EPA-560/6-77-025
ENVIRONMENTAL MONITORING
NEAR INDUSTRIAL SITES
METHYLCHLOROFORM
AUGUST 1977
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF TOXIC SUBSTANCES
WASHINGTON, D.C. 20460
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EPA-560/6-77-025
ENVIRONMENTAL MONITORING NEAR INDUSTRIAL SITES
METHYLCHLOROFORM
August 1977
BATTELLE
Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
Vincent J. DeCarlo
Project Officer
Contract No. 68-01-1983
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF TOXIC SUBSTANCES
WASHINGTON, B.C. 20460
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NOTICE
This report has been reviewed by the Office of
Toxic Substances, Environmental 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
endorsement or recommendation for use*
ii
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TABLE OF CONTENTS
Page
1. INTRODUCTION 1-1
2. SAMPLING RATIONALE 2-1
3. SAMPLING PROTOCOL 3-1
Air 3-1
Water 3-2
Sediment 3-2
Soil 3-2
Vegetation 3-3
Tissue 3-3
Number of Samples 3-3
4. ANALYTICAL METHODS 4-1
Determination of Methylchloroform in Ambient Air 4-1
Determination of Methylchloroform in Water 4-4
Determination of Methylchloroform in Soil and Sediment . . 4-19
5. MONITORING DATA 5-1
Production Sites Monitored 5-1
User Site Monitored 5-1
Background Site Monitored 5-1
Discussion of Results 5-1
FIGURES
Number Page
4.1 Schematic of EC/GC ambient air analysis system 4-2
4.2 Calibration curves for chlorinated hydrocarbons—Varian
1200/EC detector 4-5
4.3 Calibration curves for chlorinated hydrocarbons—ATC
140A/EC detector 4-6
• •*
4.4 Schematic of a liquid-sample concentrator 4-8
iii
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FIGURES (Continued)
Number Page
4.5 Chromatogram of chlorinated solvents 4-9
4.6 Chromatogram showing 500 ppb each of methylchloroform,
trichloroethylene, and perchloroethylene using FID
detector 4-11
4.7 Chromatogram showing 50 ppb each of methylchloroform,
trichloroethylene, and perchloroethylene using FID
detector 4-12
4.8 Calibration curves for the determination of methylchloro-
form and trichloroethylene using FID detector 4-14
4.9 Calibration curves for the determination of methylchloro-
form and trichloroethylene using electron-capture
detector 4-16
4.10 Chromatogram of several chlorinated hydrocarbons using
electron-capture detector after completion of
development work 4-17
4.11 Schematic of soil and sediment analysis apparatus 4-21
4.12 Sample Chromatogram for sediment 4-23
5.1 Sampling locations at Dow Plant A, Freeport, Texas—
methylchloroform production site 5—5
5.2 Sampling locations at Vulcan Materials Company, Geismar,
Louisiana—methylchloroform production site 5-14
5.3 Sampling locations at Ethyl Corporation, Baton Rouge,
Louisiana—methylchloroform production site 5-21
5.4 Sampling locations at PPG Industries, Lake Charles,
Louisiana—methylchloroform production site 5-27
5.5 Sampling locations at Boeing Company, Auburn, Washington—
methylchloroform user site 5-33
5.6 Sampling locations at St. Francis National Forest,
Helena, Arkansas—background site 5-39
iv
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TABLES
Number Page
2.1 Sites Monitored for Methylchloroform 2-1
4.1 Operating Conditions and Performance Characteristics of
the EC/GC Systems Used for Ambient Air Measurements of
Chlorinated Hydrocarbons 4-3
4.2 Volatile Impurities in Waters 4-13
5.1 Ambient Air Measurements at Dow Chemical Plant A
(Methylchloroform Producer) 5-6
5.2 Analysis of Water, Soil, and Sediment Samples from Dow
Chemical Plant A (Methylchloroform Producer) 5-10
5.3 Descriptions of Sampling Locations at Dow Chemical
Plant A, Freeport, Texas (November 9-12, 1976) 5-11
5.4 Ambient Air Measurements at Vulcan Materials Plant
(Methylchloroform Producer) 5-15
5.5 Analysis of Water, Soil, and Sediment Samples from
Vulcan Materials Plant (Methylchloroform Producer) . . . 5-18
5.6 Descriptions of Sampling Locations at Vulcan Materials,
Geismar, Louisiana (December 2, 1976) 5-19
5.7 Ambient Air Measurements at Ethyl Corporation (Methyl-
chloroform Producer) 5-22
5.8 Analysis of Water, Soil, and Sediment Samples from Ethyl
Corporation (Methylchloroform Producer) 5-24
5.9 Descriptions of Sampling Locations at Ethyl Corporation,
Baton Rouge, Louisiana (November 18-19, 1976) 5-25
5.10 Ambient Air Measurements at PPG Industries (Methylchloro-
form Producer) 5-28
5.11 Analysis of Water, Soil, and Sediment Samples from PPG
Industries (Methylchloroform Producer 5-30
5.12 Descriptions of Sampling Locations at PPG Industries,
Lake Charles, Louisiana (December 6, 1976) 5-31
5.13 Ambient Air Measurements at Boeing/Auburn Plant
(Methylchloroform User) 5-34
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TABLES (Continued)
Number Page
5.14 Analysis of Water, Soil, and Sediment Samples from
Boeing/Auburn Plant (Methylchloroform User) 5-36
5.15 Descriptions of Sampling Locations at Boeing Company,
Auburn, Washington (January 10-12, 1977) 5-37
5.16 Ambient Air Measurements'at St. Francis National Forest
(Rural Background) 5-40
5.17 Analysis of Water, Soil, and Sediment Samples from the
St. Francis National Forest (Background Site) 5-41
5.18 Descriptions of Sampling Locations at Storm Creek Lake,
St. Francis National Forest, Helena, Arkansas
(November 30, 1976) 5-42
vi
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EXECUTIVE SUMMARY
The levels of methylchloroform in various environmental media were
determined at four production sites, one user site, and a background site.
The following sites were monitored:
Dow Chemical Co., U.S.A Freeport, Texas
PPG Industries, Inc Lake Charles, Louisiana
Ethyl Corporation Baton Rouge, Louisiana
Vulcan Materials Company .... Geismor, Louisiana
Boeing Company (User Site) . . . Seattle, Washington
St. Francis National Forest. . . Helena, Arkansas
(Background Site)
Approximately 2 days were devoted to monitoring ambient air levels
for methylchloroform and collecting water, soil, and sediment samples at
each site. The samples were returned to Battelle-Columbus Laboratories
for analyses. The ambient air level of methylchloroform was determined
on-site by direct injection of the ambient air into a gas chromatograph
followed by detection and quantification with an electron capture detector.
For the analyses of water samples, the methylchloroform was
sparged from the water and collected on a trap material using a commercial
liquid sample concentrator. The trapped organic material was then back-
flushed onto a gas chromatograph column which was connected to an electron
capture detector used to quantify the methylchloroform in the original
sample. A similar technique was used for the quantification of methyl-
chloroform in soil and sediment but the, apparatus was not of commercial
design. '
For each site, a map is presented with sampling points indicated.
The results from the analyses of the samples and detailed descriptions of
the sampling locations are given and are keyed to the site map.
Considerable variation was observed in the maximum downwind levels
of methylchloroform at various production plants. Concentrations of
methylchloroform in ambient air ranged from less than 0.3 ppb (limit of
detection) to 155 ppb.
Concentrations of methylchloroform in surface water in the vicinity
of the production and user plants was even more variable ranging from frac-
tions of a ppb to. over 16 ppm. Concentrations in soil and sediment ranged
from the limits of detection to 6.1 ppb.
VII
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1. INTRODUCTION
Methylchloroform (MC) is a chlorinated hydrocarbon which is produced
in major quantities in the U.S. and is used in a variety of solvent cleaning
operations. This compound has a relatively low boiling point; therefore,
its emission into the atmosphere probably represents one of the more signi-
ficant pathways to human exposure, To date, however, very little air
monitoring data have been generated to assess potential exposure hazards.
In particular, existing data are devoid of measurements in the environment
around manufacturing and user facilities where the highest concentrations
(and thus the highest exposures) might be expected.
This report describes the sampling rationale, the collection of
samples, that is, the sampling protocol, and the analytical methods used
to determine the environmental concentrations of methylchloroform at several
sites. The results are presented using maps in conjunction with tabulated
data and descriptions of the samples. A separate set of data is presented
for each site monitored, and these sets are grouped together under
production sites, user sites, and background site.
1-1
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2. SAMPLING RATIONALE
The objective of this sampling program was to determine levels of
methylchloroform in the environment. To do this, several important factors
were considered. Among these were the type of site (production, user, or
background); the source of the substance (discharge practices—how the
substance is released to the environment); the ecological compartments to
be sampled (air, water, soil, sediment, biota); the conditions at the
time of sampling (meteorological conditions, plant operation, geography,
interfering elements); and statistical requirements. These factors are
discussed further under specific environmental compartments in the following
section on the sampling protocol.
Sites were selected based on the fact that methylchloroform is a
volatile organic compound and is most likely to reach the environment
where it is produced and used. Table 2.1 lists the four major producers
of methylchloroform, a major user site, and a background site.
TABLE 2.1. SITES MONITORED FOR METHYLCHLOROFORM
Production Sites
Dow Chemical Company, U.S.A. . . Freeport, Texas
PPG Industries, Inc Lake Charles, Louisiana
Ethyl Corporation Baton Rouge, Louisiana
Vulcan Materials Company .... Geismor, Louisiana
User Site
Boeing Company Seattle, Washington
Background Site
St. Francis National Forest . . . Helena, Arkansas
The air sampling effort at each facility was conducted to obtain the
following information: (1) the concentration profile around the plant, (2)
•maximum concentration levels, (3) temporal variations in concentration, and
2-1
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(4) the variation in concentration as a function of distance downwind from
the plant.
Measurements were made in four quadrants surrounding the plant
location. The highest concentrations prevailed downwind from the plant
location. Therefore, the majority of the sampling and analysis effort was
then concentrated in the downwind direction to determine maximum concentra-
tions and temporal and spatial concentration variations.
The air monitoring equipment, a field electron-capture gas chromato-
graph, used for the methylchloroform analyses also permitted measurement of
trichloroethylene, carbon tetrachloride, and perchloroethylene. Therefore,
concentrations of these chlorinated hydrocarbons in ambient air were also
determined. f
In order to -detect concentration levels associated with process water
discharge, water samples were taken in the receiving stream at the plant out-
fall and upstream and downstream of the outfall. Samples of aquatic animal
tissue, usually fish, were also collected at locations upstream and downstream
of plant outfalls. In order to measure the amount present in a normal day's
discharge, which may not be accurately represented in grab samples, a 24-hour
composite of the effluent was obtained from plant personnel. Water samples
were also taken from the naturally occurring surface waters in the immediate
area.
In order to determine possible associated levels of methylchloroform
in sediments, samples were taken in close proximity to water sampling sites.
Soil, vegetation, and mammal tissue samples were also taken in the
four quadrants surrounding the plant location designated for air sampling.
Samples were taken as close to the exact site of the air sampling as possible.
The proximity of these samples should yield data suitable for associating
levels of methylchloroform in air with those found in soils.
2-2
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3. SAMPLING PROTOCOL
Air
Approximately 2 days were devoted to monitoring ambient air levels
of methylchloroform in the vicinity of each producer and user plant. On
the first day, measurements were made at several sites (usually 6 to 12)
surrounding the plant to obtain a profile of the ambient chlorinated hydro-
carbon concentrations and to identify any other emission sources in the
vicinity. At least two grab sample measurements were made at each site over
approximately a 1-hour period.
For subsequent monitoring, the sampling and analysis van was located
at downwind sites and measurements were made over a 20 to 24-hour period to
determine temporal and spatial variations and maximum concentration levels.
When necessary, the van was moved to attempt to remain centered in the plant
plume as well as possible. During this sampling period, grab samples of the
ambient air were analyzed at approximately 15 to 30-minute intervals, the
sampling rate being limited by the perchloroethylene retention time. Teflon-
bag grab samples integrated over a 15-minute collection period were taken at
upwind and crosswind sites during the period in which the van was used for
downwind measurements. During the 2-day monitoring period at each location,
approximately 50 ambient air measurements were performed.
At each site, two ambient air samples were collected on Tenax traps
for GC/MS confirmation of the field EC/GC measurement data. The samples
were collected over a 1 to 2-hour period coincident with the field measure-
ments .
Meteorological data were collected at each of the sites during the
sampling. If a U.S. Weather Bureau Station was located nearby, data were
obtained from their records. If not, a MRI Model 1071 portable weather
station was set up near the site to make meteorological measurements. The
parameters recorded on an hourly basis were wind speed and direction,
temperature, barometric pressure, relative humidity, precipitation, and
general weather conditions.
During the 2 days at each plant location, water, sediment, soil, and
biota samples were taken while personnel in the air sampling van monitored
the air for chlorinated hydrocarbons. In addition, a 24-hour composite
effluent sample was obtained from plant personnel and samples were prepared
for shipment to Battelle's Columbus Laboratories for analyses. Sampling of
each medium is described below. The analyses of these samples are described
3-1
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in subsequent sections, except for biota samples which were not analyzed
during the course of this program.
Water
Samples taken by hand were collected approximately 2 to 5 cm below
the surface of the water. Care was taken to avoid bubbling as the water
entered the bottle. Samples taken with the Teflon-lined vertical sampler
were usually taken as close to the surface as possible. In cases where the
discharge was expected to stratify in the receiving stream, different depths
in the water column were sampled at one location.
All water samples in the receiving stream were taken on the same day
in as short a time frame as possible. The request made to the plant personnel
for the 24-hour composite effluent sample was made for the day on which the
sampling was conducted.
Sample bottles and the sampler were rinsed thoroughly in the water
to be collected before the samples were taken. Samples were taken in clear
glass bottles sealed with septa and crimped metal caps. At the sites sampled
during the initial trip, 12 samples were taken at each sampling location.
During the remainder of the program the sample size was reduced to 6 per
location; 3 samples were held on wet ice and 3 at ambient temperature. At
all locations, 2 additional water samples were taken in 1-ounce amber bottles
and frozen on dry ice. Samples of the 24-hour composite and a tap-water
sample were similarly prepared.
Sediment
Whenever possible, sediment samples were taken in the same locations
at the same time as the water samples. Sediments were collected either by
a dredge or by hand. Upon collection, the sediment surface was placed in
the bottom of the sample jar. The volume collected approximated a 2-inch
soil core. Two samples were collected in glass jars at each site. Sample
jars were immediately wrapped in foil and placed in wet ice,.then frozen as
soon as possible, usually within 8 hours.
Soil
Six 2- inch soil cores were taken in each of the four quadrants around
the plant. The corer was washed and rinsed with distilled water and acetone
between each location and between each soil type at one location.
To dislodge the sample from the corer, the sampler was inverted over
a glass jar. (Soil surface was on the bottom of the jar.) Samples were
3-2
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immediately wrapped in foil, held on wet ice, and then frozen as soon as
possible.
After the initial sampling trip, the sample number was reduced to two
per location.
Vegetation
Six 1-ounce-volume vegetation samples were taken at each soil and
air sampling site. The vegetation sampled was directly associated with
(growing out of) the soil core taken. Samples were coded with subscripts to
preserve this correlation. The samples comprised live, whole plants except
in cases of large plants, where parts of several were clipped to provide a
more representative sample. Samples were collected in amber bottles, placed
on wet ice, then frozen as soon as possible. The sample size for any future
collections will be reduced to two per location.
Tissue
In the case of both fishes and mammals, specimens were held on wet
ice until dissection and/or sample preparation was completed. A minimum of
10 g of muscle tissue comprised each sample. Whenever possible, the tissue
was provided by three specimens. For fish, flank muscles were taken; for
mammals, muscle was stripped from each of the two hind legs. For both fish
and mammals, whole livers were removed. Liver and muscle tissues from the
same organisms were coded to preserve possible correlations. In the case of
small organisms whose dissection would not provide sufficient sample size,
whole bodies were taken.
Dissected tissues were placed in amber bottles; whole bodies were
placed in clear glass jars and wrapped in foil. All tissue samples were
frozen.
Sample size was dependent upon the availability of the organisms.
Six specimens of each species was considered maximum.
Number of Samples
A breakdown of the numbers of samples collected from eight locations
monitored November, 1976, through January, 1977, is given below:
3-3
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Sample Type Producer User Background
Air determinations 354 45 23
Water—clear glass 254 42 12
Water—amber glass 58 14 4
Sediment 38 4 2
Soil 112 8 2
Vegetation 112 8 2
Tissue 79 9 12
Methods were developed for the analyses of air, water, soil, and
sediment samples; and these are described in the following section. However,
no satisfactory method for the analyses of vegetation and tissue samples
could be developed with-in the time limits of this program. The vegetation
and tissue samples are stored in a frozen state for possible future analyses.
3-4
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4. ANALYTICAL METHODS
Determination of Methylchloroform in Ambient Air
A method for measurement of methylchloroform in air has been
developed and evaluated. The method involves direct injection of the
ambient air into a gas chromatograph (GC) followed by detection of the
emerging compounds with an electron-capture detecter (EC).
Equipment and Procedures—A schematic diagram of the system used
for on-site field measurements of methylchloroform is shown in Figure 4.1.
Ambient air is continuously drawn through a stainless steel line extending
about 4.2 m above the ground and passed through a 5 cc loop attached to a
Carle 6-port sampling valve. During sample injection, the carrier flow is
diverted through the sampling loop for 15 seconds and the 5 cc air sample
is swept onto the GC column. An electronic timer is used to control the
injection period and automatically start the integrator at the end of
sample injection. The integrator was used primarily to record retention
times. The chromatograms obtained from the stripchart recorder were used
to quantify the chlorinated hydrocarbon concentrations based on peak height.
Two EC/GC systems were used in the ambient air analysis program.
Measurements at Dow, Ethyl Corporation, Vulcan Materials, PPG, and
St. Francis National Forest (rural background) were performed with a
Varian 1200 EC/GC system. A system using the more sensitive Analog
Technology Corporation, Model 140A, EC detector was used for measurements
at the Boeing Company plant. The operating conditions and performance
characteristics of the two systems are given in Table 4.1.
Primary calibration of the EC/GC systems is discussed in the following
section. Secondary calibrations in the field were performed with a standard
TCE/nitrogen gas mixture. The sampling system was checked regularly for
contamination by injection of the same gas (zero oxygen nitrogen) which was
used as the carrier. Very slight, uniform residual background levels equi-
valent to about 0.1 ppbv of methylchloroform and perchloroethylene were
obtained with the more sensitive ATC system. Ambient air measurements made
with the system were corrected for these background considerations. Residual
backgrounds from trichloroethylene and carbon tetrachloride were not detected.
The gas chromatograph system was operated in Battelle's Columbus
Laboratories mobile sampling laboratory. The laboratory is equipped with a
7.6 kw gas-powered generator to provide power for sampling and analysis in
any location accessible via a roadway.
4-1
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3.18 mm stainless steel
sampling line ^4.2 m
above ground level
Carrier
Gas Inlet
QOQQQO
HP 3370A
Integrator
H
Recorder
Gas Chromatograph
Sampling Valve Operation
Inject Analyze
Position Position
Sampling
Valve
Carle No. 2018
Ballast
Tank
Diaphragm
Sampling
Pump
1. 5 ml sample loop
2. Air sample inlet
3. Sampling pump
4. 5 ml sample loop
5. Carrier inlet
6. Carrier to GC column
Figure 4.1. Schematic of EC/GC ambient air analysis system.
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TABLE 4.1. OPERATING CONDITIONS AND PERFORMANCE CHARACTERISTICS
OF THE EC/GC SYSTEMS USED FOR AMBIENT AIR MEASUREMENTS
OF CHLORINATED HYDROCARBONS
Varian 1200
ATC-140A
Column size/material
Column material
Column temperature
Carrier gas
Carrier flow
Detector
Detector temperature
Baseline adjustment
Read-out
Air sample volume
Injection time
Typical Retention
Times, sec
Chloroform
Methylchloroform
Carbon tetrachloride
Trichloroethylene
Perchloroethylene
Relative Detector Response
at 50 ppb, TCE =1.0
Methylchloroform
Carbon tetrachloride
Trichloroethylene
Perchloroethylene
Estimated Minimum
Detection Levels, ppbv
Methylchloroform
Carbon tetrachloride
Trichloroethylene
Perchloroethylene
3.18 mm x 305 cm, stain-
less steel
20% SP-2100/0.1% Carbo-
wax-1500 on 100-120 mesh
Supelcoport
50 C, isothermal
Matheson nitrogen,
oxygen free
^35 cc/min
EC, tritiated titanium
150 C
NA
Honeywell 193 recorder,
1.27 cm/min
5 cc
15 sec
326
424
498
633
1632
3.9
28.5
1.0
4.8
0.3
0.05
1.0
0.3
3.18 mm x 305 cm, stain-
less steel
20% SP-2100/0.1% Carbo-
wax-1500 on 100-120 mesh
Supelcoport
55 C, isothermal
Matheson nitrogen,
oxygen free
37.5 cc/min
EC, tritiated scandium
240 C
275
Honeywell 193 recorder,
1.27 cm/min
5 cc
15 sec
240
308
365
462
1124
1.9
8.6
1.0
2.0
0.02
<0.01
0.03
0.02
4-3
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In addition to direct injection of ambient air, grab samples were
also collected in Teflon bags for GC analysis. A stainless steel diaphragm
pump powered by a portable gas-powered generator was used for sample
collection. Analysis was performed with the Varian or ATC EC/GC systems
by attaching the Teflon bag to the inlet of the sampling loop on the Carle
valve.
Gas Chromatograph Calibration—The Varian 1200 EC/GC system was
calibrated for measurement of methylchloroform, trichloroethylene, carbon
tetrachloride, and perchloroethylene over the concentration range of 1 to
1000 ppbv. The ATC 140A system was calibrated for the four compounds over
the concentration range of about 0.1 to 100 ppbv. The calibrations were
performed by concurrently injecting the four compounds into the Battelle
smog chamber to produce initial concentrations of either 100 or 1000 ppbv.
Successive dilutions of' the chamber air were made to produce a series lower,
known concentrations to complete the calibration curve. The dilution factor
for each dilution step was determined independently by following the decrease
in concentration of methane injected into the chamber with the chlorinated
hydrocarbons. A Beckman Model 109 hydrocarbon analyzer was used for the
methane measurements.
In calibrating the Varian GC system, a Matheson 1200 ppbv TCE
standard was compared with the chamber concentration of TCE to verify that
an initial concentration of 1000 ppbv was obtained.
The calibration curves showing detector response for the Varian and
ATC systems are shown in Figures 4.2 and 4.3, respectively. Each point on
the calibration curves is the average of two determinations. Agreement
between all duplicate determinations was within 5 percent. Both systems
exhibit excellent linearity over the concentration range encountered in the
field monitoring program.
Field calibrations were performed to verify detector response and
retention times using a Matheson gas mixture of 1200 ppbv TCE in nitrogen.
Calibrations were performed before, after, and at 6 to 8-hour intervals
during the sampling program at each plant.
Determination of Methylchloroform in Water
The analytical method selected for development is based on sparging
the methylchloroform from the water with an inert gas. These compounds are
collected on a trap material and then desorbed onto a gas chromatography
column for analysis.
If an inert gas is bubbled through water containing organic compounds
which exhibit a low solubility in water, the compounds will be quantitatively
partitioned into the gas phase. The enriched gas phase is then passed
through a trap that retains the organics but allows the purge gas and most
of the water to pass through. A large concentration factor of the volatile
4-4
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100,000
10,000
c
o
•H
J-l
cd
c
a)
4J
4J
CO
a
o
•H
CO
•H
S
P
4-1
CO
6
i,ooo
Concentration vs. Peak Height
Peak Height in Chart Divisions
Chart Paper - 193-8"
Chart Speed - 2 min/inch
— 1— Carbon
Tetrachloride
Perchloroethylene
Methylchloroform
Trichloroethylene
100
10 100
Concentration, ppbv
1,000
10,000
Figure 4.2.
Calibration curves for chlorinated
hydrocarbons—Varian 1200/EC Detector
(Reference: Matheson 1.2 ppm TCE - 36.4
.divisions - Attenuation-100) .
4-5
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100,000
10,000
1,000
c
o
c
-------
organics out of the aqueous phase is accomplished. The trapped organics are
then back-flushed onto a gas chromatography column or into a mass spectro-
meter for analysis.
Instrumentation—A Tekmar Liquid Sample Concentrator, Model LSC-1,
was purchased and integrated with a Packard 1700 Series gas chromatography
instrument, as shown in Figure 4.4, which shows the purge gas entering the
flow meter, the purge-gas-rate control valve, and passing through the water
sample sparging tube. The partitioned organics enter the gas phase and are
deposited on the collection trap after passing through one path of the 6-way
gas control valve. During the water purging cycle, the gas-chromatography
carrier gas enters the 6-way control valve at the desorb gas "in" location
and passes out of the valve onto the gas chromatography column.
The desorb mode is shown in the lower portion of Figure 4.4, with
the 6-way control valve switched so the gas chromatography carrier gas back-
flushes the organics onto the gas chromatography column at the same time the
trap is heated. The water sample purge gas valve is off during this period
and another water sample can be sparged during the analysis of the first
sample.
Initial evaluation of this system was not satisfactory because of
broadening of the chromatographic peaks. The LSC-1 was modified to replace
the resistance heater wrapped around the trap column with direct resistance
heating of the stainless steel trap column. A step-down transformer, coupled
with a Variac set at 50, heated the trap to 150 C in 8 seconds compared with
the 3 minutes required for the original heater. Other modifications included
replacing some Teflon lines with stainless steel and heating the transfer
line from the LSC-1 to the gas-chromatography instrument.
Column Selection for the Gas Chromatograph—Several column materials
were evaluated for the separation of chlorinated organic compounds. The
material selected was 20 percent SP-2100 with 0.1 percent Carbowax-1500 on
100 to 120 mesh Supelcoport. Figure 4.5 shows a chromatogram from the vendor
literature for 11 chlorinated solvents. The most likely interference with
methylchloroform (1,1,1-trichloroethane), peak 5, is 1,2-dichloroethane,
peak 4.
The SP-2100 is methyl silicone. The support material is diatomaceous
earth which has been acid washed and silane treated. The addition of the 0.1
percent Carbowax is essential for high-quality chromatograms. A standard
mixture containing methylchloroform, chloroform, carbon tetrachloride,
trichloroethylene, and 1,2-dichloroethane showed the latter compound to be
extremely insensitive to the electron-capture detector.
Quantitative Analysis Using the Flame lonization Detector—The initial
quantitative evaluation of this system was done in the 50 to 500-ppb range
using a flame ionization'detector. A 3-component standard containing methyl-
chloroform, trichloroethylene, and perchloroethylene was prepared in water
tha.t had been demineralized and double distilled. A 500 ppb volume per
Volume in water at ambient temperature and a 50 ppb standard were prepared.
4-7
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Deaorb Gas
Out
Desorb Gas
In
HOPfe
Trap Column 25 C
Purge Gas
Irt
Decorb Gas + Sample•
Out
Deaorb Gas
Zn
BEStiRB. MODE
trap Cdlumri 125°C
Sampler
Flow-
iheter
Purge Gas
in
Figure 4*4. Schematic of a liquid sample concentrator.
4-8
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1. Methylene chloride
2. 1,1-dichloroethane
3. Chloroform
4. 1,2-dichloroethane
5. 1,1,1-trichloroethane
6. Carbon tetrachloride
7 - Trichloroethylene
8. 1,1,2-trichloroethane
9. Perchloroethylene
10. 1,1,1,2-tetrachloroethane
11. 1,1,2,2-tetrachloroethane
10
Figure 4.5. Chromatogram of chlorinated solvents,
4-9
-------
Instrumental conditions used for analysis of this standard were as
follows:
Liquid Sample Concentrator
Sample size - 5 cc standard water solution
Purge gas rate - nitrogen at 40 cc/min for 10 min
Degas temperature - 150 C reached in 10 sec
Trap material - Tenax plus silica gel
Gas Chromatography Conditions
Column - 10 ft x 1/8-in stainless steel packed
with 20 percent SP 2100/0.1% Carbowax
1500 on 100 to 120-mesh Supelcoport
Temperatures - Column - 55 C
Detector - 150 C
Injection - 140 C
Gas flows - Nitrogen carrier - 30 ml/min
Hydrogen - 30 ml/min
Air - 300 ml/min
Electrometer - 1 x 10"10 amp, 500 volts.
The recording system was a HP 3380A integrator which prints retention time
directly above each peak, and then records the total counts for each peak,
based on the total area under the peak. The area percentage for each peak
recorded in the right-hand column is not significant in this work because
it is based on percentage of total area and we do not know the sensitivity
factor or the identification of other peaks appearing in the chromatograms.
A reproduction of t"he actual chromatograms is shown in Figures 4.6
and 4.7. Both chromatograms show some impurities which are caused by the
dilution water and/or impurities in the compounds added to the water. The
methylchloroform has a retention time of 3.44 to 3.36 minutes and the tri-
chloroethylene 4.99 and 5.01 minutes for Figures 4.6 and 4.7, respectively.
The integrator counts representing the area under these peaks were as follows;
Compound 500 ppb 50 ppb
Methylchloroform 624,861 62,092
Trichloroethylene 1,121,598 122,636
The linearity from 50 to 500 ppb using the flame ionization detector is
excellent for these two compounds. The degas temperature for the 50 ppb
chromatogram did not reach 150 C and this probably explains why the per-
chloroethylene was not linear. The x values directly above the retention-
time values are the attenuation factors used to keep the peaks on scale.
Since both compounds were attenuated times 8 and a 5 ml sample was used, it
would appear that a sensitivity of about 500 ppt could be reached with a
20-ml sample using the FID detector, provided purer water is used for the
standards. The 50 ppb methylchloroform and trichloroethylene represents
4-10
-------
X64
12. 27
XI6
PCE
'STOP
RT
2. 63
3. 44
'4. 99'
8. 52
12. 27
flREfl 5i
TYPE
T
TM
RRER
137973
_ 624861.
ii21598
82634
893973
4. 824
21. 85__
'39. 21 _
2. "867
31. 25
HP 3330R
DLV 1.
MV/M 1. 08
STOP 38
RTTN 16
REJECT OFF
Figure 4.6.
Chromatogram showing 500 ppb each of
methylchloroform (3.44 minutes),
trichloroethylene (4.99 minutes), and
perchloroethylene (12.27 minutes) using
FID detector.
4-11
-------
INJ
3. 26 X8 MC
5. 01
X2
ft fifi
12. 41
X2 PCE
•STOP
RRER '/.
1.
1.
2.
3.
5.
8
12.
RT
35
65
65
36
01
66
41
TYPE
M
M
fiRER
181478
139296
146339
62092
122636
966^5
14751
23.
18.
1-9
8.
16.
12 .
1.
77
26
18
134
©"g "••-••" '
66
932
HP 3380R
DLV 1.
MV/M 3. 0Q
STOP 30
RTTN
REJECT OFF
Figure 4.7.
Chromatogram showing 50 ppb each of
methylchloroform (3.36 minutes),
trichloroethylene (5.01) minutes), and
perchlo-roethylene (12.41 minutes) using
FID detector.
4-12
-------
50 x 10~9 ml/ml of water or 68 and 73 ng/ml of water, respectively. Figure
4.8 shows the FID calibration curve.
Quantitative Analysis Using the Electron Capture Detector—The
instrumental settings for the liquid-sample concentrator and the gas
chromatography were the same as described above except for the detector
power source and the air and hydrogen required for the operation of the
flame. The electron-capture-detector electrometer settings were 1 x 10~10 i
and 25 V.
Preparation of standards required special treatment of the dilution
water. All distilled and demineralized water supplies checked contained
methylchloroform and trichloroethylene, including a.demineralized and
double-distilled supply. Untreated well water was lowest in these com-
pounds but had a high iron content; therefore, the well water was not used
for dilutions. The integrator counts representing total impurities in the
various waters checked are shown in Table 4.2. The Ohio State University
demineralized and double-distilled water was sparged with nitrogen while
being boiled for 3 hours, which reduced the methylchloroform and trichloro-
ethylene to undetectable amounts; therefore, this water was used to prepare
standards.
TABLE 4.2. VOLATILE IMPURITIES IN WATERS
Source of Water Impurity Counts
City Products Corp., storeroom supply 10,160,000
Tap water, City of Columbus, Ohio 8,910,000
Biology Department, glass still 5,792,000
Deionized water, analytical section 810,000
Ohio State University, double distilled 317,000
Ohio State University, sparged with nitrogen 217,000
Olentangy River, 5th Ave. and King Ave. north of dam 211,000
Ohio State University, boiled and sparged with N£ 15,825
Well water, untreated, Fairfield County 3,203a
a
All values were determined by concentrating 5 ml of water except
this well water; 20 ml was concentrated with a total impurity count
of 12,812; therefore, one-fourth this amount was reported above.
Standards containing methylchloroform and trichloroethylene at a
concentration of 500, 100, and 50 ppt were prepared in the special dilution
water using the electron-cap.ture detector. The calibration curves for these
4-13
-------
100 200 300 400
Concentration, ppb
500
Figure 4.8. Calibration curves for the determina-
tion of trichloroethylene and methyl-
chloroform using the FID detector.
4-14
-------
runs are shown in Figure 4.9. The sensitivity for methylchloroform is much
greater than that for trichloroethylene, which is reversed with the flame
ionization detector. The 500 and 100 ppt standards were analyzed by sparg-
ing 5 ml of the standard, and the 50 ppt standard was analyzed using 20 ml.
The 50 ppt concentration is equivalent to 67.5 pg/ml of water for methyl-
chloroform and 73.3 pg/ml for trichloroethylene.
These calibration curves were not used in the analysis of samples
since the HP 3380A integrator is a dedicated computer which retains data
input on a standard sample and the amount of a compound per area can be
listed for each standard peak in the chromatogram. If the amount per area
shows a sudden change under the same operating conditions, this would
indicate operation beyond the linearity range of the detector, a poor
standard or that some other instrument trouble exists. A sample run is
automatically computed from the standardization data retained by the computer.
A multiplication factor to adjust for sample size or amount of dilution can
be added to the stored data at the time each sample is injected. The
electron-capture detector was used for all sample analyses with a maximum
standard concentration of 50 ppb. If the first run on a sample indicated
that the concentration was much higher than 50 ppb, the sample was diluted
to bring it into range or minor adjustment was made by reducing the quantity
of sample. A 5-ppb standard was generally used for low concentrations and
up to 20 ml of sample.
The initial objective was to obtain chlorinated hydrocarbons through
perchloroethylene without use of our program temperature facilities; however,
as shown in Figure 4.6, the resolution would not be adequate to elute per-
chloroethylene in 13 minutes with methylchloroform, carbon tetrachloride, and
other possible impurities in industrial waters. The flow and temperature
were reduced slightly to provide a retention time of about 13 minutes for
trichloroethylene as shown in Figure 4.10. The relative concentrations of
carbon tetrachloride in the samples were not as high as shown in Figure 4.10;
therefore, many samples were analyzed with the trichloroethylene retention
time set at 10 minutes.
Preparation of Standards—Standards are prepared from the specially
prepared water described earlier. A 1-liter volumetric flask is filled with
the special water and a hypodermic syringe is used to inject a known quantity
of the compounds. The flasks are placed on a shaker for 16 hours (overnight)
and this forms the base standards which are diluted to lower concentrations.
Base standards containing 5 Vg/H of water (5 ppm) and 2 yg/£ of water have
been rediluted and analyzed on the electron-capture detector. Good agreement
was obtained that would indicate that the measurements of these small
quantities were reproducible and also that these quantities were completely
soluble in 1 liter of water. The base standards and diluted standards were
protected from light at all times. The base standards were used for 2 to 3
weeks before any concentration deterioration was noted, but the diluted
standards were made fresh daily.
Precision and Accuracy—The precision of the method was tested using
10 determinations of a standard containing 50 ppb by volume of both
4-15
-------
24
20
16
o
o
o
-*-1' i o
cd 12
)-i
oc
cu
0
100
200 300 400
Concentration, ppt
500
Figure 4.9,
Calibration curves for the determi-
nation of trichloroethylene and
methyicnloroform using the electron
capture detector.
4-16
-------
INJ
2. 21
9 52
Retention Time,
minutes
6.02
7.97
9.52
13.21
Compounds
Chloroform
Methylchloroform
Carbon tetrachloride
Trichloroethylene
Figure 4.10.
Chromatogram of several chlorinated hydrocarbons
using the electron-capture detector after
completion of development work.
4-17
-------
methylchloroform and trichloroethylene. The following precision data were
obtained:
Methylchloroform Trichloroethylene
Average 49.75 50.29
Sigma (a) 1.65 1.68
Coefficient of 3.3 3.4
variation
Five of the above analyses were made on different standards and the other
five on the same standard. Two different operators were involved.
Since no primary standards exist for this type work or no cross-
laboratory analyses among several laboratories have been performed to our
knowledge, the absolute accuracy is not known.
Water Sample Data to be Presented—In addition to the concentration
of trichloroethylene and methylchloroform in each sample, the following
information is given:
(1) Date sampled
(2) Data analyzed
(3) Amount of sediment in the sample
(4) Sparging characteristics
(5) Rough quantitative values fbr chloroform
and carbon tetrachloride
(6) Comments which indicate which samples
are composites, tap waters, or required
unusually high sample dilutions, and
other miscellaneous remarks.
The sediment in the samples was classified as C=clear, IXLight,
M=medium, and H=heavy. The sediment concentrations were judged before
shaking the samples prior to analysis. If no particles had settled on
the bottom, they were classified as clear; any observable particles on
the bottom were noted as light; if the bottom was nearly covered, it was
classified as medium; and if the bottom was entirely covered, this was
considered heavy. The samples classified as heavy contained only a very
thin coating on the bottom. Some of these sediments appeared to be a
gelatin-like substance.
The column headed "sparging foam" indicates the degree of foam
generated while sparging the compounds from the water samples. These are
designated as ND=none detected, L=light, M=medium, and H=heavy. Blank
areas indicate that we made no observation. None of the samples produced
4-18
-------
sufficient foam to cause trouble with carry-over to the collection trap;
however, many of the samples were diluted before analysis, which would
reduce foaming.
The results reported for chloroform and carbon tetrachloride were
obtained by analyzing a standard mixture containing these two compounds
plus the methylchloroform and trichloroethylene. Sensitivity ratios were
calculated based on trichloroethylene as 1 and this permitted a rough
quantitative estimation of these compounds.
Determination of Methylchloroform in Soil and Sediment
Methylchloroform is expected to be present in soil and sediment
samples at levels of the order of 10" * to 103 ppb by weight. The analysis
technique must, therefore, be capable of detecting 10"1 to 10~2 ng of each
substance in reasonably sized samples of 0.1 to 1.0 g. Furthermore, a high
level of specificity is required to avoid interferences from the many other
organic substances commonly present in soil and sediment samples.
Electron-capture gas chromatography (EC/GC) is ideally suited to
detection of these volatile chlorinated hydrocarbons because of its very
specific response to electrophilic substances at the required concentration
levels. However, before EC/GC can be applied to such samples, the tri-
chloroethylene and methylchloroform must be extracted to a phase suitable
for injection into the chromatograph. Either gaseous or liquid samples can
be handled by the chromatograph. The three methods used for these types of
samples therefore involve a preliminary conversion of the methylchloroform
sorbates to either gaseous or solution forms.
Extraction Methods—Basically three different methods for methyl-
chloroform extraction have been considered:
(1) Thermal desorption—A sample of soil is heated while
being purged by a stream of nitrogen. The eluted
methylchloroform is trapped on Tenax or other suit-
able sorbents and then injected into the chromato-
graph by flash heating of the trap.
(2) Liquid extraction—The methylchloroform is solvent
extracted using acetone and/or hexane. The resulting
solution can then be injected directly into the
chromatograph.
(3) Aqueous sparging—Inasmuch as methylchloroform has
low solubility in water, this substance can be used
to disperse soil and sediment samples to render them
susceptible to purging by nitrogen. The effluent
methylchloroform is then handled much the same as
with the thermal desorption method.
4-19
-------
Method (1) has been shown to be useful for analysis of trichloro-
ethylene and certain other chlorinated hydrocarbons in dry or only slightly
wet samples. However, the excessive amounts of water likely to be present
with sediment samples render this approach difficult at best. Furthermore,
it has been shown that certain chlorinated hydrocarbons, such as chloroform
and methylchloroform, are not recovered efficiently by this method. Indeed,
results with some model soils suggest that methylchloroform is chemisorbed
and can be recovered only as vinylidene chloride by this method.
Method (2) is efficient and satisfactory providing care is taken to
minimize sample losses during the extraction and subsequent concentration
steps of the procedure. (If aliquots of solution are analyzed, the
sensitivity of the method is reduced.)
Method (3) also suffers from poor recovery of methylchloroform that
is chemisorbed in the soil surface. However, this procedure more closely
imitates the probable mechanism for mobilization of methylchloroform and
trichloroethylene in the environment. Furthermore, Method (3) is an "on-
line" procedure with little or no chance for either losses or gains of
methylchloroform and trichloroethylene due to exposure of the sample to
laboratory air. The method is equally applicable to wet and dry samples.
The results of its application reflect the availability of methylchloroform
and trichloroethylene to the environment rather than total methylchloroform
and trichloroethylene exposure.
Apparatus—A schematic representation of the apparatus used for
sparging of soil samples is shown in Figure 4.11. In use, presparged water
(3 to 4 cc) is loaded into the fritted glass vessel, the soil sample injectdr
is mounted, and the sparger is attached to the sample trap valve. The sample
side of the system is then flushed with zero nitrogen until a suitable blank
reading for methylchloroform and trichloroethylene is obtained. Usually,
this is possible within about 10 minutes or less; but flushing is continued
for approximately the 30 minutes required for the blank analysis. The soil
sample is then injected into the water and the effluent trichloroethylene
and methylchloroform are trapped on Tenax maintained at room temperature.
During sparging of the soil-water mixture, the sample is agitated by
immersion in an ultrasonic bath. This serves to rapidly disperse the soil
and facilitate sparging. Sparging periods of 10 minutes at 30 to 40 cc/min
are sufficient. Following the sparging period, the by-pass around the
sparger is opened to permit flushing of the water vapor from the Tenax trap.
A flushing period of 5 to 6 minutes is sufficient to remove the water vapor
without removing trichloroethylene or methylchloroform from the Tenax. The
trap valve is then switched to permit flushing by the zero-nitrogen GC
carrier gas and the trap is heated rapidly (at ^500 C/min) to 190 C to
inject the methylchloroform and trichloroethylene into the chromatograph.
The soil or sediment injector is constructed as a syringe-like
device with its open end capped by a tight-fitting Teflon plug. The injector
is weighed and then used to core the analysis sample directly from the bulk
as-received sample. Reweighing and capping of the injector are done rapidly
to minimize contact with the laboratory air. The injector is then kept closed
4-20
-------
.p-
fo
I-1
By-Pass
Heated Section
Zero
Fritted Sparger
with Soil Injector
EC/GC
Tenax Trap
Ultrasonic Bath
Standard
THE
i
Zero N2
Carrier
Figure 4.11. Schematic of soil and sediment analysis apparatus,
-------
until injection of the soil into the sparger, at which time both the soil
and Teflon plug are manually ejected.
The chromatograph is a Varian 1200 equipped with a Ti(H3) detector.
The column is a 1/8-inch by 10-foot stainless steel column packed with
SP-2100 (GP 20 percent SP-2100/1 percent Carbowax-1500 on 100-120 mesh
Supelcoport). Output signals are quantified using an Infotronics Model CRS
204 integrator coupled to a TTY output.
Standardization is accomplished using a precalibrated gas standard
of TCE in nitrogen. Approximately 4-ng samples of trichloroethylene are
usually used for standardization. Such samples yield peak areas on the
order of lO4 uv/sec, and peaks on the order of 102 to 103 yv/sec can be
separated from the inherent background noise. Comparative calibrations with
methylchlorofonn and trichloroethylene indicate a relative response of 3.36
for MC/TCE at equal concentrations. The response curve of the detector is
not perfectly linear but rather varies with c1'05 in the concentration range
of interest. A sample chroiflatogram showing response obtained with one
sediment sample is shown in Figure 4.12.
Quality of Results—There are several points thajt must be recognized
in discussion of the significance of the results of trichloroethylene and
methylchloroform analyses on soil and sediment samples. Ideally, standardi-
zation should be performed using well-characterized standards of trichloro-
ethylene and methylchloroform on substrates that closely simulate those of
subject samples, and these standards should be traceable to primary standards
established by independently certified means. Such standards are not
available for methylchloroform and trichloroethylene in soils and sediments,
nor is it possible to reliably prepare such standards because of the inherent
instability of this type of specimen. Because of the general stability of
trichloroethylene in a nonoxidizing atmosphere, we have chosen to use
trichloroethylene in nitrogen as the reference standard for the current work.
Analysis of the standard was made by the manufacturer and has been cross-
checked with samples of the same concentration prepared by injection of liquid
samples into the Battelle smog chamber. The standard being used appears to
be accurate to within a few percent.
A second infringement on the quality of the results is related to the
basic heterogeneity of the samples. Any soil sample is likely to be a
composite of various organic and inorganic structures, e.g., sand particles,
clays, organic residues, plant fragments, etc. Such local heterogeneity is
likely to be reflected in appreciable local gradients in the distribution of
methylchloroform and trichloroethylene. These local-gradient tendencies are
likely to be superimposed on the natural vertical and horizontal gradients
that are caused by temporal and spatial variation in the flux of methyl-
chloroform or trichloroethylene to a given sample area. Because of the
limited size of the analytical sample, the results must therefore be consi-' •-
dered as point analyses rather than as representative analyses. This situa-
tion is magnified further with the sediment samples. With sediments, the
fraction of the sample that is present as a liquid phase is much larger than-
with the soil samples. Results can vary considerably thereby reflecting the
partitioning of methylchloroform and trichloroethylene between the solid and
liquid phases.
4-22
-------
Materials Belong To:
GJ'i'T Library
401 M Strrei, S\V (TS-7S3)
Washiiijton, DC -JO460
Sample
(atten. = 50)
Blank (atten. = 10)
Figure 4.12. Sample chromatogram for sediment.
4-23
-------
5. MONITORING DATA
The sampling rationale, sampling protocol, and analytical methods
have been described. The results are presented as a series of maps and
tables which describe the locations, the nature of the samples, and the
concentrations of methylchloroform in the samples. A separate set of data
is presented for each site.
Production Sites Monitored
For each methylchloroform production site a map is presented with
sampling points indicated (Figures 5.1 to 5.4). The results from the
analysis of the samples and detailed descriptions of the sampling locations
are presented (Tables 5.1 to 5.12).
User Site Monitored
The data obtained at a methylchloroform user site are presented
in Figure 5.5 and Tables 5.13 to 5.15.
Background Site Monitored
The data obtained at St. Francis National Forest near Helena,
Arkansas, are presented in Tables 5.16 to 5.18. This site represents a
rural background site "and is removed from known sources of methylchloroform
and major industrial activity (see Figure 5.6).
Discussion of Results
The ambient air concentration profiles around all facilities
monitored are characterized by increased concentrations of methylchloroform
in the downwind direction from the source. Upwind measurements, which
showed significantly lower methylchloroform concentrations, do not give any
evidence of other methylchloroform sources which would contribute to the
observed downwind levels.
5-1
-------
Considerable variation was observed in the maximum downwind levels
of methylchloroform at the various production plants. Maximum concentra-
tions ranged from 12 to 155 ppbv at the methylchloroform production
facilities. The variations in the observed maximum concentrations among
plants may be due to differences in (1) production processes, (2) ejnission
control equipment, (3) meteorological conditions, and (4) distance from
plant. Higher production capacity apparently does not necessarily imply
higher emissions since the maximum concentrations observed at the larger
plants were lower than those observed at the smaller operations.
Very large temporal variations were generally observed at a given
site downwind from the methylchloroform production facilities. Changes in
meteorological conditions (wind speed and direction) and/or variations in
the process emissions may account for this phenomenon. Less temporal
variation was noted in the ambient air concentrations downwind from the
methylchloroform solvent cleaning facility. Due to the nature of solvent
cleaning operations, more uniform emission rates might be expected. In
addition, meterological conditions (essentially no wind) during much of
the sampling period reduced dispersion of the plume.
Duplicate analyses on some of the soil samples suggest that sample
heterogeneity may contribute 30 to 50 percent deviation in the reported
values for individual analyses. It is interesting to .note that both soil
and sediment samples from the background site display methylchloroform
content equal to or greater than many of the plant-site samples. However,
if it is assumed that a true average background level ,can be obtained 'by
averaging all results equal to or less than the background-site levels,
there still remains a number of samples containing significantly more
methylchloroform than the background.
The highest levels of methylchloroform are generally associated
with sediment samples. Chromatograms of these high-roo:ncentration-.ley,el
samples also show the presence of appreciable quantities
-------
However, the trichloroethylene content of the water was nearly an
order of magnitude smaller in the water than in the bulk sample. While
these experiments are not conclusive, they suggest that the trichloroethylene
was truly associated with the solid phase and that the observed methylchloro-
form was primarily associated with the liquid phase. In other words, if
there is any methylchloroform absorbed on the solid phase of these samples,
it is present in a form that is not readily mobilized.
5-3
-------
MONITORING DATA
PRODUCTION SITE 1
5-4
-------
Oi
Ul
Residential
«r 0 Emission Source
Highway
Railroad
Plant Proper
Industrial
Marsh
Air Site
• Soil Site
A Water Site
* Sediment Site
Mile
0 .51
Kilometer
Figure 5.1. Sampling locations at Dow Chemical Plant A, Freeport,
Texas—methylchloroform production site.
-------
TABLE 5.1 AMBIENT AIR MEASUREMENTS AT DOW CHEMICAL PLANT A (METHYLCHLOROFORM PRODUCER)
Ul
Distance
from
Site Plant,
No. km
1A 2.6
2A 1.9
3A 3.2
4A 2.1
5A 0.8
6A 1.9
7A 2.6
'
8A 2.6
10A 3*2
Direction
from
Plant,
degrees3
300
285
265
225
120
010
080
260
350
Meteorological Observations0
Date
1976. Time
11/8 0940
1020
11/8 1055
1110
11/9 1536
11/10 1346
11/8 1140
1155
11/8 1330
1345
11/8 1420
1433
11/9 1614
11/10 1420
11/8 1610
1625
11/8 1523
1535
11/9 1450
1746
11/10 1309
11/8 1712
1738
1745
1758
1812
1825
11/9 0924
0940
1015
1030
Concentration in
Ambient Air, ppbv^
MG
2.3
£0.3
£0.3
1.1
0.7
0.5
1.2
£0.3
£(K 3
£0.3
£0.3
£0.3
0.6
0.7
£0.3
£0.3
£0.3
£0.3
1.1
0.8
0.7
£0.3
0.8
£0.3
2.2
0.8
0.4
£0.3
£0.3
£0.3
^0.3
CClfy
0.30
0.25
1.4
2.1
0.15
0.15
0.60
1.1
0.15
0.15
0.15
0.15
0.15
0.14
0.14
0.15
0.15
0.16
0.14
0.14
0.13
0.19
0.24
0.18
0.58
0.38
0.22
0.22
0.17
0.14
0.54
TGE
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
PCE
NDd
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Wind
Speed,
m/s
5-10
5-10
5-9
5-9
4-7
6-7
5-9
5-9
4-7
4-7
4-7
4-7
4-7
6-7
3-7
3-7
4-7
4-7
5-8
2-4
5
3-9
3-9
3-9
4-5
4-5
4-5
2-4
2-4
2-4
2-4
Wind
Direction,
degreesa
080
080
080
080
180
155
080
080
080
080
080
080
-180
155
065
065
080
080
185
165
155
075
075
075
070
070
070
150
150
150
150
Temper-
ature, RH, Barometer,
C % mm Hg
17
17
18
18
24
24
19
19
21
21
21
21
24
24
21
21
21
21
24
23
23
20
20
20
19
19
19
21
21
21
21
NDd
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
772
772
772
772
764
761
771
771
770
770
769
769
764
761
769
769
769
769
764
763
761
769
769
769
769
769 *
769
767
767
767
767
-------
TABLE 5.1. (Continued)
Distance Direction
from from
Site Plant, Plant, Date
No. km degrees3 1976 Time
10A 3.2 350 11/9 1900
(Cont) 1915
2200
11/10 1430
1445
1500
12A 2.6 005 11/9 1155
1210
1220
1235
1250
1305
1320
1335
1350
1405
1420
1450
1505
1630
1645
1755
2300
2315
2330
2345
2400
11/10 0020
0035
0050
0105
Meteorological Observations0
Concentration in
Ambient Air, ppbv^
MC
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
7.6
6.2
5.8
4.2
9.4
0.9
4.2
1.5
—
1.4
2.2
2.4
£0.3
£0.3
0.7
£0.3
7.2
6.5
9.8
3.0
9.8
2.2
11.5
6.5
7.6
CC14
0.25
0.22
0.22
—
0.15
0.15
0.27
0.48
0.27
0.21
0.58
0.16
0.50
0.18
0.48
0.23
0.28
0.31
0.26
0.16
0.27
0.15
0.94
2.4
3.3
1.2
3.8
0.48
1.8
1.3
3.4
TCE
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
*1
PCE
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Wind
Speed,
m/s
3-5
3-5
3-4
6
6
6
4-6
4-6
4-6
3-6
3-6
3-6
3-6
4-7
4-7
4-7
4-7
5-8
5-8
3-5
3-5
2-4
2-3
2-3
2-3
2-3
2-3
2-3
1-2
1-2
1-2
Wind
Direction,
degrees3
165
165
170
150
150
160
180
180
180
185
185
185
185
180
180
180
180
185
185
175
175
165
170
170
170
185
185
185
170
170
170
Temper-
ature, RH, Barometer,
C % mm Hg
22
22
21
23
23
23
23
23
23
24
24
24
24
24
24
24
24
24
24
24
24
23
21
21
21
21
21
21
21
21
21
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
763
763
763
761
761
761
765
765
765
764
764
764
764
764
764
764
764
764
764
763
763
763
763
763
763
763
763
763
763
763
763
-------
TABLE 5.1. (Continued)
00
Distance
from
Site Plant,
No. km
12A 2.6
13A 5.1
14A 7.8
Direction
from
Plant, Date
degrees3 1976 Time
005 11/10 0120
0135
0150
0210
0225
0245
0315
0345
0415
0445
0515
0545
0615
0645
0715
0745
0815
0845
0915
0945
1015
1045
1115
1145
1215
1245
34.5 11/10 1630
1645
355 11/10 1700
1715
Meteorological Observations0
Concentration in
Ambient Air, ppbv^
MC
1.1
£0.3
£0.3
£0.3
£0.3
1.4
£0.3
2.2
2.6
1.1
1.8
0.7
£0.3
£0 . 3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
0.5
£0.3
£0.3
CC14
1.2
0.33
0.58
0.84
0.18
0.84
0.14
0.14
0.14
0.10
0.14
0.14
0.10
0.14
0.14
0.18
0.14
0.14
0.14
0.14
0.11
0.10
0.13
0.15
TCE
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
PCE
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Wind
Speed,
m/s
1-2
2
2
2
2
2
2
2
2
2-3
2-3
2
2
2-3
2-3
2-3
2-3
4-5
4-5
2-5
2-5
4-6
4-6
4
4
4
2-5
2-5
2-5
2-5
Wind
Direction,
degrees3
170
160
160
160
160
155
155
• 170
170
155
155
140
140
120
120
110
110
155
155
155
155
165
165
165
165
165
155
155
155
155
Temper-
ature, RH,
C %
21
21
21
21
21
21
21
21
21
21
21
21
21
22
22
23
23
23
23
23
22
22
22
22
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Barometer,
mm Hg
763
763
763
763
763
763
763 '
762
762
762
762
762
762
763
763
763
763
763
762
762
761
761
761
761
-------
FOOTNOTES FOR TABLE 5.1
Ui
VO
- 360°.
•L q
To convert to )ig/m at 25 C multiply ppbv by
MC 5.46
CC14 — 6.29
TCE — 5.37.
Q
General weather conditions:
11/18/76 Clear, sunny, no precipitation
11/9/76 Clear, sunny, no precipitation
11/10/76 Slightly cloudy in morning, clearing in
afternoon, no precipitation.
ND = not determined.
-------
TABLE 5.2. ANALYSIS OF WATER, SOIL, AND SEDIMENT SAMPLES FROM
DOW CHEMICAL PLANT A (METHYLCHLOROFORM PRODUCER)3
K
o
Sample
No.
Date
Sampled
Date
Analyzed
Sediment Sparging Concentration, ppb by
in Sample Foam
MC
TCE CHC13
weight
CC14
Comments
Water
A-l
A-2
A-5
A-6
A-7
A-8
A- 9
1
Sample
No.
A-2
A-4
A-7
A-12
11/9/76
11/9/76
11/9/76
11/9/76
11/9/76
11/10/76
11/13/76
11/12/76
Sample
Weight,
g
0.166
0.141
0.155
0.628
11/23/76
11/28/76
11/23/76
11/23/76
11/17/76
11/19/76
11/30/76
12/1/76
Soil
Water
Content ,
%
11.4
7.8
21.3
20.5
Clear
Light
Heavy
Heavy
Heavy
Medium
Clear
Light
Light
Light
Light
Light
ND
Medium
ND
Medium
117
119
0
1
0
12
17
35
Concentration,
ppbb
MC
0.20
NDC
ND
0.68
TCE
ND
NDC
0.22
0.045
Sample
No.
A-l-S
A-5-S
A-7-S
126
122
.8 5
13
.1 0
2
19
76
Sample
Weight ,
g
0.616
0.240
0.244
82
25
1
3
.9 1
' 2
<0.1
12
Sediment
Water
Content ,
%
71.3
46.8
49.0
116
32
5
7
0.3
0.3
<0.1
24
Surface
Bottom
Surface
Bottom
Surface
Surface
Tap water
Composite
Concentration ,
ppt
MC
6.1
0.34
0.31
>b
TCE
0.21
ND
0.036
Notes: ND = none detected.
for description of terms.
Dry basis, ppb by weight.
See "Determination of Methylchloroform in Water"
"Practical detection limits: MC = 6 pg; TCE = 10 pg.
-------
TABLE 5.3. DESCRIPTIONS OF SAMPLING LOCATIONS AT DOW CHEMICAL PLANT A,
FREEPORT, TEXAS (NOVEMBER 9-12, 1976)
WATER
(Water sample sites Al, A2, A5, A6, and A7 are not shown on the map, Figure 2.32. These sites are
upstream, west of the boundaries of this map, and are upstream and downstream of the location
where the canal from Dow Chemical Plant A discharges into the Brazos River.)
Al - Surface sample, effluent canal from Plant A taken approximately 10 meters upstream in canal
from confluence with Brazos River—moderate current, turbid.
A2 - Bottom sample (approximately 2-1/2 meters deep)—same location as Al.
A5 - Surface sample, 400 meters downstream of plant outfalls in Brazos River—taken in center of
channel—30 meters wide, 5-6 meters deep—swift current, turbid.
A6 - Bottom sample, same location as A5--taken 4 meters deep.
A7 - Surface sample, 800 meters upstream from plant outfalls in Brazos River—30 meters wide, 5-6
meters deep—steep banks bounded by recreational areas—swift current, turbid.
A8 - Shoreline surface sample in East Union Bayou—corresponds to air sampling site 12A—bayou bound-
ed by dredge spoils—40 meters wide—moderate current, clean.
A9 - Tap water from Lake Jackson, Holiday Inn, Freeport, Texas.
1 One 24-hour composite effluent sample collected November 11-12, 1976.
SEDIMENT
A1S - Effluent canal from Plant A, 10 meters upstream in canal from confluence with Brazos River—
light tan, compacted sheet-like clay.
-------
TABLE 5.3. (Continued)
SEDIMENT
ASS - 400 meters downstream of plant outfalls in Brazos River—fine textured, dark loam.
A7S - 800 meters upstream plant Outfalls in Brazos River—brown, fine textured silt/clay.
SOIL
A2 - Northeast of Freeport, south of turning basin on flood control levee—corresponds to air samp-
ling site 2A—light industrial and commercial area—dredge spoil/gumbo—hard sand/silt over
hard, compact clay.
A4 - 400 meters east of Phillips petroleum plant—corresponds to air sampling site 4A—sand/shell
spoil and root-bound sandy silt.
A7 - Overgrown vacant lot 200 meters south of Shrimp Hut in Surfside—residential area on Gulf—
fine sand, some roots.
A12 —250 meters south off Route 332 near East Union Bayou—corresponds to air sampling site 12A—
open dredge spoil area—fine sand eroded from spoil piles and roadway, some roots.
-------
MONITORING DATA
PRODUCTION SITE 2
5-13
-------
Enrission Sourc
Highway
Plant Proper
Residential
Air Site
Soil Site
Water Site
Sediment Site
Figure 5.2.
Sampling locations at Vulcan Materials Company,
Geismar, Louisiana—methylchloroform production
site.
5-14
-------
TABLE 5.4. AMBIENT AIR MEASUREMENTS AT VULCAN MATERIALS (METHYLCHLOROFORM PRODUCER)
Ui
M
Ui
Distance Direction
from from
Site Plant, Plant, Date
No. kma degrees** 1976 Time
1 0.4 090 12/2 0950
1015
1040
1135
1150
2025
2055
12/3 0005
0032
0101
Ol29
0156
0225
0252
0320
0348
0415
0443
0511
0539
0606
0634
0702
0734
0802
1035
2 0.3 010 12/2 1215
1230
2115
2145
12/3 1030
Meteorological
Concentration in
Ambient Air, ppbvc
MC
£0.3
£0.3
£0.3
£0.3
£0.3
2.0
0.8
1.2
2.5
0.8
1.6
18
3.8
8.8
5.0
17
16
8.8
7.0
6.7
3.5
2.7
2.4
2.2
1.6
0.6
£0.3
£0.3
2.7
7.0
140
CC14
0.
0.
0.
0.
0.
5.
3.
23
18
8.
8.
20
11
14
8.
15
15
8.
7.
6.
4.
4.
5.
4.
3.
6.
0.
0.
24
42
30
22
17
73
7
7
0
0
0
2
6
8
6
8
3
3
5
3
20
17
TCE
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
20 ^1
22
sl
Wind
Speed,
PCE
£0
£0
£0
<0
£0
0
£0
1
1
0
0
7
1
3
1
2
2
3
1
1
0
0
0
0
£0
0
£0
£0
1
2
2
.3
.3
.3
.3
.3
.8
.3
.1
.1
.5
.8
.2
.1
.0
.4
.3
.3
.6
.9
.0
.8
.8
.5
.5
.3
.5
.3
.3
.5
.3
.3
m/s
5
5
5
4
4
0
0
0
0
0
0
1
1
0
0
0
0
1
1
0
0
1
1
2
2
1
4
4
0
0
1
Observations^
Wind Temper-
Direction, ature, RH, Barometer,
degrees3 C % mm Hg
320
320
340
360
360
—
—
—
—
—
—
010
010
—
—
—
—
070
070
—
—
060
060
060
060
060
260
260
—
—
060
12
12
12
13
13
4
4
1
1
1
-
0
0
0
0
-1
-1
1
1
1
1
2
2
2
2
14
13
13
3
3
14
51
51
52
50
50
71
71
84
84
84
84
84
84
86
86
88
88
88
88
89
89
90
90
90
90
63
50
50 '
76
76
63
765
765
765
765
765
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
764
765
765
764
764
764
-------
TABLE 5.4. (Continued)
Ul
i
Distance Direction
from from
Site Plant, Plant, Date
No. kma degrees13 1976 Time
2 0.3 010 12/3 1057
1150
1220
1330
1357
1425
1453
1520
1545
3 0.3 230 12/2 1252
1303
12/3 0928
1000
4 0,4 150 12/2 1330
1355
1425
1451
1520
5 0.6 3.40 12/2 1555
1625
6 0.6 120 12/2 1645
1720
1745
1815
1845
1910
7 0,4 045 12/2 2215
2240
2310
2335
Meteorological Observations^
Concentration in
Ambient Air, ppbvc
MC
77
31
9.2
5.6
£0.3
27
1.2
92
140
£0.3
£0.3
^0.3
£0.3
£0.3
75
8.6
41
8,8
155
5.5
11
14
4.2
3.8
1.4
1.2
4.0
1,4
2,7
1,4
CC14
8,8
6.4
3.4
1.7
0.18
4.5
4.1
10
12
0.20
0,20
4.2
0.88
0,73
10
2.2
68
1
10
0.28
11
10
3.6
7,0
10
6.3
10
5.9
52
50
TCE
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
*l
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
PCE
3.6
<0.3
—
1.1
*0.3
1.1
0.6
2.3
4.2
0.3
0.3
0.3
0.3
0.3
23
7.5
2.0
19
7
0,3
4.3
6.2
0.8
0.5
0.3*
0.3
2.3
3.6
6.7
3.6
Wind
Speed,
m/s
1
4
4
2
2
2
3
3
3
4
4
4
4
3
3
4
4
4
4
4
3
3
0
0
0
0
0
0
0
0
Wind
Direction,
degrees3
060
140
140
290
180
180
170
170
190
260
260
100
100
290
290
360
360
360
280
280
.280
280
__
—
—
—
—
00
. —
—
Temper-
ature, KH, Barometer,
C % mm Hg
14
15
15
14
13
13
18
18
18
13
13
13
13
14
14
14
14
14
15
15
14
14
9
9
6
6
3
3
1
1
63
63
63
62
62
62
38e
38e
46e
51
51
60
60
52
52
53
53
53
54
54
54
54
58
58
64
64
78
78
80
80
764
764
764
763
762
762
762
762
762
764
764
764
764
764
764
764
764
764
764
764
766
766
764
764
764
764
764
764
764
764
-------
TABLE 5.4. (Continued)
Distance
from
Site Plant,
No. km a
8 0.3
9 3
Direction
from
Plant , Date
degreesb 1976 Time
190 12/3 0835
0902
1252
030 12/3 1615
1645
Meteorological Observations d
Concentration in
Ambient Air, ppbv°
MC
0.8
£0.3
£0.3
0.5
£0.3
cci4
6.7
1.4
0.23
1.2
0.7
TCE
£1
£1
£1
£1
£1
PCE
1.0
£0.3
£0.3
£0.3
£0.3
Wind
Speed.
m/s
3
3
2
3
3
Wind
Direction,
degrees3
110
110
290
150
150
Temper-
ature, RH,
C %
10
10
17
18
18
82
82
58
46
46
Barometer,
mm Hg
764
764
763
762
762
Ul
I
Distance and direction estimated scaled map unavailable.
bNorth - 360°.
c 3
To convert to pg/m at 25 C multiply ppbv by MC — 5.46
CC14 — 6.29
TCE — 5.37
PCE — 6.78.
d
General weather conditions: 12/2/76 Partly cloudy in morning becoming clear about
1600 hours, no precipitation
12/3/76 Clear, sunny, no precipitation.
Q
Possible malfunction of RH instrument.
-------
TABLE 5.5. ANALYSIS OF WATER, SOIL, AND SEDIMENT SAMPLES FROM
VULCAN MATERIALS PLANT (METHYLCHLOROFORM PRODUCER)3
Sample Date
No . Sampled
Date
Analyzed
Sediment Spargj
in Sample Foai
Lng Concentration^ ppb by
a MC
IT*/"ITO OTJf^l **
ICrli L.nL.J.3
weight
CC14 Comments
Water
V
K-"
gp
E-l 12/2/76
E-2 12/2/76
E-3 12/2/76
E-4 12/2/76
E-5 12/2/76
Sample
Sample Weight,
No. g
E-6 0.298
E-7 0.304
12/30/76
12/28/76
12/27/76
12/29/76
12/29/76
Soil
Water
Content ,
%
26.3
20.4
Light
Light
Light ,.
Medium
Clear
ND
Heavy
ND
2
344
169
3,314
16,500
Concentration ,
ppbb
MC
0.45
0 . 94
TCE
0.62
0.18
Sample
No.
E-l-S
E-3-S
4,
Sample
Weight
8
0.209
0.255
5 6
74 394
24 ' 226
360 152
300 31,675
Sediment
Water
, Content,
%
54.3
27.7
2
193
92
629 Diluted 1-KLOO
9,060 Composite
Concentration,
ppbb
MC TCE
0.13 0.25
2.6 3.2
1+500
Tifotes: ND = none detected. See "-Determination of Methylchleroform in Water1'
for description of terms.
Dry basis, ppb by weight.
-------
TABLE 5.6. DESCRIPTIONS OF SAMPLING LOCATIONS AT VULCAN MATERIALS,
GEISMAR, LOUISIANA (DECEMBER 2, 1976)
WATER
El- Surface sample taken from bank of Mississippi River 30 meters upstream from plant outfall—
area used for barge mooring—moderate current, turbid.
E 2 - Surface sample taken at end of submerged outfall pipe in Mississippi River—effluent dis-
charged subsurface—moderate current, turbid.
E 3 - Surface sample from bank of Mississippi River 75 meters downstream from plant outfall—barge
moored within 20 meters of sampling point—moderate current, turbid.
E 4 - Roadside ditch 60 meters north of Vulcan office (1 meter wide, 1-3 centimeters deep)—ditch
received runoff from heavily trafficked road.
E 5 - Twenty-four-hour composite effluent sample from inside plant.
SEDIMENT
E1S - Shoreline sample in Mississippi River 30 meters upstream from plant outfall—gray-black silt/
sand, oil texture.
ESS - Shoreline sample in Mississippi River 75 meters downstream from plant outfall—gray-black silt/
sand, oily texture.
SOIL
E 6 - 100 meters east of Vulcan office—road cut in front of plant—sandy soil.
E 7 - 200 meters south of plant—strip between service road and railroad--sandy silt, little humus
or roots.
-------
MONITORING DATA
PRODUCTION SITE 3
5-20
-------
Ul
NJ
t-1
Emission Source
Highway
Railroad
Plant Proper
Industrial
Residential
Air Site
Soil Site
Water Site
Sediment Site
Mile
1/2
Kilometer
Figure 5.3. Sampling locations at Ethyl Corporation, Baton Rouge,
Louisiana—methylchloroform production site.
-------
TABLE 5.7. AMBIENT AIR MEASUREMENTS AT ETHYL CORPORATION (METHYLCHLOROFORM PRODUCER)
Ui
I
to
Ni
Distance Direction
from from
Site Plant, Plant, Date
No. km degreesa 1976 Time
1 0.4 240 11/18 0815
0845
2 0.2 195 11/18 0915
0945
11/19 0300
1014
1100
1200
3 2.4 150 11/18 1015
1730
1800
1930
2000
2030
2100
2130
2200
2230
2300
2330
2400
11/19 0030
0100
0130
0200
0545
0615
0700
0730
0800
0830
Meteorological Observations0
Concentration in
Ambient Air, ppbv^
MC
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
0.6
1.1
1.0
1.5
1.0
—
2.2
3.9
0.6
1.5
0.9
0.9
1.6
£0.3
£0.3
£0.3
£0.3
£0.3
0.5
cci4
7.3
1.9
0.80
4.8
1.1
2.4
47
0.90
0.15
0.16
0.12
0.12
0.13
0.15
0.15
0.21
0.33
0.26
—
0.52
0.50
2.7
1.9
1.3
0.9
0.33
0.37
0.32
0.26
0.26
0.22
TCE
5.6
1.9
£1
£1
£1
5.4
7.2
2.4
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
PCE
5.2
1.6
0.7
3.2
£0.3
5.1
37
8.5
£0.3
£0.3
£0.3
0.5
0.6
0.6
0.6
1.0
1.0
0.8
0.6
0.4
0.4
0.5
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
Wind
Speed,
m/s
4
4
4
4
3
4
4
4
4
0
0
2
2
0
0
0
0
0
0
0
1
0
0
0
1
2
2
4
4
3
3
Wind
Direction,
degrees3
020
020
060
060
120
030
060
030
060
'360
360
360
360
360
360
360
360
360
360
360
140
360
360
360
120
090
090
060
070
060
060
Temper- RH, %
ature , (Free . , Barometer ,
C cm) mm Hg
14
14
16
16
12
11
11
11
18
17
17
17
17
16
16
16
16
16
16
16
14
14
14
12
12
12
12
10
10
11
11
NDd
ND
ND
ND
(trace)
(trace)
(0.1)
(0.4)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
(0.02)
ND
(0.02)
(0.02)
ND
.(0.02)
ND
(trace)
ND
761
761
761
761
758
758
758
758
761
759
759
759
759
759
759
759
759
759
759
759
759
759
759
759
758
759
759
758
758
758
758
-------
TABLE 5.7 (Continued)
w
Distance Direction
from from
•Site Plant, Plant,
No . km degrees3
3 2.4 150
4 2.6 180
5 2.2 095
6 0.7 010
7 2.2 330
8 3.2 240
Meteorological
Date
1976
11/19
11/18
11/18
11/18
11/19
11/18
11/18
11/19
Concentration in
Ambient Air, ppbv^
Time
0900
0930
1000
1055
1125
1155
1225
1255
1355
0345
0415
0445
0515
1445
1545
1615
1300
1330
MC
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
SQ.3
SQ. 3
SQ.3
SQ. 3
SQ. 3
£0.3
£0.3
£0.3
SQ.3
cci4
0.21
0.19
0.18
0.12
0.12
0.11
0.17
0.85
0.36
0.38
1.3
0.18
0.43
0.16
0.14
0.13
0.67
0.17
TCE
^
^1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
PCE
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
0.5
0.4
£0.3
0.6
£0.3
£0.3
SQ. 3
£0.3
£0.3
£0.3
SQ.3
Wind
Speed ?
m/s
4
4
4
2
2
1
1
1
2
2
2
1
1
0
2
2
4
4
Wind
Direction,
degrees3
060
060
030
020
020
070
070
240
340
350
350
340
340
360
080
080
040
040
Observations0
Temper- ^ %
ature, (Free., Barometer,
C cm) mm Hg
11
11
11
18
18
18
18
19
19
12
12
12
12
18
18
18
11
11
(trace)
ND
(trace)
ND
ND
ND
ND
ND
ND
(trace)
ND
(0.07)
ND
ND
ND
ND
(0.7)
ND
758
758
758
761
761
761
761
761
761
758
758
758
758
761
761
761
757
757
- 360°.
b 3
To convert to yg/m at 25 C multiply ppbv by MC
"General weather conditions:
— 5.46
CC14 — 6.29
TCE — 5.37
PCE -- 6.78.
11/18/76 Clear in morning becoming cloudy about 1400 hours with light
intermittent rain beginning about 2200 hours
11/19/76 Cloudy all day, intermittent rain throughout the day.
ND
not determined.
-------
TABLE 5.8. ANALYSIS OF WATER, SOIL, AND SEDIMENT SAMPLES FROM
ETHYL CORPORATION (METHYLCHLOROFORM PRODUCER)3
I
NJ
Sample
No.
C-l
C-2
C-3
C-8
C-9
Sample
No.
C-4
C-5
C-6
C-7
Date
Sampled
11/18/76
11/18/76
11/18/76
11/18/76
11/19/76
Sample
Weight ,
g
0.246
0.261
0.274
0.192
Date
Analyzed
12/22/76
12/22/76
12/21/76
12/22/76
12/22/76
Soil
Water
Content ,
%
26.3
20.5
27.5
17.3
Sediment Sparging Concentration, ppb by
in Sample Foam MC
Water
Light ND 74
Heavy Heavy 0 .
Heavy Heavy 20
Clear Light 10
Clear ND 0 .
* t
Concentration,
ppb^ Sample
MC TCE No.
0.20 NDC C-2-S
0.25 ND C-3-S
0 . 13 ND
0.28 ND
TCE CHC13
128 105
4 0.4 6
37 37
10 32
05 0.4 2
Sediment
Sample Water
Weight, Content,
g %
1.07 27.2
0.330 77.5
weight
CC14
67
0.1
23
12
0.2
Comments
Surface
Surface
Composite
Tap water
Concentration ,
ppb
MC
0.81
ND
b
TCE
ND
116
"Notes: ND = none detected.
for description of terms.
b
Dry basis, ppb by weight.
See "Determination of Methylchloroform in Water"
"Practical detection limits: MC = 6 pg; TCE = 10 pg.
-------
TABLE 5.9. DESCRIPTIONS OF SAMPLING LOCATIONS AT ETHYL CORPORATION,
BATON ROUGE, LOUISIANA (NOVEMBER 18-19, 1976)
WATER
Cl - Effluent sample taken immediately above the settling pond weir to receiving bayou—strong aro-
matic odors—light blue-green color, very slippery feel.
C2 - Surface sample taken in receiving bayou 200 meters upstream from plant outfall (7 meters wide,
0.5-1.5 meters deep)—moderate current; anaerobic odor; black murky color with oil slick and
tar globules on surface (bayou flows through heavily industrialized area and under railroad
tracks).
C3 - Surface sample taken in receiving bayou 300 meters downstream from plant outfall (7 meters
wide, 1-2 meters deep)—moderate flow; water quality appearance same as at C2 with additional
slippery feel.
I C8 - 24-hour composite effluent sample—6:00 a.m. November 18 to 6:00 a.m. November 19, 1976.
KJ »
-------
MONITORING DATA
PRODUCTION SITE 4
5-26
-------
Ul
10
Emission Source
Highway
Railroad
Industrial
Plant Proper
Residential
Marsh
Tailings Pond
Air Site
Soil Site
Water Site
Sediment Site
Figure 5.4. Sampling locations at PPG Industries, Lake Charles,
Louisiana—methylchloroform production site.
-------
TABLE 5.10. AMBIENT AIR MEASUREMENTS AT PPG INDUSTRIES (METHYLCHLOROFORM PRODUCER)
Cn
NJ
00
Distance Direction
from from
Site Plant, Plant, Date
No. km degrees3 1976 Time
1 1.3 215 12/6 1014
1043
2 4.2 140 12/6 1123
1152
3 3.5 1 85 12/6 1302
1330
12/7 0900
4 2.7 40 12/7 1512
1540
5 1.4 195 12/6 2100
2129
2157
2226
2254
6 4.0 150 12/6 2331
2400
12/7 0028
0056
0125
0153
0222
0249
0317
0345
0413
0441
0509
0537
0605
0633
0701
Meteorological Observations0
Concentration in Wind
Ambient Air, ppbv^ Speed,
MC
1.
0.
£0.
£0.
£0.
SO.
0.
0.
SO.
SO.
SO.
SO.
SO.
SO.
SO.
sO.
SO.
0.
1.
SO.
SO.
1.
5.
8.
0.
so.
6.
SO.
1.
1.
1.
3
8
3
3
3
3
7
5
3
3
3
3
3
3
3
3
3
4
7
3
3
5
0
5
7
3
5
3
4
2
4
cci4
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
0
.24
.17
.13
.19
.13
.20
.24
.21
.17
.18
.15
.15
.17
.20
.17
.31
.28
.20
.88
.19
.20
.64
.21
.31
.19
.20
.92
.15
.17
.26
.17
TCE
2.7
2.2
si
Si
si
si
si
si
si
si
si
si
si
si
si
si
si
si
15
si
si
6.6
si
2.2
si
si
12
si
si
si
si
PCE
0.4
0.3
SO. 3
SO. 3
SO. 3
SO. 3
0.4
SO. 3
SO. 3
SO. 3
so. 3
SO. 3
so. 3
SO. 3
SO. 3
SO. 3
SO. 3
SO. 3
3.8
0.4
£0.3
2.5
SO. 3
0.7
^0.3
£0.3
5.0
£0.3
^0.3
£0.3
£0.3
m/s
8
8
7
7
9
9
7
7
7
10
10
10
9
9
7
7
6
6
6
7
7
6
6
7
7
7
7
6
6
7
7
Wind
Direction,
degrees3
150
150
160
160
160
160
340
330
330
360
•360
350
350
350
350
350
360
360
360
360
360
340
340
340
340
340
340
350
350
350
350
Temper-
ature, RH, Barometer,
C % mm Hg
15
15
17
17
17
17
6
8
8
14
14
12
12
12
12
12
12
12
12
11
11
9
9
8
8
7
7
6
6
6
6
87
87
90
90
87
87
76
60
60
80
80
80
77
77
76
76
74
74
74
80
80
80
80
80
80
79
79
79
79
79
79
755
755
754
754
753
753
759
760
760
756 -
756
756
756
756
756
756
756
756
756
757
757
757
757
757
757
758
758
758
758
758
758
-------
TABLE 5.10. (Continued)
Ul
i
N>
IO
Distance
from
Site Plant,
No. km
6 4.0
7 0.6
8 1.3
Direction
from
Plant, Date
degreesa 1976 Time
150 12/7 0727
0755
0823
0855
0958
1015
1030
1045
1100
1205
1232
1259
1328
1358
360 12/7 1030
265 12/7 1052
Meteorological Observations0
Concentration in Wind
Ambient Air, ppbv^ Speed,
2
5
5
£0
£0
£0
£0
£0
£0
2
£0
5
2
£0
£0
0
MC
.6
.0
.3
.3
.3
.3
.3
.3
.3
.4
.3
.0
.1
.3
.3
.4
cci4
0.65
0.96
0.73
0.20
0.15
0.15
0.13
0.15
0.23
0.40
0.20
0.64
0.26
0.20
0.21
0.75
TCE
5.8
8.0
5.8
£l
£l
£l
£l
£l
£l
4.6
£l
7.0
4.6
£l
£l
£l
PCE
2.9
3.2
3.2
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
1.8
£0.3
£0.3
£0.3
£0.3
£0.3
0.4
m/s
7
6
6
7
8
8
7
7
7
6
7
7
6
6
7
7
Wind
Direction,
'degrees a
350
350
350
340
320
320
320
320
320
320
340
340
340
340
320
320
Temper-
ature,
C
6
6
6
6
5
5
5
5
5
6
6
6
7
7
6.7
6.7
RH, Barometer,
% mm Hg
79
76
76
76
76
76
73
73
73
73
70
70
68
68
73
73
758
758
758
759
759
759
760
760
760
760
760
760
760
760
760
760
aNorth - 360°.
|_ O
To convert to g/m at 25 C multiply ppbv by MC — 5.46
CC14 — 6.29
TCE — 5.37
PCE — 6.78.
°General weather conditions: 12/6/76 Cloudy, rainfall recorded from 1000 to 2100 hours,
very heavy at times
12/7/76 Cloudy with very slight clearing in late afternoon,
no precipitation.
-------
TABLE 5.11. ANALYSIS OF WATER, SOIL, AND SEDIMENT SAMPLES FROM
PPG INDUSTRIES (METHYLCHLOROFORM PRODUCER)3
Sample
No.
Date
Sampled
Date
Analyzed
Sediment Sparj
in Sample Fo<
?ing Concentration, ppb by
im MC
TCE CHC13
weight
CC14 Comments
Water
Ul
i
UJ
o
F-l'
F-2
F-3
F-4
F-5
F-10
Sample
No.
F-6
F-7
F-8
F-9
12/7/76
12/7/76
12/7/76
12/7/76
12/7/76
12/7/76
Sample
Weight,
g
0.337
0.286
0.232
0.782
1/5/77
vim
vim
1/6/77
1/4/77
12/13/76
Soil
Water
Content ,
%
12.2
22.5
19.6
28.3
Heavy
Heavy
Heavy
Heavy
Heavy
Clear
* «
Concentration,
ppbb
MC TCE
0.14 0.11
1.0 NDC
0.61 0.077
0.22 ND
132
181
58
161
5
0
Sample
No.
F-l-S
F-2-S
F-3-S
F-4-S
353
447
179
403
29
.3 0.
Sample
Weight,
g
0.263
— d
0.265
..d
11
85
30
34
12
1 <0.1
Sediment
Water
Content ,
%
72.6
71.0
29
40
12
38
<0.1
<0.1 Tap water
Concentr at ion ,
ppbb
MC TCE
2.2 146
1.1 15
Notes: ND - none detected. See "Determination of Methylchloroform in Water"
for description of terms.
Dry basis, ppb by weight.
Practical detection limits: MC - 6 pg; TCE = 10 pg.
Samples damaged in shipping (including duplicates).
-------
TABLE 5.12. DESCRIPTIONS OF SAMPLING LOCATIONS AT PPG INDUSTRIES,
LAKE CHARLES, LOUISIANA (DECEMBER 7, 1976)
WATER
Fl - Surface sample 50 meters upstream from plant outfall in Bayqu d'lnde (10 meters wide, 2.5 -3
meters deep)—slow current; high conductivity (>8000 microohms/cm); dark colored, turbid.
F2 - Surface sample—confluence of northernmost PPG effluent canal in Bayou d'lnde--5 meters wide,
1 meter deep.
F3 - Surface sample—confluence of southernmost PPG effluent canal in Bayou d'lnde—200 meters below
confluence of first canal (F2); 5 meters wide, 1 meter deep.
F4 - Surface sample—50 meters downstream of southernmost PPG effluent canal (F3) in Bayou d'lnde—
10 meters wide, 2-3 meters deep.
Y1 F5 - Surface sample taken at mouth of Calcasieu River in Prien Lake, downstream of PPG outfall.
CO
H
F10 - Top water taken from the Sheraton Motel, Lake Charles, Louisiana.
SEDIMENT
FlS - 50 meters upstream from plant outfall in Bayou d'lnde—black ooze.
F2S - Confluence of northernmost PPG effluent canal in Bayou d'lnde—black, oily ooze.
F3S - Confluence of southernmost PPG effluent canal in Bayou d'lnde—black, oily ooze.
F4S - 50 meters downstream of southernmost PPG effluent canal (F3) in Bayou d'lnde—black, oily ooze.
SOIL
F6 - Lake Shore Drive near Port of Lake Charles—residential area—sand/clay roadfill.
F7 - 1210 drainage ditch 400 meters north of bridge over Prien Lake—ditch composed of both concrete
and sandy clay.
-------
MONITORING DATA
USER SITE
5-32
-------
Emission Source
Highway
Railroad
Industrial
Plant Proper
Residential
Air Site
Soil Site
Water Site
Sediment Site
0 .5 1
Kilometer
Figure 5.5 Sampling locations at Boeing Company, Auburn,
Washington-~methylchloroform user site.
5-33
-------
TABLE 5.13. AMBIENT AIR MEASUREMENTS AT BOEING COMPANY, AUBURN PLANT (METHYLCHLOROFORM USER)
Ul
I
U3
Distance Direction
from from
Site Plant, Plant, Date
No. km degrees3 1977
1 0.7 335 1/10
1/11
2 0.6 125 1/10
3 0.9 165 1/10
1/11
1
4 1.1 280 1/10
1/11
5 0.9 005 1/10
6 0.4 050 ;L/1L
7 1.2 215 1/11
Meteorological Observations0
Concentration in Wind Wind
Ambient Air, ppbv*5 Speed, Direction,
Time
1330
1350
1410
1925
0750
0810
0900
1630
1455
1515
1542
1602
1006
1027
1655
1715
1735
1630
1655
1550
1610
1825
1945
0.9Z3.
0943
1120
1140
1200
1220
1240
1325
MC
10.
4.
6.
0.
3.
5.
2.
1.
0.
0.
0.
0.
2.
3.
4.
4.
5.
0.
0.
6.
5.
5.
0.
0
6
8
8
8
0
0
6
4
5
4
,4
3
0
5
9
0
6
6
2
2
2
9
0-6
2.
6.
7.
7.
7.
6.
7.
3
9
3
3
4
9
3
CC14
0.11
0.10
0.11
0.11
0.09
0.06
0.09
0.10
0.11
0.13
0.13
0.13
0.10
0.07
0.10
0.11
0.11
0.14
0.13
0.11
0.11
0.14
0.15
0..09.
0.13
0.09
0.09
0.08
0.10
0.10
0.10
TCE
0.38
0.15.
0.15
0.14
0.64
0.64
0.26
0.26
0.34
0.14
0.14
0.14
1.8
0.92
0.83
0.80
0.90
0.14
0.14
0.90
0.76
0.92
0.18
GUIS
0.30
0.80
0.84
0.76
1.0
1.0
1.0
PCE
0.29
0.18
0.29
0.29
0.20
0.25
0.69
0.69
0.08
0.11
0.06
0.06
0.98
1.4
0.60
0.66
0.66
0.08
0.11
0.94
0.94
0.69
0.42
0.65
0.76
0.90
0.73
0.69
0.73
0.78
0.82
m/s
0.8
0.8
1.4
d
d
d
"d
0.6
1.4
1.2
1.2
0.6
0.6
0.6
0.6
0.5
0.7
0.7
0.5
0.5
__ d
— d
— d
— d
d
n
0
0.5
0.5
— d
degrees3
180
180
180
— d
— d
— d
— d
150
180
180
180
50
50
150
150
150
150
150
210
210
— d
— d
d
Q
Q^
— d
Q_
360
360
— d
Temper-
ature, RH, Barometer,
C % mm Hg
-1
-1
0
-1
-1
0
0
3
0
-2
-2
1
1
3
3
2
2
2
3
3
2
1
-1
-1
1
1
1
2
2
2
86
86
86
88
92
92
92
93
86
87
87
92
92
93
93
93
87
94
94
94
88
92
92
92
92
92 f
93
93
93
761
761
761
761
758
758
758
754
760
761
757
757
753
753
753
761
754
754
753
761
758
758
757
757
757
757
757
757
-------
TABLE 5.13. (Continued)
i
uj
Ul
Site
No.
7
8
9
>
10
Distance Direction
from from
Plant, Plant,
km degrees3
1.2
2.0
2.9
1.1
215
210
200
255
Meteorological Observations0
Date
1977
1/11
1/11
1/11
1/11
Concentration in Wind
Ambient Air, ppbv^ Speed,
Time
1805
1345
1405
1430
1450
1510
1530
MC
4.8
7.8
8.4
4.4
4.0
7.0
8.1
CC14
0.10
0.10
0.09
0.11
0.11
0.10
0.10
TCE
0.80
1.0
1.1
0.82
0.78
1.2
1.1
PCE
0.66
0.90
1.0
0.69
0.65
0.97
1.0
m/s
__d
__d
0.6
0.6
0.5
0.5
. Wind
Direction,
degrees3
__d
d
180
180
210
210
Temper-
ature, RH,
\J 10
2
2
2
3
3
3
3
93
93
93
93
93
93
93
Barometer,
mm Hg
753
756
756
756
756
756
756
- 360°.
•L. O
To convert ug/m to ppbv multiply by MC — 5.46
CC14 — 6.29
TCE — 5.37
PCE — 6.78.
°General weather conditions: 1/10/77 Heavy overcast of fog; no precipitation
1/11/77 Heavy overcast of clouds, fog; light rain from 0600 to 1500 hours.
vfind speed below starting threshold of 0.75 mph for MRI 1071 weather station.
-------
TABLE 5.14. ANALYSIS OF WATER, SOIL, AND SEDIMENT SAMPLES FROM
BOEING COMPANY, AUBURN PLANT (METHYLCHLOROFORM USER)3
Sample
No.
J-2
J-3
J-4
J-5
J-6
J-10
Sample
No.
J-l
J-7
J-8
J-9
Date
Sampled
1/11/77
1/11/77
1/11/77
1/11/77
1/11/77
1/12/77
Sample
Weight ,
g
0.258
0.238
-T-C
c
Date
Analyzed
2/8/77
2/8/77
2/8/77
2/8/77
2/8/77
2/8/77
Soil
Water
Content ,
%
33.3
32.6
Sediment Sparging Concentration, ppb by
in Sample Form MC TCE CHC13
Light
Light
Light
Light
Light
Light
ND
ND
ND
ND
ND
ND
•*•»
Concentration ,
PP
MC
0.40
0.65
bb
TCE
0.33
0.43
Water
18 30 4
12 17 7
6 82
6 5 0.4
18 26 8
26 44 24
Sediment
Sample Water
Sample Weight, Content,
No, g %
J-4-S 0.694 28.2
J-5-S 0.805 28.8
weight
CC14
<0.1
0.6
0.2
0.2
0,4
1.0
Comments
5-hr composite
Concentration ,
PI
MC
0.039
NDd
)b0
TCE
0.42
ND
Notes: ND = none detected. See "Determination of Methylehloroform in Water"
for description of terms.
b
Dry basis, ppb by weight,
c
Sample primarily roots and peat moss—-could not be run as soil sample.
Practical detection limits: MC = 6 pg; TCE = 10 pg.
-------
TABLE 5.15. DESCRIPTIONS OF SAMPLING LOCATIONS AT BOEING COMPANY,
AUBURN, WASHINGTON (JANUARY 10-12, 1977)
^
WATER
J2 -Surface sample—Boeing outfall from settling pond—taken as effluent spilled from concrete cul-
vert—water clear, warm, smelled of chlorine, slippery to touch.
J3 -Surface sample 1 meter upstream in outfall canal to Stuck River 3 kilometers downstream of plant
outfall (1 meter wide, 0.5 meter deep)—clear, moderate current.
J4 -Surface sample 100 meters downstream from plant outfall in Stuck River (50 meters wide, 0.5-1
meter deep)—swift current, turbid, very cold, ice cover near shore; receives runoff from land-
moving operation near banks.
J5 -Surface sample 30 meters upstream from plant outfall in Stuck River (40 meters wide, 0.5-1
meter deep)—turbid, very cold, ice cover near bank, swift current.
J6 -Surface sample—Boeing outfall canal 1.5 kilometers downstream from plant outfall—residential
area; 3-4 meters wide; 0.5 meter deep; taken below bridge; clear, moderate current.
J10 - 5-hour composite effluent sample—undiluted—first 5 hours of 8-hour discharge.
SEDIMENT
J4S - 100 meters downstream from plant outfall in Stuck River—compact, fine sand.
J5S - 30 meters upstream from plant outfall in Stuck River—compact, fine sand.
SOIL
Jl - dead end road northwest of plant—corresponds to air sampling site 4; overgrown vacant lot at
side of road—20 meters north of intersection, light to moderate traffic—root-bound sandy clay.
J7 - 0.5 kilometers southwest of southern plant guard gate—corresponds generally to air sampling
site 3—taken 10 meters east off moderately trafficked blacktop road—wet, sandy clay.
J8 -Ditch paralleling railroad tracks on northwest corner of plant property, 50 meters from plant
fence—corresponds to air sampling site 1—loam.
J9 -Ditch between C Street and railroad tracks east of plant, 30-40 meters from plant fence—peri-
odically heavy train and auto traffic—corresponds to air sampling site 6—loose textured, root-
bound loam.
-------
MONITORING DATA
BACKGROUND SITE
5-38
-------
Figure 5.6.
Sampling locations at St. Francis National Forest,
Helena, Arkansas—background site.
5-39
-------
TABLE 5.16. AMBIENT AIR MEASUREMENTS AT ST. FRANCIS NATIONAL FOREST (RURAL BACKGROUND)
Ul
I
Concentration in
Ambient Air, ppbva Wind Speed,
Date Time
11/30/76 1030
1055
1125
1146
1216
1243
1308
1334
1400
1426
1452
1517
1545
1611
1636
1700
1730
1800
1825
1850
1917
1955
2022
MC
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
£0.3
CC14
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
15
15
13
14
15
12
11
14
14
13
15
14
15
14
14
15
15
14
15
14
14
15
15
TCE
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
£1
PCE
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
£0.
3
3
3
3
3
3
3
3
3
3
3
3 .
3
3
3
3
3
3
3
3
3
3
3
m/s
1
1
1
2
2
3
3
3
3
3
4
.„ 4
3
3
2
2
2
2
2
2
2
4
4
Meteorological Observations0
Wind Direction,
degreesb
170
170
170
210
210
230
230
225
225
225
220
220
160
160
165
165
165
165
165
160
160
170
170
Temperature, RH,
C %
3
3
3
5
5
4
4
5
5
4
4
' 4
4
4
2
2
1
1
1
1
1
2
2
41
41
41
38
38
39
39
42
42
44
44
44
49
49
58
58
66
66
66
70
70
73
73
Barometer,
mm Hg
761
761
761
760
760
760
760
759
759
759
759
759
759
759
759
759
759
759
759
759
759
758
758
a 3
To convert to pg/m at 25 C multiply ppbv by MC -- 5.46; CC14 — 6.29; TCE — 5.37; PCE — 6.78.
bNorth - 360°.
c
General weather conditions: Clear, sunny, no precipitation.
-------
TABLE 5.17. ANALYSIS OF WATER, SOIL, AND SEDIMENT SAMPLES FROM
THE BACKGROUND SITEa
Ul
I
Sample
No.
D-l
D-3
Sample
No.
D-2
D-2
Date
Sampled
11/30/76
11/30/76
Sample
Weight ,
g
0.200
0.641
Date
Analyzed
12/20/76
12/14/76
Soil
Water
Content,
25.8
24.3
Sediment Sparging Concentration, ppb by weight
in Sample Foam MC
Water
Clear ND 0 .
Clear ND 0.
Concentration,
ppbb Sample
MC TCE No .
0.54 0.63 D-l-S
0.29 <0.42C D-l-S
TCE CHC13
4 <0.
4 22
Sample
Weight,
g
0.198
0.115
05 2
3
Sediment
Water
Content ,
45.0
54.0
CC1A
Comments
0.2
<0.1 Tap water
Concentration,
ppbb
MC
0.67
0.23
TCE
2.2
NDd
Notes: ND = none detected. See "Determination of Methylchloroform in Water"
for description of terms.
Dry basis, ppb by weight.
c
Possible interference present.
Practical detection limits: MC = 6 pg; TCE = 10 pg.
-------
TABLE 5.18. DESCRIPTIONS OF SAMPLING LOCATIONS AT STORM CREEK LAKE,
ST. FRANCIS NATIONAL FOREST, HELENA, ARKANSAS (NOVEMBER
30, 1976)
WATER
Dl - Surface sample taken from concrete boat dock on Storm Creek Lake
100 meters south of parking lot—little wave action; clear.
D3 - Top water taken from the Holiday Inn, Helena, Arkansas.
SEDIMENT
DlS - Taken from boat dock on Storm Creek Lake 100 meters south of
parking lot—mud and sand with cover of light leaf litter; snail
and mussel shells abundant.
SOIL
D2 - west-facing slope north of boat ramp 75 meters west-southwest of
parking lot—sandy humus with decomposing leaf litter and many
roots—dense undergrowth of honeysuckle vines.
5-42
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-56075-77-02 S
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
ENVIRONMENTAL MONITORING NEAR INDUSTRIAL SITES
METHYLCHLOROFORM
5. REPORT DATE
August 1977
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Battelle Columbus Laboratories
8. PERFORMING ORGANIZATION REPORT \Z
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Battelle Columbus Laboratories
505 King Avenue
Columbus, Ohio 43201
10. PROGRAM ELEMENT NO.
11. CONTRACT/0WWPWNO.
68-01-1983
12. SPONSORING AGENCY NAME AND ADDRESS
Environmental Protection Agency
Office of Toxic Substances
Washington, D.C. 20460
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
The levels of methylchloroform (MC) in various environmental media were determined
at four production sites, one user site, and a background site. The ambient air
level was determined on-site by direct injection of the ambient air into a gas
chromatograph followed by detection and quantification with an electron capture
detector. Water, soil, and sediment samples were returned to Battelle for analyses.
For the analyses of water samples, MC was sparged from the water collected on a trap
material using a commercial liquid sample concentrator. The trapped organic
material was then backflushed onto a gas chromatograph column which was connected
to an electron capture detector used to quantify the MC in the original sample. A
similar technique was used for the quantification of MC in soil and sediment. The
results from the analyses and detailed descriptions of the sampling locations are
given and keyed to site maps. Considerable variation was observed in the maximum
downwind levels of MC at various production plants. Concentrations in ambient air
ranged from less than 0.3 ppb to 155 ppb. Concentrations in surface water in
vicinity of production and user plants was even more variable ranging from fractions
of a ppb to over 16 ppm. Concentrations in soil and sediment range from the limits
of detection to over 6.1 ppm.
7.
KEY WORDS AND DOCUMENT ANALYSIS
a. DESCRIPTORS
Me thy 1 chlo ro f o rm
18. DISTRIBUTION STATEMENT
Distribution! unlimited
b.lDENTIFIERS/OPEN ENDED TERMS
Environmental monitoring
19. SECURITY CLASS (This Report}
Unclassified
20. SECURITY CLASS (This page)
Unclassified
c. COSATI F-'icld,'Group :
21. NO. OF PAGES
74
22. PRICE
EPA Form 2220-1 (Revi 4-77) PREVIOUS EDITION is OBSOLETE
------- |