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Reference
Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2010-09-30 - 2010-11-05
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
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. QA statement)
Type of method:
HPLC estimation method
Media:
other:
Specific details on test material used for the study:
Sponsor's identification: Amine C8
Description: dark brown liquid
Batch number: T7-271109
Date received: 21 September 2010
Expiry date: 31 December 2011
Storage conditions: room temperature in the dark
Radiolabelling:
no
Test temperature:
Not applicable
Details on study design: HPLC method:
Method
The determination was carried out using the HPLC screening method, designed to be compatible with Method C19 Adsorption Coefficient of Commission Regulation (EC) No 440/2008 of 30 May 2008.
To satisfy the requirements of the guidelines which state that for ionisable substances the test should be performed with both ionised and non-ionised forms, two determinations were performed in buffered mobile phase; one at pH 5.5 and one at pH 7.5.

Procedure
Preparation of mobile phase
Phosphate buffer at pH 5.5 was prepared as follows:
Solution A: 13.61 g/l potassium dihydrogen phosphate in reverse osmosis water.
Solution B: 35.82 g/l disodium hydrogen phosphate in reverse osmosis water.
The solutions were mixed in proportions of 967 ml of Solution A plus 36 ml of Solution B and then adjusted to pH 5.5 using 1 M sodium hydroxide.
Mobile phase A: methanol:buffer pH 5.5 (55:45 v/v), adjusted to pH 5.5 using 1 M hydrochloric acid.
Mobile phase B: methanol:buffer pH 7* (55:45 v/v), adjusted to pH 7.5 using 1 M hydrochloric acid.

Preparation of sample solutions
Test item (0.5014 g) was diluted to 20 ml with mobile phase A.
Test item (0.5068 g) was diluted to 20 ml with mobile phase B.
*Buffer pH 7, Fisher Scientific, code J/2850/24.

Preparation of dead time solutions
The dead time was determined by measuring the retention time of formamide (purity*, 99.5%, 1.10 x 10E4 mg/l solution in mobile phase A and 1.03 x 10E4 mg/l solution in mobile phase B).
Preparation of reference standard solutions
Solutions of reference standards (see following table) were prepared in methanol.
Table 11.1
Standard Purity (%)* Concentration (mg/l)
Acetanilide 99+ 1.05 x 10E4
Phenol >98 1.14 x 10E4
Atrazine 97.4 9.49 x 10E3
Isoproturon 99.9 1.07 x 10E4
Triadimenol 98.4 1.05 x 10E4
Linuron 99.5 1.07 x 10E4
Naphthalene 98.0 1.05 x 10E4
Endosulfan-diol 99.8 5.02 x 10E3
Fenthion 98.3 9.21 x 10E3
Endosulfan 99.6 1.05 x 10E4
Phenanthrene 97.0 1.02 x 10E4
Diclofop-methyl 99.5 1.09 x 10E4
DDT 98 1.11 x 10E4

* value quoted by supplier

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 workstation
Column: CN Optimal 5µm (150 x 4.6 mm id)
Column temperature: 35ºC
Mobile phase : Determination 1: Mobile Phase A (pH 5.5)
Determination 2: Mobile Phase B (pH 7.5)
Flow rate: 1.0 ml/min
Injection volume: 10 µl
Refractive index detector: polarity: positive
temperature: 35ºC
Construction of calibration curve
A calibration curve was constructed from the retention time data of the dead time and reference standard solutions (Figures 11.1 and 11.2). The capacity factors (k) for the reference standards were calculated using Equation 11.1.
Adsorption coefficient of sample
The capacity factors were calculated using Equation 11.1 and the log10 Koc value determined using Equation 11.2 with reference to the calibration curve (Figures 11.1 and 11.2).
Please see attached Fig and Equations & Typical Chromatography
Key result
Type:
Koc
Remarks:
Percentage of test item measured was 89.6%
Value:
< 17.8 dimensionless
pH:
5.5
Type:
Koc
Remarks:
Percentage of test item measured 10.4%
Value:
141 dimensionless
pH:
5.5
Key result
Type:
Koc
Remarks:
Percentage of test item measured was 82.5%
Value:
< 17.8 dimensionless
pH:
7.5
Type:
Koc
Remarks:
Percentage of test item measured was 17.5%
Value:
29.8 dimensionless
pH:
7.5
Details on results (HPLC method):
Due to the nature and tabular content of this information it is not possible to input this data within this section therefore please see any other information on results.
Transformation products:
not measured

Results

Calibration

Determination 1 (pH 5.5)

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

2.188

2.188

2.188

Standard

Retention Time (mins)

Mean Retention Time (mins)

Capacity Factor (k)

Log10k

Log10Koc

Injection 1

Injection 2

Acetanilide

2.830

2.827

2.829

0.293

-0.534

1.25

Phenol

2.911

2.914

2.913

0.331

-0.480

1.32

Atrazine

3.332

3.327

3.330

0.522

-0.283

1.81

Isoproturon

3.648

3.650

3.649

0.668

-0.175

1.86

Triadimenol

4.484

4.488

4.486

1.05

2.13 x10-2

2.40

Linuron

5.417

5.415

5.416

1.48

0.169

2.59

Naphthalene

4.964

4.967

4.966

1.27

0.104

2.75

Endosulfan-diol

6.764

6.763

6.764

2.09

0.320

3.02

Fenthion

8.686

8.683

8.685

2.97

0.473

3.31

a-Endosulfan

10.155

10.165

10.160

3.64

0.562

4.09

Phenanthrene

8.563

8.558

8.561

2.91

0.464

4.09

Diclofop-methyl

10.476

10.479

10.478

3.79

0.578

4.20

DDT

22.648

22.651

22.650

9.35

0.971

5.63

 


Determination 2 (pH 7.5)

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

2.176

2.176

2.177

Standard

Retention Time (mins)

Mean Retention Time (mins)

Capacity Factor (k)

Log10k

Log10Koc

Injection 1

Injection 2

Acetanilide

2.813

2.805

2.809

0.291

-0.537

1.25

Phenol

2.888

2.891

2.890

0.328

-0.485

1.32

Atrazine

3.306

30307

3.307

0.519

-0.285

1.81

Isoproturon

3.644

3.646

3.645

0.675

-0.171

1.86

Triadimenol

4.467

4.467

4.467

1.05

2.22 x 10-2

2.40

Linuron

5.323

5.324

5.324

1.45

0.160

2.59

Naphthalene

4.949

4.950

4.950

1.27

0.105

2.75

Endosulfan-diol

6.619

6.616

6.618

2.04

0.310

3.02

Fenthion

8.534

8.533

8.534

2.921

0.465

3.31

a-Endosulfan

10.059

10.045

10.052

3.62

0.559

4.09

Phenanthrene

8.524

8.530

8.527

2.92

0.465

4.09

Diclofop-methyl

10.325

10.315

10.320

3.74

0.573

4.20

DDT

22.182

22.196

22.189

9.195

0.964

5.63

 


Figure 11.1  Calibration Curve - Determination 1 (pH 5.5) - see attachment


Figure 11.2  Calibration Curve - Determination 2 (pH 7.5) - see attachment


Adsorption coefficient of sample

Determination 1 (pH 5.5)

The retention times, capacity factors and log10Kocvalues determined for the sample at pH 5.5 are shown in the following table:

Peak No.

Injection

Retention Time (mins)

Capacity Factor (k)

Log10k

Log10Koc

Mean % Area

1

1

2.141

<0.293

<-0.534

<1.25

89.6

2

2.145

<0.293

<-0.534

<1.25

2

1

3.907

0.786

-0.105

2.15

10.4

2

3.916

0.790

-0.105

2.15

Mean log10Koc:                 In the range <1.25 to 2.15
Adsorption coefficient:      In the range <17.8 to 141

Determination 2 (pH 7.5)

The retention times, capacity factors and log10Kocvalues determined for the sample at pH 7.5 are shown in the following table:

Peak No.

Injection

Retention Time (mins)

Capacity Factor (k)

Log10k

Log10Koc

Mean % Area

1

1

1.894

<0.293

<-0.534

<1.25

0.1

2

1.898

<0.293

<-0.534

<1.25

2

1

2.041

<0.293

<-0.534

<1.25

0.7

2

2.042

<0.293

<-0.534

<1.25

3

1

2.182

<0.293

<-0.534

<1.25

7.6

2

2.184

<0.293

<-0.534

<1.25

4

1

2.318

<0.293

<-0.534

<1.25

32.8

2

2.320

<0.293

<-0.534

<1.25

5

1

2.489

<0.293

<-0.534

<1.25

41.3

2

2.492

<0.293

<-0.534

<1.25

6

1

3.181

0.462

0.336

1.47

17.5

2

3.185

0.463

0.334

1.47

Mean log10Koc:                 In the range <1.25 to 1.47
Adsorption coefficient:      In the range <17.8 to 29.8

Validity criteria fulfilled:
yes
Conclusions:
The adsorption coefficient of the test item has been determined to be <17.8 for test material concentrations of 89.6% and 82.5% and pH of 5.5 and 7.5 respectively which correspond to Log Koc of <1.25.
Executive summary:

Adsorption Coefficient. The adsorption coefficient (Koc) of the test item has been determined using the HPLC screening method, designed to be compatible with Method C19 Adsorption Coefficient of Commission Regulation (EC) No 440/2008 of 30 May 2008. The results are presented in the following table:



































pH



Percentage of
Test Item (%)



Adsorption Coefficient



Log10Koc



5.5



89.6



<17.8



<1.25



10.4



141



2.15



7.5



82.5



<17.8



<1.25



17.5



29.8



1.47




 

Description of key information

The endpoint is covered with the study of Butler & White (2010), which is performed according to the EU Method C.19. The adsorption coefficient (Koc) of the substance was determined to range from <17.8 (test material concentration of 89.6%) to 141 (test material concentration of 10.4%) at pH 5.5 and <17.8 (test material concentration of 89.6%) to 29.8 (test material concentration of 10.4%) at pH 7.5. The study is assigned a Klimisch score of 1 and is carried out according to GLP.

Key value for chemical safety assessment

Koc at 20 °C:
141

Additional information