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/ N frU -0 5 2 .5
ACUTE TOXICITY TO FISH
TEST SUBSTANCE_______________________________________________
Identity: Perfluorooctanoic acid, ammonium salt; may also be referred to as PFOA ammonium salt, Ammonium perfluorooctanoate, PFO, FC116, FC-126, FC-169, FC-143 or as the major component of FC1015. (Octanoic acid, pentadecafluoro-, ammonium salt, CAS # 3825-26-1)
Remarks: The test sample is FC-1015. It's purity was not sufficiently characterized, though current information indicates is a 30% straight carbon chain version of FC-143 in 80% water. The 3M product lot number was "HOGE 205".
The following summary applies to the test sample as a mixture of the test substance in water solution with incompletely characterized concentrations of impurities. Data may not accurately relate toxicity of the test sample with that of the test substance. Data was used to compare toxicity of the branched/straight chain ammonium perfluorooctanoate homologue mixture in FC-143 vs. what is supposed to be the 100% straight carbon chain ammonium perfluorooctanoate in
FC-1015.
METHOD:________________________________________________________
Method: USEPA - TSCA 1993. 797.1400
Type: Static acute
GLP: No
Year completed: 1996
Species: Pim ephales prom elas
Supplier: Aquatic Biosystems, Fort Collins, Colorado
Analytical monitoring: Temperature, pH, conductivity, and DO
Exposure period: 96-hours
Statistical methods: LC50 values calculated using the Stephan computer
program, 1983
Test fish age: Juvenile
Length and weight:
Average length = 35 mm
Average weight = 0.36 g (wet)
Loading: 0.24 g fish/L
Pretreatment: None.
Test conditions:
Dilution water: Deionized water adjusted to a hardness of 40 - 48
mg/L (as C a C 0 3) and passed through a particulate filter, ultraviolet
sterilizer, and activated carbon.
Dilution water chemistry:
Hardness:
44 mg/L as C a C 0 3
Alkalinity:
29-30 mg/L as C a C 0 3
__, ^
004049
TOC:
<1 mg/L
Lighting: Cool-white fluorescent lights at 30 foot-candles. A daily
photoperiod of 16 hours light and 8 hours dark with a 15 minute transition
period was maintained throughout the testing period.
Stock and test solution preparation: Test solutions were created by direct
individual weight additions. Concentrations dosing rate: Once Stability of the test chemical solutions: Not noted Exposure vessels: 20 L glass aquaria containing 15 liters test solution at an approximate depth of 18 cm. Number of replicates: two Number of fish per replicate: 20 Number of concentrations: five plus a blank control Water chemistry during the study:
Conductivity range: (0-96 hours) 1 8 0 - 1 9 0 pmhos/cm (control exposure) 300 - 320 pmhos/cm (2100 mg/L exposure)*
pH range (0-96 hours):
7.3 - 7.9 (control exposure) 7.2 - 7.7 (2100 mg/L exposure)* Temperature range (0-96 hours): 22.0 - 22.4 C (control exposure) 21.8 - 22.5 C (2100 mg/L exposure)* Dissolved oxygen range (0-96 hours): 5.8 - 9.2 mg/L (control exposure) 5.7 - 9.2 mg/L (2100 mg/L exposure)* * 2100 mg/L (second highest concentration) exposure values used because the highest concentration used resulted in total mortality at 72
hours.
RESULTS________________________________________________________
Nominal concentrations: Bk control, 530, 830, 1330, 2100, and 3330 mg/L Element values: 96-hour LC50 = 2470 (2100 - 3330) mg/L
96-hour NOEC = 830 mg/L
Element values based on nominal concentrations
Remarks: Testing was conducted on the mixture of the test substance as described in the test substance remarks field. The values reported apply to that mixture and not the test substance.
CONCLUSIONS___________________________________________________
The test sample 96-hour LC5ofor fathead minnow was determined to be 2470 mg/L with a 95% confidence interval of 2100 to 3330 mg/L.
004050
Submitter: 3M Company, Environmental Laboratory, P.O. Box 33331, St. Paul, Minnesota, 55133 DATA QUALITY___________________________________________________ Reliability: Klimisch ranking 2. Testing meets the criteria for quality testing. However, sample purity was not properly characterized and it lacks analytical confirmation of test substance concentrations. REFERENCES____________________________________________________ Test was conducted by T.R. Wilbury Laboratories, Inc., of Marblehead, Massachusetts at the request of the 3M Company, Lab Request number P1624, 1996. OTHER________________________________________________________ Last changed: 5/25/00
004051
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study Ziti Acut Toxicity of rc-1015 to th Fathead Minnow, Plaephal* proaelas
Data Requirement! Guidalin number U.8. EPA-TSCA, Guidalin* 797.1400
Authors i 1 Timothy J. Ward
Jacqueline Neviua Robert L. Boeri
(
i study Completed
j1 1 May 15, 1996
" Sponsor 3M Company Environmental Laboratory 935 Bush Avenue Building 2-3E-09 St. Paul, Minnesota 55144
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Z I . XMDBX o r SABLES AMD FXQUltBS
Table 1.
Chemical characterization of a representative sample of dilution water used for tbs toxicity test with fathead minnows, Pimephaies proms!as, and FC-1015.
Tabla 2.
Test system summary for the toxicity test with rc-1015 and fathead minnows, Pimephaies promelas.
Table 3.
survival and sublethal effect data from the toxicity test with fathead minnows, Pimephaies promelas, and FC-1015.
Table 4.
Median lethal concentrations (LCSOs) from the toxicity test with fathead minnows, Pimephaies promelas, and FC-1015.
Table A.l.
Dissolved oxygen concentration, conductivity, pH, and temperature measured during the toxicity test with fathead minnows, Pimephaies promelas, and FC-1015.
Figure 1. survival of fathead minnows, Pimephaies promelas, exposed to FC-1015 for 96 hours. .
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III. SUXKARX
The acuta toxicity of FC-1015 to tba fathead minnow. Pimaphalaa promelas, 1 described in this final report. The test was conducted for 3M Company for 96 hours from April 11 to IS, 1996, at T.R. Wilbury Laboratories, Ino. in Harblahead, Massachusetts. it was conducted by Jacqueline Nevlus, Jeanne Magazu, Xeven Stevens, Peter Kowalski, Robert Boeri, and Timothy Hard according to the procedures of the u.S. environmental Protection Agency (1993). PC-1015 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 21.7 to 22.5*c. The dilution water was filtered deionized water collected at Marblehead, Massachusetts and adjusted to a hardness of 44 mg/L as CaCO^.
Nominal concentrations of FC-1015 were 0 (control), S30, 830, 1,330, 2,100, and 3,330 mg/L. Fathead minnows used in the test were procured from a commercial supplier and acclimated to test conditions at T.R. Wilbury Laboratories. After 96 hours of exposure the control fieh had an average wet weight (blotted dry) of 0.36 g and an average total length of 35 mm. All fish were in good condition at the beginning of the study.
Exposure of fathead minnows to FC-1015 resulted in a 96 hour median lethal concentration (LC50) of 2,470 mg/L, with a 95* confidence interval of 2,100 to 3,330 mg/L. The 96 hour no observed effect concentration (NOEC) is 830 mg/L.
HSTHOT AVAILABLE
Material Taatadt sponsor
Test substance shipped From:
Reported Purityi Experimental start Date: Experimental Completion Datet'..'::-.
FC-1015
3M Company Environmental Laboratory : 935 Bush Avenue Building 2-3E-09 st. Paul, Minnesota 55144
3H Company Environmental Laboratory 935 Bush Avenue Building 2-3E-09 st. Paul, Minnesota 55106
100*
April 11, 1996
April 15, 1996
Archive Location for the Biological Raw Data and a Copy of the Final Report
T.R. wilbury Laboratories, Inc. Marblehead, Massachusetts
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V. ZRTRODUCTIOX
This study was sponsorsd by 3H Coupany, st Paul, Mlnnaaota. Tha objective of tbs study was to datarains tha 24, 48, 72, and 96 hour median lathal concantrations (LC50s) of tha taafc aubstanca to tha fsthsad minnow, PisMpbslss pramelas, a frasbwatar fish, under atatlo conditions. Tha study w a s .conducted following U.s. EPA (TSCA) guldalinas but at tha Sponsor's request it was not conducted according to Good laboratory Practice (GLP) rules. The report 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 the test.
VI. METHODS AMD MATERIALS
TEST SUBSTANCES
The sample of FC-1015 (T.R. wilbury Laboratories Sample Humber 604) was delivered to T.R. wilbury Laboratories on April 4, 1996. The sample was delivered in a metal can within a cardboard box at ambient temperature. The test substance was contained in 1 250-ml plastic bottle. The label attached to the bottle contained the following informations "FC1015, (LR P1624), see MSDS, Susan A. Beach, 2-3E-09, (612) 778-7452, 4/2/96" .
FC-1015 (a clear liquid) was supplied by 3M Company, St Paul, Minnesota. Prior to use the test substance was stored in the dark at room temperature. The test substance was assumed to have a purity of 100% 'active ingredient and to be stable under storage and testing conditions. Unused test substance is returned to the sponsor.
DILUTION MATER I
Water used for acclimation of test organisms and for all toxicity 3,4. .tasting was deionized water collected at T.R. Wilbury Laboratories in
Marblehead, Massachusetts. Water was adjusted to a hardness of 40-48 mg/L :as CaCO, and stored in 500-gallon polyethylene tanks where it was aerated iand continuously passed through a particle filter, ultraviolet sterilizer, iand activated carbon, water used for the test had a hardness of 44 mg/L, I'iwd acidity of 24 mg/L and an alkalinity of 29-30 mg/L as CaCO,, and it contained'<10 mg/L particulate matter and <1 mg/L:total-organic; carbon. 'Results:,of chemical analysis of a representative')''sample;- of; water are presented;i n ;Table 1. A sample of dilution water?-wae sent' to Lancaster Laboratories ^Lancaster, PA for analysis of total1'organic carbon. The
sample*was determined to contain < 1.0 mg/L totali-organic carbon.
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Table 1.
chemical characterization of a representative sample of tha
deionized water uaad to formulate the freshwater dilution
water for the toxicity teat with fathead minnows, Pimephaiaa promaiaa, and r c - 1 0 1 5 .
Parameter1
Unit of Measurement
Detection Limit
Measured Value
Metals
Aluminum
Araenio
Boron
Cadmium
,chromium
Cobalt
coppar
Iron
lead
Marcury
Nickel
Silver
Zinc
Nitrate
Chloride
rluoride
Total organic
Carbon
Total Phosphorus
organochlorine
Pesticides
Toxaphene
Organophoaphorus
Pesticides
Dimethoate
TEPP
' -jj*-.1`Honocrotophos .
ft
'JflW \
P1-C*B.S 4If*t'
ti' "
X
mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L mg/L as N mg/L mg/L
mg/L mg/L
pg/L pg/L
pg/L pg/L pg/tpg/L pg/L
0.1
0.01 0.5 0.0002 0.01 0.03 0.005 0.03 0.005 0.0003 0.03 0.02 0.02 0.05
1 0.1
1
0.03
0.5 2
0.5 2.0 2.0 2.0 0.5
HD*' - ' ND HD HD ND ND ND 0.03 ND ND : ND ND ND ND
..A
ND
ND ND
ND . ND ~
'^ V,
HD
ND
.
, HD
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TEET ORGANISMI
Juvenile fathead minnows, JUasphalss proawl, employed as test organisms wara iron a single source and wara proourad from Aquatic Biosystems, rort Collins, Colorado on March 26, 1996. Tha apaciaa of tha fiah waa verified ualng an appropriate taxonomic key. Prior to taating tha fiah vara maintained under flow through eonditione in a 270 liter fiberglaaa tank. During acclimation fiah vara not treated for dieeaae, and they rare free of apparent sickness, injuriaa, and abnornalitiea at the beginning of the teat. Mortality during the final 48 houra of acclimation vaa leaa than 3t.
During the 14 day period before the start of the test the acclimation temperature range was 22.0 to 22.9*c and the dissolved oxygen concentration was always at least 7.6 mg/L. During acclimation fish were fad a dry commercial food (Tetra Min* staple rood. Lot t TM06) daily except during the 48 houra immediately preceding the teat, riah were not fed during the test. At the conclusion of the test the control fish had an average total length of 35 mm and an average wet weight of 0.36 g (loading during the toxicity teat was 0.24 g/L).
TOXICITY TESTING I
The toxicity test waa performed according to the procedures of the u . s . Environmental Protection Agency (1993). A summary of the test system
ia presented in Table 2.
A screening test was not conducted because nominal concentrations
for the definitive teat were provided by the sponsor. The definitive teat
was performed from April 11 to 15, 1996 with five concentrations of teat substance and a dilution water control. Nominal concentrations of p c-101 5 were 5 3 0 , 830, 1 ,3 3 0 , 2 ,1 0 0 , and 3 ,3 3 0 mg/L. Appropriate amounts of test
substance were added directly to dilution water in test vessels without
the use of a solvent.,
i . i ........
,.->.5, ml.
Twenty fathead minnows were indiscriminately and equally distributed among two replicates of each treatment. The teat was performed in 20 liter glass aquaria that contained 15 liters of test solution (water depth waa 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.
`'.The test was conducted at 22 t 2*C. A 16 hour light and 8 hour dark
photoperiod 'with' a '15'- minute', transition period was automatically
1maintained withicool-white^fluorescent lights that provided a light
intensity of, 30 footcandles.
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Table 3 .
Survival and sublathal effe c t data iro n tha to x ic ity ta a t w ith fa th e a d minnows, PiJMjphaia* proaulaa, and r c - 1 0 1 5 .
Xoadnal
Concentration ,
o f rc-iois ,
(mg/t>
Nuabar A iiva
0 24 48 72 86
Rap. h r hr hr hr h r
Dunbar A ffected
0 24 48 72 96
hi h r h r hr h r
0 (control) 530 830 1,330 2,100 3,330
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 9 1 10 10 10 8 8 2 10 10 10 9 9 1 10 10 2 0 0 2 10 7 2 0 0
00000 00000
00000 00000
00000 00000
00000 00000
00000 00000
0 0
4 2
0 0
0 0
_ -
Wotai At 2 hours s ix o f th e seventeen surviving fis h exposed to 3 ,3 3 0 mg/L rc -1 0 1 5 e x h ib ite d le th arg y and a lo s s o f e q u ilib riu m .
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Table 4.
Kedian lethal concentration (LCSOa) iron the toxicity teat with fathead minnow, Plaaphtl promela, and rc-1015.
Exposure period
LC50
95 percent confidence limit
Calculation method
24 hour >3,330 mg/L
48 hour
2,890 mg/L
72 hour
2,470 mg/L
96 hour
2,470 mg/L
--
2,100 to 3,330 mg/L
Binomial
2,100 to 3,330 mg/L
Binomial
2,100 to 3,330 mg/L
Binomial
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ASTM. 1986. standard Practica for Conducting Acuta Toxicity Taata with Piahaa , Kacroinvartabrataa, and Amphibians. E-729-60. la Annual Booh of standards.
staphan, C.S. 1983. computar Program for tha calculation of LCSO valuas. U.S. EPA. Duluth, MN. Farsonal Communication.
U.S. EPA. 1993. Toxic substances Control Act Tast Guidelines} Pinal Rules. Section 797.1400.
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IX. SXOKAXURI F M
U
Jacqueline M. study Director Biologist
ivius
. (5^<d
Robert L Boari Coauthor
Ar
Jeanne P. MagaiuA Aquatic Toxicologist
'He
/tr. f.;Liii... Pri Keven H. Stevens
Biologist
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Peter I>. Kowalski Aquatic Toxicologist
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Table A.l. Diaaolved oxygen concantration, conductivity, p a , and taaparature Beaaurod during the toxicity teat with fathead minnowa, pinaphaiaa pronaiaa, and rc-1015.
Nominal
concantration .
Of FC-1015
(mg/L)
Rap.
Diaaolved oxygen (mg/L)
-------------- ;-------- 0 24 48 72 96
hr hr hr hr hr
conductivity (pnhoa/cn)
---------------------0 24 48 72 96
hr hr hr hr hr
0 (control) 530 830
1,330 2,100 3,330
1 2
1 2
1 2
1 2
1 2
1 2
9.2 7.0 5.8 6.0 6.0 9.2 7.1 6.2 6.2 6.4
9.2 6.5 6.2 6.2 5.9 9.2 6.8 6.1 6.0 6.1
9.2 6.9 6.1 6.0 5.8 9.2 6.8 6.1 6.0 5.9
9.2 6.7 6.0 6.0 5.8 9.2 6.8 5.6 5.7 5.6
9.2 6.5 6.0 5.9 5.8 9.2 6.6 6.0 5.9 5.7
9.2 7.2 5.7 5.6 9.2 7.0 5.8 5.6
.
--
1B0 180 180 180 190 180 180 180 180 190
210 210 200 200 220 210 210 200 200 220
220 230 230 230 230 220 230 230 230 230
250 250 250 250 270 250 250 250 250 270
320 300 300 300 310 320 300 300 300 320
390 390 390 390 a . 370 380 390 390 --
K S tO FIM M U U i
Tabi* A.l. Continuad.
Dominai nocmunun
of rc-1015 (mg/L)
Rp.
PH
0 24 48 72 96 hr hr hr hr hr
T*mp*r*tur* (*C)
0 24 48 72 96 hr hr hr hr hr
0 (control) 530 830 1,330 2,100 3,330
i 2
1 2
1 2
1 2
1 2
1 2
7.9 7.5 7.3 7.4 7.4 7.9 7.5 7.3 7.4 7.4
7.9 7.5 7.3 7.4 7.4 7.8 7.4 7.3 7.4 7.4
7.8 7.4 7.2 7.3 7.4 7.8 7.4 7.3 7.3 7.4
7.8 7.4 7.3 7.3 7.4 7.7 7.4 7.3 7.3 7.4
7.7 7.4 7.2 7.3 7.4 7.7 7.4 7.2 7.3 7.4
7.6 7.5 7.3 7.3 7.6 7.4 7.2 7.3
__
--
22.1 22.4 22.0 22.0 22.0 22.1 22.3 22.0 22.0 22.0
22.1 22.5 22.0 22.0 22.0 21.9 22.4 21.9 22.0 21.9
21.9 22.4 21.9 22.0 21.9 21.9 22.4 22.0 22.0 21.9
21.7 22.4 21.9 21.9 21.B 21.9 22.4 21.9 21.9 21.9
21.8 22.4 21.9 21.9 21.8 22.0 22.5 21.9 22.0 22.0
21.7 22.3 21.8 21.9 __ 21.9 22.4 21.8 21.9 --
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