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Administrative data

Endpoint:
short-term toxicity to fish
Type of information:
experimental study
Adequacy of study:
key study
Study period:
December 8, 2003-December 12, 2003
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2004
Report date:
2004

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
OECD Guideline 203 (Fish, Acute Toxicity Test)
Deviations:
no
GLP compliance:
yes

Test material

Constituent 1
Chemical structure
Reference substance name:
1-BUTANESULFONAMIDE, 1,1,2,2,3,3,4,4,4-NONAFLUORO-N-METHYL-
EC Number:
614-396-3
Cas Number:
68298-12-4
Molecular formula:
C5H4F9NO2S
IUPAC Name:
1-BUTANESULFONAMIDE, 1,1,2,2,3,3,4,4,4-NONAFLUORO-N-METHYL-
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

Sampling and analysis

Analytical monitoring:
yes
Details on sampling:
- Concentrations: 4.7, 9.4, 19, 38, 75, 150 mg/L
- Sampling method: Samples of the exposure solutions were collected at 0, 24, and 96 hours. Samples were taken from the batch preparation vessel for each treatment and control group. Before renewal of test solutions at 24 hours and test termination, samples were also collected from each test chamber of the treatment and control groups. Samples were collected from middle of each vessel and transferred to a 20 mL glass sintillation vials.
- Sample storage conditions before analysis: Samples were analyzed immediately.

Test solutions

Vehicle:
no
Details on test solutions:
PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
- Method: Stock solution was prepared by dissolving MeFBSA in dilution water to a nominal concentration of 450 mg/L. Primary stock for the first test day was sepearated into five, 2L aliquots and sonicated (60 minutes). The primary stock was then recombined into one vessel and mixed via stainless steel whisk for 1-2 minutes. Test solutions were prepared via dilution of aliquots to reach test concentrations (4.7, 9.4, 18, 38, 75, and 150 mg/L). Test concentrations were not corrected for active ingredient of the test substance. Solutions were again mixed with whisk and 7.5L aliquots were placed in each respective test chambers. At 24, 48 and 72 hours, a 2.5L primary stock was prepared due to 100% mortality of fish in the 75 and 100 mg/l test chambers.
- 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

Test organisms

Test organisms (species):
Pimephales promelas
Details on test organisms:
TEST ORGANISM
- Common name: Fathead minnow
- Source: Chesapeake Cultures, Hayes Virginia
- Age at study initiation: Hatched October 31, 2003 (~38 days old)
- Length at study termination: Average of 10 fish (negative control) was 2.3 cm (Range: 1.9-2.5 cm)
- Weight at study termination: Average of 10 fish (negative control) was 0.091 g (Range 0.056 - 0.12 g)

ACCLIMATION
- Acclimation period: 14 days
- Acclimation conditions: Same as test during final 51 hours. Prior to this, acclimation temperature was ca. 3 °C lower than test temperature. Water from the same source was used in both acclimation and test period
- Type and Feeding frequency during acclimation: Fed a commercially-prepared diet supplied by Zeigler Brothers Inc., daily until 48 hrs before the test frequency.
- Health during acclimation (any mortality observed): No disease nor mortalities noted during acclimation period.
- Feeding During Test: No

Study design

Test type:
semi-static
Water media type:
freshwater
Limit test:
no
Total exposure duration:
96 h

Test conditions

Hardness:
120 mg/L CaCO3
Test temperature:
21.0-22.8°C
pH:
8.2-8.6
Dissolved oxygen:
6.5-8.7 mg/L
Conductivity:
295 umhos/cm
Nominal and measured concentrations:
Nominal: Negative control, 4.7, 9.4, 19, 38, 75, 150 mg/L
Mean measured: 4.0, 7.9, 16, 31, 62, 122 mg/L
Details on test conditions:
TEST SYSTEM
- Test vessel: 9-L glass aquaria
- Fill volume: 7.5L
- Aeration: None
- Renewal rate of test solution: At 24, 48, and 72 hours .:
- No. of organisms per vessel: 10 animals
- No. of vessels per concentration (replicates): 2
- No. of vessels per control (replicates): 2
- Biomass loading rate: 0.12 g fish/L

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Well water from 40 m deep on Wildlife Internation Ltd. site.
- Metals: All less than detection limits add
- 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: 187 mg CaCO3 (Range:184-190)
- 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: 319 lux

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) : Mortality and other effects (including visible abnormalities such as lethargy, erratic swimming, surfacing, or lying on bottom of tank) at 2, 24, 48, 72 and 96 hours.

TEST CONCENTRATIONS
- Spacing factor for test concentrations: 2x
- Range finding study: A range finding study was conducted and used to establish definitive test concentrations. However, details were not provided.
Reference substance (positive control):
no

Results and discussion

Effect concentrations
Key result
Duration:
96 h
Dose descriptor:
LC50
Effect conc.:
44 mg/L
Nominal / measured:
meas. (initial)
Conc. based on:
test mat.
Basis for effect:
mortality (fish)
Remarks on result:
other:
Remarks:
95% CI: 31 to 62 mg/L
Details on results:
- Behavioural abnormalities: At 16 mg/L, 1 fish exhibited erratic swimming at 48 hours but appeared normal at 72 hours. At 31 mg/L (24 hours) 2 fish were lethargic which grew to all 20 fish at 48 hours. At 72 hours 18 of the fish were lethargic and two fish were surfacing. At 96 hours 17 fish were lethargic and 3 were surfacing, but no mortality was observed at the end of the experiment. At 62 mg/L (2 hours), 5 fish were surfacing and 8 were lethargic. All fish were dead by 24 hours.
- Mortality of controls: None
- 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 96 hour LC50 and 95% CI's were calculated binomial probability with nonlinear interpolation using US EPA methods.

Any other information on results incl. tables

Sublethal observations / clinical signs:

Table 1. Measured concentrations of MeFBSA in Freshwater

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

-

 

 

4.7

0

4.18

88.9

4.0

85

 

1

3.78

80.3

 

 

 

1

3.87

82.4

 

 

 

4

3.98

84.7

 

 

 

4

4.03

85.6

 

 

9.4

0

8.34

88.7

7.9

84

 

1

7.84

83.4

 

 

 

1

7.62

81.1

 

 

 

4

7.89

83.9

 

 

 

4

7.80

83.0

 

 

19

0

17.0

89.5

16

84

 

1

15.9

83.7

 

 

 

1

15.6

82.3

 

 

 

4

15.4

81.8

 

 

 

4

15.4

81.1

 

 

38

0

34.1

89.8

31

82

 

1

31.0

81.6

 

 

 

1

31.0

81.5

 

 

 

4

29.4

77.3

 

 

 

4

30.4

80.0

 

 

75

0

66.7

89.0

62

83

 

1

60.4

80.6

 

 

 

1

59.7

79.6

 

 

 

4*

-

-

 

 

 

4*

-

-

 

 

150

0

132

88.3

122

81

 

1

117

78.1

 

 

 

1

117

78.0

 

 

 

4*

-

-

 

 

 

4*

-

-

 

 

* indicates that no sample was submitted due to 100% mortality at previous sampling.

LOQ was 1.00 mg/L, calculated as the product of the lowest calibration standard (0.1 mg/L) and the dilution factor of the matrix blanks (10.0)

Table 2. Cumulative Mortality and Clinical Observations

Mean Measured concentration (mg/L)

Replicate

# Fish Exposed

2 Hours: # Dead/ Effects

24 Hours: # Dead/ Effects

48 Hours: # Dead/ Effects

72 Hours: # Dead/ Effects

96 Hours: # Dead/ Effects

Cumulative % Mortality

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

4.0

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

7.9

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

16

A

10

0/ 10 AN

0/ 10 AN

0/ 10 AN

0/ 10 AN

0/ 10 AN

0

 

B

10

0/ 10 AN

0/AN

0/ 9 AN, 1 E

0/ 10 AN

0/ 10 AN

0

31

A

10

0/ 10 AN

0/ 8 AN; 2 C

0/ 10 C

0/ 10 C

0/ 1 A; 9 C

0

 

B

10

0/ 10 AN

0/ 10 AN

0/ 10 C

0/ 2 A; 8 C

0/ 2  A; 8C

0

62

A

10

0/ 5A; 1 R: 4C

10/-

10/-

10/-

10/-

100

 

B

10

0/ 2 AN; 4 A; 4 C

10/-

10/-

10/-

10/-

100

122

A

10

10/-

10/-

10/-

10/-

10/-

100

 

B

10

10/-

10/-

10/-

10/-

10/-

100

Observed effects: AN-Appear normal, R-lying on bottom, C-lethargy, E-erratic swimming, A-surfacing.

Applicant's summary and conclusion

Validity criteria fulfilled:
yes
Remarks:
<10% mortality in controls (0%), DO >60% (5.2 mg/L) ASV (6.5-8.7 mg/L)
Conclusions:
96 hour LC50 of 44 mg/L (OECD 203) in Pimephales promelas.
Executive summary:

The 96 hour LC50 of MeFBSA to Pimephales promelas was determined according to OECD 203 guidelines. Nominal concentrations of 4.7, 9.4, 19, 38, 75, 150 mg/L (measured concentrations of 4.0, 7.9, 16, 31, 62, 122 mg/L) and a negative control, were run using 10 animals per tank, with two replicates per concentration. Sublethal effects with no mortality were observed at 31 mg, while complete mortality occurred within 24 hours at 62 mg/L.  An LC50 of 44 mg/L (measured concentrations) was determined.

This study was sufficiently documented, followed an international standard method, and is GLP compliant. As such, it was given a Klimish rating of 1, reliable without restrictions. The results from this study are considered suitable for Risk Assessment, Classification and Labeling, and PBT analysis.

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