Registration Dossier

Administrative data

Endpoint:
sediment toxicity: long-term
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other: GLP compliant, guideline study, available as an unpublished report, no restrictions, fully adequate for assessment

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2013
Report date:
2013

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
OECD Guideline 218 (Sediment-Water Chironomid Toxicity Test Using Spiked Sediment)
Deviations:
yes
Remarks:
There was no analysis of the pore water as the analytical method was not sufficiently sensitive. This was not considered to affect the validity of the test.
GLP compliance:
yes (incl. QA statement)

Test material

Constituent 1
Reference substance name:
Diamminedichloropalladium (II)
IUPAC Name:
Diamminedichloropalladium (II)
Constituent 2
Chemical structure
Reference substance name:
Diamminedichloropalladium
EC Number:
238-269-3
EC Name:
Diamminedichloropalladium
Cas Number:
14323-43-4
Molecular formula:
Cl2H6N2Pd
IUPAC Name:
Diamminedichloropalladium
Test material form:
solid: particulate/powder
Remarks:
migrated information: powder
Details on test material:
- Name of test material (as cited in study report): Diamminedichloropalladium (II)
- Molecular formula (if other than submission substance): Cl2H6N2Pd
- Molecular weight (if other than submission substance): 211.39 g/mole
- Physical state: yellow powder
- Analytical purity: >99.5%
- Composition of test material, percentage of components: 50.35% Palladium
- Lot/batch No.: 10912
- Expiration date of the lot/batch: 28 August 2014
- Storage condition of test material: Room temperature (15 - 30°C)

Sampling and analysis

Analytical monitoring:
yes
Details on sampling:
At the start of the (after 72h equilibration) samples of sediment were removed from one (additional) test vessel per treatment for the analytical determination of the test item concentration in the sediment. At the test end samples of sediment were removed from one vessel of all treatments for the analytical determination of the test item concentration in the sediment. Samples of the overlaying water were analyzed at the start and at the end of the test fromone vessel of the lowest (0.027 mg DDP/kg), a mid-point (2.2 mg DDP/kg) and the highest (60 mg DDP/kg) treatment. Analysis of the pore water analysis was not possible because of the sensitivity of the analytical methods..

Test substrate

Vehicle:
no
Details on sediment and application:
Artificial sediment was prepared with a water content of 20%. The respective test item was added to artificial sediment individually for each replicate as an aqueous solution prepared in deionised water. The application solution was mixed thoroughly with the sediment in the vessels and left alone for 3 h before addition of the overlying water.

Test organisms

Test organisms (species):
Chironomus riparius
Details on test organisms:
TEST ORGANISM
- Common name: Midge
- Source: Bayer Crop Science AG, 40789 Monheim, Germany.
- Age at study initiation: 4-24 hours old

Study design

Study type:
laboratory study
Test type:
static
Water media type:
freshwater
Type of sediment:
artificial sediment
Limit test:
no
Exposure duration
Duration:
28 d
Exposure phase:
total exposure duration

Test conditions

Hardness:
The total hardness at test start was 120 – 130 mg/L as CaCO3. The total hardness at test end was 190 – 210 mg/L as CaCO3 equivalents in the controls and 160 - 180 mg/L as CaCO3 equivalents in the highest test concentration.
Test temperature:
Temperature: 19.9 – 20.7 °C. The temperature did not differ more than ± 1°C between vessels and was maintained within the temperature range of 20 ± 2°
pH:
pH: 7.7 – 8.6 throught the test. The pH of overlaying water was in the 6 – 9 range in all test vessels
Dissolved oxygen:
Oxygen at start of the test was 107 - 109% and at the end of the test was between 79-94% of the air saturation level. At the end of the test the dissolved oxygen concentration was at least 60% of the air saturation level. On one occasion in one test vessel an air saturation level of 50% was recorded.
Ammonia:
The NH4+ concentration at test start was 1.1 – 1.8 mg/L. The NH4+ concentration at test end was 13 - 22 mg/L in the controls and 13 - 18 mg/L in the highest test concentration
Nominal and measured concentrations:
Definitive test: nominal concentrations: Control, 0.014, 0.041, 0.13, 0.37, 1.1, 3.4, 10 and 30 mg Pd per kg dry sediment,
corresponding to Control,0.027, 0.082, 0.25, 0.74, 2.2, 6.7, 20 and 60 mg DDP/kg dry sediment.
Arithmetic mean measured concentrations: control, 0.009, 0.032, 0.11, 0.31, 0.90, 3.3, 9.3 and 27.4 mg Pd/kg dry sediment,
corresponding to 0.018, 0.063, 0.22, 0.61, 1.8, 6.5, 18.4 and 54.3 mg DDP/kg dry sediment
Details on test conditions:
TEST SYSTEM
- Test vessel: Round glass beakers (600 mL)
- Type: closed, covered with glass pane. After 10 days, emergence traps were placed on the test vessels, the glass plates were rested on the emergence traps to avoid evaporation
- Material, size, headspace, fill volume: The vessels were filled up with 119 g of wet artificial sediment (corresponding with 95 g dry mass). The height was 1.5 cm. The overlaying water was 6 cm high (ratio sediment:water about 1:4).
- Dilution water: Purified tap water.
- Food: TetraMin® at 0.25 – 0.5 mg TetraMin® /larvae/day up to day 10 and then increased up to 0.5 – 1.0 mg TetraMin® /larvae/day
- Light intensity:522 – 591 Lux
- Aeration: Continuous
- No. of organisms per vessel: 20
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 80


TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Purified tap water.
- Culture medium different from test medium: No
- Intervals of water quality measurement: pH and temperature measured once per week. Dissolved oxygen measured twice per week. Other parameters measured at the start and end of the test.
OTHER TEST CONDITIONS
- Adjustment of pH: No
- Photoperiod: 16 hours light: 8 hours dark
Reference substance (positive control):
yes
Remarks:
2-chloracetamid

Results and discussion

Effect concentrationsopen allclose all
Duration:
28 d
Dose descriptor:
EC10
Effect conc.:
> 54.3 mg/kg sediment dw
Nominal / measured:
meas. (arithm. mean)
Conc. based on:
test mat.
Remarks:
DDP
Basis for effect:
emergence rate
Remarks:
development rate and development time
Remarks on result:
other: 95% CL: not determined
Duration:
28 d
Dose descriptor:
EC50
Effect conc.:
> 54.3 mg/kg sediment dw
Nominal / measured:
meas. (arithm. mean)
Conc. based on:
test mat.
Remarks:
DDP
Basis for effect:
emergence rate
Remarks:
development rate and development time
Remarks on result:
other: 95% CL: not determined
Duration:
28 d
Dose descriptor:
NOEC
Effect conc.:
>= 54.3 mg/kg sediment dw
Nominal / measured:
meas. (arithm. mean)
Conc. based on:
test mat.
Remarks:
DDP
Basis for effect:
emergence rate
Remarks:
development rate and development time
Duration:
28 d
Dose descriptor:
EC10
Effect conc.:
> 27.4 mg/kg sediment dw
Nominal / measured:
meas. (arithm. mean)
Conc. based on:
element
Remarks:
Palladium
Basis for effect:
emergence rate
Remarks:
development rate and development time
Remarks on result:
other: 95% CL: not determined
Duration:
28 d
Dose descriptor:
EC50
Effect conc.:
> 27.4 mg/kg sediment dw
Nominal / measured:
meas. (arithm. mean)
Conc. based on:
element
Remarks:
Palladium
Basis for effect:
emergence rate
Remarks:
development rate and development time
Remarks on result:
other: 95% CL: not determined
Key result
Duration:
28 d
Dose descriptor:
NOEC
Effect conc.:
>= 27.4 mg/kg sediment dw
Nominal / measured:
meas. (arithm. mean)
Conc. based on:
element
Remarks:
Palladium
Basis for effect:
emergence rate
Remarks:
development rate and development time
Reported statistics and error estimates:
The emergence rate was calculated as the number of emerged divided by the number of introduced individuals measured at the end of the test. The development rate is the reciprocal of the development time, the mean time span between the introduction of larvae (day 0 of the test) and the emergence of the experimental cohort of midges. The data were analysed using a regression model (Probit analysis assuming log-normal distribution of the values) in order to estimate the concentration that would cause x % reduction in emergence (e.g. EC10, EC50, etc.).mean values per treatment level were compared with control values to determine the lowest observed effect concentration (LOEC) by suitable statistical methods (Chi2 2 x 2 for emergence rate and Williams t.test for development rate). The sensitivity differences between sexes were statistically judged by a Chi2 r x 2 table test. Statistical calculations were done with ToxRat® Pro 2.10.

Any other information on results incl. tables

Table 1: Development and emergence at the end of the test.

DM = Dry mass; Concentrations given as arithmetic mean measured values. No significant deviation when compared with control (Chi² 2x2 table test with Bonferroni correction, p < 0.05; one-sided or Williams Multiple Sequential t-test, p < 0.05; one-sided).

Control

0.018 mg DDP 0.009 mg Pd per kg DM

0.06 mg DDP 0.03 mg Pd per kg DM

0.22 mg DDP 0.11 mg Pd per kg DM

0.61 mg DDP 0.31 mg Pd per kg DM

1.8 mg DDP 0.9 mg Pd per kg DM

6.5 mg DDP 3.3 mg Pd per kg DM

18.4 mg DDP 9.3 mg Pd per kg DM

54.3 mg DDP 27.4 mg Pd per kg DM

 

Emerged midges [Ind.]

66

65

68

60

69

58

64

66

63

 

Emergence rate midges [%]

83

81

85

75

86

72

80

82

79

 

Development time midges

16.4

16.1

18.4

18.1

17.6

17.1

18.4

17.2

16.8

 

Development rate midges

0.061

0.062

0.055

0.056

0.057

0.058

0.055

0.059

0.060

 

Applicant's summary and conclusion

Validity criteria fulfilled:
yes
Conclusions:
Diamminedichloropalladium (DDP) had no adverse chronic effect on Chironomus riparius in a 28 day sediment-water study with spiked sediment under the chosen test conditions. There were no affects on emergence or development up to and including 54.3 mg DDP/kg dry sediment (based on arithmetic mean measured concentrations) or 27.4 mg Pd kg dry sediment (based on arithmetic mean measured concentrations). Accordingly, the NOEC was found to be ≥ 54.3 mg DDP/kg dry sediment (27.4 mg Pd/kg dry sediment).
Executive summary:

The effects of Diamminedichloropalladium (DDP) were considered in a 28 day sediment-water study with spiked sediment conducted according to OECD 218 (Fraunhofer, 2013). The sediment was spiked with the test item at nominal concentrations of 0.027, 0.082, 0.25, 0.74, 2.2, 6.7, 20 and 60 mg test item kg dry sediment, corresponding with 0.014, 0.041, 0.13, 0.37, 1.1, 3.4, 10 and 30 mg Pd/kg dry sediment. The initial measured concentrations (based on concentration of palladium) in the sediment were between 77 % and 101% of nominal concentrations and at the end of the test were between 60 % and 93 % of nominal concentrations. The results were based on arithmetic mean measured concentrations of palladium. There were no affects on emergence or development at any test concentration up to and including 54.3 mg test item/kg dry sediment (based on arithmetic mean measured concentrations) or 27.4 mg Pd/kg dry sediment (based on arithmetic mean measured concentrations). Accordingly, the NOEC was found to be ≥ 54.3 mg test item/kg dry sediment (27.4 mg Pd/kg dry sediment).

The study was conducted in accordance with GLP and the validity criteria were met. The study was well-documented and adhered to guideline procedures and has been given a reliability rating of 1. This is considered to be a key study for this endpoint.