Flue dust, portland cement

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:

2010-03-15 to 2010-03-18

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP study, according to the OECD 202 technical guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

no

GLP compliance:

yes

Analytical monitoring:

no

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
- Method: A stock solution (100 mg/L) was prepared with dilution water one day prior to application and shaken with 20 rpm for 24 h at room temperature. After a separation phase of 1 h the WAF was taken from the homogeneous liquid phase.
- Eluate: Dilution water
- Differential loading: WAF with a nominal loading of 100 mg/L.
- Controls: Four replicates of dilution water without test item tested under the same conditions as the test groups.

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: Daphnia magna (STRAUS)
- Strain: Clone 5
- Source: Institut für Wasser-, Boden- Lufthygiene (WaBoLu), further own breeding
- Age at study initiation (mean and range, SD): 2 to 24 h
- Method of breeding: In 2-3 L glass vessels with appr. 1.8 L culture medium, at 20 +/- 2 °C, in an incubator, 16 h illumination, illumination strength max. 20 µExm-2 x s-1
- Feeding during test: No feeding

ACCLIMATION
- Acclimation period: 2 h
- Acclimation conditions (same as test or not): Same as test
- Type and amount of food: No feeding
- Health during acclimation (any mortality observed): Healthy, no mortality observed

Test type:

static

Water media type:

freshwater

Limit test:

yes

Total exposure duration:

48 h

Post exposure observation period:

No

Hardness:

Dilution water at test start: 263 (mg CaCO3/L)

Test temperature:

20.4 °C

pH:

Water Quality Parameters at Test Start (0 h, New Media)
(measured in one additional replicate of the WAF, the pH-control and the control)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] pH-Value
100 (pH control)* 6.84
100 10.48
Control 7.65


Water Quality Parameters at Test End (48 h, Old Media)
(measured in all replicates)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] pH-Values
Replicates
1 2 3 4
100 (pH control)* 7.22 7.19 7.17 7.16
100 7.41 7.43 7.45 7.46
Control 7.68 7.59 7.68 7.53

Dissolved oxygen:

Water Quality Parameters at Test Start (0 h, New Media)
(measured in one additional replicate of the WAF, the pH-control and the control)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] Dissolved O2 - Concentration

[mg/L]
100 (pH control)* 8.48
100 8.45
Control 8.89

Water Quality Parameters at Test End (48 h, Old Media)
(measured in all replicates)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] Dissolved O2 - Concentration [mg/L]
Replicates
1 2 3 4
100 (pH control)* 8.50 8.53 8.52 8.51
100 8.56 8.57 8.58 8.60
Control 8.58 8.44 8.45 8.46

Salinity:

Freshwater

Details on test conditions:

TEST SYSTEM
- Test vessel: Glass beakers, 50 mL
- Type (delete if not applicable): closed with parafilm
- Material, size, headspace, fill volume: Glass beakers (4 cm ID x 7 cm H), 50 mL
- Aeration: No
- Renewal rate of test solution (frequency/flow rate): One application at test start, static test
- No. of organisms per vessel: 5
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 4
- No. of vessels per vehicle control (replicates): None


TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Acc. to Directive 92/69/EEC Method C.2, Annex 1
- Conductivity: Dilution water at test start: 640 µS/cm
- Culture medium different from test medium: Elendt M4 acc. to ELENDT (1990), modified to a total hardness of 160 to 180 mg CaCO3/L
- Intervals of water quality measurement: At test start and test end


OTHER TEST CONDITIONS
- Adjustment of pH: No
- Photoperiod: 16:8 light:dark cycle
- Light intensity: Diffuse light, illumination strength max. 20 µE x m-2 x s-1


EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :


TEST CONCENTRATIONS
- Spacing factor for test concentrations: None, limit test
- Range finding study:
Immobilization Rates of the Preliminary Range Finding Test
(n = 20, divided into 2 replicates with 10 daphnids each)
Nominal Loading
of the
Water Accommodated Fraction (WAF)
[mg/L] IMMOBILIZATION [%]
24 h 48 h
Replicates Replicates
1 2 MV 1 2 MV
100 0 0 0 0 0 0
(pH control)*
100 0 0 0 0 0 0
10 0 0 0 0 0 0
Control 0 0 0 0 0 0

Reference substance (positive control):

yes

Remarks:

Potassium dichromate

Duration:

48 h

Dose descriptor:

NOEC

Effect conc.:

100 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mobility

Details on results:

- Behavioural abnormalities: None
- Mortality of control: 0%
- Other adverse effects control: None
- Abnormal responses: None
- Any observations (e.g. precipitation) that might cause a difference between measured and nominal values: None

Results with reference substance (positive control):

- Results with reference substance valid? Yes
- EC50/LC50: 1.44 (CI 1.35 - 1.54) mg/L

Reported statistics and error estimates:

The effects of the WAF were determined directly from the observation data.
EC50-value was only calculated for the reference item by sigmoidal dose-response regression. The confidence interval for EC50 was calculated from the best-fit values, the standard error and the t-distribution with the software GraphPad prism.

Immobilization Rates of the Finding Test

              (n = 20, divided into 2 replicates with 10 daphnids each)       

Nominal Loading of the Water Accommodated Fraction (WAF) [mg/L]	IMMOBILIZATION [%]
	24 h			48 h
	Replicates			Replicates
	1	2	MV	1	2	MV
100 (pH control)*	0	0	0	0	0	0
100	0	0	0	0	0	0
10	0	0	0	0	0	0
Control	0	0	0	0	0	0

Validity criteria fulfilled:

yes

Conclusions:

At the water accommodated fraction (WAF)* of the test item Flue Dust S with a nominal loading of 100 mg/L no effect to Daphnia magna was observed.

Executive summary:

In the acute immobilization test with Daphnia magna (STRAUS) the effects of the water accommodated fraction (WAF)* with a nominal loading of 100 mg/L as a limit concentration of the test item Flue Dust S(batch number: Not specified) were determined according to OECD 202 (2004). The limit test was conducted under static conditions over a period of 48 h from 2010-03-15 to 2010-03-18 with the definitive exposure phase between 2010-03-16 to 2010-03-18 at Dr. U. Noack-Laboratorien, Käthe-Paulus-Str. 1, D-31157 Sarstedt, Germany.

20 test organisms were exposed to the water accommodated fraction, the pH-control and the control. No analytical determination of the test item concentration was carried out, because the test item is a mixture of various inorganic compounds with different properties.

The water quality parameters (pH-value and dissolved oxygen concentration), measured at 0 and 48 h, were determined to be within the acceptable limits. The validity criteria of the test guideline were fulfilled.

EL-Values, NOEL and LOEL

(based on the nominal loading level of the test item)

	Test Duration [h]	Nominal Loading Level of the Test Item [mg/L]	Confidence Interval p = 95% [mg/L]
EC50	24	> 100	not applicable
	48	> 100	not applicable
EC100	24	> 100	---
	48	> 100	---
NOEC	48	100	---
LOEC	48	> 100	---

At the water accommodated fraction (WAF)* of the test item Flue Dust S
with a nominal loading of 100 mg/L no effect to Daphnia magna was observed.

Reference 2

Endpoint:

short-term toxicity to aquatic invertebrates

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2010-03-15 to 2010-03-18

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP study, according to the OECD 202 technical guideline

Qualifier:

according to guideline

Guideline:

OECD Guideline 202 (Daphnia sp. Acute Immobilisation Test)

Deviations:

no

GLP compliance:

yes

Analytical monitoring:

no

Vehicle:

no

Details on test solutions:

PREPARATION AND APPLICATION OF TEST SOLUTION (especially for difficult test substances)
- Method: Water accommodated fractions (WAF) were prepared with dilution water one day prior to application. The WAF’s were shaken with 20 rpm for 24 h at room temperature. After a separation phase of 1 h the WAF’s were taken from the homogeneous liquid phase.
- Eluate: Dilution water
- Differential loading: Five water accomodated fractions (WAF) were tested in a geometric series with a dilution factor 2:
6.25 - 12.5 - 25.0 - 50.0 - 100 mg/L.
- Controls: Four replicates of dilution water without test item tested under the same conditions as the test groups.

Test organisms (species):

Daphnia magna

Details on test organisms:

TEST ORGANISM
- Common name: Daphnia magna (STRAUS)
- Strain: Clone 5
- Source: Institut für Wasser-, Boden- Lufthygiene (WaBoLu), further own breeding
- Age at study initiation (mean and range, SD): 2 to 24 h
- Method of breeding: In 2-3 L glass vessels with appr. 1.8 L culture medium, at 20 +/- 2 °C, in an incubator, 16 h illumination, illumination strength max. 20 µExm-2 x s-1
- Feeding during test: No feeding

ACCLIMATION
- Acclimation period: 2 h
- Acclimation conditions (same as test or not): Same as test
- Type and amount of food: No feeding
- Health during acclimation (any mortality observed): Healthy, no mortality observed

Test type:

static

Water media type:

freshwater

Limit test:

no

Total exposure duration:

48 h

Post exposure observation period:

No

Hardness:

Dilution water at test start: 263 (mg CaCO3/L)

Test temperature:

20.4 °C

pH:

Water Quality Parameters at Test Start (0 h, Fresh Media)
(measured in one replicate per loading level, pH-control and control)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] pH-Value



100 (pH control)* 6.88
100 10.23
50.0 8.14
25.0 7.99
12.5 8.10
6.25 7.83
Control 7.65

Water Quality Parameters at Test End (48 h, Old Media)
(measured in all replicates)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] pH-Values
Replicates
1 2 3 4
100 (pH control)* 7.10 6.93 7.01 7.04
100 7.35 7.37 7.34 7.34
50.0 7.42 7.46 7.37 7.40
25.0 7.64 7.64 7.63 7.60
12.5 7.68 7.59 7.67 7.69
6.25 7.57 7.69 7.50 7.65
Control 7.68 7.59 7.68 7.53

Dissolved oxygen:

Water Quality Parameters at Test Start (0 h, Fresh Media)
(measured in one replicate per loading level, pH-control and control)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] Dissolved
O2-Concentration

[mg/L]
100 (pH control)* 8.42
100 8.61
50.0 8.63
25.0 8.63
12.5 8.68
6.25 8.68
Control 8.89

Water Quality Parameters at Test End (48 h, Old Media)
(measured in all replicates)
Nominal Loading of the Water Accommodated Fraction (WAF)
[mg/L] Dissolved O2 -Concentration [mg/L]
Replicates
1 2 3 4
100 (pH control)* 8.48 8.45 8.38 8.43
100 8.48 8.45 8.46 8.46
50.0 8.46 8.43 8.45 8.38
25.0 8.46 8.50 8.46 8.47
12.5 8.45 8.46 8.37 8.41
6.25 8.36 8.38 8.40 8.38
Control 8.58 8.44 8.45 8.46

Salinity:

Freshwater

Nominal and measured concentrations:

Measured Concentrations and Recovery Rates of Acetessigsäuremethylester
at the Definitive Test
Sampling date 2009-09-01
Test start (0 hours) 2009-09-03
Test end (48 hours)
Start of analysis 2009-09-01 2009-09-03
Nominal
Test Item
Concentration
[mg/L] Acetessigsäuremethylester
Meas. conc.
[mg/L] RR
[%] Meas. conc.
[mg/L] RR
[%]
100 97.5 98 93.1 93
Control < LOQ < LOQ
Meas. conc. = Measured concentration, mean value of 2 injections (dilution factor taken into account)
RR = Recovery rate related to the nominal concentration of the test item Acetessigsäuremethylester
LOQ = Limit of quantification of the analytical method (7.5 mg/L)

Details on test conditions:

TEST SYSTEM
- Test vessel: Glass beakers, 50 mL
- Type (delete if not applicable): closed with parafilm
- Material, size, headspace, fill volume: Glass beakers (4 cm ID x 7 cm H), 50 mL
- Aeration: No
- Renewal rate of test solution (frequency/flow rate): One application at test start, static test
- No. of organisms per vessel: 5
- No. of vessels per concentration (replicates): 4
- No. of vessels per control (replicates): 4
- No. of vessels per vehicle control (replicates): None


TEST MEDIUM / WATER PARAMETERS
- Source/preparation of dilution water: Acc. to Directive 92/69/EEC Method C.2, Annex 1
- Conductivity: Dilution water at test start: 640 µS/cm
- Culture medium different from test medium: Elendt M4 acc. to ELENDT (1990), modified to a total hardness of 160 to 180 mg CaCO3/L
- Intervals of water quality measurement: At test start and test end


OTHER TEST CONDITIONS
- Adjustment of pH: No
- Photoperiod: 16:8 light:dark cycle
- Light intensity: Diffuse light, illumination strength max. 20 µE x m-2 x s-1


EFFECT PARAMETERS MEASURED (with observation intervals if applicable) :


TEST CONCENTRATIONS
- Spacing factor for test concentrations: 2
- Range finding study: No

Reference substance (positive control):

yes

Remarks:

Potassium dichromate

Duration:

48 h

Dose descriptor:

NOELR

Effect conc.:

50 mg/L

Nominal / measured:

nominal

Conc. based on:

test mat.

Basis for effect:

mobility

Details on results:

- Behavioural abnormalities: None
- Mortality of control: 0%
- Other adverse effects control: None
- Abnormal responses: None
- Any observations (e.g. precipitation) that might cause a difference between measured and nominal values: None

Results with reference substance (positive control):

- Results with reference substance valid? Yes
- EC50/LC50: 1.44 (CI 1.35 - 1.54) mg/L

Reported statistics and error estimates:

As no immobilization after 24 h and mean immobilization rates of The EC50-value for the reference test was calculated by using sigmoidal dose-response regression. The confidence interval for the EC50-value was calculated from the best-fit values, the standard error and the t-distribution with the software GraphPad prism.
The EL10-value after 48 h was calculated with the software GraphPad prism by using sigmoidal dose-response regression, respectively. The concentration effect relationship after 48 h is presented graphically.

Immobilization Rates of the Definitive Test after 24 and 48 h of Exposure

                 (n = 20, divided into 4 replicates with 5 daphnids each)

IMMOBILIZATION [%]
Flue Dust T Nominal Loading of the Water Accommodated Fraction (WAF) [mg/L]	24 h					48 h
	Replicates					Replicates
	1.	2.	3.	4.	MV	1.	2.	3.	4.	MV
100 (pH control)*	0	0	0	0	0	0	0	0	0	0
100	0	0	0	0	0	40	60	80	20	50
50.0	0	0	0	0	0	0	0	0	0	0
25.0	0	0	0	0	0	0	0	0	0	0
12.5	0	0	0	0	0	0	0	0	0	0
6.25	0	0	0	0	0	0	0	0	0	0
Control	0	0	0	0	0	0	0	0	0	0

Validity criteria fulfilled:

yes

Conclusions:

Based on the nominal loading levels of the test item Flue Dust T the 48-h EL50 for Daphnia magna was estimated to be 100 mg/L.
The NOEL after 48 h was determined to be 50.0 mg/L as the highest tested loading level with no biologically significant effect (Immobilization rates of  10 % are seen to be not significant according to the guideline). The LOEL after 48 h was determined to be 100 mg/L as the lowest tested loading level with a biologically significant effect (Immobilization rates of > 10 % are seen to be significant according to the guideline).

Executive summary:

In the acute immobilization test with Daphnia magna (STRAUS) the effects of the test item  Flue Dust T(batch number: 12-2009) were determined according to OECD 202 (2004) from 2010-03-15 to 2010-03-18, with the definitive exposure phase from 2010-03-16 to 2010-03-18, at Dr.U.Noack-Laboratorien, Käthe-Paulus-Str.1, D-31157 Sarstedt.

The study was conducted under static conditions over a period of 48 h with 5 water accommodated fractions (WAF)* with nominal loadings ranging from 6.25 to 100 mg/L set up in a geometric series with a dilution factor of 2. Additionally a pH-control was tested within the test series. 20 test organisms were exposed to each loading level, the pH-control and the control.

No analytical determination of the test item concentration was carried out, because the test item is a mixture of various inorganic compounds with different properties. All effect values, presented in Table 1, are based on the nominal loading levels of the test item Flue Dust T.

The water quality parameters (pH-value and dissolved oxygen concentration), measured at 0 and 48 h, were determined to be within the acceptable limits. The validity criteria of the test guideline were fulfilled.

Table 1:    EL₁₀-, EL₅₀- (with Confidence Interval), EL₁₀₀ - Values, NOEL and LOEL

              (based on the nominal concentrations of the test item Flue Dust T)

	Test Duration [h]	Nominal Loading of the Test Item Flue Dust T [mg/L]	Confidence Interval p = 95% [mg/L]
EL10	24	> 100	---
	48	84.3	---
EL50	24	> 100	Not applicable
	48	100	Not applicable
EL100	24	> 100	---
	48	> 100	---
NOEL	48	50.0	---
LOEL	48	100	---

Description of key information

No acute (short term) toxicity to aquatic invertebrates due to a Klimisch 1 study result.

Key value for chemical safety assessment

Fresh water invertebrates

Fresh water invertebrates

Effect concentration:

100 mg/L

Additional information

Short-term toxicity testing with Daphnia magna was carried out according to the OECD 202 guidance taking into account GLP and thus resulting in a Klimish 1 score. Based on the nominal loading levels of the two test items Flue Dust T and Flue Dust S the 48-h EL50 for Daphnia magna was estimated to be 100 mg/L. The NOEL after 48 h was determined to be 50.0 mg/L (Flue Dust T) and 100.0 mg/L (Flue Dust S) as the highest tested loading level with no biologically significant effect (Immobilization rates of < 10 % are seen to be not significant according to the guideline). The LOEL after 48 h was determined to be 100 mg/L as the lowest tested loading level with a biologically significant effect (Immobilization rates of > 10 % are seen to be significant according to the guideline).