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Adsorption / desorption

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Reference
Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Testing was conducted between 01 June 2010 and 03 June 2010
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
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
Qualifier:
according to
Guideline:
OECD Guideline 121 (Estimation of the Adsorption Coefficient (Koc) on Soil and on Sewage Sludge using High Performance Liquid Chromatography (HPLC))
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
HPLC estimation method
Media:
soil/sewage sludge
Radiolabelling:
no
Test temperature:
Not applicable to HPLC method
Details on study design: HPLC method:
Method
- The determination was carried out using the HPLC screening method, designed to be compatible with Method 121 of the OECD Guidelines for Testing of Chemicals, 22 January 2001 and Method C19 Adsorption Coefficient of Council Regulation (EC) No 440/2008 of 30 May 2008.

Procedure
- Preparation of dead time solution: The dead time was determined by measuring the retention time of formamide (purity 99.5%, 753 mg/l solution in methanol:water (55:45 v/v)).
- Preparation of reference standard solutions: Solutions of reference standards (See 'any other information on materials and methods' section) were prepared in methanol.
- Preparation of sample solution: Test item (1.0076 g) was diluted to 100 ml with methanol.
- Determination of retention time: The sample, dead time and reference standard solutions were injected in duplicate using the following HPLC parameters: HPLC System: Agilent Technologies 1100, incorporating autosampler and workstation; Column: CN OPTIMAL 5µ (150 x 4.6 mm id); Column temperature: 40°C; Mobile phase: methanol:water (55:45 v/v); pH of mobile phase: 7.1; Flow-rate: 1.0 ml/min; Injection volume: 10 µl; UV detector wavelength: dead time and reference standards: 210 nm - sample: 220 nm
Typical chromatography: See attachments:
- Construction of calibration curve: A calibration curve was constructed from the retention time data of the deadtime and reference standard solutions (see attachment: curve). The capacity factors (k) for the reference standards were calculated using equation in attachment (calculations).
- Adsorption coefficient of sample: The capacity factor was calculated using equation in attachment (calculations) and the log10Koc value determined using equation in attachment (calculations) with reference to the calibration curve (see attachment: curve).
Key result
Type:
log Koc
Value:
2.62
Remarks on result:
other:
Remarks:
The log Koc is related to the major peak in the chromatogram covering 85.9% of the area
Type:
Koc
Value:
417
Remarks on result:
other:
Remarks:
The log Koc is related to the major peak in the chromatogram covering 85.9% of the area
Details on results (HPLC method):
Due to the nature and tabular content of this information it would be rendered less comprehensible by splitting this information between sections. Therefore please see 'any other information on results' section.
Transformation products:
not measured

Results

Calibration

The retention times of formamide and the retention times, capacity factors (k) and log10 Kocvalues for the reference standards are shown in the two following tables:

Dead Time

Retention Time (mins)

Mean Retention Time (mins)

Injection 1

Injection 2

Formamide

1.985

1.987

1.986

Standard

Retention Time (mins)

Mean Retention Time (mins)

Capacity Factor (k)

Log10k

Log10Koc

Injection 1

Injection 2

Acetanilide

2.550

2.551

2.551

0.284

-0.546

1.25

Phenol

2.603

2.613

2.608

0.313

-0.504

1.32

Atrazine

2.994

2.996

2.995

0.508

-0.294

1.81

Triadimenol

3.969

3.972

3.971

0.999

-3.28 x 10-4

2.40

Linuron

4.646

4.649

4.648

1.34

0.127

2.59

Naphthalene

4.365

4.372

4.369

1.20

7.91 x 10-2

2.75

Endosulfan-diol

5.907

5.915

5.911

1.98

0.296

3.02

Fenthion

7.427

7.384

7.406

2.73

0.436

3.31

a-Endosulfan

8.609

8.489

8.549

3.31

0.519

4.09

Phenanthrene

7.371

7.410

7.391

2.72

0.435

4.09

Diclofop-methyl

8.588

8.581

8.585

3.32

0.521

4.20

DDT

16.962

16.974

16.968

7.54

0.878

5.63

See attachement: calibration curve


Adsorption coefficient of sample

The retention times, capacity factors, log10Kocand percent area normalisation values determined for the sample are shown in the following table:

Peak Number

Injection

Retention Time (mins)

Capacity Factor (k)

Log10k

Log10Koc

Mean Log10Koc

Koc

Percent Area (%)

1

1

2.815

0.417

-0.379

1.38

1.38

23.9

7.75

2

2.809

0.414

-0.383

1.37

2

1

3.164

0.593

-0.227

1.85

1.86

71.6

0.681

2

3.173

0.598

-0.224

1.86

3

1

3.506

0.765

-0.116

2.19

2.18

153

1.39

2

3.496

0.760

-0.119

2.18

4

1

4.088

1.058

2.47 x 10-2

2.62

2.62

412

85.9

2

4.078

1.053

2.26 x 10-2

2.61

5

1

4.537

1.284

0.109

2.88

2.87

742

4.24

2

4.520

1.276

0.106

2.87

Overall log10 Koc: 1.38 to 2.87
Overall adsorption coefficient: 23.9 to 742

Validity criteria fulfilled:
yes
Conclusions:
The adsorption coefficient (Koc) of the test item has been determined to be in the range 23.9 to 742, log10 Koc of 1.38 to 2.87. By percent area normalisation, 85.9% of the test item had a log10 Koc of 2.62.
Executive summary:

The adsorption coefficient (Koc) of the test item has been determined to be in the range 23.9 to 742, log Koc of 1.38 to 2.87, using the HPLC screening method (OECD TG 121). By percent area normalisation, 85.9% of the test item had a log Koc of 2.62 (Koc is 417).

Description of key information

The adsorption coefficient (Koc) of the test item has been determined to be in the range 23.9 to 742, logKocof 1.38 to 2.87, using the HPLC screening method (OECD TG 121). By percent area normalisation, 85.9% of the test item had a log Koc of 2.62 (Koc is 417).

Key value for chemical safety assessment

Koc at 20 °C:
417

Additional information

LogKoc: 2.62