Potassium titanium oxide (K1.88-2.13Ti8O16.94-17.07)

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:

weight of evidence

Study period:

30/06/2003-04/07/2003

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

Deviations:

no

Qualifier:

according to guideline

Guideline:

ISO 7346-1 (Determination of the Acute Lethal Toxicity of Substances to a Freshwater Fish [Brachydanio rerio Hamilton-Buchanan (Teleostei, Cyprinidae)] - Part 1: Static Method)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method C.1 (Acute Toxicity for Fish)

Deviations:

no

GLP compliance:

yes

Analytical monitoring:

yes

Details on sampling:

- Concentrations: 5 µm filtered solution prepared from a 100 mg/l suspension and the control.
- Sampling method: 20 ml from the approximate centre of the test vessels
- Sample storage conditions before analysis: stored in a deep-freeze until shipment to Solvias AG, Basel, Switzerland

Vehicle:

no

Details on test solutions:

Identity and concentration of auxiliary solvent for dispersal: None.
PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
- Method: A 5 µm filtered solution prepared at a loading rate of 100 mg/l (filtered after 3 days of stirring) and dilutions containing 0.1, 1.0 and 10% of the filtrate.

Test organisms (species):

Cyprinus carpio

Details on test organisms:

TEST ORGANISM
- Common name: Carp
- Strain: Teleostei, Cyprinidae
- Source: Zodiac, proefacc, "De Haar Vissen", L.U. Wageningen, the Netherlands.
- Age at study initiation (mean and range, SD): not reported
- Length at study initiation (length definition, mean, range and SD): 2.0 ± 0.2 cm
- Weight at study initiation (mean and range, SD): 0.21 ± 0.04 g
- Method of breeding: F1 from a single parent-pair bred in UV-treated water.
- Feeding during test: No feeding from 48 hours prior to the test and during the total test period.

ACCLIMATION
- Acclimation period: At least 12 days after delivery
- Acclimation conditions (same as test or not): yes
- Type and amount of food: Trouvit
- Feeding frequency: Daily
- Health during acclimation (any mortality observed): In the batch of fish used for the test, mortality during the seven days prior to the start of the test was less than 5%.

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

96 h

Hardness:

250 mg CaCO3/L

Test temperature:

Blank control: 20.3 (day 0) to 20.9 (day 4)
0.1 % filtrate: 20.3 (day 0)
1 % filtrate: 20.4 (day 0)
10% filtrate: 20.7 (day 0)
100 % filtrate: 20.6 (day 0) to 21.0 (day 4)
Test groups represent percentages of a 5 µm filtered solution prepared at a nominal loading of 100 mg/l.

pH:

Blank control: 7.2-7.9
100 % filtrate: 7.1-8.3

Dissolved oxygen:

Blank control: 6.7-8.8
100 % filtrate: 6.3-8.8

Nominal and measured concentrations:

The nominal concentrations of Terracess L were prepared as follows: A 5 µm filtered solution prepared at a loading rate of 100 mg/l (3 days stirring) and dilutions containing 0.1, 1.0 and 10% of the filtrate.
The blank-filtrate: Test medium without test substance or other additives (0 mg/l).
Analysis of the samples taken from the 5 µm filtrate prepared at a loading rate of 100 mg/l showed that measured concentrations based on Lithium and Titanium were below the detection limit of the analytical method, i.e. below 0.1 mg/l. The Potassium concentration could be measured and remained stable at 3 mg/l during the 96-hour test period.
Extrapolating this concentration to the concentration of the test substance TERRACESS L resulted in a concentration of 13 mg/l (using the formula: K concentration analysed / 0.76* M K )* M TERRACESS L).

Details on test conditions:

TEST SYSTEM
- Test vessel: 6.5 litres, all-glass.
- Aeration: The test media were not aerated during the test.
- Type of flow-through: static
- No. of organisms per vessel: 3 ( for the 0.1, 1 and 10 % of the filtrate) and 7 ( for the blank-control and 100 mg/L filtered through 5 um filter)
- No. of vessels per concentration (replicates): 1
- No. of vessels per control (replicates): 1
- Biomass loading rate: Control and 100 mg/l filtrate: 0.37 g fish/litre, i.e. 7 fish per 4 litres of test medium; Dilutions: 0.16 g fish/litre, i.e. 3 fish per 4 litres of test medium.


TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: ISO-medium, formulated using Milli-Ro water (tap-water purified by reverse osmosis; Millipore Corp., Bedford, Mass., USA) with the following composition:
CaCl2.2H2O 293.8 mg/l
MgSO4.7H2O 123.3 mg/l
NaHCO3 64.8 mg/l
KCl 5.8 mg/l


- Culture medium different from test medium: no
- Intervals of water quality measurement: pH, nitrate and nitrite concentration and ammonia concentration: once a week. Temperature: every day.

OTHER TEST CONDITIONS
- Photoperiod: 16 hours photoperiod daily

TEST CONCENTRATIONS
- Spacing factor for test concentrations: 10
- Justification for using less concentrations than requested by guideline: not applicable
- Range finding study: no
- Test concentrations: Test groups (0.1; 1; 10 and 100) represent percentages of a 5 µm filtered solution prepared at a nominal loading of 100 mg/l (filtrate).
- Results used to determine the conditions for the definitive study: No mortality or clinical effects observed in the limit/range finding test.

Reference substance (positive control):

yes

Remarks:

pentachlorophenol (PCP)

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 3 mg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

element

Remarks:

Potassium

Basis for effect:

mortality (fish)

Remarks on result:

other: (> WSL)

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 17.62 mg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

test mat.

Remarks:

Terracess L

Basis for effect:

mortality (fish)

Remarks on result:

other: (> WSL)

Details on results:

- Behavioural abnormalities: none
- Mortality of control: no
- Other adverse effects control: no

Results with reference substance (positive control):

- Results with reference substance valid? yes
Under the conditions of the present test PENTACHLOROPHENOL induced no lethal effects in carp at or below 0.15 mg/l. The 96h-LC50 for carp exposed to PCP was 0.21 mg/l (95 % confidence interval between 0.19 and 0.27 mg/l). The 24h-LC50 was 0.24 mg/l (95% confidence interval between 0.21 and 0.30 mg/l), and remained unchanged until 72h. The range of the 96h-LC50 for carp is generally between 0.10 and 0.46 mg/l based on historical data of reference tests performed approximately every 3 months from April 1988 until the end 2000, and annually since then. The response observed in carp originating from the present batch falls within this range.

Validity criteria fulfilled:

yes

Conclusions:

Under the conditions of the present test TERRACESS L induced no visible effects in carp at or below a 5 µm filtered solution prepared at a loading rate of 100 mg/I.
In conclusion: Owing to the extremely poor solubility of TERRACESS Lin water, concentration levels toxic for fish could not be reached. Therefore, the 96h-LC50 for Carp exceeded the maximum solubility of TERRACESS L in water at a loading rate of 100 mg/I, the regulatory limit concentration.

Executive summary:

96-Hour Acute Toxicity Study in Carp with TERRACESS L.

The study procedures described in this report were based on the ISO International Standard 7346-1: 'Water quality - Determination of the acute lethal toxicity of substances to a freshwater fish [Brachydanio rerio Hamilton-Buchanan (Teleostei, Cyprinidae)]" - Part 1: Static method, Second edition, 1996-06-15. In addition, the guidelines met the EEC directive 92/69, Part C.1. "Acute toxicity for fish11 ; and the OECD guideline No. 203: "Fish Acute Toxicity Test", Adopted 17 July, 1992.

The batch of TERRACESS L tested was a white powder with a purity of 100%. The inorganic substance TERRACESS L was not soluble in water based on the information supplied by the sponsor.

Seven fish per concentration were exposed to a blank-control and a 5 µm filtered solution prepared at a loading rate of 100 mg/I. The 100 mg/I loading was stirred for three days prior to testing. Such a procedure ensured that maximum saturation was reached. Filtration removed the major part of the undissolved fraction of the test substance(> ea. 5 µm). In the combined range-finding test, three fish per concentration were exposed to dilutions of the filtrate corresponding to 0.1, 1.0 and 10% of the filtrate. Samples for analytical confirmation of actual exposure concentrations were taken from the control and the filtrate at the start, after 24 hours of exposure and at the end of the test.

Analysis of the samples taken from the filtrate showed that measured concentrations based on Lithium and Titanium were below the detection limit of the analytical method, i.e. below 0.1 mg/I. The Potassium concentration could be measured and remained stable at 3 mg/I. Extrapolating this concentration to the concentration of the test substance TERRACESS L resulted in a concentration of 13 mg/I. The study met the acceptability criteria prescribed by the protocol and was considered valid.

TERRACESS L induced no visible effects in carp at or below a 5 µm filtered solution prepared at a loading rate of 100 mg/I.

In conclusion: Owing to the extremely poor solubility of TERRACESS Lin water, concentration levels toxic for fish could not be reached. Therefore, the 96h-LC50 for Carp exceeded the maximum solubility of TERRACESS L in water at a loading rate of 100 mg/I, the regulatory limit concentration.

Reference 2

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

weight of evidence

Study period:

18 October 2000-02 May 2001

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method C.1 (Acute Toxicity for Fish)

Version / remarks:

(1992)

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

Version / remarks:

(1992)

Deviations:

no

GLP compliance:

yes

Analytical monitoring:

yes

Details on sampling:

- Concentrations: 0 (control) and 100 mg/L nominal (filtered and unfiltered)
- Sampling method: 10 mL from the approximate centre of the test vessels
- Sample storage conditions before analysis: in a deep freeze until shipment to Solvias AG, Basel, Switzerland.

Vehicle:

no

Details on test solutions:

Supersaturated solutions were prepared at nominally 100 mg/L and magnetically stirred for three days to achieve maximum solubility. Then, two of the solutions were filtered through a paper filter to remove the larger undissolved test substance particles (ca. > 5 µm). The filtered solution was used to prepare three lower concentrations (0.1, 1 and 10% of the filtrate) . The other solution was not filtered and used as such (100 mg/L nominal).

The unfiltered solution was a turbid whitish dispersion with undissolved test substance particles. The undiluted filtered solution was slightly turbid, while the dilutions of the filtrate were clear and colourless.

Test organisms (species):

Cyprinus carpio

Details on test organisms:

TEST ORGANISM
- Common name: Carp
- Strain: Cyprinus carpio, Teleostei, Cyprinidae
- Source: Zodiac, proefacc, "De Haar Vissen", L.U. Wageningen, the Netherlands.
- Length at study initiation (length definition, mean, range and SD): 2.14 ± 0.12 cm
- Weight at study initiation (mean and range, SD): 0.24 ± 0.05 g
- Method of breeding: F1 from a single parent-pair bred in UV-treated water.
- Feeding during test: No feeding from 48 hours prior to the test and during the total test period.

ACCLIMATION
- Acclimation period: at least 12 days after delivery
- Acclimation conditions (same as test or not): yes
- Type and amount of food: Trouvit
- Feeding frequency: Daily
- Health during acclimation (any mortality observed): In the batch of fish used for the test, mortality during the seven days prior to the start of the test was less than 5%.

NUMBER OF FISH
100 mg/l filtered and unfiltered and control: 7 fish per test group.
dilutions: 3 fish per test group.

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

96 h

Hardness:

250 mg CaCO3/L

Test temperature:

Blank control: 20.8 (day 0) - 21.0 (day 4)
100% filtrate: 20.9 (day 0) - 20.5 (day 4)
100 mg/l: 20.6 (day 0) - 20.5 (day 4)

pH:

Blank control: 8.0 (day 0) - 7.6 (day 4)
100% filtrate: 8.9 (day 0) - 7.7 (day 4)
100 mg/l: 9.0 (day 0) - 7.8 (day 4)

Dissolved oxygen:

Blank control: 9.3 (day 0) - 7.6 (day 4) mg/l
100% filtrate: 7.4 (day 0) - 7.4 (day 4) mg/l
100 mg/l: 9.0 (day 0) - 7.7 (day 4) mg/l

Nominal and measured concentrations:

A filtered and unfiltered solution prepared at nominally 100 mg/l and dilutions of the filtrate containing 0.1, 1.0 and 10% filtrate.
Blank-control Test medium without test substance or other additives (0 mg/l).

Analysis of the samples taken from the unfiltered test solution showed that the titanium concentration measured in the water phase decreased during the test period from 19420 µg/l to 28 µg/l after 96 hours. This was due to precipitation and deposition of the undissolved test substance particles. The concentration measured in the filtered test solution decreased from 2688 µg/l to 146 µg/l during the test period. This could be due to the fact that filtration had not been complete. Hence, measured concentrations in both the filtered and unfiltered solution remained above the calculated water solubility (< 10 µg/l based on titanium corresponding with < 36 µg/l for TERRACESS P).

Details on test conditions:

The test media were not aerated during the test.
16 hours photoperiod daily
Loading: 100 mg/L filtered and unfiltered and control: 0.34 g fish/L, i.e. 7 fish per 5 litres of test medium. Dilutions: 0.24 g fish/L, i.e. 3 fish per 3 litres of test medium.

Reference substance (positive control):

yes

Remarks:

pentachlorophenol

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 1 417 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

element

Remarks:

titanium

Basis for effect:

mortality (fish)

Details on results:

During the 96-hour test period no visible effects were observed in any of the concentrations tested. The test substance induced no visible effects in carp when exposed to a filtered or an unfiltered solution prepared at 100 mg/L. Owing to the extremely poor solubility of the test substance in water, concentration levels toxic for fish could not be reached.  Therefore, the 96h-LC50 for Carp exceeded the maximum solubility of TERRACESS P in water at a loading of 100 mg/L, the regulatory limit concentration.

Results with reference substance (positive control):

The 96h-LC50 for carp exposed to the reference substance was already reached after 48 hours of exposure and was 0.14 mg/L with a 95 % confidence interval between 0.13 and 0.18 mg/L.

Reported statistics and error estimates:

The range of the 96h-LC50 for carp is generally between 0.10 and 0.46 mg/L based on historical data.

Validity criteria fulfilled:

yes

Conclusions:

Under the conditions of the present test TERRACESS P induced no visible effects in Carp when exposed to a filtered or an unfiltered solution prepared at 100 mg/I.
In conclusion: Owing to the extremely poor solubility of TERRACESS Pin water, concentration levels toxic for fish could not be reached. Therefore, the 96h-LC50 for Carp exceeded the maximum solubility of TERRACESS P in water at a loading of 100 mg/I, the regulatory limit concentration.
TERRACESS P was not toxic for Carp and will therefore not be classified.

Executive summary:

96-Hour Acute Toxicity Study in Carp with TERRACESS P.

The study procedures described in this report were based on the EEC directive 92/69, Part C.1. 11 Acute toxicity for fish"; and the OECD guideline No. 203: 11 Fish Acute Toxicity Test", Adopted 17 July, 1992.

The batch of TERRACESS P tested was a white powder with unknown purity. The inorganic substance TERRACESS P was not soluble in water based on the information supplied by the sponsor. The water solubility of TERRACESS P based on the titanium content (28%) was determined to be below the limit of quantification (LOQ) i.e. below 10 µg/1 (NOTOX Project 300792). This value corresponded with a TERRACESS P concentration of < 36 µg/1.

Seven fish per concentration were exposed to a blank-control, a 5 µm filtered solution prepared at 100 mg/I and to an unfiltered supersaturated solution of 100 mg/I. The 100 mg/I solutions were stirred for three days prior to testing. Such a procedure ensured that maximum saturation was reached. Filtration removed the major part of the undissolved fraction of the test substance (> ea. 5 µm). In the combined range-finding test, three fish per concentration were exposed to dilutions of the filtrate corresponding with 0.1, 1.0 and 10% of the filtrate. Samples for analytical confirmation of actual exposure concentrations were taken at the start, after 24 hours of exposure and at the end of the test.

As expected, analysis of the samples taken from the unfiltered test solutiorn showed that the titanium concentration measured in the water phase decreased during the test period from 19420 µg/I to 28 µg/1 after 96 hours. This was due to precipitation and deposition of the undissolved test substance particles. The concentration measured in the filtered test solution decreased from 2688 µg/1 to 146 µg/L during the test period. This could be due to the fact that filtration had not been complete. Hence, measured concentrations in both the filtered and unfiltered solution remained above the calculated water solubility ( < 10 µg/I based on titanium corresponding with.< 36 µg/1 for TERRACESS P).

TERRACESS P induced no visible effects in Carp when exposed to a filtered or an unfiltered solution prepared at 100 mg/I.

In conclusion: Owing to the extremely poor solubility of TERRACESS P in water, concentration levels toxic for fish could not be reached. Therefore, the 96h-LC50 for Carp exceeded the maximum solubility of TERRACESS P in water at a loading of 100mg/l, the regulatory limit concentration.

TERRACESS P was not toxic for Carp and will therefore not be classified.

Reference 3

Endpoint:

short-term toxicity to fish

Type of information:

read-across based on grouping of substances (category approach)

Adequacy of study:

key study

Justification for type of information:

1. HYPOTHESIS FOR THE CATEGORY APPROACH (ENDPOINT LEVEL)
Please see attached justification.
2. CATEGORY APPROACH JUSTIFICATION (ENDPOINT LEVEL
Please see attached justification.

Reason / purpose for cross-reference:

read-across source

Reason / purpose for cross-reference:

read-across source

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 17.62 mg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Remarks on result:

other: Result is based on read across substance Terracess L

Key result

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

> 1 417 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

element

Basis for effect:

mortality (fish)

Remarks on result:

other: Result is based on read across substance Terracess P

Description of key information

The 96 hour LC50 for fish exceeds the maximum solubility of the substance in water in studies on two similar substances. Therefore the weight of evidence shows that Terracess TF will not be toxic to fish.    

Additional information

The 96h-LC50 for Carp exceeded the maximum solubility of the test substance in water at a loading rate of 100 mg/L.

The 96h-LC50 for Carp exceeded the maximum solubility of the test substance in water at a loading rate of 100 mg/L. The calculated 96h-LC50 for Carp is > 1417 µg/L. This is an average of the measured Ti concentrations in the filtered test solutions that decreased from 2866 µg/L to 146 µg/L during the test period. the calculated 96h-LC50 is 5141 µg Terracess P/L.