DEQp00022491

DuPont Automotive
CERTIFIED MAIL - RETURN RECEIPT REQUESTED
Mr. Gregory Nizich
NC DEHNR - DEM
Water Quality Section
Permits & Engineering Unit
P. O. Box 29535
Raleigh, NC 27626-0535
RE: Renewal of NPDES Permit No. NC0003573
Nafion® Process Wastewater Discharge to Outfall 002
Dear Mr. Nizich,
DuPont Automotive
P.O. Drawer
Fayetteville, NC 28302
March 15, 1996
Z
"I
This letter is to provide you information to modify the referenced NPDES Permit to allow for the
non -biodegradable Nafion® process wastewater to be discharged directly to Outfall 002, thereby
bypassing the site's Wastewater Treatment Plant (WWTP), or to be discharged to the WWTP as
is done currently.
The reason for this requested modification is that future expansions of the Nafion® area will
unnecessarily increase the hydraulic loading to the WWTP, with no benefit to the environment by
treating the non -biodegradable wastewater in the WWTP.
Enclosed are two updated wastewater flow diagrams which should replace the current diagrams
submitted with the NPDES Permit Renewal Application. These updated flow diagrams show the
two alternate routes for the non -biodegradable Nafion® process wastewater.
To characterize the Nafion® wastewater, both physical testing and aquatic toxicity testing were
performed on 24-hour composite samples taken of the Nafion® HFPO Process Scrubber and
Waste Gas Scrubber effluents, the main source of process wastewater from the Nafion® area.
SUMMARYi
Both the Nafion® HFPO Process Scrubber and Nafion® Waste Gas Scrubber _,4ave no
measurable BODS value, do exhibit measurable COD and Fluoride levels, and e it acce b�ggb
aquatic toxicity levels at the worst-case concentration at Outfall 002. 30-
--9
E. I. du Pont de Nemours and Company ® Printe rm Recycled Paper
Z-544 Rev. 8/95

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
Page 2
The testing indicates a high TSS level for the HFPO Process Scrubber effluent, which had a large
amount of salt crystals after neutralization with sulfuric acid,. Analysis of those crystals show
that they are potassium sulfate, which has a solubility in water of 12% by weight. Since this
scrubber effluent would be less than 0.05% of the Outfall 002 flow, these salts would be
completely dissolved, thereby eliminating the TSS concern.
Our NPDES permit requires monitoring of BODS, COD, Fluoride, and Bioassay at Outfall 002,
so the above parameters would be monitored under the existing permit requirements. The
OCPSF Priority Pollutants are currently monitored only at Outfall 001, so monitoring of the
Nafion@ wastewater which bypasses the WWTP may be required for the appropriate OCPSF
Priority Pollutants.
A second Nafion@ Waste Gas Scrubber is being installed as part of a new Vinyl Ethers Process
expansion. The effluent from this new scrubber should be identical to the existing Waste Gas
Scrubber, therefore it, as well as all future non -biodegradable, non-toxic wastewaters should be
allowed to bypass the WWTP.
If this site elects to bypass the Nafion@ wastewater around the WWTP, it will undoubtedly be
done with a pipeline, therefore any required monitoring will be simplified. The permit should be
writ -ten so that any monitoring is required only when Nafion@ wastewater is bypassing the
WWTP.
BASIS FOR TESTING CONCENTRATIONS
The performed tests were based on two potential operational schemes. The two schemes evalu-
ated were:
1) Bypassing the Nafion@ HFPO Process Scrubber effluent around the WWTP and
discharge it directly to the site's woodlined ditch which is discharged as Outfall 002,
and discharge all other Nafion@ process wastewater streams to the WWTP and
ultimately through Outfall 001; or
2) Bypassing both the Nafion@ HFPO Process Scrubber and Nafion@ Waste Gas Scrubber
effluents around the WWTP and discharge them directly to the site's woodlined ditch
which is discharged as Outfall 002, and discharge all other Nafion@ process wastewater
streams to the WWTP and ultimately through Outfall 001.
The anticipated flows for the two subject scrubber effluents following an upcomm e
the HFPO process, and the three-year low flow condition for Outfall 002 are as foll
J i.; i- SO 1996
CENTRAL FILES

Is
Mr. Gregory Nizich Page 3
NC DEHNR
March 15, 1996
1) The Nafion@ HFPO Process Scrubber normal daily flow = 5,330 gal/day
2) The Nafion@ Waste Gas Scrubber normal daily flow = 5,760 gal/day I �,0q0 5?4,
3) The Outfall 002 low flow condition = 11.83 MGD
The contribution of the two process streams to Outfall 002's flow is obviously very small.
All physical analyses were performed on the undiluted scrubber effluents.
The 48 -hr acute toxicity testing was performed on process samples diluted with laboratory water
to a concentration representative of the ratio of normal process flow(s) to Outfall 002 low flow.
No additional dilution was taken for the dilution effect of the Cape Fear River.
The 7 -day chronic bioassay testing was performed on process samples diluted with Outfall 002
composite effluent to a concentration representative of the ratio of normal process flow(s) to
Outfall 002 low flow. The bioassay testing was then performed at both a 3.3% dilution (the test
concentration specified on our NPDES Permit) and at a 6.6% dilution (twice the concentration
specified on our NPDES Permit).
PHYSICAL TESTING RESULTS
The results of the physical analytical testing of the scrubber effluents are presented in Table 1.
Both the HFPO Process Scrubber and Waste Gas Scrubber effluents exhibit no measurable level
of BODS. This is expected since the Nafion@ manufacturing area produces only fluorocarbon
compounds which should be totally non -biodegradable. The absence of BODS material supports
our request to allow this material to bypass the WWTP.
Both scrubber effluents exhibit levels of COD and TOC. Using the highest measured
concentrations and the normal scrubber flows, the COD discharge from the two scrubbers would
be approximately 400 lb/day. The permit currently requires monitoring of COD at Outfall 002
on a monthly basis. We feel this frequency is adequate to monitor the COD discharge in the final
effluent.
As described in the summary, the high TSS level for the HFPO Process Scrubber effluent results
from the formation of potassium sulfate as a by-product of the pH adjustment using sulfuric acid.
The dilution of this waste stream with the other streams comprising Outfall 002 will completely
dissolve the potassium sulfate salts, thereby eliminating the TSS concern. The lowed TSS'result
for the February 13, 1996, sample is believed to be the result of incomplete mixing 1,suspend
the salts in the neutralized sample.
L JUL SO 1996
CENTRAL FILES

r'
Mr. Gregory Nizich
NC DEHNR
March 15, 1996
Page 4
The BFPO Process Scrubber effluent contains from 2% to 3% fluoride, and the Waste Gas
Scrubber effluent contains approximately 1% fluoride. After the upcoming HFPO Process
expansion, the combined fluoride discharge from these two scrubbers would be approximately
2,400 lb/day, which is well below the permitted limit of 5,000 lb/day fluoride. Fluorides are non -
biodegradable, and only a small amount of the fluorides are retained in the sludge, therefore
virtually all of the fluorides currently entering the WWTP are discharged in the treated effluent to
Outfall 002.
AQUATIC TOXICITY TESTING RESULTS
To ensure that the two subject scrubber effluent streams are not toxic to aquatic organisms, both
acute and chronic testing using both invertebrates (ceriodaphnia) and vertebrates (fathead
minnows) were performed with the HFPO Process Scrubber effluent separately, and with a
mixture of both the HFPO Process Scrubber and the Waste Gas Scrubber effluents.
The 48 -hr acute toxicity testing dilution series was based on a concentration representative of the
ratio of normal scrubber flow(s) to the Outfall 002 low flow. For the HFPO Process Scrubber
effluent, the worst-case concentration was 0.00045 (5,330 gal/day - 11.83 MGD). For the
combined HFPO Process Scrubber and Waste Gas Scrubber effluents, the worst-case
concentration was 0.00094 ((5,330 gal/day + 5,760 gal/day) _ 11.83 MGD). No additional
dilution was taken for the Cape Fear River.
The acute testing was performed on 24-hour composite samples of the two scrubber effluents
taken on January 30, 1996 and on February 13, 1996. The results of the January 30th testing
were used to better define the dilution series for the February 13th testing.
Table 2 and Table 3 give the results of the acute testing using the HFPO Process Scrubber
effluent. The ceriodaphnia was the more sensitive species, with the January 30, 1996, test
indicating an LC50 of 0.00084 volume Scrubber/volume diluent versus the worst-case
concentration of 0.00045 volume Scrubber/volume diluent. The January 30, 1996, test of
Fathead Minnow had an LC50 of 0.00257 volume Scrubber/volume diluent versus the worst-case
concentration of 0.00045 volume Scrubber/volume diluent.
Table 4 and Table 5 give the results of the acute testing using the combined BFPO Process
Scrubber and Waste Gas Scrubber effluents. The ceriodaphnia was again the more sensitive
species, with the February 13, 1996, test indicating an LC50 of 0.00148 volume
Scrubbers/volume diluent versus the worst-case concentration of 0.00094 volume
Scrubbers/volume diluent. The January 30, 1996, test of Fathead Minnow ha
0.00540 volume Scrubbers/volume diluent versus the worst-case concentration''
volume Scrubbers/volume diluent.
JUL 30 1996
CENTRAL FILES

y
Mr. Gregory Nizich
NC DEHNR
March 15, 1996
Page 5
The acute toxicity testing summary sheets from Burlington Research are attached as supporting
documentation.
The North Carolina 7 -day chronic bioassay testing using ceriodaphnia dubia was also based on
the worst-case concentration representative of the ratio of the normal scrubber flow(s) to the
Outfall 002 low flow. For the chronic testing, the Outfall 002 24 -hr composite sample was used
as the diluent. The HFPO Process Scrubber effluent worst-case concentration was 0.00045
(5,330 gal/day _ 11.83 MGD). The combined HFPO Process Scrubber and Waste Gas Scrubber
effluents worst-case concentration was 0.00094 ((5,330 gal/day + 5,760 gal/day) _ 11.83 MGD).
The chronic bioassay testing was then performed at both a 3.3% dilution (the test concentration
specified in our NPDES Permit) and at a 6.6% dilution (twice the concentration specified in our
NPDES Permit).
Table 6 gives the results of the chronic bioassay testing for the two tests conditions. In both the
January 30 and February 13, 1996, testing, both the HFPO Process Scrubber effluent, and the
combined HFPO Process Scrubber and Waste Gas Scrubber effluents, passed at the 3.3% and the
6.6% concentrations.
The chronic bioassay testing summary sheets from Burlington Research are attached as
supporting documentation.
CONCLUSION
The physical testing of the Nafion@ HFPO Process Scrubber and Waste Gas Scrubber effluents
shows there is no benefit gained by treating these waste streams in this site's biological treatment
facility. Furthermore, the measured parameters of these effluents show that the current permit
limits established at Outfall 002 are adequate if the two scrubber effluents are bypassed around
the WWTP and are discharged directly to Outfall 002.
The NPDES Permit may need to include a new annual monitoring requirement for the bypassed
Nafion@ wastewater for the appropriate OCPSF Priority Pollutants. Otherwise, the current
permit requirements for Outfall 002 would be sufficient to adequately monitor pollutants from
the Nafion@ wastewater.
Aquatic toxicity testing of the subject scrubber effluents indicate that they are not toxic even at
the worst-case concentrations described in this letter.
Therefore, we request that the renewed NPDES Permit include language to allow for this site to
discharge the non -biodegradable Nafion@ process wastewaters either through the Wastewater
Treatment Plant (Outfall 001 and Outfall 002) or directly to Outfall 002. -
JUL 30 1996
CENTRAL FILES

1'
Mr. Gregory Nizich
NC DEHNR
March 15, 1996
Page 6
Based on the above, I hope that you are satisfied that enough information has been submitted to
allow for this permit modification.
If you have any questions, please feel free to call me at [phone].
Enclosures
Michael E. Johnson
Environmental Coordinator
1,
JUL 3b 1996
CENTRAL FILES

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
m
TABLE 1
PHYSICAL TESTING RESULTS
NAFION® HFPO PROCESS SCRUBBER EFFLUENT
Page 7
DATE
BODS
(m /L)
COD
(m /L)
TOC
(m /L)
TSS
(m )
FLUORIDE
(m )
12/13/95
<2
677
---
---
21,000
01/04/96
<2
2,070
---
---
20,400
01/30/96
<2
1,010
3,480
4,300
28,000
02/13/96
<2
928
3,160
361
32,900
NAFION® WASTE GAS SCRUBBER EFFLUENT
DATE
BODS
(m /L)
COD
(m )
TOC
(m )
TSS
(m )
FLUORIDE
(m )
01/30/96
<2
6,390
2,760
25
10,500
02/13/96
<2
204
409
67
8,620
ht: ;
JUL .' •96
CENTRAL FILES

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
r'
Page 8
TABLE 2
ACUTE AQUATIC TOXICITY TESTING RESULTS
HFPO PROCESS SCRUBBER EFFLUENT
Ceriodaphnia dubia
Test Concentration
(vol Effluent/vol Test Sample)
1/30/96 Testing
(% Mortality)
2/13/96 Testing
(% Mortality)
0
0
0
0.00018
10
0.00020
5
0.00028
5
0.00045
(worst case conc.)
10
0.00050
5
0.00072
0
0.00115
20
0.00150
100
0.00184
35
0.00295
100
0.00450
100
0.12160
100
0.13500
100
0.40500
100
LC50 = 0.00084
LC50 = 0.00183
JUL 30 1996
`C�N'T`i7AL .f iLE�

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
1.
Page 9
TABLE 3
ACUTE AQUATIC TOXICITY TESTING RESULTS
HFPO PROCESS SCRUBBER EFFLUENT
Fathead Minnow (Pimephales promelas)
Test Concentration
(vol Effluent/vol Test Sample)
1/30/96 Testing
(% Mortality)
2/13/96 Testing
(% Mortality)
0
0
0
0.00010
0
0.00020
5
0
0.00045
(worst case cont.
0
0.00050
0
0.00095
0
0.00150
0
0.00202
5
0.00429
0
0.00450
100
0.00909
100
0.1216
100
0.135
100
0.405
100
LC50 = 0.00257
LC50 = 0.00614
" ;
��NYRAL FILS3
,A

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
Page 10
TABLE 4
ACUTE AQUATIC TOXICITY TESTING RESULTS
NAFION® HFPO PROCESS SCRUBBER & WASTE GAS SCRUBBER
COMBINED EFFLUENTS
Ceriodaphnia dubia
Test Concentration
(vol Effluent/vol Test Sample)
1/30/96 Testing
(% Mortality)
2/13/96 Testing
(% Mortality)
0
0
0
0.00030
5
0.00037
5
0.00059
5
0.00094
(worst case conc.)
5
0.00100
10
0.00150
50
0.00241
100
0.00310
100
0.00385
100
0.00616
100
0.00844
100
0.00940
100
0.02531
100
0.02810
100
LC50 = 0.00160
LC50 = 0.00148
A ,1UL0 1996
C��TRAI, �1L�

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
m
Page 11
TABLE 5
ACUTE AQUATIC TOXICITY TESTING RESULTS
NAFIONO BFPO PROCESS SCRUBBER & WASTE GAS SCRUBBER
COMBINED EFFLUENTS
Fathead Minnow (Pimephales promelas)
Test Concentration
(vol Effluent/vol Test Sample)
1/30/96 Testing
(% Mortality)
2/13/96 Testing
(% Mortality)
0
0
0
0.00021
0
0.00030
0
0.00045
0
0.00094
(worst case conc.)
0
0.00100
0
0.00197
0
0.00310
0
0.00415
5
0.00840
100
0.00871
100
0.00940
100
0.01828
100
0.02531
100
0.02810
100
LC50 = 0.00540
LC50 = 0.00579
CENTRAL FILES

Mr. Gregory Nizich
NC DEHNR
March 15, 1996
TABLE 6
CHRONIC BIOASSAY TESTING RESULTS
Ceriodaphnia dubia
Page 12
Tested Effluent
1/30/96 Testing
2/13/96 Testing
(Pass/Fail)
(Pass/Fail)
HFPO Process Scrubber Effluent
Pass
Pass
3.3% Concentration
HFPO Process Scrubber Effluent
Pass
Pass
6.6% Concentration
Combined HFPO Process Scrubber
& Waste Gas Scrubber Effluents
Pass
Pass
3.3% Concentration
Combined HFPO Process Scrubber
Pass
Pass
& Waste Gas Scrubber Effluents
6.6% Concentration
JUL 30 1996
7
CENTRA. FILES

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STORM MATER
AVERAGE FLOWS IN THOUSANDS OF GALLONS PER DAY.
SOME FLOWS ARE ESTIMATED TO GIVE INTAKE AND
OISEHARGE TOTALS
SCHEMATIC WATER FLOW
EAU PONT OE NEMOURS & CO.
FAYETTEVILLE WORKS
PAGE 1 OF 2
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JUL 30 1996
CENTRAL FILES '

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SCHEMATIC WAITER FLOW
PROCESS USES
E.I, DU PONT DE NEMOURS & CO.
FAYETTEVILLE WORKS
PAGE 2 OF 2
PB7
AUL 30 1996
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Aquatic Bioass4y Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Envirdnmental Assessments • NPDES Testing
[Ell Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
X Comments:
Signat7a of Operator in Responsible Charge
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LC50/Acute Toxicity Test Sample temp @ receipt 1.6
(Mortality expressed as %, combining replicates) (deg. C)
0 0.018 0.028 0.045 0.072 0.115 0.184 0.295 Concentration (%)
0 10 5 10 0 20 35 100 Mortality (%)
LC50 = 0.2 % Method of Determination
95% Confidence Limits (%) Moving Average Probit
0.2 to 0.2 Spearman Karber X Other
Start End Start End
Organism Tested: 7.73 8.14 Control 8.1 8.1
Ceriodaphnia dubia 7.7 8.01 1 High 8.5 8.4
PH Conc. D.O.
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1/96
BRI rev. 12/93 h:\gpro\bri\atlform
JUL 30 1996
CUAMAL MM

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BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/15/96 THROUGH 2/16/96
WORK ORDER #: 6b220-003
CHEMICAL: HFPO
SPECIES: Ceriodaphnia dubia
DURATION: 24 HOURS
RAW DATA
CONCENTRATION(%) 0.018 0.028 0.045 0.072 0.115 0.184 0.295
Ln CONCENTRATION -4.02-3.58-3.10-2.63-2.16-1.69-1.22
NUMBER EXPOSED 21 20 21 20 20 20 21
MORTALITIES 0 0 0 0 1 7 21
SPEARMAN-KARBER TRIM: 0.00
SPEARMAN-KARBER ESTIMATES LC50: 0.2 % `�. v
2, c5ozo�j� �,O,00�- v_ vc�av
95% LOWER CONFIDENCE: 0.2
95% UPPER CONFIDENCE: 0.2
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
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ORGANISMS AFFECTED
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JUL 30 1996
CENTRAL FILES

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/15/96 THROUGH 2/17/96
WORK ORDER #: 6B220-003
CHEMICAL: HFPO
SPECIES: Ceriodaphnia dubia
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(%) 0.018 0.028 0.045 0.072 0.115 0.184 0.295
Ln CONCENTRATION -4.02-3.58-3.10-2.63-2.16-1.69-1.22
NUMBER EXPOSED 21 20 21 20 20 20 21
MORTALITIES 2 1 2 0 4 7 21
SPEARMAN-KARBER TRIM: 6.10
SPEARMAN-KARBER ESTIMATES LC50: 0.2 Y 0. (�,o7 QC,
95% LOWER CONFIDENCE: 0.2 % J
95% UPPER CONFIDENCE: 0.2
NOTE MORTALITY PROPORTIONS WERE NOT MONOTONICALLY INCREASING
ADJUSTMENTS WERE MADE PRIOR TO SPEARMAN-KARBER ESTIMATION.
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
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JUL 30 1996
CROW AUS

Aquatic Bioassay Testing * Aquatic Toxicity Reduction Evaluations
Ell
Chemical Product Environmental Assessments * NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street e Burlington, NC 27215-6935 9 [phone] * Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
X Comments:
Signature of Orator in Responsible Charge
HFPO
X =
Signature of 1?aboratory Supervisor
BRI# 6B220-004
. ............
Test Start Date: 12/15/96
Collection Start Date: 2 13196
.............
...............
X Sample Type/Duration
Grab Uomura ion
............
X 124 HOUR I Tox
Dilution Sample
Hardness(mg/L) 44.88
... ... .......
.. . .....
.. ......
Spec. Cond.(micromhos) 121.4 2980
...... .....
Xi ....... ......
. ........ .
..........
..........
.......... N/A
....... ........ ....... Chlorin e(mg/L)
LC50/Acute Toxicity Test Sample temp @ receipt 1.6
(Mortality expressed as %, combining replicates) (deg. C)
0 0.01 0.021 0.045 0.095 0.202 0.429 0.909 Concentration
0 0 0 0 0 5 0 100 Mortality (%)
LC50 = 0.6 % Method of Determination
95% Confidence Limits (%) Moving Average Probit
0.6 to 0.6 Spearman Kerber X Other
Start End Start End
Organism Tested: 7.08 7.67 Control 8.1
Pimephales promelas 7.5 7.98 High 8.5
pH Conc.
Modified from DEM form AT -1 (3/87) rev, 8/91
BR -2 1/96
BRI rev. 12/93 h:\gpro\bri\attform
CENTRAL FILES

BURLINGTON RESEARCH, INC• y
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/15/96 THROUGH 2/17/96
WORK ORDER #: 6B220-004
CHEMICAL: HFPO
SPECIES: Pimephales promelas
DURATION: 48 HOURS
RAW DATA
CONCENTRATION M 0.01 0.021 0.045 0.095 0.202 0.429 0.909
Ln CONCENTRATION -4.61-3.86-3.10-2.35-1.60-0.85-0.10
NUMBER EXPOSED 20 20 20 20 20 21 20
MORTALITIES 0 0 0 0 1 0 20
SPEARMAN-KARBER TRIM: 0.00
0-006
V l v
SPEARMAN-KARBER ESTIMATES LC50: 0.6 %
95% LOWER CONFIDENCE: 0.6 %
95% UPPER CONFIDENCE: 0.6 %
NOTE MORTALITY PROPORTIONS WERE NOT MONOTONICALLY INCREASING
ADJUSTMENTS WERE MADE PRIOR TO SPEARMAN-KARBER ESTIMATION.
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
I r5��
JUL 30, 1996
:r
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JUL `JU 1796

Aquatic Bioassay Testing - Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments - NPDES Testing
R
ll Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street a Burlington, NC 27215-6935 a [phone] 9 Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/27/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cent. # 002
X Comments:
Signatu of Operator in Responsible Charge
BOTH
x 7e u
Signature of Laboratory Supervisor
BRi# 613220-005
............
. . . . . . . . . . . . . . . . . . . . . . . . . . .
XX .
.................................
Test Start Date: 2/15/96
*i Collection Start Date: 2/12/96
ifsi
Sample Type/Duration
Grab I Comp, ura on
19A HOUR X Tox
Dilution Sample
Hardness( mg/L) 44.88
Spec. Cond.(micromhos) 124.1 2490
.......... X Chlorine(mg/L N/A
... . .. - ------
LC50 Acute Toxicity Test Sample temp @ receipt . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.5
(Mortality expressed as %, combining replicates) (dog. C)
0 0.037 0.059 0.094 0.15 0.241 1- 01385 0.616 Concentration
0 5 5 5 50 100 1 100 , 100 , Mortality
LC50 = 0.1 % Method of Determination
95% Confidence Limits (%) Moving Average Probit
0.1 to 0.2 Spearman Karber X Other
Start End Start End
Organism Tested: 7.73 7.8:1] Control 8.1 8.4
I Cerlodaphnia dubia 7.69 8.29 1 High 8.4 8.3
1 PH Conc. D.O.
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1/96
BRI rev. 12/93 h:\qpro\bri\atl form
JUL 30 1996
CENTRAL IFILE15

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/15/96 THROUGH 2/16/96
WORK ORDER #: 6B220-005
CHEMICAL: BOTH
SPECIES: Ceriodaphnia dubia
DURATION: 24 HOURS
RAW DATA
CONCENTRATION(%) 0.037 0.059 0.094 0.150 0.241 0.385 0.616
Ln CONCENTRATION -3.30-2.83-2.36-1.90-1.42-0.95-0.48
NUMBER EXPOSED 21 20 20 20 20 20 20
MORTALITIES 0 1 0 9 20 20 20
SPEARMAN-KARBER TRIM: 0.00
SPEARMAN-KARBER ESTIMATES LC50: 0.2 % ', loo 0, 00
Dc'
95% LOWER CONFIDENCE: 0.1
95% UPPER CONFIDENCE: 0.2
NOTE MORTALITY PROPORTIONS WERE NOT MONOTONICALLY INCREASING
ADJUSTMENTS WERE MADE PRIOR TO SPEARMAN-KARBER ESTIMATION.
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C -.4845
N 0
A N
T C -.3876 +
X
U E
R N
A T -.2907 +
L R
A
L T -.1938 +
X
0 I
G 0
N -9.690
0
X
X
X
10 25 50 75 100
ORGANISMS AFFECTED

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/15/96 THROUGH 2/17/96
WORK ORDER #: 6B220-005
CHEMICAL: BOTH
SPECIES: Ceriodaphnia dubia
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(%) 0.037 0.059 0.094 0.150 0.241 0.385 0.616
Ln CONCENTRATION -3.30-2.83-2.36-1.90-1.42-0.95-0.48
NUMBER EXPOSED 21 20 20 20 20 20 20
MORTALITIES 1 1 1 10 20 20 20
SPEARMAN-KARBER TRIM: 4.76
SPEARMAN-KARBER ESTIMATES LC50: 0.1 % ', i�D = 0.001 ���� ( 0. 00 a
95% LOWER CONFIDENCE: 0.1
95% UPPER CONFIDENCE: 0.2
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C -.4845
N 0
A N
T C -.3876
U E
RN
A T -.2907
L R
A
L T -.1938
0 I
G 0
N -9.690
0
X
X
X
X
10 25 50 75 100
ORGANISMS AFFECTED
JUPL 30 1996
Ft
�ENT�� FIDES

Aquatic Bioassay Testing,* Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street a Burlington, NC 27215-6935 • [phone] a Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
x Comments:
Signature of Operator in Responsible Charge
BOTH
x
Sig ture of Laboratory Supervisor
BRI# 66220-006
..:................ n......r .. ...:....:.....:. .:...:.:..:.....'•F.{.•,fi}}:•:•:•}::4}:fii•:ifi}}:fi:•}Y.:fifi:•:fi}:•::4:4}:•::v:•}::•:::•}::.}:::h}:•:•:
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¢%O?�%:•i:%:%ii:%:>+%:%:%ii:::%:%i:%:%:+::%:%i ii }$i i i i::%:�:�:i:� %:%::,L:%:%:%i i:� %:%:::¢i i'%�%;%i r:%:%i is+%:%::%i:%}:�}: i:.%;� %{i sv};{{:%:C;{%i:%'i�ri;%•;i:::,::::{:iso:::i':;:�:%:ti::,}�:{:yr:%::?: �%:W::::•:•
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XX
Test Start rt Date: 21596
.:.
•. Collection Start Date: 2/12/96
.;'•:,%$y:i::i:;yyi`•:•ks;:;:ikii::}:%:}.ii9%i:ii:::i ::%i:i:i::::SS:ii:ifit%::::.'•}iii{$iii: :i:%+.%:•:iii
Sample Type/Duration
P
Grab I Uomp. ura ion
x124 HOUR Tox
Dilution Sample
Hardness9 ) 4.88
m L 4
2.}}}Y.}.r::4:ifiti4:•:•::i•:tifi::4:L:itififi}}Y:}}:4}:{:•}}:fitititififi}:ifi;^;4}:•}:4:•}}}}:4:•:+ii•::•}}}}}:•:is titifi}:{{{•}:•}:titifi}:ti^:-0}}}}}:tifiv:}:
::;:::..:::::.::::}:.}r:::::::.:::.:::::::::::::::.:.�::::::::::::::::::::::::::::::.:::::::<.::.}:.:.:«.:}:.:}:.}:.}:.>}:.}:.}}::.}:.}:.>}:•::.}}}::.::.:<• 124.1 2490
,. Spec. Cond.(micromhos)
Chlorine m L
( '• N A
9
<<
LC50/Acute Toxicity Test Sample temp @receipt ::;;�;,;.}:.;,. 2.5
(Mortality expressed as %, combining replicates) (deg. c)
0 0.021 0.045 0.094 0.197 0.415 0.871 1.828 Concentration (%)
0 0 0 0 0 5 100 100 Mortality (%)
LC50 = 0.6 % Method of Determination
95% Confidence Limits (%) Moving Average Probit
0.5 to 0.6 Spearman Karber X Other
Start End Start End
Organism Tested: 7.04 7.52 Control 8.5 8.1
Pimephales promelas 7.53 7.83 High 8.5
PH Conc. D.O.
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1/96
BRI rev. 12(93- h:\gpro\brilatiform
JUL 3�01 1996
CENTRAL FILM

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/15/96 THROUGH 2/17/96
WORK ORDER #: 6220-006
CHEMICAL: Both
SPECIES: Pimephales promelas
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(%) 0.021 0.045 0.094 0.197 0.415 0.871 1.828
Ln CONCENTRATION -3.86-3.10-2.36-1.62-0.88-0.14 0.60
NUMBER EXPOSED 21 20 20 20 20 22 20
MORTALITIES 0 0 0 0 1 22 20
SPEARMAN-KARBER TRIM: 0.00
SPEARMAN-KARBER ESTIMATES LC50: 0.6 % `�� O.00�� U/L%
95% LOWER CONFIDENCE: 0.5 % C9, x)5-
95% UPPER CONFIDENCE: 0.6 % o(D v
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C .6032
N 0
A N
T C .4825
U E
R N
A T .3619
L R
A
L T .2412
0 I
G 0
N .1206
0
10 25 50 75 100
ORGANISMS AFFECTED
P-
JUL 30 P96
MOTRAL Fk►

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of.NTRAL FILES

Aquatic Bioassely Testing * Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments * NPDES Testing
[Ell Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street * Burlington, NC 27215-6935 e [phone] 9 Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573
Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
X Comments:
Signaturef Operator in Responsible Charge
HFPO
X
Signatulrle of Laboratory Supervisor
BRI#
6BO01-003
...........................
........................
..........................
. ..... . ...................................
. . ..... ....
Test Start Date: 12/1 /96 1
..........
Collection Start Date: 11/30/96
............. *i*i
Sample Type/Duration
Grab I Gornp• ura on
X OA HOUR To x
XXX
Dilution Sample
Hardness (m9 48.5
X •
Spec. Cond.(micromhos) 138.7 2980
X ...
........ .
Chlorine (mg/L) N/A
LC50/Acute Toxicity Test
I
Sample temp @ receipt
(Mortality expressed as %, combining replicates)
—2.2
(deg. C)
0 0.002 0.005 0.015 0.045 0.135
0.405 1.216 Concentration
0 5 5 100 100 100
100 100 Mortality
LC50 = 0.084 % Method of'Determination
95% Confidence Limits (%) Moving Average
Probit
N/R to Spearman Karber X
Other
Start End Start End
Organism Tested:
7.7 7.:92:] Control[ 8.6 8.9
Ceriodaphnia clubia
8.34 8.78 1 High 8.7
pH Cone.
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1/96
BRI rev. 12/93 h:\gpro\bri\atlf
JUL 30 1996
C Mf RAL PILUS

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/1/96 THROUGH 2/3/96
WORK ORDER #: 6B001-003
CHEMICAL: Dupont h FPO
SPECIES: Ceriodaphnia dubia
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(%) 2 5 15 45 135 405 1216
Ln CONCENTRATION 0.69 1.61 2.71 3.81 4.91 6.00 7.10
NUMBER EXPOSED 20 20 20 20 20 20 20
MORTALITIES 1 1 20 20 20 20 20
SPEARMAN-KARBER TRIM: 5.00
SPEARMAN-KARBER ESTIMATES LC50: 8.4 %
95% CONFIDENCE LIMITS
ARE NOT RELIABLE
ot, d. 000�� vIV
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C 7.103
N 0
A N
T C 5.682
U E
R N
A T 4.261
L R
A
L T 2.841
0 I
G 0
N 1.420
L
10 25 50 75 100
ORGANISMS AFFECTED
jU 19 6

Aquatic Bioassay Testing * Aquatic Toxicity Reduction Evaluations
Ell
Chemical Product Environmental Assessments * NPIDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street 9 Burlington, NC 27215-6935 * [phone] e Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
X Comments:
Signature of Operator in Responsible Charge
X &11' 4-11-1-1-
HFPO
Signiture of Laboratory Supervisor
BRi# 6BO01-003
. . . . . . . . . . . . . . . . . . . . . . . .
4.
.. .......................................... .. . .... NX
..... ........
. . . . . . . . . . . .
Test Start Date: 2/1/96
�jjjjjjjj Collection Start Date: 1/3 0/96
j:j:j:j::
N X: Sample Type/Duration
Grab I Uornp. I Duration
:g:
X 24 Tox HOUR
....
Dilution Sample
...... ........... Hardness (mg/L) 48.5
...... ..........
Spec. Cond.(micromhos) 138.7 2980
..........
..........
.... ..........
....... ........ .
.... .......
...... ....... .
............ Chlorine( mg/L) N/A
. . . . . . . . . . . ... ..
LC50/Acute Toxicity Test Sample temp @ receipt 2.2
(Mortality expressed as %, combining replicates) (deg. C)
0 0.002 0,005 0.015 0.045 0.135 0.405 1.216 Concentration
0 5 5 100 100 100 100 100 Mortality
LC50 = 0.257 % Method of Determination
95% Confidence Limits (%) Moving Average Probit
N/R to Spearman Karber X Other
Start End Start End
Organism Tested: 8.03 7.:7:] Control 8.6 8.4
Pim9phales promelas 8.34 8.54 1 High 8.7
PH
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1/96
BRI rev. 12/93 h:\qpro\bri\atlfzo,
JUL
C5NTRA rit 8

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/1/96 THROUGH 2/3/96
WORK ORDER #: 6BO01-003
CHEMICAL: Dupont rE Ff v
SPECIES: Pimephales promelas
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(%) 2 5 15 45 135 405 1216
In CONCENTRATION 0.69 1.61 2.71 3.81 4.91 6.00 7.10
NUMBER EXPOSED 20 20 20 21 20 20 22
MORTALITIES 1 0 0 21 20 20 22
SPEARMAN-KARBER TRIM: 1.67
SPEARMAN-KARBER ESTIMATES LC50: 25.7 % / 1011 = �''�f 0 0C)'�$
95% CONFIDENCE LIMITS
ARE NOT RELIABLE
NOTE MORTALITY PROPORTIONS WERE NOT MONOTONICALLY INCREASING
ADJUSTMENTS WERE MADE PRIOR TO SPEARMAN-KARBER ESTIMATION.
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C 7.103
N 0
A N
T C 5.682
U E
R N
A T 4.261
L R
A
L T 2.841
O I
G 0
N 1.420
C
10 25 50 75 100
ORGANISMS AFFECTED
lauro
JUL1996
CENTRAL FfLi

,.
clq (14 pO pO M
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Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street a Burlington, NC 27215-6935 • [phone] • Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
x I Comments:
of Operator in Responsible Charge
x BOTH
Si ature of Laboratory Supervisor I BRI# 6BO01-004
LC50/Acute Toxicity Test
(Mortality expressed as %, combining replicates)
Test Start Date: 2/1/96
Collection Start Date: 11/30/96
Sample Type/Duration
0.003
0.01
Grab I Comp. I Duration
0,094
0.281
X 24 HOUR
2,351
Tox
5
Dilution
Sample
Hardness(mg/L)
48.5
Spec. Cond.(micromhos)
138.7
2490
Chlorine(mg/L)
N/A
Sample temp @ receipt
2
(deg. C)
0
0.003
0.01
0.031
0,094
0.281
0.844
2,351
0
5
10
100
100
100
100
100
LC50 = 0.16 % Method of Determination
95% Confidence Limits (%) Moving Average
0.133 to 0.193 1 Spearman Karber
Organism Tested:
Ceriodaphnia dubia
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1196
Concentration (%)
Mortality (%)
Probit
Other
Start End Start
7.7 8,19 Control 8.6
8.25 8.86 High 8.5
PH Conc.
BRI rev. 12/93 h:\gpro\bri\ati
End
8.8
8.6 __ —. ---
JUL vet 1996 0

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/1/96 THROUGH 2/3/96
WORK ORDER #: 6B001-004
CHEMICAL: Dupont Q,ci li
SPECIES: Ceriodaphnia dubia
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(X) 3 10 31 94 281 844 2531
Ln CONCENTRATION 1.10 2.30 3.43 4.54 5.64 6.74 7.84
NUMBER EXPOSED 20 20 20 20 20 20 20
MORTALITIES 1 2 20 20 20 20 20
SPEARMAN-KARBER TRIM: 5.00
SPEARMAN-KARBER ESTIMATES LC50: 16.0 X /L0 Or 0,0016 co 13 U, 0019
95% LOWER CONFIDENCE: 13.3 %
95% UPPER CONFIDENCE: 19.3 X
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C 7.836
N 0
A N
T C 6.269
U E
R N
A T 4.701
L R
A
L T 3.134
0 I
G 0
N 1.567
0
10 25 50 75 100
% ORGANISMS AFFECTED
JUL 0 1996
`

Ag Aquatic Bioassay Testing Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
Effluent Toxicity Report Form - Acute LC50 Date: 2/14/96
Facility DUPONT, FAYETTEVILLE NPDES# NC0003573 Pipe# County BLADEN
Laboratory Performing Test Burlington Research, Inc. - Cert. # 002
x Comments:
Signature f Operator in Responsible Charge
x BOTH
Signatu a of Laboratory Supervisor BRI# 6BO01-004
LC50/Acute Toxicity Test
(Mortality expressed as %, combining replicates)
Test Start Date: 2/1/96
Collection Start Date: 11/30/96
Sample Type/Duration
uran I comp. 1 uuration
0.003
0.01
X 24 HOUR
0.094
Tox
0.844
Dilution
Sample
0
0
Hardness(mg/L)
48.5
100
Spec. Cond.(micromhos)
138.7
2490
Chlorine(mg/L)
N/A
Sample temp @ receipt
2
(deg. C)
0
0.003
0.01
0.031
0.094
0.281
0.844
2.351
0
0
0
100
100
100
100
100
LC50 = 0.54 % Method of Determination
95% Confidence Limits (%) Moving Average Probit
N/R to Spearman Karber X Other
Organism Tested:
Pimeohales ioromelas
Modified from DEM form AT -1 (3/87) rev. 8/91
BR -2 1/96
Concentration (%)
Mortality (%)
Start End Start End
7.7 8 Control 8.68
8.25 8.52 High 8.5` 1
pH Conc. t=
BRI rev. 12/93 h:\gpro\bri\at1 lUiL 3 096
tog-tea c

BURLINGTON RESEARCH, INC.
TRIMMED SPEARMAN-KARBER METHOD FOR CALCULATION OF
EC50 AND LC50 VALUES IN BIOASSAYS
DATE: 2/1/96 THROUGH 2/3/96
WORK ORDER #: 6BO01-004
CHEMICAL: Dupont j{ FPI
SPECIES: Pimephales promelas
DURATION: 48 HOURS
RAW DATA
CONCENTRATION(%) 3 10 31 94 281 844 2531
Ln CONCENTRATION 1.10 2.30 3.43 4.54 5.64 6.74 7.84
NUMBER EXPOSED 21 20 20 20 20 20 20
MORTALITIES 0 0 0 20 20 20 20
SPEARMAN-KARBER TRIM: 0.00
SPEARMAN-KARBER ESTIMATES LC50: 54.0 % �� v ' y C r
95% CONFIDENCE LIMITS
ARE NOT RELIABLE
REFERENCE: M.A. HAMILTON, R.C. RUSSO, AND R.V. THURSTON. 1977. TRIMMED SPEARMAN-
KARBER METHOD FOR ESTIMATING MEDIAN LETHAL CONCENTRATIONS IN TOXICITY BIOASSAYS.
ENVIRON. SCI. TECHNOL. 11:714-719; CORRECTION 12:417 (1978).
C 7.836
N 0
A N
T C 6.269
U E
R N
A T 4.701
L R
A
L T 3.134
0 I
G 0
N 1.567
0
10 25 50 75 100
ORGANISMS AFFECTED
SYffP Y,L < LFw
JUL 2.0 1996

Aquatic Noassay Testing • Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6BO01-001
REPORT TO: Mr. Mike Hamilton RECEIVED: 01/31/96
REPORTED: 02/14/96
SAMPLE DESC: SPECIAL STUDY, 3.3
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 01/30/9609:00 to 01/31/9609:00 SITE: HFPO 3.3
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 01/31/96 18:30 PASS
NCDEM 9/89 Analyzed 02/14/96 by JCB
Page 1
BR -2 1/96
JUL .meg' 1"'96
r,ENTP,AL FILE -S

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50 ' Date: 02/14/96
Facility: HFPO SPIKED NPDES#: NC0003573 Pipe#: County: BLADEN
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments:
X
Signature of Operator in Responsible Charge
S Aature of Laboratory Supervisor I * PASSED: -5.62% Reduction *
Work Order: 6BO01-01 vironment Sciences Branch
MA 7t�RI('f�NAL T0: Di of Envir mental Ma gement �+
N.C. Dept. of NR
4401 edy Creek oad
Raleigh, N rth Caro 'na 27607-6445
Chronic Pass/Fail Reproduction Toxicity Test
:ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 1
# Young Produced 113713712513111613012913113113013112811
Adult Wive (D)ead IIL IL IL IL IL IL IL IL IL IL IL IL
affluent %: 3.3%
REATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
18.369%
# Young Produced 17 28 35 33 37 34 33 33 30 37 29 30 % control orgs
producing 3rd
brood
Adult (Dive (D)ead L L L L L L L L L L L L 92%
Chronic Test Results
Calculated t =
Tabular t =
Reduction = -5.62
Mortality
Avg.Reprod.
0.00
29.67
Control
Control
0.00
31.33
Treatment 2
Treatment 2
PASS FAIL
X
Check One
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 01/31/96
Control 7.62 7.90 7.76 7.40 7.72 7.97 Collection (Start) Date
Sample 1: 01/30/96 Sample 2:
Treatment 2 7.81 7.89 7.76 7.92 7.78 7.95 Sample Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/L) 49
Control 8.6 8.7 8.8 8.9 8.5 8.5
Spec. Cond.(pmhos) 124 629
Treatment 2
Chlorine(mg/l) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(°C) 1.5
(Mortality expressed as %, combining replicates)
LotePlease
oncentration te This
n Also
Mortality
start/end start/end
Control
High
Conc.
pH D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average Probit
-- %
_
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
JUL 30 1996
CZN-f
:r

Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
Ell Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6BO01-005
REPORT TO: Mr. Mike Hamilton RECEIVED: 01/31/96
REPORTED: 02/14/96
SAMPLE DESC: SPECIAL STUDY
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 01/30/9609:00 to 01/30/9609:00 SITE: HFPO 6.6
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 01/31/9618:30 PASS
NCDEM 9/89 Analyzed 02/14/96 by JCB
Page 5
BR -2 1/96

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50' Date: 02/14/96
Facility: HFPO SPIKED NPDES#: NC0003573 Pipe#:
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments:
X
Signatury of Operator in Responsible Charge
County: BLADEN
Sig7fure of Laboratory Supervisor I * PASSED: -6.74% Reduction *
Work Order: 6BO01-01'5 nviron ntal Scie ces Bra�ch
MA�ORIGI-SAL T0: D'v. of vironment l Managdment �1(�
N. . Dept. f EHNR �� JA
440 eedy eek Road
Ralei h, North Carolina 27607-6445
�....+L. r-..... 1 ; r....:...J....L......
Chronic Pass/Fail Reproduction Toxicity Test
:ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced l�37�37�25�3l�l6�3O�29�3l�31130�3l�28�I
Adult M ive Mead JAL IL IL IL IL IL IL IL IL IL IL IL
:ff Luent %: 6.6%
REATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
18.369%
# Young Produced 15 30 36 30 31 32 35 39 33 29 36 34 % control orgs
producing 3rd
brood
Adult (L)ive Mead L L L L L L L L L L L L I
92%
Chronic Test Results
Calculated t =
Tabular t =
Reduction = -6.74
Mortality
Avg.Reprod.
0.00
29.67
Control
ControL
0.00
31.67
Treatment 2
Treatment 2
PASS FAIL
X
Check One
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 01/31/96
Control7.62 7.90 7.76 7.85
ff
E
Collection (Start) Date
Sample 1: 01/30/96 Sample 2:
Treatment 2 7.79 38.7 7.79 7.85 7.84 7.98 Sample Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P_
1st sample 1st sample 2nd sample
D.O. Hardness(mg/L) 49
...............
Control 8.6 8.7 8.8 8.9 8.8 8.5
Spec. Cond.(pmhos) 124 629
Treatment 2
Chlorine(mg/l) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(°C) 1.5
(Mortality expressed as %, combining replicates)
%
%
%
%
%
%
%
%
%
%
Note: Please
Concentration Complete This
Section Also
Mortality
start/end start/end
Control
it
High
Conc.
off D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Prob
-- %
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
J * C
„UL 3 19§6
U'PllflkAi FILES

Aquatic Bioassay Testing • Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6BO01-002
REPORT TO: Mr. Mike Hamilton RECEIVED: 01/31/96
REPORTED: 02/14/96
SAMPLE DESC: SPECIAL STUDY
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 01/30/9609:00 to 01/31/9609:00 SITE: Both 3.3
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 01/31/9618:30 PASS
NCDEM 9/89 Analyzed 02/14/96 by JCB
Page 2
EtVth'A1 F LtS i
BR -2 1/96

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50 Date: 02/14/96
Facility: BOTH SPIKED NPDES#: NC0003573 Pipe#:
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments.
SignZz� re of Operator in Responsible Charge
X .v�
SipKature of Laboratory Supe visor
County: BLADEN
* PASSED: 6.09% Reduction *
Work Order: 6BO01-002 E ironmental ciences ranch
MA OR
IN T0: Di of Enviro ental Ma ement NAIA-
N.C. pt. of EH
4401 y Creek d
Raleigh,N rth Carolina 27607-6445
North Carolina Ceriodaphnia
Chronic Pass/Fail Reproduction Toxicity Test Chronic Test Results
Calculated t =
Tabular t =
CONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 % Reduction = 6.09
# Young Produced 27 35 37 36 35 36 37 31129134126131
Adult (L)ive Mead L L L L L L L L L L L L
Effluent %: 3.3%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
11.891%
# Young Produced 30 31 35 36 31 32 16 35 28 33 33 30 % control orgs
producing 3rd
brood
Adult (L)ive Mead L L L L L L L L L L L L 100%
Mortality
Avg.Reprod.
0.00
32.83
Control
Control
0.00
30.83
Treatment 2
Treatment 2
PASS FAIL
X
Check One
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 01/31/96
Control7.62 8.03 7.76 7.74
ff
E
Collection (Start) Date
SampLe 1: 01/30/96 Sample 2:
Treatment 2 7.73 8.01 7.83 7.83 7.83 7.87 SampLe Type/Duration 2nd
1st P/F
s
s
s
95% Confidence Limits
Moving Average _ Probit _
Grab
Comp.
Duration
D
t e
t e
t
e
I S S
a n
a n
a
n
Sample 1
X
24 hrs
L A A
r d
r d
r
d
U M M
t
t
t
Sample 2
hrs
T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/l) 49
Control 8.6 8.4 8.8 8.9 8.8 8.3
Spec. Cond.(pmhos) 124 686
Treatment 2
ChLorine(mg/l) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(OC) 1.8
(Mortality expressed as %, combining replicates)
Concentration
Mortality
start/end
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Probit _
-- %
Spearman Karber _ Other
pH
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
Note: Please
Complete This
Section Also
start/end
Control
High
Conc.
D.O.
h
H
JUL
...0

Aquatic Bioassay Testing - Aquatic Toxicity Reduction Evaluations
Chemical Product Environmental Assessments • NPDES Testing
[ED11 Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6BO01-006
REPORT TO: Mr. Mike Hamilton RECEIVED: 01/31/96
REPORTED: 02/14/96
SAMPLE DESC: SPECIAL STUDY, 6.6
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 01/30/9609:00 to 01/30/9609:00 SITE: BOTH 6.6
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 01/31/9618:30 PASS
NCDEM 9/89 Analyzed 02/14/96 by JCB
5� .6 '9.w�"�43oaric blf �� 1
JUL 80 1995
Page 61vN�4t,
BR -2 1/96 - .14

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50` Date: 02/14/96
Facility: BOTH SPIKED NPDES#: NC0003573 Pipe#: County: BLADEN
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments:
X
Signature of Operator in Responsible Charge
LSigna e of Laboratory Supervisor I * PASSED: 0.25% Reduction
Work Order: 68001-06 vironmen L Sci \ces anch
NIL NIGIN� T Di of Env onmenMan ement. ept. o HNR4401edy Cre Roa
Raleigh North Carolina 27607 6445
Chronic Pass/Fail Reproduction Toxicity Test
:ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced 27 35 37 36 35 36 37 31 29 L34 26 f.31
Adult (L)ive (D)ead IL 11L L IL IL IL IL IL IL L IL IL
:ff Luent %: 6.6%
REATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
11.891%
# Young Produced 39 34 33 36 32 30 32 20 37 30 36 34 % control orgs
producing 3rd
brood
Adult (L)ive Mead L L L L L L L L L L L L 100%
Chronic Test Results
Calculated t = 0.046
Tabular t = 2.508
Reduction = 0.25
Mortality
Avg.Reprod.
0.00
32.83
Control
Control
0.00
32.75
Treatment 2
Treatment 2
PASS FAIL
X
Check One
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 01/31/96
Control7.62 8.03 7.76 7.74
ff�E
Collection (Start) Date
Sample 1: 01/30/96 Sample 2:
Treatment 2 7.77 8.02 7.82 7.87 7.79 7.87 Sample Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/L) 49 `:�� �•i�•iii�
Control 8.7 8.4 8.6 8.7 8.8 8.2
Spec. Cond.(pmhos) 124 686
Treatment 2
Chlorine(mg/l) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(°C) 1.8
(Mortality expressed as %, combining replicates)
%
Note: Please
Concentration Complete This
Section Also
Mortality
start/end start/end
Control
obit
High
Conc.
pH D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Pr
-- %
Spearman Karber _ Other
JUL SO 1996
Note: Please
Concentration Complete This
Section Also
Mortality
start/end start/end
Control
obit
High
Conc.
pH D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Pr
-- %
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
JUL SO 1996

Aquatic Bioassay T;epting ! Aquatic Toxicity Reduction Evaluations
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Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6B220-001
REPORT TO: Mr. Michael Johnson RECEIVED: 02/14/96
REPORTED: 02/28/96
SAMPLE DESC: FEB. MONITORING, TOXICITY
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 02/12/9612:00 to 02/13/9612:00 SITE: HFPO 3.3
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 02/14/9613:05 PASS
NCDEM 9/89 Analyzed 02/27/96 by JCB
JUL «IO 1996
Page 1
'rRA flet
BR -2 1196

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50f Date: 02/22/96
facility: HFPO SPIKED NPDES#: N00003573 Pipe#: County: BLADEN
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments:
Signature of Operator in Responsible Charge
4J
Seture of Laboratory Supervisor I * PASSED: 4.62% Reduction *
Work Order: 66220-001 E vironmen l Scie ces ranch r v
Mi►IL 0 GINA�O: Di of Env onmen l Ma agement 1Y�
N.0 Dept. o EHNR J
4401 Reedy Cr k Roa
Ralei h, North arolina 27607-6445
Chronic Pass/Fail Reproduction Toxicity Test
:ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 1
# Young Produced 1131127129132122131130124124112136
Adult (L)ive Mead JAL IL IL IL IL IL IL IL IL IL IL IL
:ff Luent %: 3.3%
REATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
22.786%
# Young Produced 23 29 29 18 31 28 27 20 24 27 29 25 % control orgs
producing 3rd
brood
Adult (Dive Mead L L L L L L L L L L L L 92%
Chronic Test Results
Calculated t = 0.591
Tabular t = 2.508
Reduction = 4.62
Mortality
Avg.Reprod.
0.00
27.08
Control
Control
0.00
25.83
Treatment 2
Treatment 2
PASS FAIL
1X1 11
CheckOne
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 02/14/96
Control7.61 7.69 7.47 7.71 7.68H
Collection (Start) Date
Sample 1: 02/12/96 Sample 2:
Treatment 2 7.58 7.71 7.64 7.75 7.77 7.96 Sample Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/t) 45
Control 8.3 7.9 8.6 8.2 7.9 8.3
Spec. Cond.(pmhos) 124 651
Treatment 2
Chlorine(mg/l) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(°C) 2.2
(Mortality expressed as %, combining replicates)
Note: Please
Concentration Complete This
Section Also
Mortality
start/end start/end
Control
it
High
Conc.
PH D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Prob
-- %
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
JUL1996
� i -IN � :

Aquatic Bioassay Taepting - Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6B220-007
REPORT TO: Mr. Michael Johnson RECEIVED: 02/14/96
REPORTED: 02/28/96
SAMPLE DESC: FEB. MONITORING, TOXICITY
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 02/12/9612:00 to 02/13/9012:00 SITE: HFPO 6.6
PARAMETER DATE/TIME/ANALYST RESULT
* * Ceriodaphnia Pass/Fail Chronic Started 02/14/9613:43 PASS
NCDEM 9/89 Analyzed 02/27/96 by JCB
* * Sample received out of hold time
leas -e t'oj✓! d�e� 5 a r»p le �^ e c e,'v� of o—�k .
Page 7
BR -2 1/96

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50Date: 02/22/96
Facility: HFPO SPIKED NPDES#: NC0003573 Pipe#: County: BLADEN
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
X
Signature of Operator in Responsible Charge
Work Order: 6B220-001
r
Comments:
* PASSED: 6.46% Reduction *
E viron ental Sciences Branch
, MA�L`BRIG14AL TO: Di of vir°gmen L Manag ment
1 N.C. Dept. of ENjJR�
1 4401 eedy reek ytoad
Raleigh, North Carolina 27607-6445
IVI-NI balVlllia lcl 1-VII[Itu
Chronic Pass/Fail Reproduction Toxicity Test Chronic Test Results
Calculated t =
Tabular t =
:ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 % Reduction = 6.46
Mortality Avg.Reprod.
# Young Produced 31 27 29 32 22 31 30 24 24 12 36 27 %
0.00 27.08
Control Control
Adult (L)ive Mead
L
L
L
L
L
L
L
L
L
L
L
L
0.00
Treatment 2
25.33
Treatment 2
!ffluent %: 6.6%
'REATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
Control CV
22.786%
PASS FAIL
# Young Produced
21
29
8
31
26
28
26
25
29
22
30
29
% control orgs
producing 3rd
ECheL_
brood
Adult (Dive Mead
L
L
L
L
L
L
L
L
L
L
L
L
92%
1st sample 1st sample 2nd sample Complete This For Either Test
PH Test Start Date: 02/14/96
Control7.61 7.b9 7.47 7.71
E�H
Collection (Start) Date
Sample 1: 02/12/96 Sample 2:
Treatment 2 7.62 7.73 7.61 7.76 7.78 7.92 Sample Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/l) 45
Control 0210
Spec. Cond.(pmhos) 124 651
Treatment 2
Chlorine(mg/L) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(OC) 2.2
(Mortality expressed as %, combining replicates)
Note: Please
Concentration Complete This
Mortality
Section Also
start/end start/end
Control
obit
High
Conc.
PH D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Pr
-- %
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
JUS 3a 1996

Aquatic Bipassay, Tppting • Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6B220-002
REPORT TO: Mr. Michael Johnson RECEIVED: 02/14/96
REPORTED: 02/28/96
SAMPLE DESC: FEB. MONITORING, TOXICITY
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 02/12/9612:00 to 02/13/9612:00 SITE: Both 3.3
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 02/14/96 13:43 PASS
NCDEM 9/89 Analyzed 02/27/96 by JCB
JUL SO 1996
Page 2
BR -2 1/96

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute•LC50 Date: 02/22/96
Facility: BOTH SPIKED NPDES#: NC0003573 Pipe#: County: BLADEN
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
Comments:
X
Sign ure of Operator in Responsible Charge
X (,�
SPhiture of Laboratory Supervisor * PASSED: 5.16% Reduction
Work Order: 68220-002 E ironment\Creek
ces�nA
MA.I,_.OR'IIGINAJ- 16� Di of Enval M !gem t ��
N.C. pt.
4401 Re ad
Raleigh, North Carolina 27607-6445
Chronic Pass/Fail Reproduction Toxicity Test
:ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 1
# Young Produced 28 39 32 32 21133132122132131 32 34
11
Adult Wive Mead L L L L L L L L L L L L
:ff Luent %: 3.3%
TREATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
16.175%
# Young Produced 31 33 33 27 25 20 27 33 24 35 34 27 % control orgs
producing 3rd
brood
Adult Wive Mead L L L L L L L L L L L L 100%
Chronic Test Results
Calculated t = 0.800
Tabular t = 2.508
Reduction = 5.16
Mortality
Avg.Reprod.
0.00
30.67
Control
ControL
0.00
29.08
Treatment 2
Treatment 2
PASS FAIL
X
Check One
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 02/14/96
Control7.61 7.85 7.47 7.87 7.68 7.83 Collection (Start) Date
Sample 1: 02/12/96 Sample 2:
Sam
Treatment 2 7.93 7.78 7.55 7.90 7.94 7.78 ple Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/L) 45
Control 8.3 8.3 8.6 8.4 7.9 8.4
Spec. Cond.(pmhos) 124 529
Treatment 2 8.1 8.3 8.55 8.3 8.5 8.3
ChLorine(mg/L) n/a
LC50/Acute Toxicity Test Sample temp. at receipt(OC) 2.1
(Mortality expressed as %, combining replicates)
SEEM®®®®®®
Method of Determination
95% Confidence Limits
Moving Average _ Prob
-- %
Spearman Karber _ Other
®®®®®®®®®®
Note: Please
Concentration Complete This
Section ALso
Mortality
start/end start/end
Control
it
High
Conc.
off D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Prob
-- %
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
JUL 30 1996
Nf

Aquatic Bioassay,Tepting . Aquatic Toxicity Reduction Evaluations
Ell Chemical Product Environmental Assessments • NPDES Testing
Reporting & Data Handling Services
BURLINGTON
RESEARCH 1302 Belmont Street • Burlington, NC 27215-6935 • [phone] • Fax [phone]
ANALYTICAL REPORT
CUSTOMER: DUPONT FAYETTEVILLE WORK ORDER #: 6B220-008
REPORT TO: Mr. Michael Johnson RECEIVED: 02/14/96
REPORTED: 02/28/96
SAMPLE DESC: FEB. MONITORING, TOXICITY
SAMPLE TYPE: WASTEWATER, COMPOSITE
COLLECTED: 02/12/9612:00 to 02/13/9612:00 SITE: BOTH 6.6
PARAMETER DATE/TIME/ANALYST RESULT
Ceriodaphnia Pass/Fail Chronic Started 02/14/9613:05 PASS
NCDEM 9/89 Analyzed 02/27/96 by JCB
�r
JELL 30 1996
Page 8 s'*jTL Piet
BR -2 1/96

Effluent Toxicity Report Form - Chronic Pass/Fail and Acute LC50 Date: 02/22/96
Facility: BOTH SPIKED NPDES#: NC0003573 Pipe#:
Laboratory Performing Test: BURLINGTON RESEARCH, INC.
[Comments:
X
Signature of Operator in Responsible Charge
County: BLADEN
X /
Signa o Laboratory Supervisor * PASSED: 2.72% Reduction
Work Order: 6B220-002 EnvironmentaL Sciences Branc
�n1\ MAORINA1\T0N_ DiEnviro ental anagem t
1� 1 N.C. Dep of E
4401 eedy Creekad
RaLei h, Nor h Caro ina 27607-6445
- - --
-. a wl ...W �r •.w
Chronic Pass/Fail Reproduction Toxicity Test
ONTROL ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12
# Young Produced ��28�39�32132121�33�32122132131132�34��
Adult (L)ive Mead JAL IL IL IL IL IL IL IL IL IL IL IL
ffluent %: 6.6%
'REATMENT 2 ORGANISMS 1 2 3 4 5 6 7 8 9 10 11 12 Control CV
16.175%
# Young Produced 34 26 31 36 28 36 28 32 29 26 22 30 % control orgs
producing 3rd
brood
Adult Wive Mead L L L L L L L L L L L L 100%
Chronic Test Results
Calculated t = 0.442
Tabular t = 2.508
Reduction = 2.72
Mortality
Avg.Reprod.
0.00
30.67
Control
Control
0.00
29.83
Treatment 2
Treatment 2
PASS FAIL
X
Check One
1st sample 1st sample 2nd sample Complete This For Either Test
pH Test Start Date: 02/14/96
Control7.61 7.85 7.47 7.87
E
8 7.83 Collection (Start) Date
Sample 1: 02/12/96 Sample 2:
Treatment 2 7.77 7.79 7.51 7.78 7.82 7.76 Sample Type/Duration 2nd
1st P/F
s s s Grab Comp. Duration D
t e t e t e I S S
a n a n a n Sample 1 X 24 hrs L A A
r d r d r d U M M
t t t Sample 2 hrs T P P
1st sample 1st sample 2nd sample
D.O. Hardness(mg/l) 45':`:`:
Control 8.3 8.3 8.6 8.4 7.9 8.4
Spec. Cond.(pmhos) 124 529
Treatment 2
Chlorine(mg/L) i' n/a
LC50/Acute Toxicity Test Sample temp. at receipt(OC) 2.1
(Mortality expressed as %, combining replicates)
Note: Please
Concentration Complete This
Section Also
Mortality
start/end start/end
Control
it
High
Conc.
PH D.O.
LC50 = %
Method of Determination
95% Confidence Limits
Moving Average _ Prob
-- %
Spearman Karber _ Other
Organism Tested: Ceriodaphnia dubia Duration(hrs):
Copied from DEM form AT -1 (3/87) rev. 11/95 (DUBIA ver. 4.30)
Min
,JUL 30 1996

oUPONT
DuPont Automotive
DuPont Automotive
P.O. Drawer Z
Fayetteville, NC 28302
March 22, 1996
Mr. Gregory Nizich
NC DEHNR - DEM
Water Quality Section
Permits & Engineering Unit
-
P. O. Box 29535
;
L�; _
Raleigh, NC 27626-0535
CA
RE: Renewal of NPDES Permit No. NC0003573
Re -analysis for di-n-octyl phthalate at Outfall 002
C3
Dear Mr. Nizich,
Enclosed are the results from two additional Outfall 002 analyses for di-n-octyl phthlate
which shows that this compound was below the method's detection limit. These results
should verify that the initial analysis of 23 µg/L di-n-octyl phthlate as reported in the
NPDES Permit renewal application was probably from cross -contamination of the
sampler's synthetic rubber gloves.
If you have any questions, please feel free to call me at [phone].
Enclosures
E. I. du Pont de Nemours and Company
Michael E. Johnson
Environmental Coordinator
C 0.1 4 • -
s
ri 'JUL 80 1996
0 Printed on Recycled Paper
Z-544 Rev. 8/95

Industrial & Environmental Analysts, Inc. (IEA)
BASE/NEUTRAL EXTRACTABLES SW -846 METHOD 8270
IEA Project Number: 2101-077
IEA Sample Number: 9512448-01 Date Received: 12/13/95
Client Name: Dupont Date Sampled: 12/13/95
Client Project ID: Waste Water Treatment Date Extracted: 12/18/95
Sample Identification: 4046 Date Analyzed: 12/28/95
Matrix: Water Analysis By: Van Lare
Dilution Factor: 1.0
Quantitation Results
Limit Concentration
Number Compound (ug/L) (ug/L)
1 Di-n-octylphthalate 10 BQL
Comments:
Sample specific quantitation limits may be calculated by multiplying
the quantitation limit by the dilution factor.
BQL = Below Quantitation Limit
(1) Cannot be separated from Diphenylamine
(,3) Hexachlorocyclopentadiene does not recover by this method.
'1
FORM 8270B (1) Rev. 041795
_ L 6

Comments:
*This compound is no longer provided as a normal target deliverable for
Method 625. Please contact your account representative for further
information.
Sample specific quantitation limits may be calculated by multiplying
the quantitation limit by the dilution factor. �.
BQL - Below Quantitation Limit '
FORM 625B (1) Rev. 081792
JUL $0 1996;
`CE; t`AL MES _t1
2/7
Industrial & Environmental
Analysts, Inc. (IEA)
GC/MS BASE/NEUTRAL EXTRACTABLES EPA 625 COMPOUND LIST
IEA Project Number: 2101-104
IEA Sample Number: 9602195-05
Date Received:
02/07/96
Client
Name: Dupont
Date Sampled:
02/07/96
Client
Project ID: LFN-182117
Date Extracted:
02/12/96
Sample
Identification: 060206-002
Date Analyzed:
02/18/96
Matrix:
Water
Analysis By:
Van Lare
Dilution Factor:
1.0
Quantitation
Results
Limit Concentration
Number
Compound
(ug/L)
(ug/L)
1
Di-n-octylphthalate
10
BQL
Comments:
*This compound is no longer provided as a normal target deliverable for
Method 625. Please contact your account representative for further
information.
Sample specific quantitation limits may be calculated by multiplying
the quantitation limit by the dilution factor. �.
BQL - Below Quantitation Limit '
FORM 625B (1) Rev. 081792
JUL $0 1996;
`CE; t`AL MES _t1

♦ VA.
MAIL TO
NORTH CAROLINA,
Cumberland County.
ST
AFFIDAVIT F PUBLICATION
i the basis of thorough
review and application of
Before the undersigned, a Notary Public of said County and State, duty
commissioned and authorized to administer oaths, affirmations, etc., personally
appeared
who, being duly sworn or affirmed, according to law, doth depose and say that
Article 21 of Chapter 143, Gen. he/she is
eral Statutes of North Carolina,
Public law 92.500 and other of THE FAYETTEVILLE PUBLISHING COMPANY, a corporation organized
lawful standards and re ula-
tions, the North Carolina Envi- and doing business under the Laws of the State of North Carolina, and publishing
lop, Management Com-
mission proposes to issue a a newspaper known as THE FAYETTEVILLE OBSERVER, in the City of
permit to discharge to the per-
i sons listed
su below
m special Fayetteville, County and State aforesaid, and that as such he/she makes this
conditions. affidavit; that he/she is familiar with the books, files and business of said
Persons wishing to comment
upon or object to the proposed Corporation and by reference to the fi&s -of said publication the attached
determmabons are invited to
submit same in writing to the advertisement of r
above address no later than
6/19/96. All comments received RECOVED
prior to that date will be con.
sidered in the formulation of fi-
nal determinations regardingI) r9jn�
the proposed permit. A public NAY L
meeting may be held where
the Director of the Division of
Environmental Management of
finds a significant degree Ofd was inserted in the aforesaid newspaper in
public interest m a proposed �so.�ckJ 4li(VOAV follows:
permit. 1 "
A copy of the draft permit is
available by writing or calling
the Division of Environmental
Management, P.O. Box 29535,
Raleigh, North Carolina
27626.0535, [phone].
and at t The application and other in-
formation may be inspected at'ation The. Fayetteville Observer was a newspaper meeting all the requirements and
these locations during normal
qUa11f1Ca office hours. Copies of the in- ,. No. 1-597 G. S. of N. C.
le
The upontrequestd payment
n on fanare bof A from the books and files of the aforesaid corporation and publication.
the costs of reproduction. All
such comments or requests re-
garding a proposed permit
should make reference to the
NPDES permit.
Date April 17, 1996.
A. Preston Howard Jr.
P.E. Director
Division of
Environmental Title
Management
Public Notice of intent to is-
sue a State NPDES permit to Sworn or affirmed to, and subscribed before me, this da
the following: Y
1. NPDES No. NC0003573,
E.L. DuPont de Nemours &
Co., Inc. PO Drawer Z Fayette- �f _ _ _ , A.D., 19
villa, NC 28302 has applied for
a permit renewal for a facility
located at Fayetteville works, In Testimony Whereof, I have hereunto set m hand and affixed m official seal,
NC Highway 87,. Duart, Bladen _ Y y
county. The facility discharges .he day and year aforesaid.
2.0 MGD of treated domestic
and industrial wastewater from
outfall 001, and outfall 003, and
non -contact cooling water, boil-
er blowdown, condensate and i
filter backwash from outfall 002
into the Cape Fear River, a Notary PUbI1C
Class C stream in the Cape
Fear River Basin which has a
7010 flow of 791.00 cis. Flour-
ide is water quality limited. For
this parameter, the available
My Comm load capacny of the immediate day of 19
receiving water will be Con-
sumed. This may affect future
water quality based effluent
limitations for additional dis-
chargers within this portion of
the watershed. 5648
5/13
£ _
1
JUL 30 1996;
�r •
'CENTRAL FILES