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1. EXHIBIT ~
2. REPORT QUALITY ASSURANCE RECORD

•

B~F..GOODFUCH

HENRY

PLANT SITE

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FIGURE 8

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FIGURE

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850

800

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RESULTS OF AN ACUTE TOXICITY IDENTIFICATION

EVALUATION (TIE) ON A FILTER EFFLUENT

SAMPLE FROM BF GOODRICH

Preparedfor:

BF Goodrich

R.R. 1, Box 15

Henry, Illinois 61537

and

Gardner, Carton and Douglas

Chicago, Illinois

EA Engineering,

Prepared

Science, and

by:

Technology,

Inc.

15 Loveton Circle

Sparks, Maryland 21152

March 1999

EA Project No. 70003.10

Report Number 3020

E H~BIT~

EA Project No.

70003.10

RESULTS OF AN ACUTE TOXICITY IDENTIFICATION

EVALUATION (TIE) ON A FILTER EFFLUENT

SAMPLE FROM BF GOODRICH

Preparedfor:

BF Goodrich

R.R. I, Box 15

Henry, Illinois 61537

and

Gardner, Carton and Douglas

Chicago, Illinois

Prepared by:

EA Engineering, Science, and Technology, Inc.

15 Loveton Circle

Sparks, Maryland 21152

~A~

“i’

William

G~odf9~~,Jr.

Date

Project Manager

W~Ct11o~h

Pate

Senior Scientist

March 1999

Report Number 3020

1. INTRODUCTION

At the request ofGardner, Carton and Douglas, EA Engineering, Science, and Technology

conducted an acute Toxicity Identification Evaluation (TIE) on a grab sample of filter effluent

from BF Goodrich, Henry, Illinois. The acute TIE methodology consisted ofthe EPA Phase I

proôedures (U.S. EPA 1991) and was performed using

Ceriodaphnia dubia

(water flea) as the

test species. The objective ofthe TIE study was to characterize the physical/chemical properties

of the compound(s) contributing to acute toxicity in the sample.

2. MATERIALS AND METHODS

2.1

SAMPLE DESCRIPTION

A grab sample of filter effluent was collected on 7 January 1999 from BF Goodrich’s Henry

facility, and shipped on wet ice via overnight carrier to EA’s Ecotoxicology Laboratory in

Sparks, Maryland. Upon receipt, the sample was logged in and assigned Aquatic Toxicology

Accession Number AT9-002. Table 1 summarizes the sample collection data. Alkalinity,

hardness, conductivity, salinity, ammonia, pH, dissolved oxygen and total residual chlorine

measurements were made on the effluent sample using methods described in APHA (1998) and

US EPA (1979), and these results are also presented in Table 1. The sample was stored in the

dark at 4°Cwhen not being used for testing.

2.2 TEST ORGANISMS

Ceriodaphnia dubia

were cultured in EA’s laboratory using synthetic moderately hard

freshwater as described below. The cultures were kept in an environmentally controlled room

at 25±2°Cwith a 16-hour light/8-hour dark photoperiod. Organisms were fed daily as

described in US EPA 1993 and thinned as necessary to maintain healthy, productive cultures.

Adults were separated from the bulk cultures at least one week prior to test initiation, placed in

individual 30-ml plastic cups (15-mi volume) in brood boards, and fed heavily. Gravid adults

were reisolated and fed the evening before the test to ensure that neonates (young) were less

than 24-hours old at test initiation.

2.3 DILUTION WATER

The laboratory water used in culturing and testing the

C. dubia

was synthetic moderately hard

freshwater (US EPA 1993). Batches of this water were made by passing deionized water

through activated carbon, adding reagent grade chemicals, and aerating overnight. The water

was stored at 25°Cunder gentle aeration until needed.

2.4

TOXICITY IDENTIFICATION EVALUATION

2.4.1 Toxicity Identification EvaluationProcedures

Chronic toxicity tests were initiated on 7 January 1999 with

Ceriodaphnia dubia

and

Pimephales

promelas,

using a suite ofthree grab samples offilter e4iluent provided by BF Goodrich. The

results ofthese test indicatedthat the second sample ofthe suite ofthree (AT9-002, collected 7

January 1999) was acutely toxic to both test species. The acute toxicity was confirmed through

the performance of acute toxicity tests initiated on this sample on 9 January. The results from

these tests are presented and discussed in EA Report #3016. An acute TIE was performed on

sample AT9-002, using

C. dubia

as the test species to allow forsmaller test solution volumes

and thus conserve sample.

The acute TIE methodology included selected manipulations from the Phase I TIE procedures

presented in U.S. EPA. 1991. This procedure is a tiered approach and involves fractionation of

the wastewaterand testing each ofthe individual fractions for acute toxicity (Figure 1). All of

the various treatments include system blanks which help ensure that potentially toxic artifacts

•

resulting from fractionation procedures are detected.

Sample AT9-002 was evaluated to determine whether treatments such as aeration, filtration, or

various pH treatments (pH3, P11ii and the initial pH of the sample at receipt pH i) were

successful in reducing the observable acute toxicity ofthe sample. Comparison ofthe aerated

versus unaerated sample test results provides an indication of the acute toxicity associated with

volatile compounds. The filtration (1.0 ~m glass fiber) treatment is designed to determine

whether toxicity is present in the suspended particulate phase or the soluble phase ofthe sample.

In addition, C18 column solid phase extraction (SPE) was performed on the composite sample

adjusted to pH3, pHi, and pH9. Removal of the nonpolar organic compounds is accomplished by

‘

passing the sample through a 6 ml C18 solid phase extraction colunm (J.T. Baker Chemical

Company, Phillipsburg, NJ). Sufficient sample volume is passed through the column (1,000 ml),

and the pass-through is evaluated for acute toxicity. Nonpolar organic compounds (molecular

weight less than 2000) that were in the effluent sample are absorbed onto the C18 column, and

thus the C18 pass-through contains a greatly reduced concentrations ofpotentially toxic non-polar

organic compounds. The C18 column can also sorb certain surfactants and several metals (e.g.,

copper).

Methanol elution was also performed on the C18 colunm. In this procedure, two 2-mi subportions

ofhigh quality methanol (total of4 ml) are passed through the column and nonpolar organic

compounds are eluted from the column. Assuming 100 percent extraction and elution efficiency,

the theoretical concentration back calculated to the original sample is 25,000 percent; or the

nonpolar organic compounds are concentrated 250 times in the methanol elutions as compared to

the original effluent concentrations. The toxicity tests forthe C18 column methanol elution take

advantage ofthe ability to concentrate the nonpolar organic compoundsby dosing the highest

treatment at fourtimes the theoretical concentration ofthe effluent (i.e., theorectical effluent

concentration of400 perccnt). This approach is conservative because not all nonpolarorganics

have 100 percent extraction and elution efficiencies using the C1~columns.

As part ofthe EPA Phase I TIE, the composited sample was evaluated using the EDTA Chelation

Test for cationic metals, and treatment with sodium thiosulfate, which reduces oxidants. It

•

should be pointed out, that these treatments are not entirely specific to either metals or oxidants,

• -

and can interact with other components in the sample. Also, these compounds do not remove the

potential toxicants from the sample; they only reduce the toxicant’s biological availability.

Evaluations were also performed on aliquots ofthe composite sample which had been pH

adjusted to pH 6.0, 7.0 and 8.0 (graduated pH test). The test pH has a substantial effect on the

toxicity of many compounds found in effluents. Changes in pH can affect the solubility, polarity,

volatility, and speciation ofa compound thereby affecting its bioavailability as well as it’s

toxicity. The graduated pH test employed the hydrogen ion buffers MES (2-N-morpholino

ethanesulfonic acid; pH

6.2), MOPS (3-N-Morpholino propanesulfonic acid; pH=7.2), and

POPSO (Piperazine-N, N’-bis’2-hydroxypropanesulfonic acid; pH=8 .2).

Figure 1 shows step-by-step procedures employed forthis TIE Phase I assessment. When the

tests on the TIE manipulated samples were initiated, the unmodified whole sample was again

evaluated (baseline test) for its acute toxicity to

C. dubia

to determine if the toxicity ofthe

composited sample changed with storage time.

Limited-scale acute toxicity tests were conducted at eac~hindividual fractionation step. The

limited-scale acute tests were used to quantifythe toxicity reduction resulting from each

fractionation treatment. Details concerning the acute toxicity testing procedures are presented in

Section 2.4.2.

A summary ofTIE Phase I (Tier I) treatment steps utilized in this study included the following:

• Initial toxicity

• Baseline toxicity (pH i)

• pH Adjustment (pH3,

pH

• Aeration (p113,pH i, pH ~

• Filtration (p113, pH i, pH ~

• C18 SPE Column (pH3,

pH i, pH 

• MeOH Elution (pH3,

pH i, pH 

• EDTA Chelation (pH i)

• Oxidant Reduction (using sodium thiosulfate)(pH i)

• Graduated pH (pH 6.0, 7.0, 8.0)

2.4.2 Acute Toxicity Tests on Fractionation Treatments

The 48-hour

C.dubia

acute toxicity tests conducted on the fractionation treatments were initiated

on 19 and 20 January 1999. Test chambers were 30 ml plastic cups containing 15 ml oftest

solution. The test organisms used in the fractionation tests were exposed to a laboratory control

ofmoderately hard synthetic freshwater, and to 100, 30, 10 and 3 percent concentrations ofeach

treatment (with the following exceptions). The baseline tests (pH

which were initiated on 19

and 20 January had five exposure concentrations (100, 30, 10, 3 and 1 percent). The tests

performed on the methanol elution fractions included 3 exposure concentrations (100, 200 and

400 percent). The graduated pH tests consisted of25 and 50 percent concentrations and a

laboratory water control. The sodium thiosulfate and EDTA tests had 3 concentrations and a

control (100, 30 and 10 percent treatment). Each test concentration and control had two

replicates of five

C. dubia

each. The system blanks were also tested with 2-replicates of 100

percent concentration with five

C. dubia

per replicate. Test concentrations were measured using

Class A glassware. Small volumes ofeffluent and dilution water were first measured in Class A

pipets, added to a graduated cylinder, and brought to volume with dilution water. All tests were

performed at 25±1°Cwith a 16-hour light/8-hour dark photoperiod. Prior to preparation oftest

solutions, a subsample ofeffluent and dilution water was brought to the target test temperature,

using a water bath.

The

C. dubia

were fed daily with a trout chow/yeast/cereal leaves solution supplemented with

algae (S.

capricornutum)

as described in USEPA (1993). Forty-eight hour LC5O values were

calculated from mortality observations performed at the end ofthe 48-hour exposure period

following Stephan (1977). Acute Toxic Units (TUa) were also calculated for each LC5O value.

The term Acute Toxic Unit is defined as:

Acute Toxic Unit (TU)

100

LC5O

where the

C. dubia

48-hourLC5O value is expressed as percent effluent.

2.5

REFERENCE

TOXICANT TESTS

conformance with EA’ 

quality assurance/quality control program, a reference toxicant test

was performed with the species tested. The

C. dubia

were exposed to the reference toxicant

sodium chloride (NaC1) to determine the 48-hour acute response of these test organisms. The

test was performed with a graded concentration series of toxicant and a dilution water control.

The results were compared to the established control chart limits set by EA.

2.6

ARCHIVES

Original data sheets, records, memoranda, notes, and computer printouts are archived at EA’s

Baltimore Office in Sparks, Maryland. These data will be retained for a period of

years

unless a longer period of time is requested by Gardner, Carton and Douglas.

3. RESULTS

The results ofthe acute toxicity tests conducted on the whole effluent sample (baseline tests) and on

the individual fractionation treatments are summarized in Table 2. The baseline tests, initiated on 19

and 20 January 1999 had a 48-hour LC5O of 17.3 percent effluent (TUa

5~8).

This was very

similar to the 48-hour LC5O value from the acute toxicity test initiated with this sample on 9 January

1999 (16.9 percent effluent) as discussed in EA Report #3016, indicating that the observed toxicity

was persistent with time.

None ofthe fractionation treatments were successful in removing, or significantly reducing the

observed acute toxicity. There were no surviving organisms in the 30 or 100 percent concentrations

of any fractionation treatment; and survival in the 10 concentrations ranged from 80

—

100 percent.

None ofthe tested methanol concentrations (100, 200 or 400 percent) had surviving organisms after

48 hours ofexposure. Similarly, with one exception, there were no surviving organisms in the 25 or

50 percent concentrations ofthe graduated pH treatments. The exception was 10 percent survival in

the pH6 25 percent concentration.

With one exception, the treatment blanks performed during this TIE had a minimum of 90 percent

survival after48 hours ofexposure, suggesting that the fractionation manipulations did not introduce

acute toxicity to the treatments. The aeration pH11 blank had 80 percent survival.

The salinity for sample AT9-002 was 6.4 ppt. Ifthis salinity was composed ofonly NaC1, it would

yield an approximate 48-hour LC5O of33 percent effluent. Since the 48-hourLC5O for this sample

ranged between 16.9 and 17.3, the observed acute toxicity could likely be caused by factors other

than the salinity, such as ammonia and non-polar organics.

The 48-hour LC5O value for the reference toxicant test performed during the month ofJanuary on

EA-cultured

C. dubia

was 1.6 g/L NaCl. The acceptable ranged based on EA Ecotoxicology

Control Charts was 1.3

—

2.5

g/L NaCl.

4. REFERENCES

American Public Health Association, American Water Works Association, Water Environment

Federation. 1998. Standard Methods for Examination of Water and Wastewater, 20th

Edition. APHA, Washington, D.C.

Stephan, C.E. 1977. Methods for calculating an LC5O, ~ Aquatic Toxicology and Hazard

Evaluation (F.L. Mayer and J.L. Hamelink, Eds.) ASTM STD 634. ASTM, Philadelphia,

Pennsylvania.

U.S. EPA. 1979. Methods for Chemical Analysis of Water and Wastes. EPA/600/4-79/020.

Environmental Monitoring and Support Laboratory, Cincinnati, Ohio.

U S EPA 1991 Methods for Aquatic ToxicityIdentification Evaluations Phase I Toxicity

Characterization

Procedures (Second Edition). EPA-600/6-91 -003. Duluth, Minnesota.

EPA. 1993. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to

Freshwater

and Marine Organisms. Fourth Edition. EPA/600/4-90/027F. U.S.

Environmental Protection Agency, Environmental Monitoring Systems Laboratory,

Cincinnati, Ohio.

-I

TABLE

I  SAMPLE COLLECTION/RECEIPT AND 

INITIAL WATER QUALITY DATA

FOR

THE BF GOODRICH FILTER EFFLUENT SAMPLE COLLECTED

7 JANUARY

1999

EA Accession Number:

AT9-002

Sample Description:

Filter Effluent

Sample Collection:

1300, 7 January 1999

Sample Receipt:

1450,

January 1999

Temperature (°C):

11.0

pH:

6.8

AlkalInity

(mg/L):

108

Hardness

(mgIL):

Conductivity (uS/cm):

15,940

Total Residual Chlorine (mg/L):

0.01

Salinity (ppt):

6.4

Dissolved Oxygen (mg/L):

5.3

Ammonia (mg/L):

194

TABLE 2

RESULTS OF ACUTE TOXICITY IDENTIFICATION EVALUATION ON EFFLUENT SAMPLE

FROM BF GOODRICH

Percent Survival (48-hours)

48-hrLC5O

~~tment

Control

j~f~~

J.Q~

3.~o

j.Q’o

(percent sample)

fli~

Baseline

(1/19/99)

100

17.3

5.8

48-hr LC5O

Control

j.Q~o

(percent sample)

ILin

pH

Adjustment

pH3

100

14.1

7.1

pH,

100

15.4

6.5

pH11

14.1

7.1

Aeration

pH3

100

17.3

5.8

pH1

100

17.3

5.8

pH11

100

17.3

5.8

Filtration

pH3

100

17.3

5.8

pH1

100

17.3

5.8

pH11

100

15.4

6.5

C~8Column

pH3

100

15.4

6.5

pH1

100

14.1

7.1

pH9

100

17.3

5.8

Sodium Thiosulfate

2.5

mg/L

100

•

17.3

5.8

5.Omg/L

100

17.3

5.8

10.0

mg/L

15.4

6.5

EDTA Chelation

0.2 mg/L

100

17.3

5.8

0.4 mgfL

100

17.3

5.8

0.8 mgfL

100

17.3

5.8

TABLE 2

(Continued)

PercentSurvival (48-hours)

48-hr LC5O

Treatment

Control

.i~

.thL~~

(nercent sample)

IL~

Baseline

(1/20/99)

100

17.3

5.8

Control iQQ~k’Q 2Q~ 4~’o

48-hr LC5O

ILi~

MeOH Elution

pH3

100

1.0

pH,

100

1.0

pH9

100

1.0

Graduated pH

Control

25~

~S2~

48-hr LC5O

TUa

pH6

100

4.0

•pH7

100

4.0

pH3

100

4.0

TABLE 3

TOXICITY IDENTIFICATION EVALUATION SYSTEM BLANKS PERFORMED

FOR

TESTING

ON SAMPLE AT9-002 COLLECTED 7 

JANUARY

1999

48-hour Survival 

•

Treatment System Blanks       

(percent) 

pH Adjustment

pH3

100

PHIl

100

Filtration

p113

100

pHi

100

pH11                

100

Aeration

100

pHi

91

pH11                

80(a)

C18

Colunm

Extraction

pH~

100

pHi

100

pH9

100

MeOH Elution

pH~

100

pHi

100

pH~

EDTA Chelation

0.2

100

0.4

100

0.8

100

Sodium Thiosulfate

2.5mg/L

100

5.Omg/L

100

10.0 

mg/L

100

(a)

Replicate B is considered anomalous and was not included in the reported data.

REPORT QUALITY ASSURANCE RECORD

Client:

Gt~-~r

Ci~r.s

O~o~

EAReportNo.:

3C~—6

Project Number:

Type Analysis:

Author:\/ir-~prl,O

-~\i~

Test

Organisms:

~.a~-~_iO ~

REPORT CHECKLIST

QA/QC

ITEM

Samples collected, transported, and received

according to

study plan requirements.

2. Samples prepared and processed according to

study plan requirements.

Data collected using calibrated equipment.

Calculations checked:

Hand calculations checked

Documented and verified statistical

procedure used.

5. Data input/statistical analyses complete and

correct.

6. Reported results

and

facts checked against

original sources.

7. Data presented in figures and tables correct

and

in agreement with text.

8. Results reviewed for compliance with study

plan requirements.

REVIEWER

_______

____

DATE

~/J~*~

~/isi99

~ ~

c//~/~9

2/i~/99

c~4

3/~/r~

?,~4 3/34’f

~J4

9. Commentary reviewed and resolved.

-.~ ~,.-_--—

_~_..

_________________

10. All study plan and quality assurance/control requirements have been met and the report is

approved:

PROJECT MAI14’AGE

DATE

ALITY

TROL

FFLC~t’

.37~/ff

DATE

SENIOR ECHN

L EVIEWER

DATE

AUTHOR

~2.

-, - -

DATE

/~?!OQ

ATS-QAl 2

3110/93