Nickel iron chromite black spinel

Short-term toxicity to aquatic invertebrates

Administrative data

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2013-10-22 to 2013-10-24

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2014

Report date:

2014

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Version / remarks:

, adopted 2004-04-13

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method C.2 (Acute Toxicity for Daphnia)

Version / remarks:

, 2008

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

other: OECD Series on testing and assessment, Number 29. Guidance document on transformation/dissolution of metals and metal compounds in aqueous media. ENV/JM/MONO (2001)9, 23-July 2001.

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

signed 2011-02-07

Test material

Test material information

Constituent 1

Reference substance name:

Nickel iron chromite black spinel

EC Number:

275-738-1

EC Name:

Nickel iron chromite black spinel

Cas Number:

71631-15-7

Molecular formula:

(Ni,Fe)(Fe,Cr)2O4

IUPAC Name:

Nickel iron chromite black spinel

Test material form:

solid: particulate/powder

Remarks:

migrated information: powder

Details on test material:

- Name of test material (as cited in study report): nickel iron chromite black spinel
- Molecular formula: Ni1-xCr2-y-zFeyMnx+zO4 (spinel structure type (Ni, Fe)(Fe, Cr)2O4)
- Physical state: solid, black powder, odourless
- Stability: December 31, 2023
- Storage condition of test material: store separate from food and drinks, dry in closed containers and protected places. Keep containers air-tight.
- Relative density: 5.16

Specific details on test material used for the study:

Details on properties of test surrogate or analogue material (migrated information):
not applicable

Sampling and analysis

Analytical monitoring:

yes

Details on sampling:

- Sampling method/Sample storage conditions before analysis:
The concentrations of dissolved chromium, iron, manganese and nickel in the aqueous phase of the test were measured. Dissolved chromium, iron, manganese and nickel concentrations were measured in all test solutions sampled at the beginning of the test prior to addition of the daphnids and in pooled samples from each treatment level after 48 hours of exposure.

Duplicate samples of approximately 20 mL were taken. The solutions were examined for soapy bubbles or particles floating on the surface. The samples were filtered (0.2 μm polyether-sulphone membrane syringe filter) at room temperature (20 - 25°C). The solutions were then transferred into disposable polyethylene vials (Scintillation vials, Sarstedt, Nuembrecht, Germany), acidified with HNO3 (final concentration 1 – 3 % HNO3), and stored at 4°C until further analysis.

Test solutions

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION
- Method:
Since the test item is a multi-component substance and of low water solubility, toxicity was determined using water accommodated fractions (WAFs). The WAFs for the various test concentrations were prepared individually in accordance with the OECD guidance document on transformation/dissolution of metals and metal compounds in aqueous media No. 29 (2001)*.

Appropriate amounts of nickel iron chromite black spinel were transferred into glass flasks and were brought to the volume of 0.5 L with dilution water to obtain nominal loadings of 1.0, 10.0, 32.0, 100 and 320 mg/L.

The bottles were shaken at 100 rpm for 7 days at room temperature (~ 20°C). After this time the insoluble part of solutions was separated from the aqueous phase by filtration through a 0.2 μm filter (Polyether sulfone, PES, e.g. DIA-Nielsen GmbH & Co. KG, Düren, Germany). The filtrated WAF solutions were subsequently used as test media in the acute toxicity test.

- Controls: control consisting of dilution water only was used as the negative control treatment.

*Reference
- OECD Series on testing and assessment, Number 29. Guidance document on transformation/dissolution of metals and metal compounds in aqueous media. ENV/JM/MONO (2001)9, 23-July 2001.

Test organisms

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Species: Daphnia magna (Branchiopoda, Daphniidae); Clone V
- Source: German Federal Environment Agency, Location Berlin-Marienfelde, Ecotoxicology Lab., 12307 Berlin, Germany
- Age: 4-24 hours old (juvenile)
- Method of holding: batches of 30 to 50 D. magna were held at room temperature in approximately 1.8 L of dilution water. The water was changed once per week. Newborn D. magna were separated by sieving, the first generation was discarded. Individuals applied in the test were transferred from this culture with a bore Pasteur pipette a few hours after sieving from the population to ensure selection of healthy specimens.
- Food type/Amount: daphnids were fed with an algal suspension (Desmodesmus subspicatus) and Artemio® Fluid (JBL, Germany). Algae growing in the log-phase were centrifuged and the pellet was re-suspended with Artemio® Fluid. Of this suspension, 30 mL were given to 1 L of D. magna medium.
The daphnids were not fed during the test.
- Frequency: daily

Study design

Test type:

static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

48 h

Test conditions

Hardness:

1.1 mmol/L

Test temperature:

20.4°C at test start and 20.0°C at test end

pH:

test start: 8.44 – 8.48
test end: 8.64 – 8.69

Dissolved oxygen:

Oxygen saturation:
test start: 6.1 – 8.1 mg O2/L
test end: 8.4 – 8.6 mg O2/L

Salinity:

not applicable

Nominal and measured concentrations:

Nominal concentrations: 1.0, 10.0, 32.0, 100 and 320 mg/L

Details on test conditions:

TEST SYSTEM
- Test vessel: 60 mL glass beakers
Approximately 50 mL of each test medium was added to each replicate test vessel followed by five D. magna less than 24 hours old.
The test vessels were not aerated during the test.
- No. of organisms per vessel: 5 daphnids
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 4

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: dechlorinated local tap water was used in accordance with the OECD guideline 202 (2004). The tap water was sourced from the Schmallenberg district water production plants, mostly fed by small springs and percolation. The purification process occurs on site at the laboratory and included filtration with activated charcoal, passage through a lime-stone column, and aeration to the point of oxygen saturation. To avoid copper contamination, plastic water pipes were used in the test facilities.
All water quality measurements were considered to be within the specifications recommended in the OECD 202 test guideline.
Physical properties of the dilution and holding water used in the test:
- Conductivity: 238.6 µS/cm
- pH: 8.3
- dissolved oxygen: 104%
- nitrate: 1.3 mg/L
- nitrite: <0.005 mg/L*
- ammonium: <0.010 mg/L*
- phosphate: <0.100 mg/L*
- total hardness: 1.1 mmol/L
- alkalinity: 1.8 mmol/L
- calcium: 0.8 mmol/L
- magnesium: 0.3 mmol/L
- NPOC: 0.336 mg/L
- chromium: <0.309 µg/L
- cadmium: < 0.286 µg/L*
- copper: < 1.83 µg/L*
- iron: < 2.20 µg/L*
- manganese: < 0.567 µg/L*
- nickel: < 0.882 µg/L*
- lead: < 2.61 µg/L*
- zinc: < 2.80 µg/L*
- total residual chlorine: < 0.02 mg/L*
* < LOD: value below the respective limit of detection

OTHER TEST CONDITIONS
- Photoperiod: 16 light / 8 dark
- Light intensity: 730 lux at test start and 711 lux at test end
The test was conducted in a temperature- and light-controlled incubator.

EFFECT PARAMETERS MEASURED:
- number of immobile daphnids in each treatment was visually determined daily and any immobile daphnids were removed.
- any abnormalities in appearance and behaviour
- daphnids were classed as immobile when they did not swim 15 seconds after perturbation.

TEST CONCENTRATIONS
- Range finding study:
A non-GLP range-finding test was performed prior to the definitive test with WAF loadings of 1 mg/L, 10 mg/L and 100 mg/L. Four replicates of the test organisms (five daphnids per replicate) were exposed to the test item for a period of 48 hours. A chemical analysis was not performed. Immobilisation was not observed during the test at any of the tested loadings.

Reference substance (positive control):

yes

Remarks:

potassium dichromate

Results and discussion

Effect concentrations

Effect concentrations 1

Duration:

24 h

Dose descriptor:

EL50

Effect conc.:

> 320 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Remarks:

water accommodated fraction at 320 mg/L after 7 days

Basis for effect:

mobility

Effect concentrations 2

Duration:

24 h

Dose descriptor:

other: LOEL

Effect conc.:

> 320 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Remarks:

water accommodated fraction at 320 mg/L after 7 days

Basis for effect:

mobility

Effect concentrations 3

Duration:

24 h

Dose descriptor:

other: NOEL

Effect conc.:

>= 320 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Remarks:

water accommodated fraction at 320 mg/L after 7 days

Basis for effect:

mobility

Effect concentrations 4

Duration:

48 h

Dose descriptor:

EL50

Effect conc.:

> 320 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Remarks:

water accommodated fraction at 320 mg/L after 7 days

Basis for effect:

mobility

Effect concentrations 5

Duration:

48 h

Dose descriptor:

other: LOEL

Effect conc.:

> 320 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Remarks:

water accommodated fraction at 320 mg/L after 7 days

Basis for effect:

mobility

Effect concentrations 6

Duration:

48 h

Dose descriptor:

other: NOEL

Effect conc.:

>= 320 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Remarks:

water accommodated fraction at 320 mg/L after 7 days

Basis for effect:

mobility

Details on results:

After 24 hours and 48 hours, there were not any immobilisation effects caused by WAFs of nickel iron chromite black spinel.
- Behavioural abnormalities/ other biological observations: there were not any signs of disease or stress, e.g. discolouration or abnormal behaviour, observed in any replicate during the test. All surviving specimens appeared normal.

Results with reference substance (positive control):

The nominal 24-h EC50 is 1.19 mg/L (November 2013) and thus in the range of 0.6 - 2.1 mg/L as set in the ISO standard 6341.2012 (Anonymous, 2012)*.

* Reference:
Water quality - Determination of the inhibition of the mobility of Daphnia magna Straus (Cladocera, Crustacea) - Acute toxicity test (ISO 6341.2012).

Reported statistics and error estimates:

The endpoint of the test was immobilisation. As there were not any immobilisation effects, the ELx and NOEL were not statistically derived. The effective loadings are reported as higher than the highest test loading.

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

Based on the lack of observed acute effects on agility and survival of daphnids, a NOEL of ≥ 320 mg/L (WAF loading) and an EL50 of > 320 mg/L (WAF loading) for WAFs of nickel iron chromite black spinel can be derived. All concentrations are based on WAF loadings.