tetraammine palladium (II) hydrogen carbonate

Short-term toxicity to aquatic invertebrates

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

23 August to 5 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other: GLP compliant, guideline study, available as unpublished report.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 202 (Daphnia sp. Acute Immobilisation Test)

GLP compliance:

yes (incl. QA statement)

Analytical monitoring:

yes

Details on sampling:

Water temperature was recorded daily throughout the study. Dissolved oxygen concentrations and pH were recorded at the start and the termination of the study. Water samples were taken from the control and all the test groups (replicates pooled) at 0 and 48 hours and stored at -20°C until despatch to Butterworth Laboratories Limited for analysis of palladium content. Analysis was also carried out on the 10 and 100 mg/l stock solution used to prepare the test series. Moreover, water samples from the 0.010, 0.032, 0.10, 0.32 and 1.0 mg/l 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:

100 mg of test material were dispersed in reconstituted water with the aid of ultrasonication and the volume adjusted to 1 litre to give a 100 mg/l stock solution. Serial dilutions were prepared form this to give further stock solutions of 10 and 1.0 mg/l. Aliquots (20, 36, 64, 112, 200, 360, 640 and 1120 ml) of this stock solution were each separately dispersed in reconstituted water and the volume adjusted to 2 litres to give the 0.010, 0.018, 0.032, 0.056, 0.10, 0.18, 0.32 and 0.56 mg/l test concentrations respectively.

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: Water flea
- Source: Daphnia magna were maintained in a laboratory culture originating from a strain supplied by the Institut National de Recherche Chimique Appliquee (IRCHA), France
- Age at study initiation: 1st instar Daphnia magna
- Method of breeding: Culture conditions ensured that reproduction was by parthenogenesis. Gravid adults were isolated 24 hours prior to the initiation of the test, the young daphnids produced overnight were then removed for testing.
- Feeding during test: no feeding

ACCLIMATION
- Acclimation conditions (same as test or not): same as test
- Type and amount of food: suspension of mixed algae (predominantly Chlorella ssp.)
- Feeding frequency: daily

Test type:

static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

48 h

Hardness:

270 mg/l as CaCO3

Test temperature:

21 °C

pH:

8.0 to 8.1

Dissolved oxygen:

7.2 to 7.9 mg/l

Salinity:

n/a

Nominal and measured concentrations:

Analysis of the test preparation at 0 and 48 hours was carried out. At 0 hours, analysis of the test preparations gave concentrations of 56% to 140% of nominal value. However, measured concentrations of the stock solutions used to prepare the test series at 0 hours were observed to be near nominal. After 48 hours a decline in measured concentrations was observed with values ranging from less than the limit of quantitation of the analytical method to 51% of nominal. These apparently variable results were not considered to reflect the true dosed concentrations. Given the variability of the results, it was considered justifiable to base the EC50 values on time weighted mean measured concentrations. The time weighted mean measured concentrations could not be calculated for the 0.010, 0.018 and 0.032 mg/l test groups due to analysis at 48 hours giving measured concentrations of less than the limit of quantitation of the analytical method.

Details on test conditions:

TEST SYSTEM
- Test vessel: 250 mL glass jars
- Type (delete if not applicable): closed
- Fill volume: 200 mL test solutions
- Aeration: No aeration
- Renewal rate of test solution (frequency/flow rate): none
- No. of organisms per vessel: 10
- No. of vessels per concentration (replicates): 2
- No. of vessels per control (replicates): 2
- Type and source of exposure medium: reconstituted water

OTHER TEST CONDITIONS
Photoperiod: 16 light :8 dark

EFFECT PARAMETERS MEASURED (with observation intervals if applicable)
Any immobilisation or adverse reactions to exposure were recorded at 24 and 48 hours after the start of the exposure. The criterion of effect used was that Daphnia were considered to be immobilised if they were unable to swim for approximately 15 seconds after gentle agitation.

TEST CONCENTRATIONS
A range-range finiding study was initially performed at 0.01, 0.1, 1, 10 and 100 mg/l test concentrations. The results showed no immobilisation at the test concentrations of 0.01 and 0.1 mg/l. However, immobilisation was observed at 1, 10 and 100 mg/l. Based on this information test concentrations of 0.010, 0.018, 0.032, 0.056, 0.10, 0.18, 0.32, 0.56 and 1 mg/l were selected for the definitive study.

Reference substance (positive control):

no

Duration:

24 h

Dose descriptor:

EC50

Effect conc.:

0.29 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Remarks on result:

other: 95% Confidence Limits: 0.26 - 0.33 mg/l

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

0.22 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Remarks on result:

other: 95% Confidence Limits: 0.20 - 0.25 mg/l

Duration:

24 h

Dose descriptor:

NOEC

Effect conc.:

0.18 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

0.1 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Duration:

24 h

Dose descriptor:

EC50

Effect conc.:

0.18 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Remarks on result:

other: 95% Confidence Limits: 0.16 - 0.20

Key result

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

0.13 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Remarks on result:

other: 95% Confidence Limits: 0.11 - 0.14

Duration:

24 h

Dose descriptor:

NOEC

Effect conc.:

0.12 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

0.06 mg/L

Nominal / measured:

meas. (TWA)

Conc. based on:

test mat.

Basis for effect:

other: Immobility

Details on results:

Given the variability of the results of the test preparation analysis, the effective concentrations were calculated for both, nominal and measured (time weighted mean measured), concentrations.

Reported statistics and error estimates:

Immobilisation data was evaluated using the moving average method of Thompson (1947). The EC50 95% CL were also calculated.

Validity criteria fulfilled:

yes

Conclusions:

In an OECD- and GLP-compliant study, the 48-hour EC50 determined for tetraamminepalladium(II) hydrogen carbonate was 0.13 mg/L (based on the time weighted average (TWA) measured concentrations).

Executive summary:

Tetraamminepalladium(II) hydrogen carbonate was tested for acute toxicity towards Daphnia magna. The GLP compliant study followed OECD test method 202. In order to investigate the acute toxicity to Daphnia magna, any immobilisation or adverse reactions to exposure were recorded at 24 and 48 hours after the start of the exposure.

Following a preliminary range-finding study, twenty daphnids (2 replicates of 10 animals) were exposed to an aqueous dispersion of the test material at concentrations of 0.010, 0.018, 0.032, 0.056, 0.10, 0.18, 0.32, 0.56 and 1 mg/l for 48 hours under static test conditions. The 48-hour EC50 toDaphniabased on nominal test concentrations was 0.22 mg/l, with a 95% confidence limits of 0.20 - 0.25 mg/l; the NOEC was 10 mg/l. However, an analysis of the test preparations at 0 and 48 hours showed a high variability between nominal and measured concentrations. Hence, it was considered justifiable to base the EC50 values on the time weighted mean measured concentrations also. The 48-hour EC50 based on the time weighted mean measured concentrations was 0.13 mg/l with a 95% confidence limits of 0.11 - 0.14 mg/l. The NOEC was 0.06 mg/l. All the validity criteria are fulfilled.

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

Reference 2

Endpoint:

short-term toxicity to aquatic invertebrates

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 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

yes

Remarks:

Due to good solubility, stirring time was reduced during test media preparation; analytical samples of test media had to be filtered prior to analysis

GLP compliance:

yes (incl. QA statement)

Analytical monitoring:

yes

Details on sampling:

Samples were taken from the test media at test start and after 48 hours. At test start a sample of fresh control media and freshly prepared test media of each treatment were taken just before distributing the test media to the test containers. After 48 hours all samples of the replicate vessels from each treatment were pooled prior to analysis. Duplicate samples of 20mL were taken and filtered (0.45 µm) at room temperature. Solutions were acidified with nitric acid (final concentration 1-3% HNO3). If samples were not analysed immediately they were stored deep-frozen at -20°C until analysis

Vehicle:

no

Details on test solutions:

Test 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.

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: water flea
- Strain: Clone V
- Source: German Federal Environment Agency, Location Berlin-Marienfelde, Ecotoxicology Lab, 12307 Berlin, Germany
- Age at study initiation (mean and range, SD): 4 - 24 hours old

Test type:

static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

48 h

Hardness:

70 - 120 mg/L as CaCO3

Test temperature:

At test start: 20.1°C
At end of test: 20.5°C

pH:

At test start: 8.03 - 8.07
At end of test: 7.93 - 8.05

Dissolved oxygen:

At test start: 8.9 - 9.7 mg/L
At end of test: 8.7 - 9.2 mg/L

Salinity:

Not relevant

Nominal and measured concentrations:

Range finding test: nominal concentrations 10, 100 and 1000 µg palladium/L
Definitive test: nominal concentrations: Control, 6.25, 12.5, 25, 50 and 100 µg palladium/L,
corresponding to Control, 12.4, 24.8, 49.7, 99.3 and 198.7 µg DDP/L.
Mean measured concentrations: control, 4.73, 9.69, 20.52, 40.1 and 81.28 µg palladium/L,
corresponding to 9.4, 19.25, 40.77, 79.67 and 161.49 µg DDP/L

Details on test conditions:

TEST SYSTEM
- Test vessel: beaker
- Type: closed, covered with glass pane
- Material, size, headspace, fill volume: glass beakers filled with 50 mL test solution
- Aeration: No
- No. of organisms per vessel: 5
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 4


TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Purified drinking water: filtered through activated charcoal, passed through a limestone column and aerated
- Conductivity: 171.6 µS/cm
- Culture medium different from test medium: No
- Intervals of water quality measurement: 0 and 48 hours

OTHER TEST CONDITIONS
- Adjustment of pH: No
- Photoperiod: 16 hours light: 8 hours dark
- Light intensity: 592 - 597 lux

EFFECT PARAMETERS MEASURED (with observation intervals if applicable) : immobilisation was determined daily and abnormalities in appearance noted

TEST CONCENTRATIONS
- Spacing factor for test concentrations: 2
- Range finding study: yes
- Test concentrations:10, 100, 1000 µg palladium/L
- Results used to determine the conditions for the definitive study: ) 0% immobilisation at 10µg palladium/L, 100% immobilisation in 100 µg palladium/L at 24 and 48 hours.

Reference substance (positive control):

yes

Remarks:

potassium dichromate

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

35.19 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

element

Remarks:

palladium

Basis for effect:

mobility

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

69.91 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

test mat.

Remarks:

Diamminedichloropalladium

Basis for effect:

mobility

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

20.52 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

element

Remarks:

palladium

Basis for effect:

mobility

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

40.77 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

test mat.

Remarks:

Diamminedichloropalladium

Basis for effect:

mobility

Duration:

48 h

Dose descriptor:

LOEC

Effect conc.:

40.1 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

element

Remarks:

palladium

Basis for effect:

mobility

Duration:

48 h

Dose descriptor:

LOEC

Effect conc.:

79.67 µg/L

Nominal / measured:

meas. (arithm. mean)

Conc. based on:

test mat.

Remarks:

Diamminedichloropalladium

Basis for effect:

mobility

Details on results:

- Behavioural abnormalities: None observed
- Mortality of control: None

Results with reference substance (positive control):

24-hour EC50 0.77 mg/L

Reported statistics and error estimates:

Determination of EC50 values was performed by probit analysis. NOEC and LOEC values were determined by the Fisher's Exact Binomial Test with Bonferroni correction.

Validity criteria fulfilled:

yes

Conclusions:

The 48-hour EC50 for Diamminedichloropalladium is 69.91 µg/L, corresponding to 35.19 µg Pd/L. The 48-hour NOEC is 40.77µg/L, corresponding to 20.52 µg Pd/L.

Executive summary:

A GLP compliant, OECD guideline study to assess the acute immobilisation of Daphnia magna was carried out (Fraunhofer 2012). It

is considered to be suitable for use as the key study for this endpoint.

Reference 3

Endpoint:

short-term toxicity to aquatic invertebrates

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 unpublished report; minor restrictions in design and/or reporting but otherwise adequate for assessment.

Qualifier:

according to guideline

Guideline:

other: Commission Directive 92/69/EEC Annex Part C, C.2; OECD Guideline 202; OECD Guidance Document for Testing and Assessment, No.23 (Aquatic Toxicity Testing of Difficult Substances and Mixtures).

Deviations:

no

GLP compliance:

yes

Specific details on test material used for the study:

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

Analytical monitoring:

yes

Details on sampling:

Samples taken at 0 hours (in duplicate) and at 48 hours (by pouring the content of the test beakers into sampling flasks)

Vehicle:

no

Details on test solutions:

Since the test item degrades in water very quickly (<1 hr) in the present test the hydrolysis products were tested, according to the guidance document on aquatic toxicity testing of difficult substances. Therefore, the test medium at a test concentration of 100 mg/L was prepared twice by suspending 50mg test item in 500ml test water and stirring for approx. 4hr in the dark at room temp. Thus, the main part of the test item was hydrolysis products. Then, the undissolved test item was separated by filtration (0.45um Cellulose Nitrate filter) and the pH value was adjusted to 7.8 with NaOH. The two filtrates were poured together and stirred for 5 mins. Adequate volumes of the filtrate were mixed with test water to obtain the required concentrations.

Test organisms (species):

Daphnia magna

Details on test organisms:

Test organisms (species): Daphnia magna (Straus), clone 5
Source: Supplied in 1997 by the Umweltbundesamt, Institut fur Wasser-Boden-und Lufthygiene, Berlin, Germany
Holding conditions prior to test: Held under similar temperature and light conditions as in the test.
Life stage of test species used:Not first brood progeny, aged 8-24 hrs, female

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

48 h

Hardness:

2.5 mmol/L (=250 mg/L) as CaCO3

Test temperature:

21°C

pH:

7.6-7.8

Dissolved oxygen:

9.6-10.4 mg O2 / L

Salinity:

Not applicable

Nominal and measured concentrations:

Nominal 100 mg/L

Details on test conditions:

Test vessel: glass beakers of 100ml volume with 80ml test medium
Photoperiod: 16h light : 8h dark
Light intensity: 80-190 lux

Reference substance (positive control):

yes

Remarks:

For the evaluation of the quality of the Daphnia clone and the experimental conditions the substance potassium dichromate p.A. Is tested at least twice a year to demonstrate satisfactory test conditions.

Key result

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

0.021 mg/L

Nominal / measured:

nominal

Conc. based on:

element

Basis for effect:

other: swimming or mortality

Duration:

48 h

Dose descriptor:

EC50

Effect conc.:

0.107 other: mg test item / L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: swimming or mortality

Remarks on result:

other: 95% confidence values 0.092-0.125 mg test item/L

Duration:

48 h

Dose descriptor:

EC0

Effect conc.:

0.03 other: mg test item / L;

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: swimming or mortality

Duration:

48 h

Dose descriptor:

EC100

Effect conc.:

0.263 other: mg test item / L;

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: swimming or mortality

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

0.045 other: mg test item / L;

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: swimming or mortality

Duration:

48 h

Dose descriptor:

LOEC

Effect conc.:

0.097 other: mg test item / L;

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

other: swimming or mortality

Details on results:

Recalculated concentration of test item from analysis of concentration of Pd.

Reported statistics and error estimates:

95% confidence limits were calculated by Probit analysis.

Mortality in control <10%; dissolved oxygen ≥3 mg/L

Validity criteria fulfilled:

yes

Conclusions:

The acute EC50 for dihydrogen tetrachloropalladate for Daphnia magna was 0.107 mg test item / L corresponding to 21.4 µg Pd/L.

Executive summary:

This information is taken from a GLP compliant, guideline study and is considered reliable and suitable for use as the key study for this endpoint.The acute EC50 for dihydrogen tetrachloropalladate for Daphnia magna was 0.107mg test item / L (corresponding to 21.4 µg Pd/L)

Description of key information

The 48-hour EC50 for tetraamminepalladium(II) hydrogen carbonate was determined to be 0.13 mg/L (as a time weighted average) (Wetton, 1997b), equivalent to 0.047 mg Pd/L.

The 48-hour EC50 for diamminedichloropalladium is 69.91 µg/L (Schlechtriem, 2010), corresponding to 35.19 µg Pd/L.

The 48 -hour EC50 for dihydrogen tetrachloropalladate is 0.107 mg/L (Moll and Wydra, 2005), corresponding to 21.4 µg Pd/L.