Registration Dossier

Administrative data

Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Study period:
02/12/2008 to 17/02/2009
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Study conducted to GLP in accordance with recognised 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)
Type of method:
HPLC estimation method
Media:
soil/sewage sludge

Test material

Reference
Name:
Unnamed
Type:
Constituent
Details on test material:
No further information required.
Specific details on test material used for the study:
Details on properties of test surrogate or analogue material (migrated information):
Not applicable.
Radiolabelling:
no

Study design

Test temperature:
no data available

HPLC method

Details on study design: HPLC method:
HPLC System: Agilent Technologies 1200, incorporating autosampler and workstation
Column: Zorbax SB-CN 5 µm (250 x 4.6 mm id)
Column temperature: 40°C
Mobile phase A: methanol: reverse osmosis water (55:45 v/v);
adjusted to pH 7, with 0.1M sodium hydroxide
pH of mobile phase: 7.1
Flow-rate: 1.0 ml/min
UV detector wavelength: dead time and reference standards: 210 nm sample: 269 nm
Injection volume: 10 µl

The retention times of formamide and the retention times, capacity factors (k) and log10 Koc values 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 2.826 2.833 2.830

Standard Retention Time (mins) Mean retention time (mins) Capacity Factor (k) Log10 k Log10 Koc
Injection 1 Injection 2
Acetanilide 3.844 3.845 3.845 0.359 -0.445 1.25
Phenol 3.691 3.690 3.691 0.304 -0.517 1.32
Isoproturon 5.699 5.673 5.686 1.01 4.13 x 10-3 1.86
Triadimenol 7.512 7.525 7.519 1.66 0.219 2.40
Naphthalene 6.813 6.805 6.809 1.41 0.148 2.75
Endosulfan-diol 9.259 9.271 9.265 2.27 0.357 3.02
Fenthion 11.541 11.533 11.537 3.08 0.488 3.31
a-Endosulfan 16.586 16.620 16.603 4.87 0.687 4.09
Diclofop-methyl 18.106 18.102 18.104 5.40 0.732 4.20
DDT 36.330 36.403 36.367 11.9 1.070 5.63




Batch equilibrium or other method

Analytical monitoring:
yes
Details on sampling:
Solutions of reference standards were prepared in methanol, see table:

Standard Purity** (%) Concentration (mg/l)
Acetanilide 99+ 104
Phenol 99+ 118
Isoproturon 99.8 100
Triadimenol 98.4 112
Naphthalene ≥99.0 110
Endosulfan-diol 99.8 105
Fenthion 97.8 126
a-Endosulfan 99.6 120
Diclofop-methyl 99.5 106
DDT 98 104

** value quoted by supplier
Details on matrix:
no data available
Details on test conditions:
As the test material was noted to contain numerous salted sulphonic acid groups, testing was carried out at pH 7, with the test material in its fully ionised state.
Computational methods:
The adsorption coefficient was calculated using the following equation:

Log10 Koc = (Log10 k-A)/B

Koc = adsorption coefficient
k = capacity factor
A = intercept of the calibration curve
B = slope of the calibration curve

Results and discussion

Adsorption coefficientopen allclose all
Type:
Koc
Value:
< 17.8
Type:
log Koc
Value:
< 1.25

Results: HPLC method

Details on results (HPLC method):
The dead time was determined by measuring the retention time of formamide (purity ≥99.5%, 1.02 x 10^3 mg/l solution in mobile phase).

HPLC System: Agilent Technologies 1100, incorporating autosampler and workstation
Column: Zorbax SB-CN 5 µm (250 x 4.6 mm id)
Column temperature: 40°C
Mobile phase A: methanol: reverse osmosis water (55:45 vlv);
adjusted to pH 7, with 0.1M sodium hydroxide
pH of mobile phase: 7.1
Flow-rate: 1.0 ml/min
UV detector wavelength: dead time and reference standards: 210 nm sample: 269 nm
Injection volume: 10 µl

The retention times of formamide and the retention times, capacity factors (k) and log10 Koc values 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 2.826 2.833 2.830

Standard Retention Time (mins) Mean retention time (mins) Capacity Factor (k) Log10 k Log10 Koc
Injection 1 Injection 2
Acetanilide 3.844 3.845 3.845 0.359 -0.445 1.25
Phenol 3.691 3.690 3.691 0.304 -0.517 1.32
Isoproturon 5.699 5.673 5.686 1.01 4.13 x 10-3 1.86
Triadimenol 7.512 7.525 7.519 1.66 0.219 2.40
Naphthalene 6.813 6.805 6.809 1.41 0.148 2.75
Endosulfan-diol 9.259 9.271 9.265 2.27 0.357 3.02
Fenthion 11.541 11.533 11.537 3.08 0.488 3.31
a-Endosulfan 16.586 16.620 16.603 4.87 0.687 4.09
Diclofop-methyl 18.106 18.102 18.104 5.40 0.732 4.20
DDT 36.330 36.403 36.367 11.9 1.07 5.63

Any other information on results incl. tables

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

Injection Retention Time Capacity Factor (k) Log10k Log10Koc
(mins)
1 1.654 <0.359 <-0.445 <1.25
2 1.681 <0.359 <-0.445 <1.25

Mean log10 Koc:                     <1.25

Adsorption coefficient:           <17.8

Applicant's summary and conclusion

Validity criteria fulfilled:
not specified
Conclusions:
The adsorption coefficient (Koc) of the test material has been determined to be less than 17.8, log10 Koc <1.25.
Executive summary:

In a determination of general physico-chemical properties study (Harlan project number: 0959/0224) the test material has been determined to to have an adsorption coefficient of less than 17.8, log10 Koc <1.25.

The determination was carried out using the HPLC screening method, Method C19 Adsorption Coefficient of Commission Regulation (EC) No 440/2008 of 30 May 2008.

As the test material was noted to contain numerous salted sulphonic acid groups, testing was carried out at pH 7, with the test material in its fully ionised state.