Document 106aEXn4p6GVMpXaw3RYzGqaX
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BACK TO MAIN T.R. W ilbury study Number 894-TH
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II. QUALITY ASSURANCE IZAT1MS1II
Submitted by I T.R. Hilbury Laboratori#, Inc. 40 Doaks Lana Marblehead, Massachusetts
Cartification:
T.R. Hilbury Laboratories, Inc. study number 894-TH, Acute Toxicity of N2803-4 to the Fathead Minnow, Pimephalea promalaa, was audited by the Quality Assurance unit for compliance with the protocol, standard operating procedures, and applicable Good Laboratory Practices (U.S. EPA, 1993). Quality assurance audits were performed and the findings reported to T.R. Hilbury Laboratories management and the study director on the following dates:
Aspect Audited
Audit Date
Reported to Study Director
Reported to
Managesient
Protocol: In-life: Draft Report: Final Report:
8/ 4/95 9/26/95 10/30/95 11/21/95
8 / 4/95 9/26/95 10/30/95 11/21/95
8 / 4/95 11/21/95 11/21/95 11/21/95
Quality Assurance Officer
T.R. Hilbury Study Number 894-TH
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SECTIONS
I. Good Laboratory Practice compliance statement II. Quality Assurance statement III. Table of Contents IV. Index of Tables and Figures V. Summary VI. General Information VII. Introduction vili. Methods and Materials IX. Results X. References XI. Signature Page XII. Protocol Amendments and Deviations
Appendix A. Hater Quality Data from Toxicity Teot
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2 3 4 5 6 7 8 8 13 17 18 19
20
T.R. Wilbury Study Number 894-th
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XV. INDEX OP TABLES AND PX0UNE8
Table 1.
chemical characterization of a representative ample of dilution water used for the toxicity test with fathead minnows, Pimephales promales, and N2803-4
Table 2.
Test system summary for the toxicity test with N2803-4 and fathead minnows, Pimephales promelas
Table 3.
Survival and sublethal effect data from the toxicity test with fathead minnows, Pimephales promelas, and N2803-4
Table 4.
Median lethal concentrations <LC50s> from the toxicity test with fathead minnows, Pimephales promelas, and N2803-4
Table A.l. Dissolved oxygen concentration, conductivity, pH, and temperature measured during the toxicity test with fathead minnows, Pimephales promelas, and
. N2803-4
Figure 1. Survival of fathead minnows, Pimephales promelas, exposed to H2803-4 for 96 hours
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11 14 16 21 15
T.R. wilbury study Number B94-TH
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The acuta toxicity of N2803-4 to tha fathaad minnow, Plmaphtlan promalaa, ia described in thia final report. Tha taut waa conducted for 3M Company for 96 hours from September 25 to 29, 1995, at T.R. Wilbury Laboratoriaa, Inc. in Marblehead, Maaaachuaatta. It waa conducted by Peter L. Kowalski, Jeanne Kagazu, Jacqueline Neviua, Keven Stevens, Peter Nevius, Robert Boeri, and Timothy Hard according to the protocol developed for T.R. Hilbury Study Number 894-TH. N2803-4 was supplied by the sponsor.
The test was performed under static conditions with five concentrations of test substance and a dilution water control at a temperature of 21.6 to 22.7*C. The dilution water was filtered deionized water collected at Marblehead, Massachusetts and adjusted to a hardness of 44 mg/L as caco,. Aeration was not required to maintain dissolved oxygen concentrations above an acceptable level.
Nominal concentrations of N2803-4 were 0 (control), 160, 250, 400, 630, and 1,000 mg/L. Fathead minnows used in the test were procured from a commercial supplier and acclimated to test conditions at T.R. Wilbur; Laboratories. After 96 hours of exposure the control fish had an average wet weight (blotted dry) of 0.19 g and an average total length of 28.6 mm. All fish were in good condition at the beginning of the study.
Exposure of fathead minnows to the test substance resulted in a 96 hour median lethal concentration (LC50) of 740 mg/L N2803-4, with a 95 confidence interval of 660 to 830 mg/L. The 96 hour no observed effect concentration (NOEC) is 400 mg/L.
T.R. wilbury study Number 894-TH
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V I . O K M R A L INFORMATION
Material Tested! sponsor!
Test Substance shipped From!
Reported Purityi
Study Initiation Date: Experimental start Date: Experimental Completion Date: Study Completion Date: Archive Location for the Biological Raw Data and a Copy of the Final Report:
N2803-4 3M Company Environmental Laboratory 935 Bush Avenue Building 2E-3E-09 St. Paul, Minnesota 55X44-1000 3M 3M center St. Paul, Minnesota 55144-1000 100
August 16, 1995 (protocol signed) September 25, 1995
September 29, 1995 November 21, 1995
T.R. Wilbury Laboratories, Inc. Marblehead, Massachusetts
T.R. Wilbury study Hujnber 894-TH
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iti rnr
V II. introduction
This study was sponsorsd by 3M Company, St Paul, Minnssota. Ths objsctivs of ths study was to datarmina tha 24, 48, 72, and 96 hour madian lathal concantrations (LC50s) of tha tast substance to tha fathaad minnow, Plaaphalaa prone!as, a frashwatar fish, undar static conditions. Tba tast protocol was basad on U.S. EPA methods (U.s. EPA, 1993). Tha raport contains sections that describe the methods and materials employed in the study, and results of the investigation. The report also contains an appendix that presents water quality data collected during tha tast.
VIIX. METHODS AND MATERIALS
TEST SUBSTANCE!
Tha sample of N2803-4 (T.R. Wilbury Laboratories Sample Number 544) was delivered to T.R. Wilbury Laboratories on September 22, 1995 in a 250 ml glass bottle within a cardboard box at ambient temperature. The attached label included the following information: "N2803-4, Corrosive, S.J. Martin, S3-4N-02778-5774, 9/13/95".
N2803-4 (a white powder) was supplied by 3M Company, St PiUl, Minnesota. Prior to use the test Bubstance was stored in the dark at room temperature. Test substance stock solutions were formulated in dilution water without the use of a solvent. The test substance was assumed to have a purity of 1 0 0 % active ingredient and to be stable under storage and testing conditions. Unused test substance will be returned to the sponsor.
DILUTION WATER:
Water used for acclimation of test organisms and for all toxicity testing was deionized water collected at T.R. wilbury Laboratories in Marblehead, Massachusetts. Water was adjusted to a hardness of 40-48 mg/L as CaC03 and stored in 500-gallon polyethylene tanks where it was aerated and continuously passed through a particle filter, ultraviolet sterilizer, and activated carbon. Results of chemical analysis of a representative sample of water are presented in Table 1.
TEST ORGANISMI
Juvenile fathead minnows, plmeptialea promelaa, employed as test
organisms were from a single source' and were procured from Aquatic
Biosystesis, tort Collins, Colorado on September 6 , 1995. The species of
the fish was verified using an appropriate taxonomic key.
:
T.R. Wilbury Study Number 894-TH
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Tab!* 1.
chamical characterization of a representative sample of dilution water uaed for the toxicity teat with fathead minnowa, Plmtphaltt promelai, and N2803-4.
Parameter1
unit of Measurement
Detection Limit
Measured Value
Metals
Aluminum
mg/L
0.1
ND*
NDArsenic
mg/L
0.01
NDBoron
mg/L
0.5
NDCadmium
mg/L
0.0002
NDChromium
mg/L
0.01
NDCobalt
mg/L
0.03
ND\
Copper
mg/L
0.005
Iron Lead Mercury
mg/L mg/L mg/L
0.03 0.005 0.0003
NN0DD.03
Nickel Silver Zinc
mg/L mg/L mg/L
0.03 0.02 0.02
NNNDDD
Nitrate Chloride Fluoride Total organic Carbon Total Phosphorus
mg/L as N mg/L mg/L
mg/L mg/L
0.05 1 0.1
1 0.03
ND ND NNDD
organochlorine Pesticides
Toxaphene
pg/L pg/L
0.5 2
NNDD
Organophosphorus Pesticides
Dimethoate TEPP Monocrotophos
PCB* 5/,;C\ '
pg/L pg/L pg/L pg/L
pg/L
0.5 2.0 2.0 2.0
0.5
NNNNDDDD ND
Noteat
1. Hetala, nitrate, chloride, fluoride, total organic carbon,
total phospborua, organochlorine pesticides, organophosphorus
pesticides, and PCBa were measured in deionized water (used to
formulate dilution water) that was collected during August,
1995 and analyzed by Pace, Inc, as part of routine water
quality testing.
;
2. ND not detected at or above the detection limit.
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Prior to testing the fish vara maintained undar flow through conditiona in a 270 liter fibarglaaa tank or a 40 liter glaaa aquarium. During acclimation fiah ware not treated for diaaaaa, they ware free of apparent sickness, injuriee, and abnorualitiea at tha beginning of tha teat, and mortality during the final 48 houra of acclimation waa laaa than 34.
During tha 14 day period before the atari of the teat the acclimation temperature range waa 2 1 . 0 to 21.9*c and the diaaolved oxygen concentration waa alwaya at leaat 7.7 mg/L. During acclimation fiah were fed a dry commercial food (Tatra Hina staple Food, Lot # TM05) daily except during the 48 houra immed.'ately preceding the teat. Fiah ware not fed during the teat. At the concluaion of the teat the control fiah had an average total length of 28.6 mm and an average wet weight of 0.19 g (loading rate during the definitive toxicity teat waa 0.13 g/L).
XOXXCXTX TESTING I
The definitive toxicity test was performed from September 25 to 29, 1995, according to T.R. Wilbury Protocol 894-TH (Acute Toxicity of N2803-4 To The Fathead Minnow, Pimephales promolas). The protocol, which was signed by the study director on August 16, 1995, is based on procedures of the u.S. Environmental Protection Agency (1993). A nummary of the teat system is presented in Table 2.
The test was conducted at a target temperature ol: 22 2*c with five concentrations of test substance and a dilution water control. Nominal concentrations of the test substance weret 0 mg/L (control), 160, 250, 400, 630, and 1,000 mg/L. Appropriate amounts of test substance were added directly to dilution water in teat vessels to formulate test media without the use of a solvent.
Twenty fathead minnows were indiscriminately and equally distributed among two replicates of each treatment. The test was performed in 20 liter glass aquaria that contained 15 liters of test solution (water depth was approximately 18 cm). Test vessels were randomly arranged in a water bath during the 96 hour test (a random numbers table was used to select the location of each vessel) and they were loosely covered. A 16 hour light and 8 hour dark photoperiod with a 15 minute transition period was automatically maintained with cool-white fluorescent lights that provided a light intensity of 30 footcandles.
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Table 2.
Test system summary for tha toxicity taat with N2803-4 and fathead minnows, Pinaphaiaa promelas.
Spaciaat
Pimephales promelns
Aga/Siza of Teat organism:
Juveniles/-0.19 grams, vet weight
Taat Duration:
96 hours
Teat Veaaala:
20 liter glass aquaria
Depth of Test Media:
18 cm
Number of Replicate Teat veaaela: 2
Organisms per Replicate:
10
Temperature Range:
21.622.7*C
Minimum Dissolved Oxygen:
6.7 sig/L
Photoperiod:
16 hours light and. 8 hours dark, with a IS minute transition period.
Light Intensity:
30 fcotcandles
Water Quality Measurements:
Dissolved oxygen, pB, temperature, and conductivity daily in each test vessel. Temperature measured at least every hour in 1 test vessel. Hardness, alkalinity, acidity, and particulate matter and TOC in the dilution water. Dilution water analysis is summarized in Table 1.
End Points:
24, 48, 72, and 96 hour LC50; 96 hour NOEC.
Acceptability Criteria:
slot control mortality and acceptable temperature range.
T.R. Wilbury Study Humb*r 894-TH
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Th* number of surviving organisms and the occurrence of sublethal effecta (immobilization, loaa of equilibrium, loaa of reflex, exoitability, diacoloration, or change in behavior) were determined viaually and recorded initially and after 24, 48, 72, and 96 houra (mortality waa monitored twice each day). Dead teat organiama were removed when firat observed. Dissolved oxygen (YSI Model 57 meter; instrument numbers 1), pH (Beckman model pHT 4 meter; instrument number 124), conductivity (Cole Parmer meter, instrument number 94), and temperature (Beckman model pHT 4 meter; instrument number 124) were measured and recorded daily in each test chamber that contained live animals. The temperature in one test vessel was recorded during the test.
STATISTICAL METHODS;
Results of the toxicity test were interpreted by standard statistical techniques. Computer methods (Stephan, 1983) were used to calculate the median lethal concentrations (LC50s). All calculations were performed by using nominal concentrations of test substance and the number of live fathead minnows. The no observed effect concentration is the highest concentration of test substance that did not cause any toxicantrelated mortality or sublethal effects.
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Tbl 3.
survival and sublethal effect data iron tha toxicity taat with fathead innow*, Platphtltt promtItt, and H2S03-4.
Nominal of N2803-4
(mg/L) 0 (control) 160
250 400
630 1,000
Rep.
Number alive
0 24 48 72 96 hr hr hr hr hr
1 10 10 10 10 10 2 10 10 10 10 10
1 10 10 10 10 10 2 10 10 10 10 10
1 10 10 10 10 10 2 10 10 10 10 10
1 10 10 10 10 10 2 10 10 10 10 10
1 10 10 10 9 8 2 10 10 8 7 7
1 10 10 2 2 2 2 10 7 0 0 0
Number affected
0 24 48 72 96 hr hr hr hr hr
00000 00000
00 00 0 00000
00000 00000
00000 00000
00000 00 000
02 000 00
Note: Affected fish were dark colored and swimming erratically.
"5*1
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Figure 1. Survival of fathead ininnova, P.Lmephales proiaelas, exposed to N2803-4 for 96 hours.
T.R. wilbury study Number 894-TH
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Tabla 4
Median lethal concantratloria (LC50) iron tba toxicity taat with fathead minnows, Plaaphalaa proaalat, and N2803-4.
Exposure period
LC50
95 percent confidence limit
Calculation method
24 hour* 48 hour* 72 hours 96 hour*
>1,000 mg/L
--
790 mg/L
630 to 1,000 mg/L
760 mg/L
630 to 1,000 mg/L
740 mg/L
660 to 830 mg/L
'-- Binomial Binomial Probit
T.R. Wilbury study Number 894-t h
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ASTM. 1966. standard practice for Conducting Acuta Toxicity Tests with Fishes, Hacroinvertebrates, and Amphibians. E-729-B0. in Annual Book of Standards.
Stephan, C.E. 1983. Computer Program for the Calculation of LC50 Values. U.S. EPA. Duluth, MM. personal Communication.
U.S. EPA. 1993. Toxic Substances Control Act Test Guidelines; Final Rules, section 797.1400.
U.S. EPA. 1993. 40 CFR Part 792. Toxic Substances Control Act (TSCA); Good Laboratory Practice standards. Code of Federal Regulations, Title 40, July 1, 1993.
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Appendix A. HATER QUALITY DATA FROM TOXICITY TEST
T.R. Wilbury Study Number 894-TH
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Tabla A.l. Diaaolvad oxygan concantration, conductivity, pH, and tamparatura maaaurad during tha toxicity taat with fathaad ninnowa, Platphtlat promalmM, and N2803-4.
Nominal
concantration
of N2803-4
(mg/L)
Rap.
Diaaolvad oxygan (mg/L)
0 24 48 72 96 hr hr hr hr hr
Conductivity (pmhoa/cm)
0 24 48 72 96 hr hr hr hr hr
0 (control) 160 250 400 630
1,000
1 2
1 2
1 2
1 2
1 2
1 2
8.5 7.2 7.5 7.2 7.5 8.5 7.4 7.5 7.3 7.6
8.5 7.7 7.5 7.1 7.4 8.5 7.7 7.5 7.2 7.5
8.5 7.8 7.5 7.1 7.6 8.5 7.8 7.5 7.0 7.6
8.5 7.7 7.5 7.1 7.4 8.5 7.6 7.5 7.1 7.2
8.5 7.6 7.4 7.0 7.1 8.5 7.4 7.4 6 . 8 7.4
8.5 7.7 7.0 6.7 7.2 8.5 7.6 7.1
140 180 160 160 150 140 180 160 160 150
160 210 170 160 160 160 210 170 170 160
170 230 180 180 180 170 230 180 180 180
190 260 210 200 2 10 190 260 2 10 2 00 2 10
250 310 270 260 260 250 310 260 260 260
280 380 340 350 340 280 380 350
T.R. Wilbury Study Number 894-TH
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Tabi* A.l. Continuad.
Nominai
PH
Concantration
ot N2B03-4
0 24 48 72 96
(mg/L)
Rap. hr hr hr hr hr
Temperatura <*C)
0 24 48 72 96 hr hr hr hr hr
0 (control) 160 250 400 630 1,000
1 2
1 2
1 2
1 2
1 2
1 2
7.3 7.4 7.5 7.5 7.6 7.3 7.0 7.5 7.5 7.6
7.4 7.4 7.5 7.5 7.6 7.4 7.5 7.5 7.5 7.6
7.5 7.5 7.5 7.5 7.6 7.5 7.4 7.5 7.5 7.6
7.5 7.5 7.5 7.5 7.6 7.5 7.5 7.5 7.5 7.5
7.5 7.4 7.5 7.5 7.5 7.5 7.4 7.5 7.5 7.5
7.5 7.4 7.5 7.5 7.5 7.5 7.4 7.5
2 2 . 2 2 2 . 2 2 2 . 1 22.5 2 2 . 1 22.2 22.2 22.0 22.6 22.1
22.0 22.1 22.1 22.6 22.1 2 2 . 1 2 2 . 1 2 2 . 1 22.7 2 2 . 0
2 1 . 8 2 2 . 0 2 2 . 0 22.5 2 2 . 0 21.9 27.0 2 2 . 2 22.4 2 2 . 0
2 1 . 6 2 2 . 1 2 2 . 1 22.5 2 2 . 0 2 1 . 8 2 2 . 1 2 2 . 0 22.5 2 2 . 0
22.0 22.1 22.0 22.6 22.0 21.9 2 2 . 1 2 2 . 0 22.5 2 2 . 0
2 1 . 8 2 2 . 0 2 2 . 0 22.5 21.9 21.8 22.0 22.1
T.R, Wilbury Study Number 894-TH
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V-T W / C_W I
u n r u TVTfT'itn_nBi- u/mjuiini vui ARCHIVED FINAL REPORT
LAB REQUEST NO. N2803 REQUESTOR NAME: SAB/GOEBEL/PICKETT DEPARTMENT: 3048 PROJECT NO: BI703004UQ DATE RECEIVED: 08/01/1995 DESC: FC-143 AND RELATED PRODUCTS ECOTOX WORK
CONTRACT LAB(S): TRWIL EXP COMP DATE: 10/04/1995 DATE COMPLETED: 03/27/1996 PROJECT LEAD: PHONE NO: 3M FAX NO: 651-778-6176
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Samples received from S.J. Martin.
Samples 1-5 sent to TRWIL on 8/11/95. An additional 4L of sample 5 sent on 8/22/95.
Sample 1 = Tetrabutyl ammonium hydroxide, 40% in water. Sample 2 = L-13492 (45% solids, 27% water, 27% IPA) Sample 3 = FC-26, 100% solids. Dissolve in 50:50 water:IPA solution. Sample 4 = FC-143, 100% solids. Sample 5 = L-13856, 15% solids. Sample 6 = L-13856, diluted by a factor of 15, tested as an effluent.
Sample #1 (Tetrabutylammonium hydroxide) - a new bottle was ordered from Aldrich because TR Wilbury needed more sample. This was lot 05922BN, red label, cat. # 17,878,0. sab 9/11/95
NOTE: All data for sample 3 (FC-26) is reported in terms of FC-26, and not
as a 50/50 mixture with isopropanol.
sab 11/21/95
NOTE: For sample #5, only a range-finding test was run for toxicity to algae. The requestor canceled the request for testing so no definitive test was run. The results for the range finder are as follows:
Test Cone.
Percent Difference in Avg. Specific Growth Rate
m0g.1/1
1 .0
296-hrs Expsure
18
11000
4 32
1000
100
EC50 (95% C.I.)
160 (100 - 1000) mg/L.
sab 2/16/96
For N2803-6, the testing was canceled before a definitive study with fish could be completed. Results reflect testing with a single concentration of 13% v/v, which showed no mortality after 96-hours, sab 3/14/96
SAMPLE DATE
CODE
DESCRIPTION RESULT
1 08/11/95 TB NH40H
Lot 10317KQ
TRWIL 48-HR-EC50 *DAPHNIA ACUTE TEST
27 MG/L
MDL or (95% C. I.) (23 - 32)
UUN I TIMO I-- LMB UM IH
04/01/2001
LAB REQUEST NO. N2803
SAMPLE DATE
CODE
ENVIRONMENTAL LABORATORY ARCHIVED FINAL REPORT
CONTINUED
DESCRIPTION RESULT
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2
MDL on (95% C.I.)
1 08/11/95 TB NH40H
Lot 10317KQ
TRWIL 96-HR-LC50 *FISH ACUTE TEST - 96 HOUR 720 MG/L
TRWIL IC50-ALGAE *ALGAE ASSAY - IC50
3.7 MG/L
(600 - 1000) (1.8 - 7.7)
2
L-13492
Lot 2
TRWIL 48-HR-EC50 *DAPHNIA ACUTE TEST TRWIL 96-HR-LC50 *FISH ACUTE TEST - 96 HOUR TRWIL IC50-ALGAE *ALGAE ASSAY - IC50
62 MG/L 960 MG/L 8.4 MG/L
(36-100) (830->1000) (5.9 - 14)
3
FC-26
Lot 135
TRWIL 48-HR-EC50 *DAPHNIA ACUTE TEST TRWIL 96-HR-LC50 *FISH ACUTE TEST - 96 HOUR TRWIL IC50-ALGAE *ALGAE ASSAY - IC50
360 MG/L 140 MG/L 90 MG/L
(300 - 500) (110 - 180) (63 - 130)
4
FC-143
Lot 427
TRWIL 48-HR-EC50 *DAPHNIA ACUTE TEST TRWIL 96-HR-LC50 *FISH ACUTE TEST - 96 HOUR TRWIL IC50-ALGAE *ALGAE ASSAY - IC50
720 MG/L 740 MG/L >1000 MG/L
5 08/16/95 L-13856
As-is
(600 - 1000) (660 - 830)
(-)
TRWIL 48-HR-EC50 *DAPHNIA ACUTE TEST TRWIL 96-HR-LC50 *FISH ACUTE TEST - 96 HOUR TRWIL IC50-ALGAE *ALGAE ASSAY - IC50
190 MG/L
(130-600)
>1000 MG/L
(-)
SEE COMMENT ABOVE
6
L -13856
1:15 diluted
TRWIL 48-HR-EC50 *DAPHNIA ACUTE TEST TRWIL 96-HR-LC50 *FISH ACUTE TEST - 96 HOUR TRWIL IC50-ALGAE *ALGAE ASSAY - IC50
1.2 % V/V
(1.0 - 1.7)
>13 % V/V
(-)
TESTING CANCELED
* = CONTRACT LAB DATA
