Document OJqQGJ0Ly9LmvbMmnG8QDJ3xv
ACUTE TOXICITY TO FISH
TEST SUBSTANCE
Identity:Perfluorooctanoiaccid,ammonium saft;may alsobe referredto as PFOA ammonium saltA,mmonium perfluorooctanoateP,FO, FC116, FC-126, FC-169, FC-143 or as the major component ofFC1015. (Octanoicacid,pentadecafluoro-a,mmonium saftC,AS 3825-26-1)
Remarks: The testsample isFC-1015. It'psuritywas notsufficiently characterizedt,hough currentinformationindicatesisa 30% straighctarbon chain versionofFC-143-in80% water. The 3M productlotnumber was
"HOGF--205".
The following summary applies to the testsample as a mixture of the 'testsubstance in water solution with Incompletely characterized concentrations of Impurities. Data may not accurately relatetoxicityof the testsample with that of the testsubstance. Data was used to compare toxicityof the branchedlstraight chain ammonium petfluorooctanoate homologue mixture In FC-143 vs. what Is supposed to be the 10001ostraightcarbon chain ammonium perfluorooctanoate In FC-1015.
METHOD:
Method:
USEPA - TSCA 1993. 797.1400
Type: Staticacute
GLP: No
Year completed: 1996
Species: Pimephalespromelas
Supplier:AquaticBiosystems,FortCollinsC,olorado
Analyticalmonitoring:Temperature,pH, conductivitayn,d DO
Exposure period:96-hours
Statisticamlethods: LCso valuescalculateudsingtheStephan computer
program, 1983
Test fishage: Juvenile
Length and weight:
Average length 35 mm
Average weight 0.36g (wet)
Loading:0.24g fish/L
Pretreatment:None.
Test conditions:
Dilutionwater:Delonizedwateradjustedtoa hardnessof40 - 48
mg/L (asCaC03) and passed througha particulaftielteurl,traviolet
sterilizearn,d activatedcarbon.
Dilutionwater chemistry:
Hardness:
44 mg/L as CaC03
Alkalinity: 29-30 mg/L as CaC03
TOC:
<1 mg/L
Lighting:Cool-whitefluorescenltightast30 foot-candiesA. daily
photoperiodof 16 hours lighatnd 8 hours darkwitha 15 minutetransition
periodwas maintainedthroughoutthetestingperiod.
Stock and testsolutionpreparation:Test solutionwsere createdby direct individuawleightadditions. Concentrations dosing rate:Once Stabilitoyf thetestchemical solutions:Not noted Exposure vessels: 20 L glassaquariacontaining15 litertsestsolutionatan approximatedepth of 18 cm. Number of replicatest:wo Number of fishper replicate:20 Number of concentrations:fiveplusa blankcontrol Water chemistry during the study:
Conductivityrange: (0-96hours) 180 - 190 pmhos/cm (controelxposure) 300 - 320 pmhos/cm (2100mg/L exposure)*
pH range (0-96hours): 7.3- 7.9(controelxposure) 7.2- 7.7(2100mg/L exposure)*
Temperature range (0-96hours): 22.0- 22.4OC (controelxposure) 21.8- 22.5-C (2100mg/L exposure)*
Dissolvedoxygen range (0-96hours): 5.8- 9.2mg/L (controelxposure) 5.7- 9.2mg/L (2100mg/L exposure)*
2100 mg/L (secondhighestconcentratione)xposurevaluesused because the highestconcentratiounsed resultedintotalmortalitayt72 hours.
RESULTS
Nominal concentrations: Bk control5,30,830,1330, 2100, and 3330 mg/L Element values: 96-hour LC50 = 2470 (2100- 3330) mg/L
96-hourNOEC = 830 mg/L
Element valuesbased on nominalconcentrations
Remarks: Testingwas conducted on themixtureofthetestsubstanceas describedinthetestsubstanceremarks fieldT.he valuesreportedapplyto thatmixtureand notthetestsubstance.
CONCLUSIONS
The testsample 96-hour LC50forfathead'minnowwas determinedtobe 2470 mg/L witha 95% confidenceintervaolf2100 to 3330 mg/L.
Submitter: 3M Company, EnvironmentalLaboratory,P.O. Box 33331, St. Paul,Minnesota,55133
DATA QUALITY -
ReliabilitKyl:imischranking2. Testingmeets the criterifaorqualitytesting. However, sample puritywas notproperlycharacterizedand itlacksanalytical confirmationoftestsubstance concentrations.
REFERENCES
Test was conducted by T.R. WilburyLaboratoriesI,nc.,of Marblehead, Massachusetts atthe requestofthe 3M Company, Lab Request number P1624,.1996.
OTHER
Last changed: 5/25/00
Study Title
Acut* Toxicity of FC-1015 to the rathead minnow, Pimephalos pz@onol&s
Data Requirement: Guideline xumlber U.S. EPA-TSCA, Guideline 797.1400
Amthors Timothy J. Ward Jacqueline NeViUS Rok>er-t L. Soeri
study c=pleted
May 15, 1996
Sponsor
3H C=pany. Environmental Laboratory
935 Bush Avenue, Building 2-3E-09'@ St. Paul, Mizinesol-"@@
-Testing Faci:iit;@@.,
T.R.
tilhury@,Laborat@ 40 h
Study N
r'-"l-031
racqz
1. TABLX Or COWTZXTN
SECTION:
1.
Table of Contents
ll..' Index of Tables and rigures
111..
IV. General Information
V.
Introdur-tion
Vi. methods and material@
VII. Results
VIII. References
IX. Signature Page
Appendix A. Water Quality Data from Toxicity Test
PAGE
2 3 4 5 6 6 11 15 16
17
NW: 1011bury,:Study Number 10
11. IltDKX OF TAW.XS AND RIGURLS
PAGE
Table 1.
Chemical characterization of a representative
7
sample of dilution water used for the toxicity
test with fathead minnows, Pimophalos promelas,
and FC-1015.
Table 2.
Test system su=ary for the toxicity test with
9
IIC-1015 and fathead minncywa,Pimephales pr=*Ias.
Table a- survival and sublethal effect data from the
12
toxicity teat with fathead minnows, Pinaphalea
promelas, and PC-1015.
Table 4.
median lethal concentrations (LC509) from the
14
toxicity test with fathead minnows, P.Lmophalso
promelas, and FC-1015.
Table A.l. Dissolved oxygen concentration, conductivity, pH,
18
and temperature measured during the toxicity test
with fathead minnows, Pi-mephale3promelas, and
PC-1015. L
Figure 1. survival of fathead minnows, Pimephales pzomelas,
13
exposed to FC-1015 for 96 hou-s.
ury'Otu Number 1031-TH
Pag 13'.0f@@
F
111, SUXXJLRY
The promol&s,
3M Company
acute toxicity of FC-1015 to the
is described in this final report.
for 96 hours
from April
11 to
fathead minnovi Plmophalos The test was conduct4bdfor
15, 1996, at T.R. Wilbury
Laboratories,
Inc. in Marblehead,
Massachusetts.
It was conductsd
by
Jacqueline
Novius,
Jeanne
Magazu,
Koven Stevens,
Peter Kowalski,
Robert
Bc>eri,
and Timothy
W&rd
according
to the procedures
of the U.S.
L'nVi.ronmental Protection
Agency (1993).
FC-1015 was suppliard 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 dnionized
water collected at Marblehead, Massachusetts and adjusted to a hardness of
44 Mg/L as CaCoj-
Nominal concentrations of FC-1015 were 0 (control), 530, 830, 1,330
2,100, and 3,330 Mg/L.
Fathoad minnows used in the test were prc>cur.@
from a commercial
supplier and acclimated to test conditions at T.R.---
WilbUry Laboratories.
After 96 hours of exposure the control fish had an
average 35 =.
wet weight (blotted dry) of 0.36 g and an average All fish were in good condition at the beginning
total length of of the study.
Exposure of fathead tiinnows to FC-1015 ramulted in a 96 hour median
lethal concentration of 2,100 to 3,330
(LC50) of 2,470 mg/L, with a 95% confidence interval
mg/L.
-,he 96 hour no observed effect concentration
(NOEC) is 830 mg/L.
,,Wilbury,otNuudmyberInI
IV. GC"RAL I"ORXJLT1019
Mat*rial Testeds Sponsors
Test Substa=a Shipp-ad From:
Reported Purity:
Experimental Start Date:
Experimental Date:
Corpletion
rc-lol5
3H C=pany
Environmental 14f)6i&tory
935 Bush Avenue
Building 2-3Z-O9 St. Paul, Kinnonota
55144
3M Company
Environmental Laboratory'
935 Bush Avenue
Building 2-3E-O9
St. Paul, Minnesota
55106
100%
April 11, 1996
April 15, 1996
A.rchive Location for the Biological Raw Data and a copy of the Final Report;
.R. Wilbur-y Lpboratoriox, Karblehead, maseachubetts,.
Inc.
03
tof
V.
IXTRODUCTION
This study was sponsored by 3m companyo St Paul, Minnesota. The objective of the study was to determine the 24, 4B, 72, and 96 hour median lethal concentrations (LC509) of the test substance to the fathead minnow, Pimophal*s promolafir a freshwater fish, under static conditions. The study was conducted following U.S. EPA (TSCA) guidelines but at the Sponsor's request it was not conducted according to Good Laboratory Pzar-tice (GLP) rules. The report contains sections that describe the methods and materials employed in the study, and results of the
i,nvestigation. The report also contains an appendix that presents water quality data collected during the test.
VI.
METHODS
AlrD XJLTR-RIALS
TEST SUBSTANCET
The sample of FC-1015 (T.R. wilbliryLaboratories Sample Number 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 information; -rc1015, (LR P1624), see MSOS, 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 WA=RI
Water'used for acclimation of test organisms and for all toxicity
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
and continuously passed through a particle filter, ultraviolet sterilizer,
.,activatedcarbon. Water used for the test had a hardness of.44 mg/L,.'@--,
acidity of 24 mg/L and an alkalinity of 29-30 mg/L@ as -,@CaCoi*a.nd it-"*.,
ul
<10
mg/L
particulaitseLomfatter
and <1
mg/L''tota1,.,-o,r,ganiccarbon., v
Res tstoflchemical analys
a representative amp a @t.o -da r@ ar
oo tedFi@@@Table 1. A sample of dil-I.Itiowna er,,wam sent:-
rit@6i!em*i@a,ncastar; PA for.analysisof total!,r(gaiiid carbon' The
to contain @c 1.0 mg/L total'.'brg
bo
Aa,
@.lbury. 5 udy Number 1031 H
@Pa
Table 1.
chemical characterization of a representative @ample of the dsionized water used to formulate the freshwater dilution water for the toxicity test with fathead minnows, Pimeph&los promolas, and rc-1015.
Paramet*rl
unit of Measurement
Detection Limit
Measured value
Metals
Al=in=
mg/L
0.1
ND"
Arsenic
mg/L
0.01
ND
Roron
mg/L
0.5
RD
cadmium
mg/L
0.0002
ND
chromium
*g/L
0.01
ND
cobalt
mg/L
0.03
ND
Copper
ing/L
0.005
ND
li:on
mg/L
0.03
0.03
Lead
mg/L
0.005
ND
Mercury
mg/L
0.0003
ND
Nickel
mg/L
0.03
btD
silver
mg/L
0.02
ND
Zinc
mg/L
0.02
ND
Nitrate
mg/L as N
0.05
RD
Chloride
mg/L
I
rluoride
mg/L
0.1
ND
Total organic
carbon
mg/L
I
ND
Total Phosphorus
mg/L
C.03
ND
orga,nc>chlorine
Pesticides
pg/L
0.5
ND
Toxaphons
pg/L
2
M
organophosphor-us @4
Pesticides
;jg/L
0.5
ND
Dimethoate
;jg/L
2.0
;jg/L
2.0
Manc>crotophos-,.
pg/L
2.0
PC
pg/L
0.5
N 0 t ez:
Paramoia rs were measured in deionized water (used to fa. lution'water) that was collected during AugUi'i",'@41@95'@ ilyzed'- by,@Pace,'--Inc.' as part of routine water-'qual
*sting
t datecrsa at or at>ovethe cetection' iii
w.Llbury-StuY'
10 I-TH
TXST ORGAXISMs
Juvenile fathead minnows, Pimophales promelas, employed as test organisms were from a single source and were procured from Aquatic Biosyste", rort collins,coloradoon Karch 26, 1996. The species of the fish was verified using an appropriate taxonomic key. Prior to testing the fish were maintained under flow through conditions in a 270 liter fiberglass tank. During acclimation fish were not treated for disease, and they were fro* of apparent sickness, injuries, and abnormalities at tha beginning of the test. mor-tality during the final 48 hours of acclimation was less than 3%.
During the 14 day period before the start of the test the acclimationtemperaturerange was 22.0 to 22.9*C and the dissolvedoxygen concentration was always at least 7.6 mg/L. During acclimationfish were fed a dry commercial food (Tetra Kin* Staple Food, Lot # 'rM06)daily except during the 48 hours immediately preceding the test. Fish were not fed during the test. At the conclusion of the teat the control fish had an average total length of 35 = and an average vot weight of 0.36 9 (loading during the toxicity test was 0.24 g/L).
TOXICIT'Y TESTING:
The toxicity test wan performed according to the procedures of the
U.S. Env4.ro=ental Protection Agency (1993). A summary of the test system
is presented in Table 2.
A screening test was not conducted because nc=Linal concentrations
for the definitive test were provided by the sponsor. The definiti-.,teebt
was performed from April 11 to 15, 1996 with five concentrations
of test
substance and a dilution water control. Nominal concentrations
of FC-1015
were 530, 830, 1,330, 2,100, and 3,330 mg/L. Appropriate
amounts of test
substance
were added directly to dilution water in test vessels without
the use of a solvent.
Twenty fatboad minnows were indiscriminately
among two replicates
of each treatment.
The
20 liter glass aquaria that contained 15 liters
and equally distributed
test was performed
in
of test solution (water
depth water
was approximately 18 cm) . Test vessels were randomly arranged in a bath during the-,96 hour,"iest (a random numbers table was used to
select the location'of, each 'vessel) and they were loosely covered.
--@The to at was conduct.
at, 22.t 2 C.@,JL I 6 hour light and 8 ho ur dar)@@
'@@'@photoperiod .-@@'maintained
' with',-;i'-15-'@ z@inuis@t@-transition'.. period with "c@ool@'-whitit'.f@lu@@oisconIE- lights, that
was automatically
provided
a ligh
-@zintensity, of @30,'fcot@@dl
'a-.
T.X. n
umbe
31-TH
Pa
T&ble 2.
Test system summary for the toxicity test with rC-1015 and fathead minnows, Pinephaloo promoles.
Bpeciami Age/Size of Test organisms: Test Duration:
Pimephal*s promal"
Juvenilesl-0.36 grams, wet weight
iz
96 hours
Test Vesselai
20 liter glass aqu&ria
Depth of Test Media:
18 cm
Number of Replicate Text Vesselat
2
organisms per Replicate:
10
Te=perature Range:
21.7-22.5'c
Minimum Dissolved oxygen:
5.6 mg/L
t
Photoperiod: Ligl,.tIntensity:
16 hours light and 8 hours dark
with a 15 =Linuto transition period.
ik
30 fc>otcandles
watqr Quality measure--wnts:
Dissolved oxygen, pH, ta=Parature, t,t7 and conductivity daily in each ton -' vessel. B&rdness &nd alkalinity dilution water at the eta-rt of tbe, test and in the controls at the end @f the test. Temperature meastired ott least every hour in I test
Acidity, and palrticulate matter in th*' dilution water. Dilution water-
analysis is summarized in TaLblei
End Points:
24, 48 NOEC
72, and 96 hour LC50;-96'ho
A Cceptabilit@' '@@i@e'ria tNp-
'510% control mor-ta lity an accep
0,
t
rature range.
114-"44
-4;
T.R.' Wi
Stil@y Number 03
The number of surviving organisms and the occurrence of sublethal effects ,(immobilization, loss of *quilibrium, loss of reflex, excitability, discoloration, or change in b*havior) were determined visually and recorded initially and after 24, 48, 72, and 96 hours. Dead test organisms were removed when first observed. Dissolved oxygen (Tsi model 57 motor; instrument number 1), pe (Beckman model pal 12 motor; instrument number 144), conductivity (Colo Parmor motor, instrument numb-or 94), and to rature (Backman model pal 12 motor; instrument number 144, probe pHT-5) wort measured and recorded daily in each test ch-- r that corrtained live animals. The temperature in on* test vessel was recorded at least hourly during the test.
STATISTICJLL MZTEODS:
Re ults' of -:the toxicity test were inter-proted by standard statistiIcal toohniques. co=puter methods (Stephan, 1983) were used to calculate the median lethal concentrations (LC50s). )Lllcalculations were performed using nominal concentrations cf test substance and the number of live fathoad minnows. The no observed effect concentration is the highest' concentra tion of test substance that did not cause any toxicant-related mortality or sublethal effects.
y Btu y N
1031-@TH
di 10.of 19
Vil. RZBULTB
insoluble material was not noted during the test. Biological and water quality data generated by the &cut* toxicity test are presented in
Table 3 and Appendix A, respectively.
The measured concentrations of
dissolved oxygen ranged from 5.6 to 9.2 mg/L, the temperature ranged from
21.7 to 22.5*C, conductivity ranged from 180 to 390 pmhoo/cm, and pH
ranged from 7.2 to 7.9. one hundred percent survival occurred in the
control exposure and these fathead minnows did not exhibit any sublethal
offects.
The 2 48, 72, and 96 hour LCSOs for fathead minnows exposed to rc 1015 are presented in Table 4. The 96 hour LC50 for fathead minnows exposed to FC-1015 is 2,470 mg/L, with a 95% confidence interval of 2, 100 to 3,330 m4/L, The slope of the 96 hour dose response cur-ve is 10. The 96 hour NOEC is 830 mg/L.
age 'll 0 19
TiLble 3.
furvival and subl*thal effect data from the toxicity test with fathead ainnown, Pimopmlos promelas, and FC-1015.
nollinal Conc*ntration
of rc-lol5
(MgtL)
Rep.
Number kliv*
0 24 48 72 96 hr hr hr hr hr
Number Affected
0 24 48 72 96 hr hr hr hr hr
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
000 00 000 00
000 00 000 00
0000 0 000 00
000 00 000 00
000 00 000 00
040 0020 0-
tiotat At 24 hours six of the moventeen i3urvivingfish exposed to 3o330 mg/L FC-1015 exhibited letharcjy and a loss of equilibrium.
Ir,m
@,@03'
100
go
so
70 cc
0 03
40
30
20
10
0i
530
830
1330
2100
3330
ConcentrationorFC-1015 (mg/L)
Figure 1. survival of fathead minnovs,:.Fimephalon.prome., as, e rc-1015 for 96 hou.Km.
sed to
Table 4.
Xedian lethal concentrations (LC502) from the toxicity test with fathead minnows, Plm*phalos promolas, and rc-lol5.
Exposure period
Lc50
95 percent confidence limit
calculation method
24 hours
>3,330 mg/L
48 hours
2,890 mg/L
72 hours
2,470 mg/L
96 hours
2,470 mg/L
2,100 to 3,330 mg/L 2,100 to 3,330 mg/L 2,100 to 3,330 mg/L
Binomial Binomial Binomial
-at ud y N
I o 3-
VIII. ITZFZRMCZS
A.BTM. 1986. Standard Practice for Conducting Acute Toxicity Tests with risb*x , Macroinvertebrates, and Amphibians. E-729-80. In Annual Book of standards.
StaphaLn, C.E. 1983. computer Program for the Calculation U.S. EPA. Duluth, MN. Personal Communication.
of LCSO Values.
U.S. EPA. 1993. Toxic Substances Control Act Test Cu-idelineal Final Rules. Section 797.1400.
!Ilbm St y'Number 1031-TH
Pag
ay
IX. glax&TUM PAZZ
Jacctutlino M. Wevium Study Director Biologist
Robert L. Boari Coauthor
Jeanne P. Magaiu,l Aquatic Toxicologist
1,@r@ Keven m. Stevens Biologist
@4i Pete@r L. Kowalski Aquatic Toxicologist
T thy. ward
T R7@'Wil ry'Stu y.,N ar-@.
AppoiLdix A. WATZR QUALITY DATJL rRC*g TOXICITY TZST
...
--
n wi
study. N
T&bl* A. 1.
Dimmolved
oxygen
concentration,
conductivity,
PH,
and
t- rature measurtd during the toxicity test with fathead
minnows, Pimaphaloo promelas, and rc-1015.
Nominal Concentration
of FC-1015 (mg/L)
Rep.
Dissolv*d oxygen (mg/L)
0 24 48 72 96 hr hr hr hr hr
0 (control) 1 2
530
1
2
830
1
2
1,330
1
2
2,100
1
2
3,330
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
Conductivity (;mhom/cm)
0 24
48
72
96
hr hr hr hr hr
180 180 180 180 190 iso 180 iso 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
390 390 390 390 370 380 390 390
Study NLimber 103L-wn
'aam,
Table A.I. Continued.
Nominal Concentration
of FC-1015
(mg/L)
Rep.
pH
0
24
48
72
96
hr hr hr hr br
Tompor&tLLre (*C)
0 24
48
72
96
hr hr hr hr hr
0 (control) 1 2
530
1
2
830
1
2
1,330
1
2
2,100
1
2
3,330
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 22.1
22.4 22.3
22.0 22.0
22.0 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 21.8 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
0
31-TH