  Mann, J. B., H. F. Enos, J. Gonzalez, and J. F. Thompson, Environ,
       Sci. Technol.. 8(6) :584 (1974).

16.  Aue, W. A., and P. M. Teli, J. Chromatogr.. 62J1): 15-27 (1971).

17.  Tessari, J. D., and D. L. Spencer, J. Assoc. Offie. Anal. Chem..
       54(6):1376-1382 (1971).

18.  Enagonio, D. P., W. E. May, and S. P. Cram, Paper presented at the
       25th Pittsburgh Conference on Analytical Chemistry and Applied
       Spectroscopy (1974).
                                   151

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                                   TECHNICAL REPORT DATA
                            (Please read Insinii'tions on the reverse before completing)
 1. REPORT NO.
   EPA  560/6-76-001
                              2.
                                                           3. RECIPIENT'S ACCESSION-NO. •
 4. TITLE AND SUBTITLE
   Sampling  and  Analysis of Selected Toxic  Substances
   Task  1A - Hexachlorobenzene
             5. REPORT DATE
                June 1976
             6. PERFORMING ORGANIZATION CODE
 7. AUTHOR(S)
                                                           8. PERFORMING ORGANIZATION REPORT NO
   R. T. Li, J.  L.  Spigarelli and J. E. Going
9. PERFORMING ORGANIZATION NAME AND ADDRESS
   Midwest Research  Institute
   425 Volker Boulevard
   Kansas City, Missouri  64110
                                                            10. PROGRAM ELEMENT NO.
              11. CONTRACT/GRANT NO.

                Contract No. 68-01-2646
 12. SPONSORING AGENCY NAME AND ADDRESS

   Environmental Protection Agency
   Office of Toxic Substances
   Washington, D.C.  20460
              13. TYPE OF REPORT AND PERIOD COVERED
              Final July 1974-September  1975
              14. SPONSORING AGENCY CODE
 15. SUPPLEMENTARY NOTES
 16. ABSTRACT
       Nine industrial plants were sampled to determine hexachlorobenzene (HCB) levels
  in air, water, soil and  sediment.  The plants represent  six  major industries:  per-
  chloroethylene, trichloroethylene,  carbon tetrachloride,  chlorine,  triazine herbicides
  and pentachloronitrobenzene.   In general, higher levels  of HCB were associated with
  the production of lower  chlorinated hydrocarbons than with the production of other
  chemicals.  HCB levels in  soil and  air at the pentachloronitrobenzene plant were rela-
  tively high.  The levels of HCB associated with plants producting chlorine and tri-
  azine herbicides were very low.  Several different waste-disposal methods were used at
  the perchloro-and trichloroethylene plants that were sampled.  The  highest level of
  HCB was detected in air  and soil at the plant using on-site  landfill and open pit
  storage. High HCB levels were  detected in loading and transfer areas at plants using
  off-site disposal methods.

       The highest level of  HCB  found in the air on plant property  was 24 ug/m3.  The
  HCB level in an open waste treatment pond was 306 ug/liter.  The  level of HCB in soil
  within the plant area'was  over  1,000 ug/g at three plants.   The maximum concentration
 ^_	.	(continued)	     ,   	
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS  C. COSATI Field/Group
  Monitoring  -  Air,  Water, Soil, Sediment
 Hexachlorobenzene
Organic
  Chemistry
 3. DISTRIBUTION STATEMENT
  Release Unlimited
                                              16. SECURITY CLASS (This Report/
                                               Unclassified
                           21. NO. OP PAGES
                                              20. SECURITY CLASS (THIS page)
                                               Unclassified
                           22. PRICE
EPA Form 2220-1 (9-73)
                                            152

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                           TECHNICAL REPORT DATA
16.  Abstract

of HCB in air sampled off plant property was 0.36 jig/m .  A level of 3
was detected at the boundary of another plant.  Soil taken from a cornfield
adjacent to one plant contained 1.1 ug/g, and over 3,000 ug/g were detected
along a boundary road of another.  HCB levels in water sampled beyond the
plant property exceeded 1 ug/liter at two plants.

     Samples were collected from two sewage treatment plants; negligible
quantities of HCB were detected.
                                    153

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