ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
EPA-330/2-77-022
The Potential For Pollution
Of The Little Menomonee River
From The Kerr-McGee/Moss-American Plant Site
Milwaukee, Wisconsin
(September-October 1977]
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
DENVER, COLORADO
AND
REGION V, CHICAGO, ILLINOIS I
NOVEMBER 1977
-------
ENVIRONMENTAL PROTECTION AGENCY
Office of Enforcement
EPA-330/2-77-022
THE POTENTIAL FOR POLLUTION
OF THE LITTLE MENOMONEE RIVER
FROM THE KERR-McGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN
(September-October 1977)
November 1977
National Enforcement Investigations Center - Denver
and
Region V - Chicago
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CONTENTS
I INTRODUCTION 1
II SUMMARY AND CONCLUSIONS 3
III RECOMMENDATIONS 5
IV STUDY METHODS 6
WELL AND SOIL SAMPLING SITE LOCATIONS. . 6
SAMPLING AND ANALYTICAL PROCEDURES ... 11
V GEOLOGIC OBSERVATIONS AND
ANALYTICAL RESULTS 16
TABLES
1 Location of Wells Installed -
Sept. 19-20, 19 77 8
2 Transects Used in Locating Soil
Sampling and Well Sites - Sept. 1977 . 9
3 Water Level Measurements in
Wells Drilled - Sept. 19-20, 1977. . . 12
4 Water Level Measurements in Wells
and a Spring - Oct. 19, 1977 14
5 Analytical Results
Well Water Samples 17
6 Analytical Results
Soil and Well Core Samples 19
FIGURES
1 Aerial View of
Kerr-McGee/Moss-American Site 7
APPENDICES
A Well Logs, Casing and Perforation Record
and Field Notes - 9/19-20/77
B Chain-of-Custody Procedures
C Soil and Water Sample Analyses
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I. INTRODUCTION
Creosote contamination of the Little Menomonee River from the
operation of a Kerr-McGee/Moss-American creosote plant near Milwaukee,
Wisconsin has been a long-standing problem in the area. Severe con-
tamination occurred in the past as a result of the direct discharge of
wastewater and now, even though the plant has ceased operations, con-
tinued contamination from residual creosote deposits is of concern.
The National Enforcement Investigations Center (NEIC) of the
Environmental Protection Agency (EPA) was requested by EPA1s Region V to
conduct an investigation of the plant site and recommend measures to
eliminate further pollution of the River. This investigation was
conducted in September and October of 1977. A review of the history of
the site and the resulting pollution is presented in an earlier report
by NEIC.*
Due to the highly technical and complex nature of the subject
matter concerning creosote contamination of the Little Menomonee River,
the Honorable Myron L. Gordon, U.S. District Judge (Eastern District,
Wisconsin) appointed David A. Saichek, of Gaines and Saichek, to serve
as Special Master in the matter of United States v. Kerr-McGee/Moss-
American,,Inc. All drilling, sampling and other field observations
conducted by NEIC were done in accordance with requirements specified in
a letter from the Special Master dated April 29, 1977 to Mr. Frank J.
Daily, Attorney for the defendant, and Mr. Charles H. Bohl, U.S.
* National Enforcement Investigations Center} June 1977. Impact of
Creosote Deposits in the Little Menomonee River} Wisconsin (April 1977).
Denver: Environmental Protection Agency, 330/2-77-0163 47 p.
** Case No. 75-C-277.
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2
Attorney. In addition, on-site field operations including well drilling,
sampling, water level measurements, well casing removal, well back-
filling and abandonment procedures were observed by the Special Master,
the EPA Region V Attorney, and representatives of the defendant.
This report describes the field methods used during the September
and October surveys. It also presents the results of the investigation
and recommends measures to reduce or eliminate movement of creosote from
the plant site into the Little Menomonee River.
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II. SUMMARY AND CONCLUSIONS
As requested by EPA, Region V, the National Enforcement Investigations
Center conducted an investigation of the abandoned Kerr-McGee/Moss-
American plant site near Milwaukee, Wisconsin. The objectives of the
investigation were to determine the extent of creosote contamination in
soil and groundwater, to evaluate the potential for continued pollution
of the Little Menomonee River from this site, and to determine the
measures necessary to eliminate the source of pollution.
During a site visit on September 19 and 20, 1977, six wells were
drilled, casings were installed, groundwater levels were determined and
water samples were collected from four of the wells for. analysis [Appendix
A]. In addition, core samples were collected at depths over 4.6 m (15
ft) during well drilling. Transects were laid out in relation to the
wells and to structures in the area, and more than 100 soil samples were
collected at depths up to 90 cm (3 ft) for later analysis.
Another site visit was made on October 19, 1977 to collect a second
series of water samples from the wells and to remove the well casings.
The wells were backfilled and the property was restored to its pre-
survey condition to the satisfaction of Company representatives present
on the site.
All soil and water samples were returned to the NEIC under chain-
of-custody procedures [Appendix B] and analyzed for methylene chloride
extractables [Appendix C]. The moisture content of the soil samples was
also determined. The presence of creosote in the extracts was confirmed
by gas chromatography on all of the extracts and the individual components
of creosote were confirmed by mass spectrometry analyses of selected
samples.
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4
Groundwater level at each well was measured during both visits.
These measurements plus general observations of the area and a knowledge
of geology and hydrology indicate that the groundwater flows toward the
Little Menomonee River.
The presence of creosote in water samples from two wells during
both site visits and from a third well during the October visit shows
that the groundwater is contaminated with creosote.
Analyses of core samples and soil samples taken from the transects
show that the entire area is contaminated with creosote, in some cases
to a depth of at least 4.6 m (15 ft) below ground level. In one case,
the concentration of methylene chloride extractables in the soil was
greater than 27% and it was greater than 10% in several more samples.
Such widespread and high concentrations of creosote at the Kerr-
McGee/Moss-American plant site make it evident that contamination of the
Little Menomonee River will continue unabated for years if no efforts
are made to control surface runoff and mobility of the creosote-contaminated
groundwater.
The provision of an interceptor ditch, however, would prevent the
contaminated runoff, groundwater and soil from entering the River. A
granular carbon adsorption column may be necessary if the ditch effluent
contains dissolved contaminants.
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III. RECOMMENDATIONS
The inflow to the Little Menomonee River of creosote-contaminated
surface runoff, groundwater, and soil could be prevented by installing
an interceptor ditch along the railroad track north of the site and
between the contaminated area and the Little Menomonee River [Figure 1,
Section IV].
The ditch should intercept the groundwater and surface runoff from
the Kerr-McGee/Moss-American property. A system of skimmers and ad-
sorption media (straw), placed in the ditch, would remove creosote from
the interceptor discharge before it enters the Little Menomonee River.
At 2.4 m (8 ft) deep, the ditch would collect any creosote floating on
the water table and any soil washed off during a storm.
The ditch would have to be maintained regularly to remove accumu-
lated skimmed material and solids that have settled.
If the water leaving the ditch is contaminated with soluble or
emulsified components of creosote, it may be necessary to install a
granular activated carbon column to treat the discharge from the ditch.
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IV. STUDY METHODS
WELL AND SOIL SAMPLING SITE LOCATIONS
2
The investigated site consists of approximately 44,500 m (11
acres) located in the NW 1/4, Section 8, T.8N., R.21E. near Brown Deer,
Milwaukee County, Wisconsin [Figure 1]. From an aerial photograph of
the site and an on-site inspection, the decision was made that six
observation wells would be drilled to characterize the degree of con-
tamination of the soil and the groundwater with creosote. One well was
drilled near the northeast corner of a green shed close to the former
retort area, and where it was assumed that the concentration of creosote
would be the highest. Five other wells were drilled in relation to this
"green shed" well, as described in Table 1; Figure 1 shows the approxi-
mate location of these wells. Because of surface characteristics
(water, muck, etc.), it was not practicable to drill all of the wells at
what was considered optimum locations.
Once the wells were located, transects were established in relation
to the wells and to structures in the area [Table 2]. The transects
enabled the location of sites for collection of samples of soil from the
surface and down to depths of 90 cm (3 ft) below land surface. The
analysis of the samples collected allowed a more complete evaluation of
the extent of contamination in the area.
The six observation wells were drilled on the eastern half of the
Kerr-McGee/Moss-American plant site on September 19 and 20, 1977 using a
truck-mounted continuous flight auger drill rig. In the field, a geologic
log was prepared of each hole, including observations made by studying
cuttings brought from the wells, noting rig behavior and taking drive
samples.
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,SS#^. ''.%'¦ *¦>>t*X'^ i+*-: Hi :i-ii ^"t-w"-'%
•S;-*V
NOTE: WELLS LOCATED BY LAST TWO
£3^5
NUMBERS OF STATION ONLY
EffiMK! D
SCALE : 1" = ~ 358'
*cre-jt«Bfeg
Figure l. Aerial View of Kerr-McGee/Moss-American Site 6/76
' Lf S H E' \\ '¦ "iu «»., ~ VTR*fl'tftlFairchi 1 ci National, Inc. I
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8
Table 1
LOCATION OF WELLS INSTALLED AT THE
KERR-MCGEE/MOSS-AMEEICAN PLANT SITE
MILWAUKEEs WISCONSIN
September 19-20} 1977
Well Location Description*
772401 2.4 m (8 ft) from NE corner of the green shed,
bearing 045°
772407 226 m (740 ft) from well 772401, bearing 045°
772419 315 m (1,035 ft) from well 772401, bearing 080°
772413 177 m (582 ft) from well 772401, bearing 335°
772440 About 91 m (298 ft) from well 772401 and 29 m
(96 ft) north of transect A
772431 Halfway between wells 772407 and 772419 on transect F
t All bearings were taken with magnetic compass
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9
Table 2
TRANSECTS USED IN LOCATING
SOIL SAMPLING AND WELL SITES
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN
Septembers 1977
Transect
Description
A
Line connecting wells 772401 and 772407
B
Line connecting wells 772401 and 772413
C
Line connecting wells 772407 and 772413
D
Line east from well 772413 and parallel to
railroad tracks
E
Line connecting wells 772401 and 772419
F
Line connecting wells 772407 and 772419
G
Line parallel to and 1 m (3 ft) south of retorts
H
Line parallel to and 0.3 m (1 ft) north of north
wall of retort building
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10
A drive sample was collected by removing the auger from the well
and replacing it with a "split-spoon sampler" on the bottom end of the
drill rod. The split spoon was driven into the undisturbed earth at the
bottom of the well by dropping a 59 kg (130 lb) weight. The number of
blows required to drive split-spoon sampler 46 cm (18 in) deep was
recorded at the time of sampling. These data are recorded in the drill
logs.
After the split-spoon sampler was removed, the auger was re-
installed in the hole, and drilling continued until the desired depth
was reached. Upon reaching this depth, the auger was removed from the
hole and a section of 5-cm (2-in) diameter PVC pipe, capped on the end
and perforated with hacksaw slots, was installed in the hole. Backfill
around the casing was obtained from cuttings which had been withdrawn
from the hole.
During the drilling of the green-shed well (772401), it was noted
that cores obtained from 3.0 to 3.5 m (10 to 11.5 ft) and from 4.6 to
/ \ **
5.0 m (15 to 16.5 ft) had layers of creosote filling fractures and
partings. As drilling progressed to about 6 m (20 ft), the auger began
to lift water to the surface. This water had globules of creosote
floating on the surface. As the auger was withdrawn, it was noted that
the bottom 4.6 m (15 ft) was not coated with clay as had been the experi-
ence in other holes on the site, but instead was coated with creosote.
This apparently was the result of drilling through a layer of creosote
which coated the auger and prevented any clay from adhering to the
auger.
* PolyvinyI Chloride
** Identified on the basis of odor and appearance
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11
SAMPLING AND ANALYTICAL PROCEDURES
Well Samples
Upon completing the six observation wells, the depth to groundwater
was determined, and water sampling proceeded. Depth to water, obtained
with a Powers' electric well sounder, was recorded as depth below the
undisturbed land surface [Table 3].
After the depth was recorded, a 4.6 m (15 ft) long, 2.5 cm (1 in)
diameter suction hose was installed in the casing and well was pumped
until dry or until suction was broken. This was done twice at each
well, then water samples were collected in glass containers prerinsed
with water from each well using a Homelight gasoline-powered water pump.
Water could not be obtained from two of the wells (772407 and 772419) due
to the tight clay which comprises the bulk of the formation.
During each pumping of the green-shed well (772401), the water was
noticed to contain globules of creosote, and as the pump broke suction a
creosote froth was produced.
The soil samples from the wells were taken by opening the split-
spoon sampler and placing the lower portions of the core in chemically
clean glass jars capped with Teflon-lined lids. The upper portion of
the core, which included material that fell into the hole as the auger
was being removed, was not saved as a part of the sample.
All samples, soil and water, were taken to the NEIC Laboratory for
analysis. Chain-of-custody procedures were followed throughout.
On October 19, the site was again visited by NEIC to re-sample the
wells and return the site to pre-survey conditions. Several of
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Table 3
WATER LEVEL MEASUREMENTS IN WELLS DRILLED AT THE
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE3 WISCONSIN
September 19 - 203 1977
Date Depth to water below land surface
Well (Sept.) ("cm) ' (ft)
772401 20 142 4.7
772407 19 27 0.9
772419 20 143 4.7
772413 20 33.5 1.1
772440 20 42.7 1.4
772431 20 79.2 2.6
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13
the wells, all of which had been capped with a plastic cover, had been
vandalized and the well casing was broken off at or just above the
ground surface. As before, the depth to water level at each of the
wells was measured, this time using a steel tape [Table 4]. Then the
wells were purged to a depth of 4.6 m (15 ft) and left to recover before
sampling.
Also as noted during the previous visit, the well nearest the green
shed produced a black, greasy liquid during purging. Well 772407, which
produced no water during the earlier attempt at sampling, produced a
very muddy, thick liquid during purging.
During the October visit, samples were obtained by use of a hand-
powered diaphragm pump which was rinsed with acetone between sampling at
each well. Well 772407 was difficult to sample, probably because of mud
and clay blocking the slots in the casing. To get enough sample for
analysis, it was finally necessary to use a hand-operated bailer. The
sample contained about 1,000 ml of water and 900 g of clayey sediment.
The sample from the well nearest the green shed was brownish with
an iridescent sheen on the surface. The sample was not as dark or
greasy as the material removed when the well had been purged earler in
the day.
At sampling site 772452, about 31 m (100 ft) southwest of well
772440, the discharge from a small spring flowed through a small clump
of vegetation and then toward the Little Menomonee River. A small pond
had formed which was partially covered by an oily, iridescent sheen. As
the water came up out of the ground, a sample was taken.
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14
Table 4
WATER LEVEL MEASUREMENTS IN WELLS AND A SPRING AT THE
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN
October 19, 1977
Well Depth to water below land surface
cm ft
772401
101.60
3.3
772407
36.48
1.0
772419
93.98
3.1
772413
36.83
1.2
772440
34.29
1.1
772431
76.20
2.5
772452
Surface
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15
After sampling, all casings were pulled from the wells and removed
from the site. The holes were backfilled with a mixture of sand and
bentonite clay, and the survey stakes placed during the earlier site
visit were removed.
Soil Samples
Soil samples were collected from sites on the transects described
in Table 2. At each of the sites except the wells, a small coring
device was used to collect a surface sample. An auger was then used to
excavate a hole to an intermediate depth of 30 to 50 cm'(l to 1.6 ft)
where another core sample was collected. The holes were then deepened
with the auger to final depths varying between about 55 and 90 cm (1.8
to 3.0 ft) and again a small core sample was collected from the bottom
of each hole.
Analytical Procedures
The soil and water samples were analyzed for methylene chloride
extractables. In addition, the moisture content of the soils was deter-
mined. The methylene chloride extracts were also analyzed for the
presence of creosote compounds by gas chromatography.
Individual components of creosote were also confirmed in selected
samples by mass spectrometry. In all cases, unless otherwise indicated,
most of the methylene chloride extractable material was creosote.
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V. GEOLOGIC OBSERVATIONS AND ANALYTICAL RESULTS
The entire Kerr-McGee/Moss-American plant site is underlain by a
thick section [at least 17 m (55 ft)] of plastic, clayey glacial till
with a greater percentage of gravel material in the till section along
the eastern side of the plant site near the Little Menomonee River. The
till is locally overlain by a man-made fill and/or by a section of
organic peat. In the Kerr-McGee/Moss-American plant site, the till
showed evidence of horizontal openings filled with creosote to a depth
of at least 4.6 m (15 ft) in the undisturbed core samples. Groundwater
occurs in the till section throughout the entire area of the Kerr-
McGee/Moss-American plant site investigated. In humid areas such as in
the Milwaukee vicinity, the groundwater table configuration is char-
acteristically a subdued replica of the land surface which, at the
subject site, slopes north and east across the Kerr-McGee/Moss-American
site toward the Little Menomonee River. Groundwater and soil samples
obtained from the plant site indicated evidence of severe creosote
contamination, especially in the area of the former retort building. As
the groundwater and soil are known to contain creosote and the water
table slopes toward the Little Menomonee River, any movement will be in
this direction.
As reported in Table 5, the water samples collected from the
observation well (772401) near the retort contained 4,910 mg/1 of
methylene chloride extractables in the September sample and 99 mg/1
during the October sampling. Even higher concentrations of creosote
were noted in the water standing in the well. The suction line from the
well to the pump was coated with creosote adhering to the inside of the
pipe. Cores obtained from the surface 0.5 m (0 to 1.5 ft) and from
depths within the hole -- 3.0 to 3.5 m and 4.6 to 5.0 m (10 to 11.5 ft
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Table 5
ANALYTICAL RESULTS - WELL WATER SAMPLES COLLECTED AT THE
KERR-MC GEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN
Location Methylene Chloride Extractables
Well Description Sept. 20, 1977 Oct. 19, 1977
mg/1
772401
NE corner of green shed
4,190
99
772407
NE corner of area near RR
NS+
600++
772413
Northside center
ND+++
<2+++
772419
SE corner of area
NS+
<2+++
772431
Eastside center
ND++t
<2++t
772440
Center of area
20
9
772452 Spring sample, ^100 ft southwest
of 772440 - <2
t No sample obtained due to slow water level recovery after well
development and purging.
++ Value rounded off to nearest 100 mg/l. This sample contained a
considerable amount of very finely divided clay-like mud. An
1,800 ml slurry of this material was extracted. The slurry con-
sisted of about 1,100 ml of water and 900 g of mud. The moisture
content of the mud was 457o. A small amount of the methylene
chloride extractables in this sample was creosote. The majority
of the extractable material resembled a highly weathered heavy
fuel oil.
None detected above the detection limit of methylene chloride
extractables or_ no identification as creosote by gas chroma-
tography.
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18
and 15 to 16.5 ft) -- contained large amounts (2,400 to 7,900 mg/kg) of
methylene chloride extractables [Table 6].
It appears that there is a creosote layer, probably several inches
thick, at shallow depth in the retort area. In addition, heavier
fractions of creosote are apparently sinking through the groundwater to
greater depths.
Much of the creosote may be temporarily sorbed on the soil material
but a finite portion does move toward the Little Menomonee River. A
sample of groundwater obtained from well 772440, near the center of the
storage area, was found to contain 20 mg/1 of methylene chloride extract-
ables in the September sample and 9 mg/1 during the October sample. A
core sample, taken at a depth of 3.0 to 3.5 m (10 to 11.5 ft) from this
well showed no detectable level of creosote. Creosote was not detected
in water samples from any of the other wells except that during the
October sampling, the mud-water mixture from well 772407 contained a
high concentration of methylene chloride extractables which resembled
highly weathered heavy fuel oil. A fraction of this extract was found
to contain creosote components. This may be a result of the strong
tendency for creosote to adhere to the well casing and to the pump
suction line.
Analysis of the well core samples [Table 6] showed creosote at
depths more than 4.6 m (15 ft) below the surface and concentrations of
methylene chloride extractables as high as 23,700 mg/kg (2.37%). As
previously discussed, this creosote was visible and detected by appear-
ance and odor as the cores were removed from the split-spoon sampler.
The creosote had evidently percolated through the soil and the ground-
water surface to fill voids in the soil to at least the 4.6 m (15 ft)
depth.
The presence of creosote from soil samples [Table 6] is randomly
distributed throughout the area investigated. It reached a high of
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19
Table 6
ANALYTICAL RESULTS - SOIL AND WELL CORE SAMPLES AT THE
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE3 WISCONSIN
September 19-20} 1977
Methylene
% Chloride
Description Depth Moisture Extractable
(Dry Weight)
mg/kg
STATION NO. 772401
Green shed, well 0-1.5 ft 8.7 2,500
5-6.5 ft 24.2 ND'
10-11.5 ft 16.5 7,900
15-16.5 ft 10.6 2,400
STATION NO. 772402
Transect A, 105 ft from Station 772401 Surface 11.9 9,800
62 cm 17.5 15,400
90 cm 14.9 1,700
STATION NO. 772403
Transect A, 228 ft from Station 772401 Surface 13.8 9,200
35 cm 27.4 2,100
50 cm 35.5 11,100
STATION NO. 772404
Transect A, 351 ft from Station 772401 Surface 27.0 8,500
32 cm 53.5 4,300
82 cm 30.0 1,000
STATION NO. 772405
Transect A, 474 ft from Station 772401 Surface 39.0 5,900
35 cm 51.3 13,100
65 cm 45.5 4,200
STATION NO. 772406
Transect A, 597 ft from Station 772401 Surface 40.0 9,000
¦Mid-Depth 64.5 31,800
73 cm 60.4 3,800
STATION NO. 772407
NE corner of site, well 0-1.5 ft 20.1 23,700
5-6.5 ft 22.1 NDl
10-11.5 ft 12.7 NDT
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Table 6 (Continued)
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
20
Methylene
% Chloride
Description Depth Moisture Extractable
(Dry Weight)
mg/kg
STATION NO. 772408
Transect B, 145 ft from Station 772401 Surface 7.8 4,500
50 cm 12.6 4,400
69 cm 18.7 3,500
STATION NO. 772409
Transect B, 291 ft. from Station 772401 Surface 7.5 800
40 cm 22.7 4,800
69 cm 21.6 4,300
STATION NO. 772410
Transect B, 436.5 ft from Station 772401 Surface 16.0 5,300
42 cm 29.5 3,100
68cm 29.8 1,500
STATION NO. 772413
North side, well 5-6.5 ft 21.0 1,700
10-11.5 ft 16.6 NDT
STATION NO. 772414
12 ft north of Transect E, 207 ft
from Station 772401 Surface 13.3 71,000
38 cm 20.5 10,400
55 cm 18.2 34,300
STATION NO. 772415
12 ft north of Transect E, 414 ft
from Station 772401 Surface 12.2 12,900
50 cm 24.4 ND
60 cm 22.6 ND1
STATION NO. 772416
12 ft north of Transect E, 611 ft
from Station 772401 Surface 12.0 20,000
40 cm 15.1 5,300
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21
Table 6 (Continued)
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
Methylene
% Chloride
Description Depth Moisture Extractable
(Dry Weight)
mg/kg
STATION MO. 772417
12 ft north of Transect E, 808 ft from
Station 772401 Surface 4.9 1,300
30 cm 11.5 2,400
60 cm 13.9 2,200
STATION NO. 772419
SE corner of site, well 0-1.5 ft 17.7 ND
5-6.5 ft 9.8 NDl
10-11.5 ft 14.6 ND'
STATION NO. 772420
Transect H, NW corner of retort bldg Surface 18.3 40,200
50 cm 22.7 19,300
75 cm 18.5 13,600
STATION NO. 772421
Transect H, Midpoint of retort bldg
71 ft from Station 772401 Surface 17.1 10,500
47 cm 21.3 3,800
72 cm 24.4 2,200
STATION NO. 772422
Transect H, NE corner of retort bldg Surface 8.1 4,900
33 cm 21.1 6,200
73 cm 22.9 2,200
STATION NO. 772423
Transect G, Midpoint between 5th &
6th retorts on south facing side Surface 13.0 41,900
40 cm 19.7 2,900
72 cm 23.5 13,900
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Table 6 (Continued)
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
22
Descri ption
%
Depth Moisture
Methylene
Chloride
Extractable
(Dry Weight)
mg/kg
STATION NO. 772424
Transect G, Midpoint of 4th retort
from left on south facing side Surface
11.9
92,700
38 cm
25.8
127,000
63 cm
25.9
36,400
STATION NO. 772425
Transect G, Midpoint of 2nd retort
from left on south facing side Surface
2.4
104,000
38 cm
43.2
133,000
70 cm
38.7
89,900
STATION NO. 772426
Inside retort room, 40.3 ft from NE
corner, 2 ft from north wall Surface
5.0
72,900
70 cm
26.0
7,100
STATION NO. 772427
Inside retort room, 20 ft from NW
corner, 4 ft in from north wall Surface
3.3
279,000
60 cm
20.2
5,600
STATION NO. 772430
Transect F, 168 ft from Station 772419 Surface
52 cm
60 cm
8.4
23.9
22.4
2,400
4,1Q0
ND'
STATION NO. 772431
Transect F, 336 ft from Station 772419 Surface
30 cm
55 cm
9.9
41.0
38.5
1,900
2,800
ND'
-------
Table 6 (Continued)
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
23
Description
Depth
%
Moisture
Methylene
Chloride
Extractable
(Dry Weight)
mg/kg
STATION NO. 772431
Eastside center, well 5-6.5 ft 18.2 NDA
10-11.5 ft 19.4 ND
STATION NO. 772432
Transect F, 504 ft from Station 772419 Surface 27.0 11,200
36 cm 50.8 35,800
58 cm 47.2 NDr
STATION NO. 772433
Transect D, 75 ft from Station 772413 Surface 24.2 8,800
40 cm 31.8 ND;
41.8 ND'
STATION NO. 772434
Transect D, 168 ft from Station 772413 Surface 23.3 9,100
40 cm 32.2 1,700
70 cm 50.0 3,700
STATION NO. 772435
Transect D, 261 ft from Station 772413 Surface 33.3 19,700
40cm 50.8 1,000
70 cm 55.3 1 ,000
STATION NO. 772436
Transect D, 354 ft from Station 772413 Surface 30.2 10,200
50 cm 51.0 1,100
80 cm 58.5 15,600
STATION NO. 772437
Transect C, 152 ft from Station 772407 Surface 26.0 8,600
32 cm 74.5 11,000
65 cm 73.6 2,800
STATION NO. 772438
Transect C, 304 ft from Station 772407 Surface 25.0 1,900
52 cm 59.9 3,900
70 cm 58.5 3,100
-------
24
Table 6 (Continued)
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
Description
Depth
%
Moisture
Methylene
Chloride
Extractable
(Dry Weight)
mg/kg
STATION NO.
772439
14.9
38.9
60.4
900
25,300
21,100
Transect C, 456 ft from Station 772407
Surface
38 cm
70 cm
STATION NO.
772440
ft 13.5
ND+
Center of site, well
10-11.5
STATION MO.
772441
21.9
24.2
34.6
1,600
1,100
1,400
50 ft at 280° magnetic from a
point in the RR ditch 23 ft
downstream of the confluence
with the dock ditch
Surface
37 cm
72 cm
t ND - None detected above the detection limit of 500 mg/kg or no
identification as creosote by gas chromatography.
-------
25
279,000 mg/kg (27.9%) in a sample taken inside the retort room and was
greater than 100,000 mg/kg (10%) at depths up to 38 cm (15 in) below the
ground surface at sites outside the buildings.
The absence of creosote in some of the water samples collected and
the relatively low concentrations found in wells other than the one
nearest the green shed may be an indication of the low solubility of
creosote or the strong tendency for creosote to adhere to the well
casing and to the pump suction line. It may also be an indication that
the wells were placed at the edge of a plane of higher concentration of
contaminants. This latter possibility is thought most likely because
the wells could not be drilled in optimum locations due to poor surface
conditions which precluded ready access.
The high concentrations of creosote found in the groundwater and in
the soil at all levels, particularly at the surface, indicate that the
pollution of the Little Menomonee River will continue if corrective
measures are not taken. It seems likely that a ditch dug along the
north and east boundaries of the study area would intercept both ground-
water and surface runoff. The creosote thus intercepted could be removed
by skimming and sediment removal prior to release of the water to the
River. If soluble materials in the water orove to be a problem, it may
be necessary to treat the water with activated carbon prior to discharge.
-------
APPENDIX A
WELL LOGS, CASING AND PERFORATION RECORD
AND FIELD NOTES
9/19-20/77
-------
A-l
APPENDIX A
WELL LOGS, CASING AND PERFORATION RECORD AND FIELD NOTES, 9/19-20/77
KEY TO WELL LOGS
Fill, Cinders, gravel, clay and silt
Till, gray, clayey silt, peat, vari-colored clay
Gravel and sand, dense, sandy
Peat, dark gray
Total Depth
Record of casing depth and perforations.
Record of surface of water level. Other notes
on field logs are self-explanatory.
-------
( I ' '
a_2 :EPA Na' jnal Enforcement Investigations enter
I i Dnli Log !
111!
ProjJ-ct". Number:
Hcle ;'!¦ ,-!ser: •7724-07
Drill Method: cf
Depth Ft ' Log Water
• _ __ __ 1 _ . t
1 Project: /V^ /*/
iLocation: t>f fro* A-r fa;.-*-
_Drill Crew: >,/ jfr'/'W^-Geologist:
j j ; Date: <7/St/'777
lDescription¦ '
57771
C, / be^e /-*> , C~/«J f C4 gp f'ly
! i
cfiu£. j f -f~
-iv/'-i—
re*-/-
*"y^c/i,£i /-0 4/' / „
a e o
0 4 J'o
j\£ a;
I >v
^ *»J
3
CU ^ ^
A/o/e / 1Vo/e
7^
7Q
- W c ve\^, \, ^o^f//c
j fj6 r-J Lf c^r, //r>J
-------
EPA Na' jnal Enforcement Investigations .enter
| Drill Log I I
rroject Number:
iLocation\j£cor-, t:-' w/f r,
Drill Crew: 37'>\/
Geologist: /~( 0^> <
Date:, f j/
-------
A-4 i
, ' 1
¦EPA No onal Enforcement Investigation, Renter
Dril
Log
Project Number:
Hole Number: 77Z.4-P/
Project: Re f
Location: wei Co*¦,
Drill Method: C, P~ A<"/<-c Drill C rev/: 57-5 Geologist: /yW-fr c
. j : Date: er//?//c/V7
Depth tF'f* Log Water Description 1 I
; Lj —
^A~ --
10
ii "N
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? odio^X—
z°
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pjc15 it 1
i
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C. r* e d,>v '/c /
C r eat
5 /?e o
5> a >-/i
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C~t( T^tspoO'1 iiu-^pcC
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0'"
J2o-/Jo'-\ /S~ ^ o-f xec is y ecJ^e-f\£-
teYre'-iL of^
IS
<2 //to ; jTtf/ 2-
2^/7 /
&e /-y/<: f~
Lx//
//<*>
-------
EPA Na jnal Enforcement Investigat
I Drill Log
on. enter
A-5
rroject dumber: ,
uole Number: ~7YZ-^-/3
rill Method:
Project: a& |
Loca ti on~i fij
-4t-
rx
-tfS
1 ; ' ;
— Pc^fA yi.y, roo/j\
/ / 1 1
$ f & %-x./?. {€AA.
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c r JJ
77//y ¦*> ?/i f I
! t ~fo ; eyi/'-iy
/ ^ /«.> yC' <-
ti <.
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5 G c*
7
ff/ /^y p/ 5
VTt"
|_ ££//_f±.^r/. ? y f-/^ ^i'f(r f* J/2.f /
-------
j 'A-6
EPA Ng ona
Enforcement Investigation, ^enter :
Drill Log
I
Project Number:
Hole Number: 77Z-^<-hP
.Project: He rv/r ftAC£-ee' \ !
Location\ Ajc/?r?Y- 7>"
Drill MethocfT C F A<-Drill Crew: /*%¦<- Geologist: /c' ov$-r
i i Date:_£//f2Z£ZZ
Depth,' Log Water
—5-
/' o0Z
0-~"~
— o 0—
_ 0 "
c -
TPZO
_d
£
zo
iDescription
F^.'//yj ^ ist'v* /, (^[q y 5
77//,
c/<"r'f, i
' 7 ,/p/ - * *
f/Z-o/77S
I
^7i
a/ffisfe# | / /*/$>
-------
\ j I
,EPA Na .onal Enforcement Investigation- -enter
I j Drill Log
A-7
n-oject Number: L
ile Number: /'
\K,r- - *<
Ocl$V
Ce//
-------
APPENDIX B
CHAIN-OF-CUSTODY PROCEDURES
-------
B-l
ENVIRONMENTAL PROTECTION AGENCY
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
CHAIN OF CUSTODY PROCEDURES
June 1, 1975
GENERAL
The evidence gathering portion of a survey should be characterized by the minimum
number of samples required to give a fair representation of the effluent or water body
from which taken. To the extent possible, the quantity of samples and sample loca-
tions will be determined prior to the survey.
Chain of Custody procedures must be followed to maintain the documentation necessary
to trace sample possession from the time taken until the evidence is introduced into
court. A sample is in your "custody" if:
1. It is in your actual physical possession, or
2. It is in your view, after being in your physical possession, or
3. It was in your physical possession and then you locked it up in a manner so
that no one could tamper with it.
All survey participants will receive a copy of the survey study plan and will be
knowledgeable of its contents prior to the survey. A pre-survey briefing will be held
to re-appraise all participants of the survey objectives, sample locations and Chain
of Custody procedures. After all Chain of Custody samples are collected, a de-briefing
will be held in the field to determine adherence to Chain of Custody procedures and
whether additional evidence type samples are required.
SAMPLE COLLECTION
1. To the maximum extent achievable, as few people as possible should handle
the sample.
2. Stream and effluent samples shall be obtained, using standard field samplinq
techniques.
3. Sample'tags (Exhibit I) shall be securely attached to the sample container
at the time the complete sample is collected and shall contain, at a minimum,
the following information: station number, station location, data taken,
time taken, type of sample, sequence number (first sample of the day -
sequence No. 1, second sample - sequence No. 2, etc.), analyses required and
samplers. The tags must be legibly filled out in ballpoint (v/aterproof ink).
4. Blank samples shall also be taken with preservatives which will be analyzed
by the laboratory to exclude the possibility of container or preservative
contamination.
5. A pre-printed, bound Field Data Record logbook shall be maintained to re-
cord field measurements and other pertinent information necessary to refresh
the sampler's memory in the event he later takes the stand to testify re-
garding his actions during the evidence gathering activity. A separate
set of field notebooks shall be maintained for each survey and stored in a
safe place where they could be protected and accounted for at all times.
Standard formats (Exhibits II and III) have been established to minimize
field entries and include the date, time, survey, type of samples taken,
volume of each sample, type of analysis, sample numbers, preservatives,
sample location and field measurements such as temperature, conductivity,
-------
B-2
DO, pH, flow and any other pertinent information or observations. The
entries shall be signed by the field sampler. The preparation and conser-
vation of the field logbooks during the survey will be the responsibility
ot the survey coordinator. Once the survey is complete, field logs will be
retained by the survey coordinator, or his designated representative, as a
part of the permanent record.
6. The field sampler is responsible for the care and custody of the samples
collected until properly dispatched to the receiving laboratory or turned
over to an assigned custodian. He must assure that each container is in his
physical possession or in his view at all times, or locked in such a place
and manner that no one can tamper with it.
7. Co]ored slides or photographs should be taken which would visually show the
outfall sample location and any water pollution to substantiate any con-
clusions of the investigation. Written documentation on the back of the
photo should include the signature of the photographer, time, date and site
location. Photographs of this nature, which may be used as evidence, shall
be handled recognizing Chain of Custody procedures to prevent alteration.
TRANSFER OF CUSTODY AND SHIPMENT
1. Samples will be accompanied by a Chain of Custody Record which includes the
name of the survey, samplers' signatures, station number, station location,
date, time, type of sample, sequence number, number of containers and analy-
ses required (Fig. IV). When turning over the possession of samples, the
transferor and transferee will sign, date and time the sheet. This record
sheet 31 ous transfer of custody of a group of samples in the field, to the
mobile laboratory or when samples are dispatched to the NEIC - Denver labora-
?S6n transferring a Portion of the samples identified on the sheet to
the field mobile laboratory, the individual samples must be noted in the
column with the signature of the person relinquishing the samples. The field
laboratory person receiving the samples will acknowledge receipt by siqmnq
in the appropriate column. v * 5,ynm9
2' custodian or field sampler, if a custodian has not been assigned,
?n JhSa™ . F»P°nfibimy of properly packaging and dispatching samples
nf ruetnH r ^0ru ?!^yu analysis. The "Dispatch" portion of the "Chain
of Custody Record shall be properly filled out, dated, and signed.
3. Samples will be properly packed in shipment containers such as ice chests to
avo,d breakage The shipping containers will be padlocked for shipment to
the receiving laboratory.
4. All packages will be accompanied by the Chain of Custody Record showing iden-
^"•iTk t;e.cont«nts* The ori'9lnal win accompany the shipment, and a
copy will be retained by the survey coordinator.
5. If sent by mail, register the package with return receipt requested. If sent
by common carrier, a Government Bill of Lading should be obtained. Receipts
nl°? r£S' 0 ^reS' ^ll1s lfldln9 will be retained as part of the perma-
nent Chain of Custody documentation.
6. If samples are delivered to the laboratory when appropriate personnel are not
there to receive them, the samples must be locked in a designated area within
the laboratory in a manner so that no one can tamper with them. The same per-
son must then return to the laboratory and unlock the samples and deliver
custody to the appropriate custodian.
-------
B-3
LABORATORY CUSTODY PROCEDURES
1. The laboratory shall designate a "sample custodian." An alternate will be
designated in his absence. In addition, the laboratory shall set aside a
"sample storage security area." This should be a clean, dry, isolated room
which can be securely locked from the outside.
2. All samples should be handled by the minimum possible number of persons.
3. All incoming samples shall be received only by the custodian, who will in-
dicate receipt by signing the Chain of Custody Sheet accompanying the samples
and retaining the sheet as permanent records. Couriers picking up samples at
the airport, post office, etc. shall sign jointly with the laboratory custodian.
4. Immediately upon receipt, the custodian will place the sample in the sample
room, which will be locked at all times except when samples are removed or
replaced by the custodian. To the maximum extent possible, only the custo-
dian should be permitted in the sample room.
5. The custodian shall ensure that heat-sensitive or light-sensitive samples,
or other sample materials having unusual physical characteristics, or re-
quiring special handling, are properly stored and maintained.
6. Only the custodian will distribute samples to personnel who are to perform
tests.
7. The analyst will record in his laboratory notebook or analytical worksheet,
identifying information describing the sample, the procedures performed
and the results of the testing. The notes shall be dated and indicate who
performed the tests. The notes shall be retained as a permanent record in
the laboratory and should note any abnormalties which occurred during the
testing procedure. In the event that the person who performed the tests is
not available as a witness at time of trial, the government may be able to
introduce the notes in evidence under the Federal Business Records Act.
8. Standard methods of laboratory analyses shall be used as described in the
"Guidelines Establishing Test Procedures for Analysis of Pollutants,"
38 F.R. 28758, October 16, 1973. If laboratory personnel deviate from
standard procedures, they should be prepared to justify their decision dur-
ing cross-examination.
9. Laboratory personnel are responsible for the care and custody of the sample
once it is handed over to them and should be prepared to testify that the
sample was in their possession and view or secured in the laboratory at all
times from the moment it was received from the custodian until the tests
were run.
10. Once the sample testing is completed, the unused portion of the sample to-
gether with all identifying tags and laboratory records, should be returned
to the custodian. The returned tagged sample will be retained in the sample
room until it is required for trial. Strip charts and other documentation
of work will also be turned over to the custodian.
11. Samples, tags and laboratory records of tests may be destroyed only upon the
order of the laboratory director, who will first confer with the Chief,
Enforcement Specialist Office, to make certain that the information is no
longer required or the samples have deteriorated.
-------
B-4
EXHIBIT I
EPA, NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
Station No. | Date
^'me 1 Sequence No.
Station Location
Grab
Crimp
o
_BOD
.Solids
_COD
-Nutrients
_MeJals
—Oil and Grease
J3.0.
.Bact.
-Other
Samplers:
Remarks / Preservative:
Front
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER.
DENVER, COLORADO 80225
Back
-------
EXHIBIT II
SURVEY, PHASE , DATE
rYPE OF SAMPLE
STATION
NUMBER
STATION DESCRIPTION
TOTAL VOLUME
TYPE CONTAINER
PRESERVATIVE
NUTRIENTS J
- 009
Q
o
u
TOC
TOTAL SOLIDS
SUSPENDED SOLIDS ,,
ALKALINITY
O
o
>
*
X
a
CONDUCTIVITY*
K
•
UJ
Cki
ID
>—
<
CXl
UJ
Q
5
UJ
TOTAL COLIFORM "
w
o
IL.
o
u
3
UJ
u_
TUPBIDITY C
OIL AND GREASE
K
wo
<
~—
UJ
s
BACTI "
PESTICIDES c
HEPB
trace organics
phenol
1
(
(
•
-
I
¦
¦
ne 11 a ovc
I
CJ1
-------
EXHIBIT III
Samplers:
FIELD DATA RECORD
Gage Hf
or Flow
Ft. or CFS
CONDUCTIVITY
u mhos/cm
TEMPERATURE
NUMBER
STATION
-------
EXHIBIT IV
B-7
ENVIRONMENTAL PROTECTION AGENCY
Office Of Enforcement
national enforcement investigations center
Building 53, Box 25227, Denver Federal Center
Denver, Colorado 80225
CHAIN OF CUSTODY RECORD
SURVEY
STATION
NUMBER
STATION LOCATION
DATE
TIME
SAMPLE TYPE
SEQ
NO
NO OF
CONTAINERS
ANALYSIS
REQUIRED
Water
Air
Comp
Grab
•
«
SAMPLERS: /Signature)
Relinquished by: fSigno/orej
Received by: fSignafureJ
Dafe/T ime
Relinquished by: (S tgnaturc)
RcCGlVod by: /Signature/
Date/Ti
imc
Relinquished by: (Signaturej
Received by: fSignafurej
Date/Time
Relinquished by: [SignofureJ
Received by Mobile Laboratory for field
analysis: {SignatureI
Date/Time
Dispatched by I (Stgnofurej
Date/Time
Received for Laboratory by:
Date/T
ime
Method of Shipment:
Distribution: Orig. — Accompany Shipment
1 Copy—Survey Coordinator Fiold File*
GPO «5« - »
-------
APPENDIX C
SOIL AND WATER SAMPLE ANALYSES
-------
C-l
CONFIRMATION OF CREOSOTE IN WATER AND SOIL SAMPLES
FROM THE KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN BY
GAS CHROMATOGRAPHY/MASS SPECTROMETRY
Analyses of the water extract and soil extract from Kerr-McGee
confirming creosote were completed. The samples were screened initially
on the flame ionization gas chromatograph, then analyzed utilizing
combined gas chromatography/mass spectrometry (GC/MS). The gas chroma-
tograms readily confirmed the presence of creosote when the chromato-
gram of the standard was compared to the water sample extract and the
soil extract. The major sample components in samples and standard all
occurred in the same ratio. The mass spectra of the individual com-
pounds in the standard creosote mix and standard spectra of individual
compounds run using the same instrumental conditions as the samples
were perfect matches and all were confirmed by mass spectrometry and
matching gas chromatography retention times. Table I gives the results
for the samples and the standard mix.
TABLE I
Compound
GC/MS Identification
Commercial Sample Sample
Creosote 2311 2240
Local Soil Water
Napthalene
2-methylnaphthalene
1-methylnaphthal ene
Biphenyl
1,3-dimethylnaphthalene
Acenaphthene
Dibenzofuran
Fluorene
Anthracene
CF
CF
CF
CF
CF
CF
CF
CF
CF (1)
CF CF
CF CF
CF CF
CF CF
CF CF
CF CF
CF CF
CF CF
CF CF
CF CF
CF CF
(Phenanthrene)
Carbazole
2-methylphenanthrene
Fluoranthene
Pyrene
CF (2)
CF
Good (3)
CF
CF
CF CF
CF CF
Good Good
Note: CF - confirmed
-------
These compounds confirmed by GC/MS identification, GC/MS of
standards, and coincidence of retention times with those of
standards.
Phenanthrene and anthracene have identical mass spectra and the
gas chromatography retention times are only slightly different,
with phenanthrene eluting later. It appears as a definite shoulder
on the anthacene peak with the GC conditions used when more dilute
solutions are run. Both compounds are obviously present.
This compound was identified by mass spectrometry only. A standard
was not available.
-------
C-3
ANALYTICAL METHODOLOGY - SOIL, WELL CORE AND GROUNDWATER
SAMPLES COLLECTED SEPTEMBER 19-20, 1977 AT THE
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN
On September 23, 1977, 6 water and 113 soil samples were received at
the NEIC Laboratory for creosote analysis. All samples were handled
according to chain-of-custody procedures. The waters and soils were
analyzed for methylene chloride extractables and the soils for moisture
content. The methylene chloride extracts were also analyzed for the
presence of creosote compounds by gas chromatography. The results are
summarized in Tables 5 and 7 in the body of the report.
Methodology:
A. Moisture
About 10 grams of thoroughly mixed sample was accurately weighed in
a tared 50 ml beaker and dried overnight in an oven at 105°C. The water
loss was determined by reweighing the cooled and desiccated beakers.
Calculations:
Wt. of water loss x 100 = % moisture
Wt. of sample wet
B. Methylene Chloride Extractables
Soils - 10 grams of thoroughly mixed soil was weighed into a 150 ml
beaker. Large stones, twigs, leaves, etc. were avoided. 30 grams of
granular anhydrous sodium sulfate was added to the beaker and the soil
and sodium sulfate were mixed thoroughly to obtain a coarse granular
consistency. The mixture was then transferred to a 33 x 80 mm cellulose
extraction thimble and placed in a Soxhlet extractor. 200 ml of methy-
lene chloride was placed in a 500 ml flat-bottomed flask and attached to
the extractor. The extractor was allowed to cycle for 2 to 3 hours,
with a rate of about 10 cycles per hour. Each flask was then placed on
a rotary evaporator and the solution was concentrated to a volume of
about 20 ml. The remaining solvent was quantitatively transferred to a
tared 50 ml beaker and evaporated to dryness on a warm hot plate under a
gentle stream of carbon-filtered air. Each beaker was reweighed and the
residue determined. Results were calculated on a dry weight basis using
% moisture values.
Wt. of residue in mq x 1000 =
Wt. of sediment extracted wet (gm) x wt fraction solids
mg/kg dry basis
wt fraction solids = 1.00 - wt fraction moisture
-------
C-4
Waters - From 100 ml to 3 liters of the water samples were extracted
twice with 100 ml of methylene chloride. The extracts were combined and
evaporated to dryness in tared beakers on a warm hot plate under a gentle
stream of carbon-filtered air. Each beaker was reweighed and the residue
determined.
C. Creosote Compounds
Creosote is a complex mixture of compounds, some of which can be
detected on a flame ionization gas chromatograph. These compounds give
a distinctive pattern of peaks. This pattern was used to identify the
presence of creosote.
The methylene chloride extracts were dissolved in 10 ml of acetone
and an aliquot was injected on a Hewlett-Packard 5700A gas chromatograph
equipped with an automatic sampler. Chromatograms were compared with a
"standard" creosote sample that was purchased locally. The standard
creosote sample was labelled as containing 60% creosote by weight. The
sample was cut with a light refined petroleum-based oil.
Some samples with methylene chloride residues as high as 7,000
mg/kg showed no creosote pattern by gas chromatography. These resi-
dues could be caused by either "natural background" material, non-
creosote compounds which have been extracted by methylene chloride, or
creosote compounds which are not chromatographable. The samples which
contained detectable amounts of methylene chloride residue, but which
exhibited no creosote pattern, were reported as None Detected.
-------
C-5
ANALYTICAL METHODOLOGY
GROUNDWATER SAMPLES COLLECTED OCTOBER 19, 1977 AT THE
KERR-MCGEE/MOSS-AMERICAN PLANT SITE
MILWAUKEE, WISCONSIN
On October 21, 1977 seven plant site well samples were delivered to
the laboratory in accordance with NEIC chain-of-custody procedures. The
samples were analyzed for total methylene chloride extractables and the
extracts screened by flame ionization detection - gas chromatography
(FID-GC) to determine the presence of creosote material.
FID-GC analysis showd that samples from Stations 772413, 772419,
772431, and 772452 did not contain any observable creosote material. All
other samples contained observable amounts of creosote. The results of
these analyses are presented in Table 5 in the body of the report.
Methodology:
A. Moisture
About 10 grams of thoroughly mixed sample was weighed in a tared 50
ml beaker and dried overnight in an oven at 105°C. The water loss was
determined by reweighing the cooled and desiccated beakers. Calculations:
Wt. of water loss x 100 = % moisture
Wt. of sample wet
B. Methylene Chloride Extractables
Waters - From 1,000 ml to 3.5 liters of the water samples were
extracted twice with 100 ml of methylene chloride. The extracts were
combined and evaporated to dryness in tared beakers on a warm hot plate
under a gentle stream of carbon-filtered air. Each beaker was reweighed
and the residue determined.
C. Creosote Compounds
Creosote is a complex mixture of compounds, some of which can be
detected on a flame ionization gas chromatograph. These compounds give
a distinctive pattern of peaks. This pattern was used to identify the
presence of creosote.
The methylene chloride extracts were dissolved in 10 ml of acetone
and an aliquot was injected on a Hewlett-Packard 5700A gas chromatograph
equipped with an automatic sampler. Chromatograms were compared with a
"standard" creosote sample that was purchased locally. The standard
creosote sample was labelled as containing 60% creosote by weight. The
sample was mixed with a light refined petroleum-based oil.
-------
C-6
G.C. Conditions
Instrument: Hewlett Packard Model 5700
equipped with a dual flame ionization detector and
automatic sampler
Column: 2mm ID X 3.3 M stainless steel
6% 0V-101 on 60/80 GCQ
Instrument Conditions: Carrier Gas - Helium - 25 ml/min flow
Oven temp: 80°C-230°C programmed at 8°C/min
with hold at 230°C for 16 min.
Injector: 250°C
Detector: 250°C
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