1,1,2,2,3,3,4,4,4-nonafluoro-N-methylbutane-1-sulfonamide

Short-term toxicity to aquatic invertebrates

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

November 4, 2003-November 6, 2003

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

no

GLP compliance:

yes

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch number of test material: 3M SMMD EHSR, Lot #3
- Purity: 97.25%
- Physical state: off white crystalline powder

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: Ambient conditions

Analytical monitoring:

yes

Details on sampling:

- Concentrations: 3.1, 6.3, 13, 25, 50, 100 mg/L
- Sampling method: On Day 0, samples were collected from batches of test solutions prepared for each treatment. Samples were also collected from the 24-hour old test solutions in each test chamber and at the test termination. All samples were collected at mid-depth and placed in glass vials.
- Sample storage conditions before analysis: Samples were analyzed immediately.

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
Method: A 1L stock solution was prepared via sonicating MeFBSA in dilution water (60 minutes) at a nominal concentration of 100 mg/L. Test solutions were prepared by dilution primary stock with dilution water until 3.1, 6.3, 13, 25 and 50 mg/L test concentrations were reached. Test concentrations were not corrected for active ingredient of the test substance. Solutions were then mixed via inversion. After mixing, approximately 250 mL aliquots of each test solutions were placed in each respective test chamber to condition for 24-hours. The procedure for preparing the primary stock and test solutions was repeated for exposure solutions. Solutions for 24-h renewal were freshly prepared.
- Controls: Negative control (dilution water), test medium without substance or other additives.
- Chemical name of vehicle (organic solvent, emulsifier or dispersant): No vehicle
- Evidence of undissolved material (e.g. precipitate, surface film, etc.): None, solution appeared clear and colorless
- Other relevant information: None

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: Water flea
- Age at study initiation: <24 hours
- Source: Wildlife International Ltd. Cultures
- Feeding during test : No
- Frequency: Once daily during culture
- Culture conditions: Adult daphnids were cultured in well water from the same source used during the test. During the 2 week holding period adults showed no signs of disease or stress. Water temperatures were 19.4 - 20.8°C, pH was 8.1 - 9.0, and dissolved oxygen ranged from 7.4 - 9.0 mg/L. Daphnids in the cultures were fed a mixture of yeast, Cerophyll®, and trout chow plus a suspension of freshwater green algae (Selenastrum capricornutum), daily. Neonate daphnids were obtained from four individual adults

Test type:

semi-static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

48 h

Hardness:

Day 1: 128 mg/CaCO3, Day 2: 132 mg/CaCO3

Test temperature:

19.5-20.8 °C

pH:

8.0-8.4

Dissolved oxygen:

7.8-8.4 mg/L

Conductivity:

Day 1: 310 umhos/cm, Day 2: 320 umhos/cm

Nominal and measured concentrations:

Nominal: 3.1, 6.3, 13, 25, 50, 100 mg/L
Mean measured concentrations: 2.9, 6.0, 12, 24, 47 and 90 mg/L

Details on test conditions:

TEST SYSTEM
- Test vessel: 250 mL glass beakers
- Fill volume: 225mL, 6.6 cm depth
- Aeration: No
- Renewal rate of test solution (frequency/flow rate): Renewed at 24 hours
- No. of organisms per vessel: 10
- No. of vessels per concentration (replicates): 2
- No. of vessels per control (replicates): 2

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Well water from 40 m deep on Wildlife International Ltd. site. Water was sand-filtered to remove particles >25 um and aerated in a holding tank. Prior to use, water was filtered to 0.45 um and UV sterilized.
- Metals: All less than detection limits
- Na: 18.6 mg/L
- K: 5.45 mg/L
- Ca: 28.2 mg/L
- Mg: 11.6 mg/L
- Pesticides: All less than detection limits
- Alkalinity: Average: 183 mg CaCO3 (Range:184-186)
- Ca/mg ratio: 2.43
- TOC: <1 mg C/L
- Culture medium different from test medium: No
- Intervals of water quality measurement: Water was measured in the 4 weeks preceding the test and immediately at test initiation. Temperature, DO, and pH were measured daily.

OTHER TEST CONDITIONS
- Adjustment of pH: None
- Photoperiod: 16 hour light: 8 hours dark with 30 minute transition periods. Fluorescent lights similar to natural sunlight (Colortone® 50).
- Light intensity: 283-291 lux

EFFECT PARAMETERS MEASURED : Immobilization, mortality and other signs of toxicity (lethargy) at 2, 24 and 48 hours.

Reference substance (positive control):

no

Key result

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

17 mg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

test mat.

Basis for effect:

mortality

Remarks on result:

other:

Remarks:

95% CI: 12-24 mg/L

Details on results:

- Mortality of control: One mortality in the control
- Behavioral abnormalities: Behavioral abnormalities were reported at 2 hours (all 20 invertebrates lethargic) at exposure concentration of 47 mg/L and at 48 hours, 2 invertebrates exposed at 24 mg/L, were lethargic.
- Other adverse effects control: None reported
- Effect concentrations exceeding solubility of substance in test medium: No

Results with reference substance (positive control):

No reference substance test run.

Reported statistics and error estimates:

The 48 hour EC50 and 95% CI's were calculated binomial probability with nonlinear interpolation using the computer software of C. E Stephen (Methods for Calculating an LC50, Aquatic Toxicology and Hazard Evaluations. American Society for Test and Materials. Publication Number STP 634, pp 65-84).

Table 2. Cumulative Percent Mortality, Immobility and Effects Observed

	Replicate	# Daphnia Exposed	2 Hours: Cumulative Dead/ # Immobile	Effects	24 Hours: Cumulative Dead/ # Immobile	Effects	48 Hours: Cumulative Dead/ # Immobile	Effects	% Immobile and Dead per concentration
Blank control	A	10	0/0	10 AN	0/0	10 AN	0/1	9 AN	5
	B	10	0/0	10 AN	0/0	10 AN	0/0	10 AN
2.9	A	10	0/0	10 AN	0/0	10 AN	0/0	10 AN	0
	B	10	0/0	10 AN	0/0	10 AN	0/0	10 AN
6.0	A	10	0/0	10 AN	0/0	10 AN	0/0	10 AN	5
	B	10	0/0	10 AN	0/0	10 AN	0/1	9 AN
12	A	10	0/0	10 AN	0/0	10 AN	0/1	9 AN	5
	B	10	0/0	10 AN	0/0	10AN	0/0	10 AN
24	A	10	0/0	10 AN	0/ 0	10 AN	5/5	-	90
	B	10	0/0	10 AN	0/0	10 AN	6/2	2C
47	A	10	0/0	10 C	10/ -	-	-	-	100
	B	10	0/0	10 C	10/ -	-	-	-
90	A	10	0/10	-	-	-	-	-	100
	B	10	0/10	-	-	-	-	-

Observed effects: AN-Appear normal, C-lethargy

- indicates that there was 100% mortality or immobilization in the sample

Validity criteria fulfilled:

yes

Remarks:

<10% mortality in controls (5%), Dissolved oxygen concentration was ≥ 3 mg/L during test period (DO=7.8-8.4)

Conclusions:

48 hour EC50 of 17 mg/L (OECD 202) in Daphnia magna

Executive summary:

The 48 hour EC50 of MeFBSA to Daphnia magna was determined according to OECD 202 guidelines. Nominal concentrations of 3.1, 6.3, 13, 25, 50, 100 mg/L, and a control, were run using 10 animals per vessel, with two replicate per concentration. An EC50 of 17 mg/L (measured concentration) was determined.

The study was well-documented, followed an international standard method and is GLP compliant. The study is considered reliable without restrictions. The results from this study are considered suitable for Risk Assessment, Classification and Labeling, and PBT Analysis.

Reference 2

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

November 10, 2003-November 14, 2003

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

EPA OPPTS 850.1035 (Mysid Acute Toxicity Test)

GLP compliance:

yes

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
-Source and lot/batch number of test material: 3M SMMD EHSR, Lot #3
- Purity: 97.25%
- Physical state: off white crystalline powder

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: Ambient conditions

Analytical monitoring:

yes

Details on sampling:

- Concentrations: 0.47, 0.95, 1.9, 3.8, 7.5, 15 mg/L
- Sampling method: Samples of the exposure solution were collected at test initiation, 24 hours, and test termination, to measure dissolved MeFBSA concentrations. Test initiation samples were taken from the batch preparation vessel of each treatment and control group. Prior to test solution renewal at 24 hours and test termination, samples were collected from each test chamber of each treatment and control group. All samples were collected, from mid-depth and placed in 20-mL glass scintillation vials.
- Sample storage conditions before analysis: Samples were analyzed immediately.

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances):
- Method: A primary stock solution was prepared by dissolving MeFBSA in dilution water at a concentration of 15 mg/L (highest concentration). Primary stock was separated into three, 2L aliquots and sonicated. After mixing, the primary stock solution was recombined into one stock (6L). Test solutions were prepared via dilution of aliquots to reach test concentrations of 0.47, 0.94, 1.9, 3.8, and 7.5 mg/L. Test concentrations were not corrected for percent active ingredient of the test material. All test solutions were mixed with a stainless-steel whisk. After mixing, 1500 mL aliquots of each test solution were placed in each respective test chamber. The procedure for preparing the primary stock and test solutions was repeated at each renewal period.
- Controls: Negative control (dilution water), test medium without substance or other additives.
- Chemical name of vehicle (organic solvent, emulsifier or dispersant): No vehicle
- Evidence of undissolved material (e.g. precipitate, surface film, etc.): None, solution appeared clear and colorless
- Other relevant information: None

Test organisms (species):

Americamysis bahia (previous name: Mysidopsis bahia)

Details on test organisms:

TEST ORGANISM
- Common name: Saltwater mysids
- Age at study initiation: <24 hours
- Source: Wildlife International Ltd. cultures
- Feeding during test : Yes
- Frequency: Once daily during culture and test to prevent cannibalism.
- Culture conditions: Adult mysids were cultured in saltwater from the same source at approximately the same temperature used during the test. Adults showed no signs of disease or stress during the 2 weekholding period. Water temperatures during the holding period were 25.2 - 26.0°C, pH was 7.7 - 8.0, dissolved oxygen ranged from 6.4 - 6.7 mg/L, and salinity at 20-23 ppt. Mysids in the cultures were fed brine shrimp Artemia nauplii (Brine Shrimp Direct, Ogden), occasionally enriched with ALGAMAC-2000 (Aquafauna, Hawthorne, California).

Test type:

semi-static

Water media type:

saltwater

Limit test:

no

Total exposure duration:

96 h

Test temperature:

23.3-25.3 °C

pH:

8.1-8.3

Dissolved oxygen:

6.8-7.4 mg/L

Salinity:

20 ppt

Nominal and measured concentrations:

Nominal: 0.47, 0.94, 1.9, 3.8, 7.5, 15 mg/L
Mean measured concentrations: 0.35, 0.69, 1.4, 2.8, 5.7, 12 mg/L

Details on test conditions:

TEST SYSTEM
Test vessel: 2L glass beakers
- Fill volume: 1.5 L volume, depth 12.4 cm
- Aeration: No
- Renewal rate of test solution (frequency/flow rate): Renewed at 24, 48 and 72 hours
- No. of organisms per vessel: 10
- No. of vessels per concentration (replicates): 2
- No. of vessels per control (replicates): 2

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Natural seawater collected at Indian River Inlet, Delaware. Filtered and diluted to salinity of 20‰ with well water. Seawater was passed through a sand filter to remove particles greater than 25um and a second filter (0.45um) to remove microorganisms and fine particles.
- Metals: All less than detection limits
- Na: 18.6 mg/L
- K: 5.45 mg/L
- Ca: 28.2 mg/L
- Mg: 11.6 mg/L
- Pesticides: All less than detection limits
- Ca/mg ratio: 2.43
- Culture medium different from test medium: No
- Intervals of water quality measurement: Water was measured in the 4 weeks proceeding the test and immediately at test initiation. Temperature, DO, and pH were measured daily.

OTHER TEST CONDITIONS
- Adjustment of pH: None
- Photoperiod: 16 hour light: 8 hours dark with 30 minute transition periods. Fluorescent lights similar to natural sunlight (Colortone® 50).
- Light intensity: 289 lux

EFFECT PARAMETERS MEASURED :Mortality and other signs of toxicity (lethargy, erratic swimming) at 3, 25.5, 48, 72 and 96 hours

RANGE-FINDING STUDY
- Results used to determine the conditions for the definitive study: A range finding study was conducted and used to establish definitive test
concentrations. However, details were not provided.

Reference substance (positive control):

no

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

2.4 mg/L

Nominal / measured:

meas. (not specified)

Conc. based on:

test mat.

Basis for effect:

mortality

Remarks on result:

other:

Remarks:

95% CI 1.4-2.8 mg/L

Details on results:

- Mortality of control: No mortality in the control.
- Behavioral abnormalities: See Table 2
- Other adverse effects control: None reported
- Effect concentrations exceeding solubility of substance in test medium: No
- Any observations that might cause a difference between measured and nominal values: See Table 1. For fresh medium samples, recoveries were 85.9 to 96.3%. However, old solutions had recoveries in the range of 66.0-78.4% with best recoveries of 76.2-78.4% at the highest loading rate. Initial concentrations were not measured for the renewal solutions and each replicate for the old solutions was entered into the average individually. As such, the initial concentrations skew the average recoveries. Time-weighted average concentrations could not be calculated based on the analytical results.

Results with reference substance (positive control):

No reference substance test run.

Reported statistics and error estimates:

The 96 hour LC50 and 95% CI's were calculated binomial probability with nonlinear interpolation using the computer software of C. E Stephen (Methods for Calculating an LC50, Aquatic Toxicology and Hazard Evaluations. American Society for Test and Materials. Publication Number STP 634, pp 65-84).

Table 1. Measured Concentrations in Filtered Seawater

Concentration (mg/L)	Sampling Time (Day)	Measured concentration MeFBSA (mg/L)	% of Nominal	Mean Measured concentration (mg/L)	Mean Measured % of Nominal
Blank control	0	<LOQ	-	-	-
	1	<LOQ	-
	1	<LOQ	-
	4	<LOQ	-
	4	<LOQ	-
0.47	0	0.404	85.9	0.35	74
	1	0.337	71.7
	1	0.353	75.1
	4	0.323	68.7
	4	0.330	70.2
0.94	0	0.820	87.2	0.69	73
	1	0.678	72.1
	1	0.693	73.8
	4	0.620	66.0
	4	0.641	68.2
1.9	0	1.67	88.2	1.4	74
	1	1.36	71.5
	1	1.40	73.7
	4	1.33	69.9
	4	1.31	68.7
3.8	0	3.37	88.7	2.8	74
	1	2.71	71.3
	1	2.79	73.5
	4	2.58	67.9
	4	2.68	70.5
7.5	0	6.76	90.2	5.7	76
	1	5.60	74.6
	1	5.65	75.3
	4	5.17	69.0
	4	5.32	70.9
15	0	14.4	96.3	12	80
	1	11.6	77.3
	1	11.8	78.4
	4	11.6	77.5
	4	11.4	76.2

LOQ was 0.250 mg/L, calculated as the product of the lowest calibration standard (0.005 mg/L) and the dilution factor of the matrix blanks (50.0)

Table 2. Cumulative % Mortality and Clinical Observations

	Replicate	# Mysids Exposed	3 Hours: Cumulative Dead	Effects	25.5 Hours: Cumulative Dead	Effects	48 Hours: Cumulative Dead	Effects	72 Hours: Cumulative Dead	Effects	96 Hours: Cumulative Dead	Effects	% Dead per concentration
Blank control	A	10	0	10 AN	0	10 AN	0	10 AN	0	10 AN	0	10 AN	0
	B	10	0	10 AN	0	10 AN	0	10 AN	0	10 AN	0	10 AN
0.35	A	10	0	10 AN	0	10 AN	0	10 AN	0	10 AN	0	10 AN	5
	B	10	0	10 AN	0	10 AN	0	10 AN	0	10 AN	1	9 AN
0.69	A	10	0	10 AN	0	10 AN	0	10 AN	0	10 AN	0	1 E, 9 AN	10
	B	10	0	10 AN	0	10 AN	0	10 AN	0	1 E, 9 AN	2	8 AN
1.4	A	10	0	10 AN	0	10 AN	0	10 AN	1	1 E, 2 C, 6 AN	1	2 E, 7 AN	30
	B	10	0	10 AN	0	10 AN	1	1 C, 8 AN	2	1 C, 7 AN	5	5 AN
2.8	A	10	0	10 AN	0	10 AN	2	1 C, 7 AN	3	2 E, 5 AN	4	1 C, 5 AN	55
	B	10	0	10 AN	2	8 AN	5	5 AN	5	1 E, 4 AN	7	3 NA
5.7	A	10	0	10 AN	0	10 AN	3	1 C, 6 AN	3	5 E, 2 AN	7	2C, 1 AN	55
	B	10	0	10 AN	1	9 AN	2	8 AN	2	6 E, 2 C	4	6 AN
12	A	10	0	3E; 7 AN	4	2 C, 4 AN	9	1 AN	9	1 C	10	-	100
	B	10	0	1E, 9AN	6	2 C, 2 AN	7	1 E, 2 AN	9	1 C	10	-

Observed effects: AN-Appear normal, C-lethargy, E- erratic swimming

- indicates that there was 100% mortality in the sample

Validity criteria fulfilled:

yes

Remarks:

<10% mortality in controls (0%), abnormal behavior in controls (no)

Conclusions:

96 hour LC50 of 2.4 mg/L (EPA OPPTS 850.1035) in Americamysis bahia

Executive summary:

The 96 hour LC50 of MeFBSA to Americamysis bahia was determined according to EPA OPPTS 850.1035 guidelines. Nominal concentrations of 0.47, 0.95, 1.9, 3.8, 7.5, 15 mg/L, and a control, were run using 10 animals per vessel, with two replicate per concentration. An LC50 of 2.4 mg/L (measured concentration) was determined.

The study was sufficiently well documented, followed an international standard method and is GLP compliant. The study is considered reliable with restrictions. The results from this study are considered suitable for Risk Assessment, Classification and Labeling, and PBT Analysis.

Description of key information

48 hour EC50 of 17 mg/L (OECD 202) in Daphnia magna

96 hour LC50 of 2.4 mg/L (EPA OPPTS 850.1035) in Americamysis bahia

Key value for chemical safety assessment

Fresh water invertebrates

Fresh water invertebrates

Effect concentration:

17 mg/L

Marine water invertebrates

Marine water invertebrates

Effect concentration:

2.4 mg/L

Additional information

A 48 hour EC50 of MeFBSA to Daphnia magna was determined according to OECD 202 guidelines. Nominal concentrations of 3.1, 6.3, 13, 25, 50, 100 mg/L, and a control, were run using 10 animals per vessel, with two replicate per concentration. An EC50 of 17 mg/L (measured concentration) was determined.

A 96 hour LC50 of MeFBSA to Americamysis bahia was determined according to EPA OPPTS 850.1035 guidelines. Nominal concentrations of 0.47, 0.95, 1.9, 3.8, 7.5, 15 mg/L, and a control, were run using 10 animals per vessel, with two replicate per concentration. An LC50 of 2.4 mg/L (measured concentration) was determined.

The studies were sufficiently well documented, followed an international standard method and is GLP compliant. The studies are considered reliable with restrictions. The results from these studies are considered suitable for Risk Assessment, Classification and Labeling, and PBT Analysis.