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Adsorption / desorption

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Reference
Endpoint:
adsorption / desorption, other
Remarks:
Estimation of Adsorption Coefficient Using HPLC
Type of information:
experimental study
Adequacy of study:
key study
Study period:
21.4. - 7.5.2020
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))
Version / remarks:
Council Regulation (EC) No 440/2008, Published in O.J.L 142/666, 2008.
Deviations:
no
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))
Version / remarks:
Adopted January 22, 2001.
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:
SOURCE OF TEST MATERIAL
- Source and lot/batch number of test material:
10062710
- Expiration date of the lot/batch:
10/2021
- Purity test date:
N/A

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material:
Keep container closed when not in use. Store in dry, cool, well-ventilated area. Storage temperature: 10 – 60 °C. Incompatible materials: acids and acidic substances

TREATMENT OF TEST MATERIAL
1001.47 mg of test item was weighed into a 50 ml volumetric flask, dissolved in and diluted to volume with Methanol. 5 ml of this solution was pipetted into a 10 ml volumetric flask and the flask was diluted to volume by solvent.

All prepared solutions were ultrasonicated
Radiolabelling:
no
Details on study design: HPLC method:
EQUIPMENT
pH meter inoLAB pH7310 (inventory no. 64275)
Ultrasonic bath type Sonorex Digitex (inventory no. 63738)
Liquid chromatograph – Shimadzu LC-30AC with DAD – “Nexera 1” (inventory no. 13895)
Liquid chromatograph – Shimadzu LC-20AD with DAD – “DAD 2” (inventory no. 14268)
Samples were weighed on analytical balance Mettler Toledo XS205, capable of weighing to the nearest 0.01 mg (inventory no. 13503).
Samples were weighed on analytical balance Radwag XA 82/220 4Y, capable of weighing to the nearest 0.01 mg (inventory no. 14133).
Water purification system Demiwa 10 ROSA, EWA 20 + tank, WATEK, (inventory no. 62572, 14260, 62574)


MOBILE PHASES
- Type: 550 ml MeOH and 450 ml ultra pure water were mixed together.
- Experiments with additives carried out on separate columns: no
- pH: 6.44 at 23°C
- Solutes for dissolving test and reference substances:

DETERMINATION OF DEAD TIME
- Method: by inert substances which are not retained by the column

REFERENCE SUBSTANCES
NaNO3
30.02 mg of Sodium Nitrate was weighed into a 50 ml volumetric flask and dissolved in solvent.
Acetanilide
15.34 mg of Acetanilide was weighed into a 100 ml volumetric flask and dissolved in solvent.
Atrazine
15.98 mg of Atrazine was weighed into a 100 ml volumetric flask and dissolved in solvent.
Monuron
11.07 mg of Monuron was weighed into a 50 ml volumetric flask and dissolved in solvent.
Linuron
15.42 mg of Linuron was weighed into a 50 ml volumetric flask and dissolved in solvent.
Fenthion
31.19 mg of Fenthion was weighed into a 50 ml volumetric flask and dissolved in solvent.
Phenanthrene
15.14 mg of Phenanthrene was weighed into a 50 ml volumetric flask and dissolved in Methanol. 5 ml of this solution was pipetted into a 10 ml volumetric flask and the flask was diluted to volume by solvent.


DETERMINATION OF RETENTION TIMES (see final report)


REPETITIONS
- Number of determinations: 4 (reference susbtances and mobile phase)
- Number of determinations: 15 (test item solution)

EVALUATION
Preliminary Estimation of the pKa:
- From the structural formula of Iso-decyloxypropylamine acetate, the logarithm of log POW as well as the pKa values was calculated. Estimation of values of log POW and pKa (was performed using ACD/I-Labs 2.0 – Algorithm Version: v5.0.0.184. Based on the estimation of pKa a mobile phase (55% (v/v) aqueous MeOH without adjustment pH was used).

Adsorption coefficient: log Koc = (log k - b) / a, k = (tR / t0) - 1

Where:

KOC = adsorption coefficient either on soil or sewage sludge (depends on input used)
log KOC = decimal logarithm of the adsorption coefficient (by HPLC)
k = capacity factor
t = retention time of the test compound
t0 = dead time (“retention” time of NO3(-))
a = slope of the calibration line
b = intercept of the calibration line

The calibration line is constructed through evaluation of log k of reference compounds of known log KOC.

Calibration line was constructed with a statistical software EffiValidation 3.0.2410, ©1999-2004 by EffiChem, Czech Republic, (http://www.effichem.com - valid on 2.8.2006)
The retention time of test item was determined by using of the LC Solution software, Version 6.72 SP2 (Shimadzu Corporation 2008-2016). Statistical assessment of experimental data was carried out in Excel (Microsoft Corporation).
Analytical monitoring:
no
Key result
Type:
log Koc
Value:
ca. 3.22 dimensionless
pH:
6.44
Temp.:
23 °C
Matrix:
soil
Key result
Type:
log Koc
Value:
ca. 3.46 dimensionless
pH:
6.44
Temp.:
23 °C
Matrix:
sludge
Details on results (HPLC method):
- Details of fitted regression line (log k' vs. log Koc): see final report
- Graph of regression line attached
- Average retention data for test substance: 3.782
Validity criteria fulfilled:
yes
Conclusions:
The adsorption coefficient of test item, Iso-decyloxypropylamine acetate, on soil and on sewage sludge was estimated. The HPLC method with reference compounds was used.

Estimation of the adsorption coefficient (KOC) on soil and sewage sludge at given pH of mobile phase and set temperature:


log = 3.22 ± 0.61 (pH = 6.44, 23°C)

log = 3.46 ± 1.52 (pH = 6.44, 23°C)
Executive summary:

The test was performed according to the Method C.19, Estimation of the adsorption coefficient (KOC) on soil and sewage sludge using high performance liquid chromatography (HPLC), Council Regulation (EC) No 440/2008, Published in O.J.L 142/666, 2008.

The HPLC method is applicable to chemical items with log Koc values ranging from 1.5 to 5.0 for which an appropriate detection system is available and which are sufficiently stable during the duration of the experiment. All these requirements are applicable to test item.

The adsorption coefficient of test item, Iso-decyloxypropylamine acetate, on soil and on sewage sludgewas estimated. The HPLC method with reference compounds was used.

The study gives the following values fortheestimation of adsorption coefficient (KOC) on soil and sewage sludgeIso-decyloxypropylamine acetate:

 Estimation of the adsorption coefficient (KOC) on soil and sewage sludge at given pH of mobile phase and set temperature:

 log = 3.22 ± 0.61 (pH = 6.44, 23°C)

log = 3.46 ± 1.52 (pH = 6.44, 23°C)

Description of key information

The adsorption coefficient of test item, Iso-decyloxypropylamine acetate, on soil and on sewage sludge was estimated. The HPLC method with reference compounds was used.

Estimation of the adsorption coefficient (KOC) on soil and sewage sludge at given pH of mobile phase and set temperature:

log soilOCK = 3.22 ± 0.61 (pH = 6.44, 23°C)

log sludgeOCK = 3.46 ± 1.52 (pH = 6.44, 23°C)

Key value for chemical safety assessment

Other adsorption coefficients

Type:
log Kp (solids-water in soil)
Value in L/kg:
3.22
at the temperature of:
23 °C

Other adsorption coefficients

Type:
log Kp (solids-water in activated sewage sludge)
Value in L/kg:
3.46
at the temperature of:
23 °C

Additional information

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