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CHEMICALS
INDUSTRIES
TO FROM
See Distribution
INTEROFFICE/ LAKE CHARLES
DATE SUBJECT
November 5, 1975 HCB-HCBD Survey
On September 4th and 5th Midi-rest Research Institute conducted an HCB-HCBD Survey in and around the Lahe Charles Plant. In addition to assisting the MRI team, the Laboratory also sampled and analyzed air, water, soil, and stream sediment for KCB and HCBD. A more detailed description of sampling and analytical procedure will be prepared in E=64\
Following are sample location nomenclature used in the appended data:
AX - Air sample adsorbed on Tenax
/ID - Air sample adsorbed in Dccane
AC - Air sample adsorbed on Carbon tTVv *" tt,o, ... knP ____Ji_L_C
D - Soil Sample (Composite)
S - Sediment Sample
Numerical notations refer to locations on the attached map.
MW:EG:rw
Att.
Distribution
H. J. Iloencs, Jr. T. Taylor C. A. Burns
SL 049342
HCB and HCBD in Environmental Samples
Air*
Location **2 AX **2 AD
Date/Time 9-^-75/115 thru
HCB/ ^c/M^
HCBD, hr/M3
< 0.02, < 0.02 < 0.02, < 0.02
9-5-75/1150
0.09, 0.09
4.2, 3.6
2 AC
EDC MC Tri Per Total
60
75 60 65 2S0
**5 AX
9-4-75/IIO6 thru < 0.02, <0.02 < 0.02, < 0.02
**5 AD 5 AC
9-5-75/1138
0.05, 0.10
* Weather data available in LD-l6o4
** Duplicate analyses.
1.3, 1.0
Other, Ug/M'3
VDC EDC MC Tri TCE Per Total
25 30
55 30
55 50
205
Water (9-4-75)
Description
HCB, ppb
HCBD, ppb
Water into Incinerator Scrubber
None Detected None Detected
Incinerator Scrubber Effluent Outfall
9 None Detected
PPC Canal at Mobil Bridge No. 1
2 12
Area "B" Effluent into Trap
22 16
Area "B" Effluent Outfall
22 lb
PPG Barge Slip Surface Water Over NE Landfill
None Detected 104
0.4 22
SL 049343
Description
Landfill Area Composite
4D, 5P> 7D Composite
8D, 9D, 10D Composite
Columbia-Southern Road Right-Of-Way, South of PPG - Composite
(\7
50,000 120 28
1, ^:00 600 129
194 45,000
Sediment (9-4-75)
Description
HCB, ppb v/v
PPG Canal Sediment at Mobil Bridge No. 2
120
Area "B" Effluent Sediment at Outfall
1,100
PPG Barge Ship Sediment at West Bank
None Detected
HCBD, pub w/w 120 444 46
SL 049344
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Midwest Research Institute Kansas City
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Sampling Methods
--'
--- . .
Air, water, soil, sediment, and aquatic organisms will be considered as potential sampling media. The production process and waste disposal techniques used will determine which of the above media will be sampled.
Air Sampling - Ground-level area sources such as open lagoons will be sam pled at two or three points along the downwind boundary of the source using vertical line grids of three samplers each. The shape of measured downwind concentration profiles will be analyzed to determine if the downwind bound ary of the source is, in fact, the point of maximum ground level air qual ity impact.
During each test, source activity and meteorological conditions will be monitored on site. Wind speed and direction will be measured contin uously. Other meteorological measurements will be made as required for the determination of atmospheric stability by the method of Turner. Descrip tions of source activity will include the amount of waste material trans ferred to the disposal site or processed by the disposal technique. Samples of waste material will be collected for laboratory determination of physical and chemical properties.
The sampling train for collection of HCB and EC 3D In the ambient air will consist of the following items assembled in the order given: (a) probe (directed into the wind); (b) membrane filter for collection of par ticulate matter; (c) column of Tenax^ GC resin for collection of vapor; (d) calibrated flow meter; and (e) pump. The filter and Tenax1^ plug will be self contained in holders which can be easily disconnected from the sam pling train and replaced with unused madia. Several sampling heads posi tioned in relatively close proximity to each other may be operated from a single pump. Portable gasoline-powered generators or battery powered pumps will be used to move the air through the sampling trains.
Samplers will be positioned in any array downwind of the source and at a location upwind to determine the background concentration. Spatial dis tribution of samplers will depend upon the source configuration. All sam plers will be operated simultaneously during a given run. Sampling time will be as short as possible (1/2 to 2 hr) to allow for the conduct of a test under relatively constant meteorological conditions. Sampling rates will be set to allow collection of detectable mass from atmospheres contuinLng minimal concentrations of HCB and/or HCBD.
In the case of an elevated point source such as an incinerator stack, samplers will be positioned laterally in groups of three (with intakes at 2 ill above grade) at two or three distances downwind in the vicinity of the maximum receptor point. The location of the maximum receptor point will be
SL 049346
estimated by the application of a mathematical model which describes the dispersion of the source effluent under the prevailing meteorological con ditions.
Mathematical models of atmospheric dispersion phenomena will be used to estimate the maximum ground level pollutant concentration which may occur in the vicinity of the disposal sites. In other words, the model will be used to predict the intensity of possible pollution episodes. (An episode is defined as a period greater than 1 day during which atmospheric ventil ation is at a minimum.) For an assumed (constant) rate of emissions the model extrapolates the set of measured concentrations and corresponding meteorological conditions to predicted concentrations corresponding to meteorological conditions of highest pollution potential for the geograph ical area. MRI has available in-house EPA1s UNAMAP system of models recom mended for various source configurations, concentration averaging times, and conditions of restricted dispersion.
Water Sampling - If wastes are channeled into rivers, streams, or lakes following treatment, or simply disposal of wastes in sealed lagoons is em ployed, the water will be sampled to establish the concentration gradient from the source. Sampling stations will be set up at upstream and down stream, i.e., above and below the waste inflow. Samples collected from upstream will be used as controls. If time and budget allow, it is de sirable to locate two or three sampling stations above the waste inflow to establish the rate at which unstable material, if any, is changing. A series of sampling stations will be set up downstream so as to establish the course of contamination of ECB and KCBD throughout a reach of the stream. Stations will be spread at intervals based on time-of-vater travel rather than distance. Surface floats or organic dyes, such as Rhodamine WT, can be followed downstream and timed for known distances to determine time-of-water travel. Sampling station(s) will also be set at marked changes in physical characteristics of the stream.
Water will be sampled directly with a commercial sampler (Sirco Port able Sampler Model No. MK-VS7) or by passing the water through Amberlite XAD-4--) resin at a metered flow rate. As recommended by Kittrell, samples will be taken at either 5 ft or mid-depth, whichever is less. The collec tion of quiet or even stagnant water of a quality that does not represent that of the main flow will be avoided. Sampling points usually are estab lished at approximate quarter points, or equal intervals across the width of the stream. The equal intervals will be across the main current rather than across the entire width of the river. If a stream is too wide, such as the Mississippi, Missouri, Ohio, or Tennessee, sampling may prove to be time-consuming; a single sample at the midpoint of the main current will be adequate.
SL O49347
Sampling frequency per sampling station will be determined by the waste discharge rate, current velocity, temperature stability, and other relevant factors. All these can only be determined after the presampling visit to the particular industrial plant. In general, an ideal schedule would be hourly sampling for a 24-hr period. This would provide 24 samples at each station. These samples can be combined prior to analysis to achieve maximum information concerning pollutant discharge within the time-cost limitations of the program.
Sediment Sampling - Sediment samples will be collected at each point where water samples are taken. A modified Peterson dredge will be used for col lecting sediment samples. This sampling device essentially picks up sur face sediment up to 6 in. deep. It is believed that penetration of chlor inated organic hydrocarbons such as HCB and KCBD should not go beyond 6 in.
Soil Sampling - Soil samples will be taken to assess HCB and HCBD levels due to landfill waste disposal techniques, particulate settling, vapor condensation from ground or elevated sources, and contamination from run off of surface wattr or open waste ditches.
T
A number of core samples will be taken to determine the vertical con centration profile of the pollutants. It is not probable that HCB and HCBD migrate into the soil because of their low water solubility. Surface sampling (to 6 in.) will probably be satisfactory, but this will be veri fied by the analysis of selected core samples.
Where possible, soil samples will be taken to correspond with air samples. Soil upwind (controls) and downwind of ground level and elevated sources will be sampled.
Sample Handling
No matter what sampling medium is employed, the samples will be kept at 4 to 6"C to preserve the integrity of HCB and HCBD. Upon receipt of the samples at MRI, they will be stored in a refrigerated storage room, at a constant temperature of 5C, until ready for analysis.
Water samples will be stored in 1-liter glass bottles with Teflonlined caps. The bottles will be marked, dated, and individually kept in Styrofoam containers to prevent breakage. If an Amberlite XAD-4coluntn is used for water sampling, the column will be capped and stored intact until ready to be analyzed. Sediment and soil samples, like water samples, will be stored in glass bottles and treated exactly as water samples. Aquatic samples will be wrapped In aluminum foil, and kept frozen until analysis.
SL 049348
Sample Analysis
For each air sample, the millipore filter, as well as the Tenax GC resin are extracted separately in an ultrasonic bath, each with three por tions (20, 20, 10 ml) of pesticide grade n-hexane (Matheson, Coleman, and Bell) for a period of 10 min, and made up to the mark of a 50 ml volumetric flask.
The soil samples are first sifted on a U.S, Standard No. 18 sieve to remove stones and other foreign material. A known amount of each of the samples is then weighed and extracted with n-hexane in a Soxhlet overnight. Each extract is made up and stored in 100 ml volumetric flasks.
For water samples, the grab samples are extracted with two 20-ml vol umes of n-hexane followed by one 10-ml volume of n-hexane using a 500 ml separatory funnel. The three extracts are combined and made up to the mark in a 50 ml volumetric flask.
Amberlite XAD-4 resin is Soxhlet extracted three times, each with 500 ml of n-hexane. 1 The first two volumes are combined for analysis and the third is analyzed separately to check whether the extraction was com plete .
During the analysis dilution or concentration of the samples is per formed, if necessary, in order to bring the instrument response to within the linear range of the calibration curve.
Instrumentation
A Microtek-2000R gas chromatograph equipped with an electron capture detector (tritium) is used. The output of the gas chromatograph is con nected to a Hewlett-Packard 3380a integrator-recorder, which features the printout of the chromatogram with integrated areas of individual peaks and respective retention times. A 4 ft x 1/4 in. glass column packed with 1.57, OV-17/1.957,, SF-1 coated on 100/120 mesh Supelcoport la used as the primary column for the analysis, while a 6 ft x 1/4 in. glass column packed with 37. XE-60 coated on 80/100 mesh chromosorb UHP is used to verify and differ entiate HCB from cy-BHC .
For lOO analysis, the chromatographic operating conditions arc: in
jector temperature, 200C; column temperature, 100C; detector temperature,
180C; carrier flow rate, 50 ml/min
purge flov rate, 90 ml/min N^; and
detector voltage, 10 V DC,
SL 049349
For RGB analysis, the chromatographic operating conditions are the same
as those for the analysis of KC3D except that the column temperature is
maintained at 150C; carrier flow rate, 100 ml/min
and purge flow rate,
90 ml/min
Calibration Curves
A 10 ng/nl composite standard solution of RCB and HCBD is used to ob tain the calibration curve. The standard solution is prepared by dilution of a stock solution made up from EPA reference standards obtained from Pesticides and Toxic Substances Effects Laboratory, National Environmental Research Center, Research Triangle Park, North Carolina. Concentration ranges chosen for the calibration curve are from 10 to 60 pg, and linearity is observed.
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Jo
19 20 21 22 23 24 25 26 27 ' 28 29 30 31 32 33
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36
RE:
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SL 049420
FOPM CS-4 *EV.\o/1/54
ENGINEERING DEPARTMENT
1 : 2 3 4 S 6 7 8 9 10 II 12 13 14 15 16 17 18 19 20 21 22 23 24 25 : 26 27 28 29 30 31
3
4
5 6
7
8
9 10 11 12 13
14 15 16 17
f
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..................... ^ y lDl,lC ~)bO -K^
iX . , ,
^S/ih
20
21
22
23 2O0c
24
25 26
27
28
/Dot
I'D fb^-
29 Tl&
30
31 11
32 33 34
36
RE
SL 0*9*21 Job No.
FORM. CS -4 .KPV. 10/1/54
rn`f s
ENGINEERING DEPARTMENT
12 3 4 5 6 7 8 9 10 11 12 ' 13 M 15 16 17 18 - 19 20 21 22 23 24 : 25 26 27 28 29 30 3'.
# ......................................... A/K CPimx. CAU^LWnOMs. GMI^iOkL ^ou/eC-TS
..
3 ....................... i/grp zcKu&ficzs
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21 22 23 24 25 26 27 28 29 30 31 32 33 34
36
RE:_
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-------------------------------------- ~~..................................... ~ _________________________ JohNo.^SL 049422
FORV.CS-4 HEV.1U/I/54
?
IS
ENGINEERING DEPARTMENT
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6
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22
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25 CP ibOSPn) -77/at /S
26
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36
RE:
Job No SL 049423
FORM. CS-4 REV. 10/1 /54
1 2 3 4 S 6 7 8 9 10 11 12 13 14 IS 16 17 18 : 19 20 21 22 23 24 25 26 27 28 29 30 31
2
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s~o 6/*m' u.hu>th>ik>^ -rat /,33 ^
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14
15
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17 Y?6AUUJV.
19
.(433 /i%^)(3nt) =
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20
21
22
23
24
25 26
27, 28 29 30 31
32 33 34
4
36
RE:
SL 049426
Jnh No.
FOw <-S - 4 rw. v . | O - I / b4
inC ,*;.{ n
ENGINEERING DEPARTMENT
1 2 3 4 5 6 7 8 9 10 1 1 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 3!
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.
I - etCKy C pftys
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17
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= *tQlFr% f\cr/aufL
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32
33
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36
RE;.
SL 049427 Job No..
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FORM .CS-4 REV. J0 /1 /5 4
SL 049430
2-7*/ PC^ SZJtU&d&Z
smec
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12 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 3!
3; 4
5
\
6
7
8:
9;
10
11 12
13 :
14 15
15
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19 20 21 22 23 24 25
26 fe
27 28 29 30 31
32 33 34
i
36
RE:
stack j>m
srtiwQ
Cp. 3-/7-
V/Z SC/Z+f.
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- O/C --
SL 049431
.lob i\o_____
, roR".cs-4 '>"v 10/1/54
.
m* |1 mJSm
- ENGINEERING DEPARTMENT
12 3 4 5 6 7 8 910 11 1213 14 15 16 17 1819 20 21 22 23 24 25 26 27 28 29 30 31
2 : 2-7^
L/snrrs
s-mv/Lnaz.
3 . '..................
................................. `............................ S72-SCPH,,^
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4 ................. )(
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8
QS71 SCPH^f ) Csz/WwJ =2.
V7
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10 n 12 13 14 15 16 17-
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19 20 21 22 23 24 25 26 27 28 29 30 31
32 33 34
3f-> PrV/toi. J
V................................................
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36
RE:
--
SL 049432 *
i 'v
ENGINEERING DEPARTMENT
2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 : 19 20 21 22 23 24 25 26 27 28 29 30 31
.3 ; 4 5
6
7 8 9. 10 11 12 13 14 15 16 17
t
20 21 22 23 24 25 26 27 28 29 30 31 32 33 34
36
RE:
--V.r7
4 sybZfuP
................................
...................... ....................
Srzrer For? Ul>U/hU.y Wo OF- -T&\*> fZArt~
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SL 049433
Joh iNo.
rORM ,Ci> - 4 RES' .10,1/54
12
56
. T6C g/l fit/ ENGINEERING DEPARTMENT
10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 . 27 28 29 30 31
3 4 5
6
7 8 9 10
12
13 14 15
16
17
20 21 22 23 24 25 26 27 28 29 30 31 32 33 34
36
RE:
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. /or
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....................... 3, Q& L&
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SL 049434 Job No.
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34
ENGINEERING DEPARTMENT 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 ! 26 27 28 29 30 3 1
C/W.CULflTIptJS T=D& C&NC&vT&fitOOfiJ pr PQeia*mrjr <$/&>/*J
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21 22 23 24 25 26 27 28 29 30 31
32 33 34
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RE:
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SL 049438
Job No.