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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:
2009-11-10 to 2010-02-12
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: OECD guideline, GLP study
Qualifier:
according to guideline
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. QA statement)
Type of method:
HPLC estimation method
Media:
soil/sewage sludge
Specific details on test material used for the study:
TEST ITEM:
Identification: LCE08118
Batch: 0820000006
Appearance: clear yellow limpid viscous liquid
Packaging: 1 white plastic flask with blue stopped
Quantity received: 500 g
Storage: in darkness at room temperature
Identification number for the study: 08-141

REFERENCE ITEMS:
The following reference items were used for the determination of the reference retention times:

Acetanilide:
Common name: Acetanilide
CAS number: 103-84-4
Analytical purity: 1000 g/kg
Batch number: 1343268
Origin: Fluka
Expiry date: Mai 2013

Methylbenzoate
Common name: methylbenzoate
CAS number: 93-58-3
Analytival purity: 998 g/kg
Batch number: A0227448
Origin: Acros
Expiry date: 28 february 2010

Isoproturon
Common name: Isoproturon
CAS number 34123-59-6
Analytical purity 998 g/kg
Batch number 3209X
Origin Riedel-deHaën
Expiry date 28 July 2010

1,2,3-Trichlorobenzene
Common name 1,2,3-Trichlorobenzene
CAS-Registry-Number [87-61-6]
Analytical purity 994 g/kg
Batch number A0043055001
Origin Acros
Expiry date 29 July 2010

Pyrazophos
Common name Pyrazophos
CAS-Registry-Number [13457-18-6]
Analytical purity 998 g/kg
Batch number 7116X
Origin Riedel-deHaën
Expiry date 16 April 2013

4,4’-DDT
Common name 4,4’-DDT
CAS-Registry-Number [50-29-3]
Analytical purity 966 g/kg
Batch number 2274X
Origin Riedel-deHaën
Expiry date 31 October 2009

Thiourée
Common name Thiourée
CAS-Registry-Number [62-56-6]
Analytical purity 993 g/kg
Batch number A0238628
Origin Acros
Expiry date 28 February 2010
Radiolabelling:
no
Test temperature:
The temperature during the analytical phase was around 22°C
Details on study design: HPLC method:
Analytical method for the adsorption/desorption coefficient determination
Reagents
Acetone for analysis
Methanol for HPLC
Water for HPLC
All the glassware was rinsed with acetone for analysis and air dried before use.

Apparatus
Autosampler Hitachi AS2000A
HPLC pump Hitachi L-6200A
UV visible detector Hitachi L-4250
Ultrasonic tank Transonic Type T425H
Magnetic stirrer Heidolph 94360
Balance: Accuracy ± 0.1 mg Mettler AE 100S
Usual laboratory apparatus

Safety instructions
The chemicals, solvents and equipment were used with caution. The safety rules
defined within DEFITRACES were strictly followed.

Instrumental analysis
The experimental conditions used for the determination of the retention times of the analytical reference items and of the test item by high pressure liquid chromatography equipped with an ultraviolet detector are as following:
Details on sampling:
Preparation of the mobile phase
A volume of 275 mL of water was transferred into a 500-mL graduated cylinder. A
volume of 225 mL of methanol was added. The solution was treated with ultrasounds for
5 minutes and left to stand for 10 minutes before analysis.

Preparation of the thiourea solution
The thiourea solution was prepared at a concentration of about 800 mg/L and diluted 100 then 1.5 fold with methanol/eau 5/5 before analysis.
This diluted solution was used for the t0 determination.

Preparation of the mixed analytical reference item solutions
Acetanilide, methylbenzoate, isoproturon, 1,2,3-trichlorobenzene, pyrazophos and 4,4’-DDT are the six reference items solutions chosen within the method recommended reference substances for the HPLC method.
Each reference item solution was prepared separately at a concentration of about 100 mg/L (for acetanilide, 1,2,3-trichlorobenzene, pyrazophos, 4,4’-DDT), about 200 mg/L (for isoproturon) and about 800 mg/L (for methylbenzoate) in methanol.
The reference items were mixed and diluted to about 20 mg/L (for 1,2,3- trichlorobenzene, pyrazophos and 4,4’-DDT) and about 5 mg/L (acetanilide, methylbenzoate, isoproturon) for with a mixture of methanol/water 5/5 v/v.
This solution was used as the reference item solution to obtain the calibration curve.

Preparation of the test item solution
A quantity of about 100 mg of LCE08118 was accurately weighed into a 100-mL volumetric flask and the volume was made with methanol. The solution was treated with ultrasounds for 5 minutes and left to cool and a vial was prepared for analysis.
Type:
log Koc
Value:
< 1.25
Temp.:
22 °C
Details on results (HPLC method):
First run:
Using the Capacity factor and the adsorption coefficient of the reference items, the
following calibration curve was obtained: log k’ = 0.384 log koc – 0.893 r2 = 0.9660

Second run:
Using the Capacity factor and the adsorption coefficient of the reference items, the
following calibration curve was obtained: log k’ = 0.384 log koc – 0.884 r2 = 0.9648

Variation in the retention times of the reference items are very small. Therefore a
stable configuration of the HPLC column can be assumed.
The correlation logk’/ log koc is accurate as calibration gave a coefficient of
correlation near r2 = 0.965.
Under the normal chromatographic conditions, the test item peak showed nearly no
retention on the column and no reference item with lower retention time was available.
Therefore, the log koc of the test item peak must be stated as < 1.25 (lowest value of
calibration).
Validity criteria fulfilled:
yes
Conclusions:
Using this procedure, it was shown that the adsorption / desorption coefficient of LCE08118 is lower than 1.25.
Executive summary:

Determination of the adsorption / desorption coefficient of LCE08118 In compliance with OECD Guideline No. 121 (2001)

The objective of this study was to estimate the adsorption/desorption coefficient on soil and on sewage sludge using (HPLC) High Performance Liquid Chromatography following the test method (OECD Guideline No. 121, 2001).

Using this procedure, it was shown that the adsorption / desorption coefficient of LCE08118 is lower than 1.25.

Description of key information

test material: the liquid marketed product "Proteol OAT", batch LCE08118 which contains ca.27.5% of the solid substance "Glutens, hydrozylates, reaction products with lauroyl chloride, sodium salts".

Using this procedure, it was shown that the adsorption / desorption coefficient of LCE08118 is lower than 1.25.

Key value for chemical safety assessment

Koc at 20 °C:
1.25

Additional information

[LogKoc: 0.097]