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

Short-term toxicity to fish

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 - 28 Feb 2013

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

GLP compliance:

yes (incl. QA statement)

Remarks:

Landesanstalt für Umwelt, Messungen und Naturschutz Baden-Würtemberg, Germany

Analytical monitoring:

yes

Details on sampling:

- Concentrations: control and 100 mg/L; fresh and aged test solution
- Sample storage conditions before analysis: Samples were mixed with 1 mL 65% nitric acid and stored refrigerated (nominally 1-10 °C) until analysis.

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
The necessary amount of Ammonium Niobium Oxalate was weighed on weighing scoops an transferred to a volumetric flask. Test medium was added up to the mark and the stock solution was homogenised by 5 minutes of ultrasonification and shaking. The solution was applied to the respective aquaria.
- Controls: blank control without test item

Test organisms (species):

Oncorhynchus mykiss (previous name: Salmo gairdneri)

Details on test organisms:

TEST ORGANISM
- Common name: Rainbow trout
- Source: Forellenzucht am Kocherursprung, Oberkochen, Germany
- Length at study initiation (length definition, mean, range and SD): 4 - 6 cm
- Feeding during test: none

ACCLIMATION
- Acclimation period: >= 12 days
- Acclimation conditions (same as test or not): same as test
- Type and amount of food: granular rearing food with approx. 2% of body weight
- Feeding frequency: daily
- Health during acclimation (any mortality observed): No mortality above 5% was observed throughout the acclimatisation period.

Test type:

semi-static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

96 h

Hardness:

10°dH (178 mg CaCO3/L)

Test temperature:

15.6 - 16.1 °C

pH:

6.57 - 8.21

Dissolved oxygen:

>= 92% of air saturation

Nominal and measured concentrations:

Nominal: 100 mg/L (17.2 mg/L niobium)
Measured mean initial (niobium): 110%
Measured mean aged (niobium): 78%

Details on test conditions:

TEST SYSTEM
- Test vessel:
- Material, size, headspace, fill volume: 25 L glass aquaria, fill volume 15 L
- Aeration: continuous aeration of the test tanks
- Renewal rate of test solution (frequency/flow rate): daily
- No. of organisms per vessel: 7
- No. of vessels per concentration (replicates): 1
- No. of vessels per control (replicates): 1
- No. of vessels per vehicle control (replicates): 1
- Biomass loading rate: max. 1 g fish/L

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: dechlorinated drinking water and deionised water
- Conductivity: 386 microS/cm
- Culture medium different from test medium: no
- Intervals of water quality measurement: temperature, pH-value and dissolved oxygen at 24h intervals

OTHER TEST CONDITIONS
- Photoperiod: 16 h light daily

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :
Fish were observed at 0, 3, 6, 24, 48, 72 and 96 h. Records were made on mortality and visible abnormalities, such as loss of equilibrium, swimming behaviour, respiratory function, pigmentation and all other observed events

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Details on results:

- No mortality was observed during the study.

Sublethal observations / clinical signs:

Table: Determined concentrations of the test item during the test

Test item Nominal (mg/L)	Niobium Nominal (mg/L)	Sampling (h)	Niobium
			(mg/L)	% of nominal	Mean initial	Mean aged (%)	Geomean
0	0	0 fresh 24 aged 24 fresh 48 aged 48 fresh 72 aged 72 fresh 96 aged	n.d. n.d. n.d. n.d. n.d. n.d. n.d. n.d.	- - - - - - - -	-	-	-
100	17.2	0 fresh 24 aged 24 fresh 48 aged 48 fresh 72 aged 72 fresh 96 aged	19.6 11.4 18.7 13.3 18.1 15.3 19.3 13.4	114 66 109 77 105 89 112 78	110	78	92

Reference 2

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

04 Jan - 08 Jan 2016

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

test procedure in accordance with national standard methods

Qualifier:

according to guideline

Guideline:

other: Japanese Industrial Standard (JIS K 0102-2013-71.)

GLP compliance:

yes

Analytical monitoring:

no

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION
- Method: 15.0 g Test item was dissolved in 1.5 L of ion-exchange water to prepare 10.0 g/L stock solution. This procedure was conducted twice to prepare total 3 L stock solution. An appropriate amount of stock solution was used to achieve the predicted test item concentrations.
- Controls: yes

Test organisms (species):

Cyprinus carpio

Details on test organisms:

TEST ORGANISM
- Common name: Common carp
- Source: CERI Kurume
- Age at study initiation: Yearling fish
- Length at study initiation: 3.4 - 3.7 cm

ACCLIMATION
- Acclimation period: After rearing in the underground water for 16 days, the fish were acclimatized in the dechlorinated water for 21 days
- Acclimation conditions (same as test or not): Temperature: 25±2°C
- Type and amount of food during acclimation:Feed for carp (Kyorin Food Industries)
- Feeding frequency during acclimation: Amount corresponding to approximately 3% of total body weight was fed twice a day in halves (once aday in all at holiday). Tue fish were fasted for 24 hours before sampling
- Health during acclimation (any mortality observed): Mortality during acclimatiz.ation was less than 5%

Test type:

semi-static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

96 h

Hardness:

35 mg/L (dilution water)

Test temperature:

24.5 - 24.7 °C (at the initial of exposure)
24.5 - 24.6 °C (at first renewal)

pH:

4.2 - 7.7 (at the initial of exposure)
4.1 - 7.8 (before renewal of test water)

Dissolved oxygen:

8.0 - 8.1 mg/L (at the initial of exposure)
7.2 - 7.9 mg/L (at first renewal)

Conductivity:

150 µS/µcm (dilution water)

Nominal and measured concentrations:

Control, 35.0 mg/L, 70.0 mg/L and 140 mg/L (nominal)

Details on test conditions:

TEST SYSTEM
Test vessel:
- Type: open
- Material, size, headspace, fill volume: 30 L glass tank and 30L/Level
- Aeration: no aeration
- Renewal rate of test solution (frequency/flow rate): renewal of test water every 24 h
- No. of organisms per vessel: 10

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Dechlorinated water [City water was treated by charcoal bed system (ORGANO Co., Ltd.)]
- pH: 7.7
- Particulate matter (suspended solids): < 1 mg/L
- Total organic carbon: < 0.5 mg/L
- Chemical oxygen demand: < 1 mg/L
- Metals (mg/L): Total mercury < 0.0005, Cadmium < 0.001, Chromium (VI) <0.01, Lead < 0.001, Arsenic < 0.005, Iron <0.01, Copper 0.001, Cobalt < 0.001, Manganese < 0.005, Aluminium <0.02, Zinc <0.1, Nickel < 0.001, Silver < 0.0001
- Pesticides (mg/L):1,2-Dichloropropane <0.002, Chlorothalonil < 0.001, Propyzamide < 0.0008, Chlomitrofen < 0.0001, Simazine < 0.0003, Thiobencarb < 0.001, Diazinon < 0.0005, Isoxathion < 0.0008, Fenitrothion <0.0003, EPN <0.0006, Dichlorvos <0.001, Iprobenfos <0.0008, PCB < 0.0005, Fluorine 0.4, Anionic surfactant <0.02
- Chlorine (residual): < 0.02 mg/L
- Alkalinity:38 mg/L
- Total hardness (Ca,Mg): 35 mg/L
- Intervals of water quality measurement: Date of Analysis January 5, 2016; lt was confirmed that the dilution water meets the criteria as stipulated in the standard operation procedure.

OTHER TEST CONDITIONS
- Photoperiod: 16 hours light/ 8 hours dark
- Light intensity: artificial light of white fluorescent lamp

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :

TEST CONCENTRATIONS
- Spacing factor for test concentrations: 2.0
- Range finding study: no range-finding test was performed

Reference substance (positive control):

yes

Remarks:

pentachlorophenol sodium salt

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

99 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Details on results:

- Mortality of control: No abnormalities were observed in control.

Results with reference substance (positive control):

- LC50: 0.286 mg/L

Reported statistics and error estimates:

Tue 96-hour LCso· value was estimated by the Doudoroff method

Sublethal observations / clinical signs:

Table 1: Biological Results:

Concentration (mg/L)	Cumulative Mortality (%)
	24 hours	48 hours	72 hours	96 hours
Control	0	0	0	0
35.0	0	0	0	0
70.0	0	0	0	0
140	100	100	100	100

Validity criteria fulfilled:

yes

Description of key information

LC50 (96h) > 100 mg/L with Oncorhynchus mykiss (nominal, OECD 203)

Additional information

Two studies are available 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 fish (Onchorhynchus mykiss and Cyprinus carpio) in a semi-static design under GLP.

The key study with Onchorhynchus mykiss was tested as a limit test at 100 mg/L test substance concentration and was performed according to OECD 203 (CBMM Europe BV, Key, 2013, Onchorhynchus mykiss). Analytical measurements showed the substance to be stable during the test with a 92% mean recovery for this test. Therefore it was justified to relate effects to nominal concentration. No mortalities occurred at 100 mg/L within 96 hours; thus the LC50 being > 100 mg/L.

The study with Cyprinus carpio was tested with four test item concentrations 35, 70 and 140 mg/L. No analytical measurement was performed. The LC50 was determined to be at 99.0 mg/L.