tetraammine palladium (II) hydrogen carbonate

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:

19 August to 6 December 1996

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP compliant, guideline study, available as unpublished report.

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

GLP compliance:

yes (incl. QA statement)

Analytical monitoring:

yes

Details on sampling:

Water samples were taken from the control and all surviving test groups at 0, 24 and 96 hours and stored at -20°C until despatch to Butterworth Laboratories Limited for analysis of Palladium content. Moreover, water samples from all the test groups were taken at 0 hours for the initial stability analysis and at 24 hours after storage at ambient temperature both in the light and the dark for the 24 hours stability analysis.

Vehicle:

no

Details on test solutions:

Test solutions were prepared from an original aqueous stock solution of 100 mg/L obtained by dispersing 100 mg of test material in reverse osmosis water with the aid of ultrasonication. Aliquots (20, 36, 64, 112 and 200 ml) of this stock solution were each separately dispersed in dechlorinated tap water and the volume adjusted to 20 litres to give the 0.10, 0.18, 0.32, 0.56b and 1.0 mg/L test concentrations respectively.

Test organisms (species):

Oncorhynchus mykiss (previous name: Salmo gairdneri)

Details on test organisms:

TEST ORGANISM
- Common name: Rainbow Trout
- Source: Parkwood Trout Farm, Harrietsham, Kent, UK
- Age at study initiation: juveniles rainbow trout
- Length at study initiation (mean and SD): 4.7 cm (sd=0.3)
- Weight at study initiation (mean and SD): 1.36 cm (sd=0.29)
- Feeding during test: no feeding during test or 24 hours prior to the test

ACCLIMATION
- Acclimation period: 7 day
- Acclimation conditions (same as test or not): same as test
- Type and amount of food: commercial trout pellets
- Health during acclimation (any mortality observed): 3% mortality

Fish were maintained in-house since 14 October 1996 in a glass fibre tank with "single pass" water renewal system. Fish were acclimatised to test conditions for 7 days prior to test and the lighting cycle was controlled to give a 16 hours of light and 8 hours dark.

Test type:

semi-static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

96 h

Hardness:

100 mg/l as CaCO3

Test temperature:

14 ± 1 °C

pH:

Range between 7.7 and 8

Dissolved oxygen:

Range between 9.4 and 10 mg/l

Salinity:

n/a

Nominal and measured concentrations:

Measured test concentrations were considered to be the same as nominal as they were very similar.

Details on test conditions:

TEST SYSTEM
- Test vessel: glass vessels (covered)
- Material, size, headspace, fill volume: 20 litre
- Aeration: aeration was done via narrow bore glass tubes.
- Renewal rate of test solution (frequency/flow rate): daily
- No. of organisms per vessel: 10
- No. of vessels per concentration (replicates): 1
- No. of vessels per control (replicates): 1
- Biomass loading rate: 0.68 g body weight / litre

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: laboratory tap water dechlorinated by passage through an activated carbon filter

OTHER TEST CONDITIONS
- Photoperiod: 16 light : 8 dark

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :
Any mortalities and sub-lethal effects of exposure were recorded at 3, 6, 24, 48, 72 and 96 hours after the start of the exposure. The criteria of death were taken to be the absence of both respiratory movement and response to physical stimulation.

TEST CONCENTRATIONS
A range-range finding study was initially performed at 1, 10 and 100 mg/l test concentrations. After 24 hours’ exposure a 100% mortality rate was observed at all the test concentrations. Therefore, a second range-finding study was carried out at 0.010, 0.10 and 1.0 mg/l. After 24, 48 72 and 96 hours any mortalities or sublethal effects of exposure were determined by visual inspection of the test fish. Based on these results, the following test concentrations were assigned to the definitive study: 0.1, 0.18, 0.32, 0.56 and 1.0 mg/l.

Reference substance (positive control):

no

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

0.53 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Remarks on result:

other: 95% Confidence Limits of 0.44-0.64 mg/l

Duration:

96 h

Dose descriptor:

NOEC

Effect conc.:

>= 0.32 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mortality (fish)

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

0.19 mg/L

Nominal / measured:

nominal

Conc. based on:

element

Remarks:

palladium

Basis for effect:

mortality (fish)

Remarks on result:

other: Concentration expressed as palladium, determined based on molecular weight conversion

Details on results:

- Behavioural abnormalities: sublethal effects (increased pigmentation and loss of equilibrium) of exposure were observed at the test concentration of 0.56 mg/l
- Mortality of control: zero mortality

NOEC based on zero mortalities and the absence of any sublethal effects

Reported statistics and error estimates:

The LC50 values and associated confidence limits were calculated by the moving average method of Thompson (1947).

Sublethal observations / clinical signs:

Analysis of the mortality data by the moving average method of Thompson (1947) based on the nominal concentrations

Time (h)	LC50 (mg/l)	95% confidence limits
3	>1.0	-
6	>1.0	-
24	0.75	0.56-1.0*
48	0.75	0.56-1.0*
72	0.63	0.53-0.75
96	0.53	0.44-0.64
* concentrations resulting in 0 and 100% mortalities respectively

Validity criteria fulfilled:

yes

Conclusions:

In a guideline study, to GLP, the 96-hr LC50 for tetraamminepalladium(II) hydrogen carbonate was determined to be 0.53 mg/L (0.19 mg Pd/L).

Executive summary:

Tetraamminepalladium(II) hydrogen carbonate was tested for acute toxicity towards Rainbow trout. The GLP compliant study followed the OECD test method 203.

In order to investigate the acute toxicity towards rainbow trout, mortality and any sublethal effects were recorded after 96 hours’ exposure time. Two range-finding studies were initially performed at test concentrations of 1.0, 10 and 100 mg/l and 0.010, 0.10 and 1.0 mg/l. The results showed no mortalities at the test concentrations of 0.010 and 0.10 mg/l. However, mortalities were observed at 1, 10 and 100 mg/l. Based on this information, test concentrations of 0.10, 0.18, 0.32, 0.56 and 1.0 mg/l were selected for the definitive study.

Analytical monitoring of the test concentrations was performed throughout the study and all the validity criteria were fulfilled. The 96-hour LC50 for the test material, based on nominal test concentrations, was 0.53 mg/l (with 95% confidence limits of 0.44-0.64 mg/l). The NOEC was 0.32 mg/l.

The results are fully adequate for the assessment of this endpoint.

Reference 2

Endpoint:

short-term toxicity to fish

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP-compliant, guideline study available as an unpublished report. No restrictions, fully adequate for assessment.

Qualifier:

according to guideline

Guideline:

OECD Guideline 203 (Fish, Acute Toxicity Test)

GLP compliance:

yes (incl. QA statement)

Analytical monitoring:

yes

Details on sampling:

Duplicate samples of 20 mL where taken from fresh media at test start (before addition of fish), at 48 hours from aged test solution and newly prepared solution and at test end. Samples were filtered (0.45 µm filter) and acidified with 200 µL nitric acid per sample. Samples were stored at 4°C and tested within 24 hours.

Vehicle:

no

Details on test solutions:

Stock solutions were prepared by dissolving adequate amounts of test item in purified drinking water (filtered through activated charcoal, passed through a limestone column and aerated) and stirring for one hour. Stock solution was further diluted to achieve final test concentrations.

Test organisms (species):

Oncorhynchus mykiss (previous name: Salmo gairdneri)

Details on test organisms:

TEST ORGANISM
- Common name: Rainbow trout
- Source: Sauerländer Forellen GmbH, Saalhauser Straße 8, 57368 Lennestadt-Gleierbrück, Germany
- Length at study initiation: 5.0 - 5.9 cm, mean 5.4 cm
- Weight at study initiation: 1.30 - 2.32 g, mean 1.66 g
- Feeding during test: None from 24 hours before test start

ACCLIMATION
- Acclimation conditions (same as test or not): same as test
- Type and amount of food: Fed ad libitum, type not specified
- Feeding frequency: ad libitum
- Health during acclimation (any mortality observed): Less than 5% during the last week before the study

Test type:

semi-static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

96 h

Hardness:

Ar start of test: 1.0 mmol/L

Test temperature:

15.1 - 15.9 °C

pH:

8.0 - 8.5

Dissolved oxygen:

90 -110% staturation

Salinity:

Not relevant

Nominal and measured concentrations:

Nominal: Control, 124, 248, 497, 993 and 1987 µg/L diamminedichloropalladium, corresponding to 62.5, 125, 250, 500 and 1000 µg/L palladium.
Mean (geometric) measured concentrations: Control, 93.2, 188, 409, 757 and 1636 µg/L diamminedichloropalladium, corresponding to Control, 46.9, 94.6, 206, 381 and 823 µg/L palladium.

Details on test conditions:

TEST SYSTEM
- Test vessel: Aquarium
- Material, size, headspace, fill volume: Glass, 28 L with 20 L of test solution
- Aeration: slightly aerated via a glass capillary
- Renewal rate of test solution: test solutionm replaced after 48 hours
- No. of organisms per vessel: 7
- No. of vessels per concentration (replicates): 1
- No. of vessels per control (replicates): 1

TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: purified drinking water (filtered through activated charcoal, passed through a limestone column and aerated)
- Conductivity: 180 µS/cm
- Culture medium different from test medium: No
- Intervals of water quality measurement: daily for temperature, pH and dissolved oxygen; palladium concentrations at 0, 48 and 96 hours

OTHER TEST CONDITIONS
- Photoperiod: 14 hours light: 10 hours dark

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) : mortality, sub-lethal and behavioural signs recorded at 3, 24, 48, 72 and 96 hours

TEST CONCENTRATIONS
- Spacing factor for test concentrations: 2
- Range finding study: Yes
- Test concentrations: 19.9, 1999 and 1987 µg/L diamminedichloropalladium, corresponding to 10, 100 and 1000 µg/L palladium
- Results used to determine the conditions for the definitive study: All fish dead at 1000 µg/L palladium

Reference substance (positive control):

not specified

Duration:

96 h

Dose descriptor:

LC10

Effect conc.:

180 µg/L

Nominal / measured:

meas. (geom. mean)

Conc. based on:

test mat.

Remarks:

diamminedichloropalladium

Basis for effect:

mortality (fish)

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

306 µg/L

Nominal / measured:

meas. (geom. mean)

Conc. based on:

test mat.

Remarks:

diamminedichloropalladium

Basis for effect:

mortality (fish)

Remarks on result:

other: 95% CL 203 - 443

Duration:

96 h

Dose descriptor:

LC10

Effect conc.:

90.4 µg/L

Nominal / measured:

meas. (geom. mean)

Conc. based on:

element

Remarks:

palladium

Basis for effect:

mortality (fish)

Duration:

96 h

Dose descriptor:

LC50

Effect conc.:

154 µg/L

Nominal / measured:

meas. (geom. mean)

Conc. based on:

element

Remarks:

palladium

Basis for effect:

mortality (fish)

Remarks on result:

other: 95% CL 102 - 223

Details on results:

- Behavioural abnormalities: hectic swimming observed in all fish at 3 hours at 1636 µg/L diamminedichloropalladium, 4 fish inactive and 3 fish dead at 24 hours at 409 µg/L diamminedichloropalladium
- Other biological observations: 3 fish dead at 24 hours at 409 µg/L diamminedichloropalladium, 1 and 5 fish dead at 72 hours at 188 and 409 µg/L diamminedichloropalladium, respectively, all fish dead at 24 hours at 757 and 1636 µg/L diamminedichloropalladium
- Mortality of control: None
- Other adverse effects control: None

Reported statistics and error estimates:

LC values were determined together with 95% confidence intervals using Probit analysis assuming log-normal distribution.

Validity criteria fulfilled:

yes

Conclusions:

A GLP compliant, OECD guideline study, the 96-hour LC50 is 306 µg/L diamminedichloropalladium, corresponding to 154 µg/L palladium.

Executive summary:

A GLP compliant, OECD guideline study, to assess the acute toxicity of diamminedichloropalladium to freshwater fish (Oncorrhynchus mykiss) was carried out. The 96-hour LC50 is 306 µg/L, corresponding to 154 µg Pd/L. It is considered to be suitable for use as the key study for this endpoint.

Description of key information

In a guideline study, to GLP, the 96-hr LC50 for tetraamminepalladium(II) hydrogen carbonate was determined to be 0.53 mg/L (0.19 mg Pd/L) (Wetton, 1997a).

In a GLP compliant, OECD guideline study, the 96-hour LC50 was 306 µg/L diamminedichloropalladium, corresponding to 154 µg/L palladium (Teigeler, 2012).