Calcium Manganese Titanium oxide

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:

17 July 2018 to 19 July 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

This study was conducted in accordance with international guidelines in a GLP testing laboratory.

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

yes

Remarks:

No effect at limit of solubility (<1 mg/L)

GLP compliance:

yes

Specific details on test material used for the study:

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material:
Room temperature, in the dark.
- Stability under test conditions:
See analytical results section.
- Solubility and stability of the test substance in the solvent/vehicle:
Solubility of the test item in the test media was determined to be 0.555 mg/L.
- Reactivity of the test substance with the solvent/vehicle of the cell culture medium:
No

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing:
The test sample (100 mg) and dilution water (1L) were mixed to prepare the nominal loading concentration of 100 mg/L. The solution was mixed with a magnetic stirrer for 48 h. The suspension was then filtered with a membrane filter (GV, 0.22 µm, Merck Millipore). The filtrate was stirred for 30 minutes at about 20°C to recover dissolved oxygen concentration decreased at the suction filtration to prepare the test solution, which was divided into each test vessel. This created a saturated solution.

- Preliminary purification step (if any):
No
- Final dilution of a dissolved solid, stock liquid or gel:
See above.
- Final preparation of a solid:
N/A

FORM AS APPLIED IN THE TEST (if different from that of starting material)
Solution

TYPE OF BIOCIDE/PESTICIDE FORMULATION (if applicable)
: N/A

OTHER SPECIFICS: N/A

Analytical monitoring:

yes

Details on sampling:

- Concentrations: 100 mg/L
- Sampling method: Samples were taken from a solution sampled separately from the preparation container. The mixed solution was taken out with equal volume from the middle of the test solution in the test vessels (before the renewal and at the end of exposure). Measurements were taken at the start of the exposure, before and after the renewal, and at the end of exposure.
- Sample storage conditions before analysis: N/A

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
- Method: The test sample (100 mg) and dehlorinated tap water (1L) were mixed to prepare the nominal loading concentration of 100 mg/L. The solution was mixed with a magnetic stirrer for 48 h. The suspension was then filtered with a membrane filter (GV, 0.22 µm, Merck Millipore) to make a saturated solution. The filtrate was stirred for 30 minutes at about 20°C to recover dissolved oxygen concentration decreased at the suction filtration to prepare the test solution, which was divided into each test vessel. The dilution water (dechlorinated tap water) did not contain significant amounts of chelating agents and is appropriate for use with metal compounds.

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: Daphnia magna
- Strain/clone: Clone A
- Source: The University of Sheffield, UK, date of supply of : 9 July 1990. Young daphnids produced by parents that were cultured in this test facility were used.
- Age of parental stock (mean and range, SD): 21 days
- Feeding during test: No feeding

ACCLIMATION: No details provided

Test type:

semi-static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

48 h

Hardness:

43 mg/L (Ca, Mg)

Test temperature:

20.3 °C

pH:

7.9

Dissolved oxygen:

8.6 mg/L

Salinity:

15 mg/L Na

Conductivity:

17 mS/m

Nominal and measured concentrations:

Nominal: 100 mg/L; Measured: 0.398 mg/L

Details on test conditions:

TEST SYSTEM
- Test vessel:
- Type (delete if not applicable): closed (transparent plastic lid)
- Material, size, headspace, fill volume: 100 mL glass beaker
- Aeration: N/A
- Type of flow-through (e.g. peristaltic or proportional diluter): N/A
- Water bath: Plastic tank; Warming/cooling unit; Type HCA 250 (Sato craft)
- Renewal rate of test solution (frequency/flow rate): Renewal at 24 hours after start
- No. of organisms per vessel: 5
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 5
- No. of vessels per vehicle control (replicates): 4


TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water:
- Total organic carbon: < 0.5 mg/L
- Particulate matter: Not reported
- Metals:
Total mercury: <0.0005 mg/L
Cadmium: <0.001 mg/L
Chromium: <0.01 mg/L
Lead: <0.001 mg/L
Arsenic: <0.005 mg/L
Iron: < 0.01 mg/L
Copper: <0.001 mg/L
Cobalt: <0.001 mg/L
Manganrese: <0.005 mg/L
Aluminium: <0.02 mg/L
Zinc: <0.1 mg/L
Nickel: <0.001 mg/L
Silver: <0.001 mg/L
Sodium: 15 mg/L
Potassium: 3.6 mg/L
Calcium: 11 mg/L
Magnesium: 3.5 mg/L
- Pesticides:
1,2-chloropropane: <0.002 mg/L
Chlorothalonil: <0.001 mg/L
Propyzamide: <0.0008 mg/L
Chlomitrofen: <0.0001 mg/L
Simazine: <0.0003 mg/L
Thiobencarb: <0.001 mg/L
Diazinon: <0.0005 mg/L
Isoxathion: <0.0008 mg/L
Fenitrothion: <0.0003 mg/L
EPN: <0.0006 mg/L
Dichlorvos: <0.001 mg/L
Iprobenfos: <0.0008 mg/L
PCB: <0.0005 mg/L
- Chlorine: 13 mg/L (chloride in)
- Alkalinity: 42 mg/L
- Ca/mg ratio: 3.1:1
- Conductivity: 17 mS/m
- Salinity: Not reported; 15 mg/L Na
- Culture medium different from test medium: No
- Intervals of water quality measurement: Last sampling on 9 January 2018

OTHER TEST CONDITIONS
- Adjustment of pH: No adjudtment
- Photoperiod: Room light, 16-hour light/8 hour dark
- Light intensity: Not reported

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :
- Immobility: 24 and 48 hours after start of exposure. Daphnids were considered immobile when they were not able to swim within 15 seconds after gentle agitation of the test vessel.

VEHICLE CONTROL PERFORMED: yes

RANGE-FINDING STUDY: N/A

Reference substance (positive control):

no

Key result

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

> 0.398 mg/L

Nominal / measured:

meas. (geom. mean)

Conc. based on:

test mat.

Basis for effect:

mobility

Key result

Duration:

48 h

Dose descriptor:

EL50

Effect conc.:

> 100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mobility

Details on results:

- Behavioural abnormalities: Not reported
- Observations on body length and weight: Not reported
- Other biological observations: Not reported
- Mortality/immobility of control: 0
- Other adverse effects control: Immobility in the control was 0%. No abnormal response was observed.
- Abnormal responses: Neither immobilisation nor abnormalities of behaviour or appearance were observed.
- Any observations (e.g. precipitation) that might cause a difference between measured and nominal values:
No. The test solutions and the control were colourless and clear at the start and before renewal. Any precipetates were removed during test solution preparation.
- Effect concentrations exceeding solubility of substance in test medium: No effects observed.

Table 1 Immobility

Nominal loading concentration (mg/L)	Vessel	24 hours		48 hours
		Number of immobilised daphnids/ Total daphnids	Immobility (%)	Number of immobilised daphnids/ Total daphnids	Immobility (%)
Control	A	0/5	0	0/5	0
	B	0/5		0/5
	C	0/5		0/5
	D	0/5		0/5
100	A	0/5	0	0/5	0
	B	0/5		0/5
	C	0/5		0/5
	D	0/5		0/5

Table 2 Observed Abnormal Response

Nominal loading concentration (mg/L)	Observed abnormal response
	24 hours	48 hours
Control	-	-
100	-	-

-: Normal (No abnormal response)

Validity criteria fulfilled:

yes

Conclusions:

The 24-hour and 48-hour EL50 of the test item for Daphnia magna were both > 100 mg/L.
The 24-hour and 48-hour EC50 of the test item for Daphnia magna were both > 0.398 mg/L.

Executive summary:

OECD 202 (2018) - In a 48 hour toxicity study, Daphnia magna were exposed to solutions of the test item at a nominal loading rate of 100 mg/L (four replicate flasks per concentration, 5 daphnids per replicate) for 48 hours, under a 16 -hour light/8 -hour dark lighting cycle and at a temperature of 20 ± 1°C. The test item solutions were prepared by stirring weighed amounts of test item in the medium for 48 hours. After the stirring period any undissolved test item was removed by filtration through a 0.2 µm Sartorius Sartopore filter to produce a saturated solution. Analysis of the test solution showed the geometric mean measured concentration to be 0.398 mg/L. The chemical analysis was based on measured concentrations of calcium, manganese and titanium (i.e. components of the test item) using ICP-AES and internal calibration curves. No immobility of the test organism was observed, hence the EL50 was reported to be > 100 mg/L and the EC50 was reported to be >0.398 mg/L.

 

Description of key information

Endpoints based on geometric mean measured values

48 h EC₅₀: >0.398 mg/L; OECD 202; Adachi, R. (2018)

Additional information

A single key study was submitted for this endpoint, conducted in accordance with OECD Guideline 102. The 48h EC50 for Daphnia magna was estimated to be > 0.398 mg/L while the 48h EL50 was estimated to be > 100 mg/L (Adachi, R., 2018)