Reaction mass of Ammonium bisethanedioato bisaquo niobate(V) (anhydrous form) and Ammonium hydrogen ethanedioate ethanedioic acid (anhydrous form)

Short-term toxicity to aquatic invertebrates

Link to relevant study record(s)

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

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

GLP compliance:

yes (incl. QA statement)

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)

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).