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Short-term toxicity to aquatic invertebrates

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Reference
Endpoint:
short-term toxicity to aquatic invertebrates
Type of information:
experimental study
Adequacy of study:
key study
Study period:
04 Nov 2013 – 07 Mar 2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: GLP guideline study
Qualifier:
according to
Guideline:
OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)
GLP compliance:
yes (incl. certificate)
Remarks:
Landesanstalt für Umwelt, Messungen und Naturschutz Baden-Würtemberg, Germany
Analytical monitoring:
yes
Details on sampling:
Analytical samples were taken from all test concentrations and control(s) at test start, after 24 and 48 hours. The control and all test item concentrations were analysed at 0 hours from fresh test solutions and at 24 hours from aged and fresh test solutions.
Vehicle:
no
Details on test solutions:
The necessary amount of Ammonium Niobium Oxalate for preparing the stock solution was weighed on weighing scoops and transferred to a volumetric flask. Test medium was added up to the bench mark and the solution was homogenised by shaking. The lower test solutions were prepared by dilution of the stock solution. Defined volumes of the prepared solution were transferred to each test vessels.
Test organisms (species):
Daphnia magna
Details on test organisms:
TEST ORGANISM
- Common name: water flea
- Strain: Clone V
- Source: Continuously bred in the laboratory. Originally purchased in a healthy condition from the Umweltbundesamt (Federal Environment Agency) in Berlin/Germany
- Age at study initiation (mean and range, SD): max. 24 hours old
- Method of breeding: Daphnia magna was reared as single culture where one daphnid is kept per 100 mL. The pH-value of the aerated water was within a range of 6.0 – 9.0. The dissolved oxygen was above 60 % saturation and the total hardness 140 - 250 mg/L (as CaCO3), corresponding to 7.8 - 14°dH. Daphnids reared at a temperature of 20 ± 2 °C in a climatic chamber with 16 hours of illumination and 8 hours of darkness.
- Feeding during test: none
- Food type: green alga Desmodesmus subspicatus
- Frequency: three times a week
Test type:
semi-static
Water media type:
freshwater
Limit test:
no
Total exposure duration:
48 h
Hardness:
179 mg/L CaCO3; 10 °dH
Test temperature:
18.8 – 20.1 °C
pH:
7.14 – 8.39
Dissolved oxygen:
≥ 8.6 mg/L
Nominal and measured concentrations:
control, 0.842, 2.19, 5.69, 14.8, 38.5 and 100 mg/L (nominal)
Details on test conditions:
TEST SYSTEM
- Test vessel:
- Material, size, headspace, fill volume: 100 mL glass beakers, filled with 50 mL test solution
- Aeration: none
- No. of organisms per vessel: 20
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 4
- Biomass loading rate: 10 mL of test solution for each animal

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: The test medium was water composed of dechlorinated drinking water and deionised water.
- Intervals of water quality measurement: Temperature, pH-value and oxygen concentration of the test solutions measured after 0, 24 and 48 hours. Hardness of the test water was measured on the day of application.

OTHER TEST CONDITIONS
- Photoperiod: 16 hours light, 8 hours dark

EFFECT PARAMETERS MEASURED (with observation intervals if applicable): After 24 h and 48 h the immobilised daphnids were counted. If present, behavioural changes of daphnids were recorded at 24 and 48 hours after starting the test.

TEST CONCENTRATIONS
- Spacing factor for test concentrations in main test: 2.6
- Range finding study:
Test concentrations: 0, 0.01, 0.1, 1.00, 10.0 and 100 mg/L
Reference substance (positive control):
yes
Remarks:
potassium dichromate
Duration:
48 h
Dose descriptor:
EC50
Effect conc.:
> 100 mg/L
Nominal / measured:
nominal
Conc. based on:
test mat.
Basis for effect:
mobility
Duration:
48 h
Dose descriptor:
NOEC
Effect conc.:
100 mg/L
Nominal / measured:
nominal
Conc. based on:
test mat.
Basis for effect:
mobility
Duration:
48 h
Dose descriptor:
EC50
Effect conc.:
> 34 mg/L
Nominal / measured:
meas. (geom. mean)
Conc. based on:
test mat.
Basis for effect:
mobility
Duration:
48 h
Dose descriptor:
NOEC
Effect conc.:
34 mg/L
Nominal / measured:
meas. (geom. mean)
Conc. based on:
test mat.
Basis for effect:
mobility
Details on results:
- Any observations (e.g. precipitation) that might cause a difference between measured and nominal values: After 24 and 48 hours a fine, white precipitate was observed at the test item concentration of 14.8 mg/L. More precipitate was observed at the test item concentration of 38.5 mg/L and at the highest test item concentration of 100 mg/L the bottom of the test vessel was completely covered with precipitate
Results with reference substance (positive control):
The results indicate an EC50 (24 h) of the reference item potassium dichromate between 1.0 and 2.0 mg/L. Since the results fall within the historical data generated with the reference item at the testing facility and are within the range of 0.6 – 2.1 mg/L recommended by the test guideline OECD 202, the daphnids were suitable for the determination of the toxicological effects of the test item.
Reported statistics and error estimates:
Since no immobilisation above the allowed control immobilisation of 10 % was observed at the highest test item concentration of 100 mg test item/L, no statistical determination was indicated.

Analytical monitoring:

The initial measured concentrations in the test item solutions ranged from 84% to 113% of nominal with a mean initial concentration at 101% of nominal. The measured concentrations in the aged test item solutions ranged from 11% to 45% of nominal with a mean concentration at 25% of nominal. Toxicological endpoints were therefore evaluated using nominal concentrations and actual concentrations based on the geometric means of the analysed concentration levels.

Table: Determined concentration of Ammonium Niobium Oxalate during analytical monitoring

Test item nominal [mg/L]

Nb nominal [mg/L]

Sampling

Nb

Test item actual [mg/L]

[mg/L]

% of nominal

Geometric mean*

0

0

0h fresh

n.d.

-

-

-

24h fresh

n.d.

-

24h aged

n.d.

-

0.842

0.145

0h fresh

0.147

102

67

0.564

24h fresh

0.139

96

24h aged

0.066

45

2.19

0.377

0h fresh

0.349

93

60

1.31

24h fresh

0.399

106

24h aged

0.136

36

5.69

0.979

0h fresh

0.922

94

50

2.85

24h fresh

0.987

101

24h aged

0.258

26

14.8

2.55

0h fresh

2.70

106

46

6.81

24h fresh

2.66

104

24h aged

0.52

20

38.5

6.62

0h fresh

5.59

84

33

12.7

24h fresh

7.22

109

24h aged

0.71

11

100

17.2

0h fresh

17.3

101

34

34.0

24h fresh

19.5

113

24h aged

1.94

11

Mean value fresh test solutions

101

 

 

Mean value aged test solutions

25

 

 

- = not calculated; n.d. = not detectable; LOQ = 0.251 mg/L Ammonium Niobium Oxalate corresponding to 0.0432 mg/L Nb 

*mean values of fresh test solutions and single values of aged test solutions per concentration level were used for calculation of geometric means

Table: Immobilisation of Daphnia after 48 hours

Concentration Test Item

Control

0.842

2.19

5.69

14.8

38.5

100

 

 

[mg/L]

 

immobilised daphnids after 48 h

Group 1

0

0

1

0

0

0

0

Group 2

0

0

0

0

0

0

1

Group 3

0

0

0

1

0

0

0

Group 4

0

0

0

0

0

0

0

Σ

0

0

1

1

0

0

1

%

0

0

5

5

0

0

5

 

 

Description of key information

EC50 (48h) > 100 mg/L with Daphnia magna (nominal, OECD 202)
EC50 (48h) > 34 mg/L with Daphnia magna (measured, geometric mean, OECD 202)

Key value for chemical safety assessment

Additional information

One study investigating the acute toxicity of Reaction mass of ammonium diaqua[bis(oxalate)]oxoniobate(1-) hydrate and ammonium hydrogen oxalate oxalic acid (1:1:1) dihydrate to Daphnia magna is available. The study was conducted with six concentrations of the test item in the range from 0.842 to 100 mg/L. The test was performed in a semi-static design according to OECD 202 (CBMM Europe BV, Key, 2014, Daphnia magna). After 24 hours one immobilised Daphnia each was found at 2.19, 5.69, and 100 mg/L. Thus, no significant mortality occurred at any test concentrations within 48 hours. There were, however, difficulties in the performance of the test, due to the chemical behaviour of the test item, which tends to form complexes in solution. After 24 and 48 hours a fine, white precipitate was observed at the test item concentration of 14.8 mg/L. More precipitate was observed at the test item concentration of 38.5 mg/L and at the highest test item concentration of 100 mg/L the bottom of the test vessel was completely covered with precipitate. Recovery rates were low: while analytical monitoring showed the initial mean measured concentration to be 101% of nominal, the mean measured concentration in the aged test item solutions was only 25% of nominal. The endpoints were therefore evaluated using nominal concentrations and actual concentrations based on the geometric means of the analysed concentration levels. Thus, the EC50 being > 100 mg/L (based on nominal concentration) and > 34 mg/L (based on geometric mean measured concentration).