Registration Dossier

Administrative data

Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
May 5 - May 13, 2009
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: The study was performed according to guideline. Restriction due to log Koc range of test material was outside the range of the calibration standards.

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 Signed by: Dr. Andrew J. Gray, Head, UK GLP Monitoring Authority
Type of method:
HPLC estimation method
Media:
soil/sewage sludge

Test material

Reference
Name:
Unnamed
Type:
Constituent
Radiolabelling:
no

Study design

Test temperature:
30 C

HPLC method

Details on study design: HPLC method:
EQUIPMENT

- Apparatus: Agilent Technologies 1050

- Type: HPLC

- Type, material and dimension of analytical (guard) column: Zorbax SB-CN 5 μm (250 x 4.6 mm id)
- Detection system: UV 210 nm



MOBILE PHASES

- Type: methanol:reverse osmosis water (55:45 v/v), adjusted to pH 7.0 with 0.1M NaOH

- pH: 7.0

- Solutes for dissolving test and reference substances: methanol


DETERMINATION OF DEAD TIME

- Method: by inert substances which are not retained by the column

REFERENCE SUBSTANCES ( % purity and concentrations shown in Table 1)

- Identity: Acetanilide, Phenol, Atrazine, Isoproturon, Triadimenol, Linuron, Endosulfan-diol, Fention, a-Endosulfan, Phenanthrene, Diclofop-methyl, DDT

DETERMINATION OF RETENTION TIMES

- Quantity of test substance introduced in the column: 10μl of 0.106g/100 mL methanol

- Quantity of reference substances: 10μl of 1g/L solutions in methanol:RO water (55:45 v/v)


REPETITIONS

- Number of determinations: duplicate


EVALUATION

- Calculation of capacity factors k': calculated from the dead time and retention times of reference standards as described in guideline.

- Calculation of retention times: Dead time for formamide (shown in Table 2) and retention times for standards and test material (shown in Table 3 and Table 4).

- Determination of the log Koc value: determined from a calibration plot of log k' vs. log Koc as described in guideline. Log k1 and log Koc are shown in Table 4. Calibration graph is attached in Figure 1.

Results and discussion

Adsorption coefficientopen allclose all
Type:
log Koc
Value:
< 1.25
Remarks on result:
other: 67.7 area %
Type:
log Koc
Value:
>= 1.36 - <= 5.09
Remarks on result:
other: 32.4 area %

Results: HPLC method

Details on results (HPLC method):

The test substance is a mixture of several components with log Koc values ranging from < 1.25 to 5.09

- Retention times of reference substances used for calibration (shown in Table 3):

- Details of fitted regression line (log k' vs. log Koc): R2=0.968; slope = 0.357; intercept = -0.740

- Graph of regression line attached: Yes (Figure 1)

- Average retention data for test substance: multiple components resolved by HPLC with retention times ranging from 2.043 to 36.982 minutes. See table 5.

Any other information on results incl. tables

Table 2: Determination of Dead Time (formamide)

Substance

Retention Time (min)

Dead Time (min)

Injection 1

Injection 2

Formamide

2.864

2.861

2.8625

Table 3: Retention times, capacity factor and adsorption coefficients of Reference Standards

Reference Standard

Mean Retention Time (min.)

Capacity factor(k)

Log k

Log Koc

Acetanilide

3.913

0.367

-0.435

1.25

Phenol

3.716

0.298

-0.525

1.32

Atrazine

5.609

0.959

 -.00180

1.81

Isoproturon

5.928

1.7

.0297

1.86

Triadimenol

7.881

1.75

0.244

2.40

Linuron

8.331

1.91

0.281

2.59

Endosulfan-diol

9.828

2.43

0.386

3.02

Fenthion

13.182

3.61

0.557

3.31

a-Endosulfan

17.974

5.28

0.723

4.09

Phenanthrene

14.997

4.24

0.627

4.09

Diclofop-methyl

20.809

6.27

0.797

4.20

DDT

42.279

13.8

1.14

5.63

Regression line: slope = 0.357 intercept = -0.740 R2 = 0.968

Table 4. Retention times, capacity factors and adsorption coefficient (log Koc) for test material

Peak number

Injection

Retention time (min)

Capacity factor, k

log K

logKoc

Mean log Koc

% area

1

1

2.043

-0.286

-

< 1.25

< 1.25

55.6

2

2.046

-0.285

-

< 1.25

2

1

3.848

0.344

-0.463

< 1.25

< 1.25

12.1

2

3.833

0.339

-0.470

< 1.25

3

1

4.461

0.558

-0.253

1.37

1.36

10.5

2

4.437

0.550

-0.260

1.35

4

1

5.326

0.860

-0.065

1.89

1.92

8.00

2

5.419

0.893

-0.0493

1.94

5

1

6.962

1.43

0.156

2.51

2.51

0.423

2

6.943

1.43

0.154

2.51

6

1

7.269

1.54

0.187

2.60

2.60

0.63

2

7.249

1.53

0.185

2.60

7

1

7.832

1.74

0.239

2.75

2.75

1.12

2

7.799

1.72

0.237

2.74

8

1

10.534

2.68

0.428

3.28

3.28

1.89

2

10.534

2.68

0.428

3.28

9

1

11.43

2.99

0.476

3.41

3.41

3.13

2

11.337

2.96

0.471

3.40

10

1

12.019

3.20

0.505

3.49

3.49

1.14

2

11.903

3.16

0.499

3.48

11

1

36.982

11.92

1.08

5.09

5.09

5.54

2

36.557

11.77

1.07

5.08

Applicant's summary and conclusion

Validity criteria fulfilled:
yes
Remarks:
A plot of log k vs log Koc for reference standards gave an R2 value of 0.968
Conclusions:
The log Koc determined for the test material ranged from <1.25 to 5.09
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 < 1.25 to 5.09.