Registration Dossier

Administrative data

Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
4 June 2009 - 26 August 2009
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: The study was performed according to guideline.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2009
Report Date:
2009

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
EU Method C.19 (Estimation of the Adsorption Coefficient (KOC) on Soil and Sewage Sludge Using High Performance Liquid Chromatography (HPLC))
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
Issued by: The Department of Health of the government of the United Kingdom Inspection date: 19 August 2008
Type of method:
HPLC estimation method
Media:
soil/sewage sludge

Test material

Reference
Name:
Unnamed
Type:
Constituent
Radiolabelling:
no

Study design

Test temperature:
40 degrees C

HPLC method

Details on study design: HPLC method:
EQUIPMENT

- Apparatus: Agilent Technologies 1050/1100 with autosampler and workstation

- Type: HPLC

- Type, material and dimension of analytical (guard) column: Phenosphere 5 micron CN (250 x 4.6 mm id)

- Detection system: UV at 210 nm


MOBILE PHASES

- Type: Methanol:water (55:45 v/v). The mobile phase was adjusted to 100% methanol using a gradient elution program starting from 55 minutes which was the time after eflution of the DDT standard. This adjustment was made to assure elution of all components.

- Experiments with additives carried out on separate columns: NO

- pH: 6.0

- Solvents for dissolving test and reference substances: acetonitrile


DETERMINATION OF DEAD TIME
- Method: Dead time was determined using the retention time of formamide; an inert substance not retained by the column


REFERENCE SUBSTANCES
- Identity: acetanilide, phenol, atrazine, isoproturon, triadimenol, Linuron, naphthalene, endosulfan-diol, fenthion. See Table 1 for purity and concentrations used.


DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: 10 uL of a solution of 1.0056 g/50 mL test substance in acetonitrile

- Quantity of reference substances: 10 uL of reference substance solutions in acetonitrile; concentrations in Table 1)

- Intervals of calibration: HPLC calibrated just prior to injection of test substance.


REPETITIONS
- Number of determinations: Duplicate injections of eference standards and test material were made.


EVALUATION
- Calculation of capacity factors k': Calculated from the dead time and retention times of resference standards as described in guideline

- Calculation of retention times: Dead time for formamide is shown in Table 2. Retention times for standards are shown in Table 3. Retention times for test material are shown in Tables 4.

- Determination of the log Koc value: Determined from a calibration plot of log k' vs. logKoc as described in guideline. Log k' and log Koc values are shown in Table 4.

Results and discussion

Adsorption coefficientopen allclose all
Type:
Koc
Value:
>= 1 110 - ca. 427 000
Type:
log Koc
Value:
>= 3.05 - ca. 5.63

Results: HPLC method

Details on results (HPLC method):
- Retention times of reference substances used for calibration: retention times ranged from 3.979 to 43.617 min (See Table 3 )

- Details of fitted regression line (log k' vs. log Koc): slope = 0.339 ; intercept = -0.640 ; R2= 0.972

- Graph of regression line attached: Yes See Figure 1

- Retention data for test substance: Retention times of test material ranged from 9.404 to > 60 min. (See Table 4 and Figure 2)

Any other information on results incl. tables

Table 3: Reference Standards: Retention Times, Capacity Factors and Adsorption Coefficients

Reference Standard

Injection 1

Injection 2

Mean

Capacity factor(k)

Log k

Log Koc

Acetanilide

3.978

3.980

3.979

0.464

-0.334

1.25

Phenol

3.811

3.810

3.811

0.402

-0.396

1.32

Atrazine

5.682

5.687

5.685

1.091

0.038

1.81

Isoproturon

6.007

6.021

6.014

1.213

0.084

1.86

Triadimenol

8.112

8.116

8.114

1.985

0.298

2.40

Linuron

8.496

8.500

8.498

2.127

0.328

2.59

Naphthalene

7.308

7.309

7.309

1.689

0.228

2.75

Endosulfan-diol

10.232

10.208

10.220

2.760

0.441

3.02

Fenthion

13.079

13.068

13.074

3.810

0.581

3.31

α-Endosulfan

18.882

16.942

17.912

5.590

0.747

4.09

Phenanthrene

15.182

15.188

15.185

4.587

0.662

4.09

DDT

43.709

43.524

43.617

15.047

1.177

5.63

Table 4: Test Material: Retention Times, Capacity Factors and Adsorption Coefficients

Peak number

Injection

Retention time (min)

Capacity factor, k

log K

logKoc

Mean log Koc

% area (mean)

1

1

9.404

2.460

0.391

3.040

3.05

10.8

2

9.427

2.468

0.392

3.050

2

1

10.518

2.870

0.458

3.240

3.240

10.1

2

10.552

2.882

0.460

3.250

3

1

39.838

13.657

1.135

5.240

5.240

14.7

2

39.919

13.687

1.136

5.240

4

1

> 60

> 21.079

> 1.324

> 5.63

> 5.63

64.4

2

> 60

> 21.079

> 1.324

>5.63

Applicant's summary and conclusion

Validity criteria fulfilled:
yes
Remarks:
Instrument response was linear with an R2 value of 0.972
Conclusions:
The test material contains a mixture of components with logKoc values ranging from 3.05 to > 5.63
Executive summary:

The adsorption coefficient of the test material was determined by HPLC following the guidelines in EU Method C.19. The test substance is a mixture of components with log Koc values ranging from 3.05 to > 5.63. The distribution of log Koc values by area % is:

Mean log Koc

Mean Area %

 3.05

10.8

 3.24

10.1

 5.24

14.7

>5.63

64.4