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NIC ENVIRONMENTAL SCIENCES ICO./OIV./OEPT./LOCATIOWI
SPECIAL STUDY rrvpe or report)
REPORT
REPORT NO.: JOB/PROJECT NO.:
OATE:
TITLE:
authors:
ES-83-SS-13 43-000-760.56-8700094 September 28, 1983
CONCENTRATION OF POLYCHLORINATED BIPHENYLS IN SAMPLES FROM CHOCCOLOCCO CREEK
P. R. Michael and R. 6. Kuehnel
CONCENTRATION OF POLYCHLORINATEO BIPHENYLS IN SAWLES
FROM CHOCCOLOCCO CREEK
abstract:
Composite sediment samples were collected from eight different sites along a 1-3/4 mile seg ment of Choccolocco Creek. Sediments were extracted and analyzed by gas chromatography/ mass spectrometry (GC/MS). PCB concentrations ranged from 2.1 g/g to 19.2 ug/g and averaged 9.9 vg/g.
DISTRIBUTION:
W. J. Adams - NIB I. L. Brown - 1060 D. E. Cayard - C3NC R. L. Cheever - 1060 J. H. Craddock - B3KA W. E. Gledhill - N3A T. J. Hoogheem - NIB P. R. Michael - NlE J. G. Nassif E2ND
R-inmi
MOMS 022879
ES-83-SS-I3 Page 1
CONCENTRATION OF POLYCHLORINATED 8IPHENYLS IN SAMPLES FROM CHOCCOLOCCO CREEEK
INTRODUCTION
At the request of state and federal authorities to the Monsanto plant in Anniston, Alabama, Monsanto Company agreed to provide assistance for collect ing and analyzing sediments from Choccolocco Creek. This report describes the results of the analysis of the sediments for polychlorinated biphenyls (PCB's).
SUMMARY
Composite sediment samples were collected from eight different sites along a 1-3/4 mile segment of Choccolocco Creek. Sediments were extracted and ana lyzed by gas chromatography/mass spectrometry (GC/MS). PCB concentrations ranged from 2.1 ug/9 to 19.2 ug/9 and averaged 9.9 ug/g.
DETAILS
Sailing - Samples were collected on September 20, 1983 as described In the attached Sampling Plan (Appendix I) by a team composed of representatives from Monsanto, the Alabama Department of Environmental Management, and the United States Department of Agriculture Soil Conservation Service. By mutual agree ment of the sampling team members, minor deviations were made from the Sampling Plan. They consist of:
1. Samples were collected In reverse order; l.e., beginning at the conflu ence of Snow and Choccolocco Creeks and working downstream on Choccolocco Creek to the Highway 21 bridge.
2. At one site, sampling was done in duplicate Instead of triplicate.
3. Two field blanks were prepared Instead of one.
4. Sample labeling was slightly different from that described In the Sampling Plan.
Copies of all quality assurance forms associated with sample collection are contained In Appendix II.
Analysis - Samples were analyzed according to method ES-B0-M-28, `Determination of Polychlorinated Biphenyls In Soil and Sediment*. Briefly, after sieving through a two millimeter sieve, 10 g portions of each sample were extracted with 10 mL Isooctane using a Polytroom Ultrasonic Homogenlzer. The phases were separated by centrifugation and the extracts were analyzed using GC/HS in the selected ion monitoring mode. The GC/MS was calibrated with standard solutions containing monochloroblphenyl, Aroclorm 1242, Aroclor 12S4, and Aroclor 1260. Monochloroblphenyl, not Included In method ES-80-M-28, was measured by starting the 6C temperature program at a lower temperature (100*C) and monitoring m/z 188 and 153.
HONS 022880
ES-83-SS-13 Page 2
Results - Results of the analyses are listed In Table 1. Concentrations are calculated on a wet weight basis. The samples are listed in order of collectlon. The first sample. 9-20-83-1-A, was at the confluence of Snow and Choccolocco Creeks and the last sample, 9-20-83-8-A, was at the Highway 21 bridge. The detection limits listed in Table 1 are equivalent to the lowest calibration standard. In all cases, they produced signal to noise ratios much greater than 2:1.
Quality Assurance - Results of the two duplicate samples collected at site *6 agree very closely, 5.8 vs 5.4 ug/g, which Indicates representative sampling.
The sample collected at site 44 was subdivided Into three portions in the analytical lab to assess method precision. The relative standard deviation of the analyses (assuming the three subsamples were Identical) was 325. An additional portion of the sample from site 44 was spiked with Aroclor 1254 at 30 ug/g. Recovery was 1121. A sample of Florissant/Ray soil (used for field blanks) was spiked with Aroclor 1254 at 6 ug/g and gave a recovery of 741. No
PCB's were detected in either of the field blanks or In the laboratory blank.
REFERENCES
All raw data can be found on the following notebook pages and In the associ ated file folders.
Notebook Pages
P. R. Michael
2431085
R. 6. Kuehnel
2550087
W. J. Adams
1835103-33
HONS 022 881
T
Table 1. Concentration of Polychlorinated Biphenyls In Sediment Samples from Choccolocco Creek
Environ. Science Log Nianber
Sample ID
Mono
3092201
9-20-83-1-A
(0.038)
3092202
9-20-83-2-A
0.60
3092203
9-20-83-3-A
(0.016)
3092204
9-20-83-4-A
0.13
3092205
9-20-83-5-A
0.50
3092206
9-20-83-6-A
0.17
3092207
9-20-83-6-C
(0.087)
3092208
9-20-83-7-A
0.48
3092209
9-20-83-7-FB-l ND
3092210
9-20-83-7-FB-2 ND
3092211
9-20-83-8-A
0.32
ui 0.49 3.6 0.21 0.66 3.3 1.1 0.57 2.8 ND NO 1.8
Chloroblphenyl 1Concentration (uq/g)
Trl
latra
Henta
Hexa
3.1 5.8 4.1 3.2
4.8 3.1 1.4 1.2
0.44
0.49
0.61
0.34
1.6 1.7 1.2 0.99
5.0 3.6 1.6 1.3
1.4
1.3
0.62
0.54
1.2
1.3
0.89
0.78
3.5
1.9
0.92
0.80
ND ND ND ND
ND ND ND ND
2.6
1.3
0.53
0.43
Hepta 2.5 0.73 ND 0.58 0.90 0.64 0.53 0.54 NO ND ND
Detection Limit
0.1
0.08
0.2
0.2
0.3
0.1
NO 1 None Detected ( ) Represent positive detections but are less than the lowest calibration standard.
0.4
total 19.2 15.4
2.1 6.9 16.2 5.8 5.4 10.9 ND ND 7.0
7 8 8 7 7 0 SNOW
ES-83-SS-13 Page 3
Submitted by: Prepared by: Approved by:
ES-83-SS-13 Page 4
Monsanto Industrial Chemicals Company Environmental Sciences Section - N1E 800 North Lindbergh Boulevard St. Louis, Missouri 63167
Research Group Leader
fdmtedhill
Manager, Environmental Sciences
HONS 022803
ES-83-S5-13 Page 5
APPENDIX I SAMPLING PLAN
HONS 022884
CH0CC010CC0 CREEK SAMPLING PLAN
nuiy o, ltzj
I. PURPOSE At the request of the Alabama Department of Environmental Management
(ADEN) and the United States Department of Agriculture Soil Conservation Service (USDA-SCS) to the Monsanto Anniston plant, Monsanto Company has agreed to provide technical assistance In collecting and characterizing sediments from Choccolocco Creek. This assistance was requested to assure proper disposal of sediment dredged from the creek. The section of Choccolocco Creek under study extends from the Alabama Highway 21 bridge upstream to the confluence with Snow Creek. The characterization will concern the identification of any possible polychlorinated biphenyl (PCH) content which might be present In the sediment to be dredged and removed from this stream segment. II. SAMPLE COLLECTION STRATEGY
Eight stream width/depth composites will be collected along the approximate 1.75 mile stream segment study area. Composites will be collected beginning at the Highway 21 bridge and at approximately 0.25 mile Intervals, ending at the confluence of Choccolocco Creek and Snow Creek. (See Figure 1 for approximate location of sampling sites.) Each width/depth composite will be made up on three individual depth cores taken at three equidistant locations across the width of the stream. Each depth core will represent a maximum 30 inch depth composite of bottom sediment dredge material.
HONS 022865
Page 2
III. COLLECTION EQUIPMENT Sediment cores will be collected in 3 foot coring tubes with a tube
diameter of 1 inch. These coring tubes will be made up of 3 - 1 foot sections threaded together. The coring tubes will be driven into the sediment via a driving pipe; the pipe will also screw onto the top of the 3 foot coring tube. A small sledge hammer will be used to drive the driving tube/coring tube assembly. The coring tubes will be constructed of cast iron as will the driving tube. The coring front edge of each tube will be sharpened to affect easier sample collection. A horizontal hole will be drilled through the top of the driving tube. A metal rod will be placed through the hole to facilitate removal of the driving tube/coring tube assembly from the sediment.
A stainless steel tray will be used to composite the three individu al 30 inch sample cores collected at each sampling site. If necessary, an 18 inch long, 1 inch diameter plunger rod will be used to evacuate the core from the three 1 foot coring tube sections. IV. COLLECTION PROCEDURES
The following collection procedure will be utilized at each of the eight sampling sites. Separate coring tubes will be used at each site to avoid cross contamination between sites. Each coring tube will have been detergent washed and distilled water and acetone rinsed before use in the field.
Upon reaching the sampling site, a marker will first be placed on a suitable landmark (tree, power/phone pole, etc.) to serve as a semi-permanent benchmark for future references. Next, the creek area will be visually surveyed to identify the most representative creek width
HONS 022886
Page 3
In view of the landmark. The selected river width will then be physical ly surveyed to determine the ability to collect the required samples. Bottom sediment will be examined for sand/soil/rock content. If deemed suitable for coring, the creek width will then be visually quartered. The borders of the first and second, second and third, and third and fourth quarters will be the three coring stations for the sampling site. This is shown in Figure 2. Station 1 will always be thd left most station facing upstream. Compass bearings will be taken from Station 1 to the landmark and to the center of the stream facing upstream
Figure 2.
Station
. Station
Station
To Fix the Station for Future,Reference.
The core at Station 1 will be taken by again facing upstream,
assembling the three 1 foot coring sections and the driving tube and
hammering the apparatus to a maxmium of 30 Inches or as deep as is
physically possible. The rod will be placed through the driving tube and
the entire assembly removed. A rubber stopper will be placed over the
top of the driving tube which will assist in retaining the sediment in
the coring tube.
MONS 022887
Page 4
After removal, the driving tube will be removed and the coring tube placed In the stainless steel compositing tray. The three 1 foot coring tube sections will be separated and the sediment removed from each section. If the sediment does not readily fall out of the tubes, the rod plunger will be used to force the sediment into the tray. A stainless steel spatula will be used to completely mix the sediment in the tray for a minimum time of 1 minute. It is extremely important that the sediment bo as homogeneous as possible in order that reproducible/identical samples can be taken from the tray. . After removal of the sample, the coring assembly will be cleaned in creek water, reassembled, and moved to Station 2. The collection and mixing procedure will be repeated at this Station and Station 3. The same coring assembly will' be used at all three stations; new coring assemblies will be used at each sampling site. V. SAMPLE HANDLING
After all three cores from a site have been composited in the mixing tray, large rocks, twigs, etc., will be discarded and the sediment mixed for an additional 1 minute. A stainless steel spatula will be used to transfer the homogenized sediment to two, precleaned 16 oz wide mouth jars, filling each approximately two thirds full. (The jars will have been precleaned by washing in warm soapy water followed by rinsing with deionized water and acetone and heating at 175*C for 24 hours.) Acetone rinsed aluminum foil will be placed over the mouth of the jar and the jar will be sealed with a polyethylene lined plastic cap. Additional sedi ment remaining in the tray will be discarded. The tray and all utensils will be washed with creek water and rinsed liberally with acetone.
MQNS 022888
Page 5
Each sample will be labeled with a unique identification code using a waterproof label and waterproof marking pen. The sample identification code will be patterned after the following example:
6-8-83-1-A-I
where
6-8-83 date of sample collection
1 site #
A * designation for half of the composited sediment
from a site. The other half of the sediment would be designated B.
1 sediment replicate number when applicable.
As described in the Quality Assurance section,
sediment will be collected in triplicate at one site.
The field blank (see Quality Assurance section) will also use the above
code except the A or B will be followed by "BLANK". The site number in
the field blank code will be the site at which the field blank is pre
pared. After labeling, the samples will be placed in a waterproof poly
ethylene bag and stored on ice in an insulated cooler. When the field
work is completed, "A" samples will be sent by overnight carrier to the
following address for PCB analysis.
Monsanto Company
800 North Lindbergh Blvd.
St. Louis, Ho. 63167
Attn: Paul R. Michael
Mail Zone - N1E
MONS 022889
Pag 6
The "B* samples will be retained by the USDA Soil Conservation Service
(SCS) and the Alabama Department of Environmental Management (AQEM) for
analysis by Dr. Patrick Morgan at the Auburn Pesticide laboratory. To
maintain sample identity, the samples should be analyzed as soon as
possible and should be kept refrigerated or frozen at all times prior
to analysis.
'
VI. QUALITY ASSURANCE - SAMPIIHG
To assess precision, sampling at one mutually agreed upon site will
be conducted in triplicate. At this site, three traverses of the stream
will be made and the composited sediment from each traverse will be
treated as an entirely separate sample.
A field blank will be taken at approximately the halfway point of
the sampling operation. The field blank will consist of soil previously
analyzed and shown not to be contaminated with PCB's. The soil will be
carried into the field, placed in the mixing tray and stirred, trans
ferred to a container, and preserved and shipped with the rest of the
samples.
At each site, quality assurance Form II will be completed to de
scribe the site and the conditions at the site at the time of sampling.
At each site, after the sediment cores have been composited, the sample
code and description of the sediment will be entered on Quality Assurance
Form 12. To provide for chain of custody. Quality Assurance Form 13 will
be used by the sampling personnel to demonstrate sample transmittal to
and receipt by the appropriate analytical laboratory. VII. analysis
Sediment samples sent to Monsanto will be analyzed by method ES-fiC-
M-Z8, "Determination of Polychlorinated Biphenyls in Soil and Sediment.
MONS 022090
Page 7
In this method, PCB's ere extracted from the sample and measured by
selected ion monitoring gas chromatography/mass spectrometry. The
average recovery of di- through heptachlorobiphenyl is 76S and the
precision (relative standard deviation) is 20X. The quality assurance
steps in sample analysis will include analyzing 10* of the samples in
triplicate to determine precision, spiking 10% of the samples with known
levels of PCB's to determine accuracy, and analyzing laboratory blanks to
demonstrate the absence of laboratory contamination.
VIII. PI.erOMNEL/EQUIPMEnT RESPONSIBILITY
A six person team will be used to complete the sampling. Monsanto
Company, the USDA SCS, and the AOEM will each provide two individuals.
Each individual is responsible for his/her own personal gear such as
gloves, boots, hip waders, etc. The SCS will supply a work boat suitable
for carrying field equipment and supplies. Monsanto will supply the
collection equipment Including sample containers, shipping containers,
chain-of-custody forms, preservatives, etc. ADEM will be responsible for
first aid supplies. A complete list of needed equipment and provision
responsibility is given in Table I.
IX. SCHEDULING It Is imperative that sampling be done at or near low flow stream
conditions since access to the sampling sites is by walking/wading only.
In addition, sample collection will be most easily accomplished at low
flow conditions. For this reason, a two week "window of time" will be
established by the team members during which sampling can be done by all
members. ADEM and SCS members will be responsible for calling the best
two day sampling period within this "window" based on stream flow and
predicted weather conditions. This two week "window" is tentatively
identified as September 12-23, 1983.
HONS 022891
Page 8 Once the two day sampling period is identified, Monsanto, SCS, and ADEH personnel will be on site and ready to begin within two days of notification. Members will meet at the Holiday Inn, Anniston, Alabama, at the scheduled time. Although sampling should be completed In one day, the sampling period will be established as two days to allow for any potential collection decisions/problems. IX. REPORTING Monsanto will prepare a final report describing collection, analy sis, QA/QC, and shipping procedures including results and all applicable field and QA/QC forms. SCS and ADEM will provide Monsanto with a report describing analytical results obtained on their portion of the split samples.
HONS 022892
TnM<; I. Equipment List (Tentative)
Boat Coring Tubes Driving Tube Staple Containers Shipping Containers Coapas-, Chaln-of-Custody Fonts Labels Collection Tray Spatula Landmark Markers First Aid Waders Gloves Coots Etc. Etc. Etc.
.
Page 9
. '
SCS HON HON HON Hon HON HON HON HON HON SCS ADEM ALL ALL ALL
HONS 022893
PERSONNEL SAMPLING____________ !__________________________________ ____________________________
RIVER STAGE
- FLOW RATE __________________________________TIDE CONDITIONS_____
SAMPLE SITE NAME _SAMPLE SITE NUMBER
SAMPLE COLLECTION METHOD USED DATE OF METHOD
Drawing of transect at each site and station 1 identification. (Record prominent landmarks and compass bearings).
CommentsTweatiler'condidons, problems with sampling, etc.]
HONS 022S94
QUALITY ASSURANCE FOR,'! 12
SEDIMENT SAMPLES Hater
*Conments arc required on the physical appearance of the sediment, i.e., color, coarseness
sand, clay, silt, gravel, etc., and on the presence or absence of benthic organisms and
if possible, which type of organisms are present.
.
HONS 022895
. QUALITY ASSURANCE FORM #3 SAMPLE TRANSMITTAL LETTER
Client
Project Title
Dte shipped
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Shipped by
Shipped from_________________________________________________________________________ __
Shipped to_____________________________ Attention of _____________________________
Additional shipping information or comments _________________________________
Semple description code
Comments
Semples received by _ Date samples received _ Return letter received
HONS 022896
ES-83-SS-13 Page 6 APPENDIX II SAMPLE COLLECTION QUALITY ASSURANCE FORMS
MOMS 022898
MONSANTO COMPANY
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SAMPLE SITE NAME j* J.
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Comments are required on the physical appearance of the sediment, l.e., color, coarsenes , sand, clay, silt, gravel, etc., and on the presence or absence of benthic organisms and if possible, which type of organisms are present.
HONS 022900
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QUALITY ASSURANCE FORM #4 - MIC-NATIONAL AqUATIC MONITORING PROGRAM
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MONSANTO
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Additional shipping information or comments __________________________________________________
Sample description code__________________________________________________________ Comments
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<>-30-11*-a-a_________________ '___________________________ ;_________________________________
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QUALITY ASSURANCE FORM 13 - MIC-HATIONAL AQUATIC MONITORING PROGRAM
Sample Description Code Date
SEDIMENT SAMPLES
Time
Water Depth(m)
Comments*
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Coewents are required on the physical appearance of the sediment, i.e., color, coarseness, sand, clay, silt, gravel, etc., and on the presence or absence of benthic organisms and if possible, which type of organisms are present. MONS 022903
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SAMPLE SITE NAME
SAMPLE SITE NUMBER
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SAMPLE COLLECTION METHOD USED (HUMBER)
DATE OF METIIOO
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HONS 022904
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N? 1835113
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Sample Description Code Date 9 -d?0-65'3-/J
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Sample Description Code Date
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Time
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MONSANTO COMPANY -- /&-
N? 1835119
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Consents (weather conditions, problems with saapllng, etc.)
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HONS 022910
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MONSANTO COMPANY
N? 1835125
cc
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lasg^L
QUALITY ASSURANCE FORM 13 - MIC-NATIONAL AQUATIC MONITORING PROGRAM
Sample Description Code Date
9i#-3J
SEDIMENT SAMPLES
Time
Mater Depth(m)Comnents*
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eu.-t/iArnti ofjen. i
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`Comments are required on the physical appearance of the sediment, i.e., color, coarseness, sand, clay, silt, gravel, etc., and on the presence or absence of benthic organisms and If possible, which type of organisms are present. HONS 022911
C&yL
MONSANTO COMPANY
N? 1835127
QUALITY ASSURANCE FOgM >1 - MIC-HATIOHAL AQUATIC HONITORING PROGRAM
PERSONNEL SAMPLING /dtt/t**.
/______________________________________
*IVER STAGE A- .;.f *
FLOW RATE TIDE CONDITIONS__________________
'\HPLE SITE NAME SAMPLE COLLECTION KETHOO USED (NUMBER)
SAMPLE SITE NUMBER 7 DATE OF METHOD
Drawing of transect at each site and station I identification. (Record prominent landmarks and compass bearings).
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loanentT (weather conditions, problems with sampling, etc.)
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MONS 022912
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MONSANTO COMPANY CstfoCteLLQCcj) &&# ' (C
N? 1835129
QUALITY ASSURANCE FORM 13 - MIC-NATIONAL AQUATIC MONITORING PROGRAM
Jfufle Description Code Date
SEDIMENT SAMPLES
Time
Water Depth(m)
Coements*
1
t!
<J3- 7-rt f-Jo Si
?' 7-& f-Jo-Si 3:s-o
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7~0 SCS 70 sos
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`Coaaents are required on the physical appearance of the sediment, i.e., color, coarseness, sand, day, silt, gravel, etc., and on the presence or absence of benthic organisms and If possible, which type of organisms are present. ' MOMS 022913
AO Aaao WMOMTOOO *
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MONSANTO COMPANY
N? 1835131
CieCCe/.*-'-
AT
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1NCANKO av (tICNATUNKI {/u.
I OATS
v- 7o - 1 _
QUALITY ASSURANCE FORM #1 - NIC-NATIONAL AQUATIC MONITORING PROGRAM
PERSONNEL SAMPLING
P1VER STAGE
J
^-r.AMr'iv <-. FLOW RATE
TIDE CONDITIONS _______ uu
'.AMPLE SITE NAME SAMPLE SITE NUMBER A SAMPLE COLLECTION METHOD USED (NUMBER)
___________________ DATE OF METHOO
Drawing of transect at each site and station 1 identification. (Record prominent landmarks and compass bearings).
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t
CoSSntT (wcither conditions, problems with sampling, etc.)
Oo 3.
HONS 022914
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Cke^-Ucco
MONSANTO COMPANY
k
PftCPAMCO Y HlCNATU*f>
N? 1835133
QUALITY ASSURANCE FORM 13 - MIC-NATIONAL AQUATIC MONITORING PROGRAM
Simple Description Code Pate
SEDIMENT SAMPLES
Time
Water Depth(m)Conments*
f-M-rs-f- ft
4^\ /o" s*~
^
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1
I- 2p
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'Comments ere required on the physical appearance of the sediment, l.e., color, coarseness, sand, clay, silt, gravel, etc., and on the presence or absence of benthic organisms and if possible, which type of organisms are present. HONS 022915
I