(1'R,2R)-2-Methyl-4-(2',2',3'-tri-nal and methylcyclopent-3'-en-1'-yl)-4-pent-enal

Adsorption / desorption

Link to relevant study record(s)

Reference

Endpoint:

adsorption / desorption: screening

Type of information:

experimental study

Adequacy of study:

key study

Study period:

27-02-2001 to 28-06-2001

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Guideline study performed under GLP. All relevant validity criteria were met.

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

Qualifier:

equivalent or similar 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)

Remarks:

inspected: February 2000; signature: April 2000

Type of method:

HPLC estimation method

Media:

soil/sewage sludge

Radiolabelling:

no

Test temperature:

40 °C

Details on study design: HPLC method:

EQUIPMENT
- Apparatus: WATERS 2690 HPLC with WATERS 410 Differential Refractometer.
- Type: Phenosphere Next 5μ CN (150 x 4.6 mm id)
- Type, material and dimension of analytical (guard) column: None reported.
- Detection system: RI detection

MOBILE PHASES
- Type: Methanol : purified water (55:45 v/v) Flow rate 1 mL per minute.
- Experiments with additives carried out on separate columns: No
- pH: mobile phase: pH = 5.2
- Solutes for dissolving test and reference substances: None.

DETERMINATION OF DEAD TIME
- Method: The dead time was determined by measuring the retention time of formamide (purity: 99.5%, as certified by supplier), 2190 mg/L solution in methanol : purified water (55:45 v/v). Determined in duplicate.

REFERENCE SUBSTANCES
- Identity: Acetanilide, CAS 103-84-4, Purity 99%+, log Koc 1.25 (OECD Guideline 121); concentration 2050 mg/L
- Identity: Atrazine, CAS 1912-24-9, Purity 99.2%, log Koc 1.81 (OECD Guideline 121); concentration 2010 mg/L
- Identity: Isoproturon, CAS 34123-59-6, Purity 99.9%, log Koc 1.86 (OECD Guideline 121); concentration 2000 mg/L
- Identity: Triadimenol, CAS 55219-65-3, Purity 98.5%, log Koc 2.40 (OECD Guideline 121); concentration 1060 mg/L
- Identity: Linuron, CAS 330-55-2, Purity > or = 99.5%, log Koc 2.59 (OECD Guideline 121); concentration 2040 mg/L
- Identity: Naphthalene, CAS 91-20-3, Purity > or = 99%, log Koc 2.75 (OECD Guideline 121); concentration 2090 mg/L
- Identity: Fenthion, CAS 55-38-9, Purity 98%, log Koc 3.31 (OECD Guideline 121); concentration 220 mg/L
- Identity: alpha-Endosulfan, CAS 959-98-8, Purity 99.8%, log Koc 4.09 (OECD Guideline 121); concentration 2110 mg/L
- Identity: Diclofop-methyl, CAS 51338-27-3, Purity 99.9%, log Koc 4.20 (OECD Guideline 121); concentration 2040 mg/L
- Identity: Phenanthrene, CAS 85-01-8, Purity > or = 97.0%, log Koc 4.09 (OECD Guideline 121); concentration 2040 mg/L
- Identity: DDT, CAS 50-29-3, Purity 99.3%, log Koc 5.63 (OECD Guideline 121); concentration 2100 mg/L

DETERMINATION OF RETENTION TIMES
- Quantity of test item introduced in the column: 50 μL per injection for dead time and reference items and/or 50 μL for test item; an aliquot of test item (0.2576 g) was diluted to 100 mL with methanol.
- Quantity of reference substances: 50 μL per injection; the concentration of each reference substance is indicated above injected in duplicate.
- Intervals of calibration: The calibration was performed once specific for the study; with a range of log Koc suitable for the test item which cover both substances suitable for sewage sludge and soil under OECD TG 121 guideline.

REPETITIONS
- Number of determinations: Two.

EVALUATION
- Calculation of capacity factors k': Calculated as a ratio of retention time of retained compounds relative to unretained substances after determination of the column dead time.
- Calculation of retention times: Determined empirically relative to the known column dead time.
- Determination of the log Koc value: Capacity factors (log k') for reference substances were plotted against absorption coefficients (log Koc). The log Koc for the test item was then calculated using the resultant equation for the calibration curve and the experimentally determined log k'.

Type:

log Koc

Value:

ca. 2.33 dimensionless

pH:

7

Temp.:

40 °C

Type:

Koc

Value:

ca. 212 L/kg

pH:

7

Temp.:

40 °C

Details on results (HPLC method):

EVALUATION
- Calculation of capacity factors k': Calculated as a ratio of retention time of retained compounds relative to unretained substances after determination of the column dead time.
- Calculation of retention times: Determined empirically relative to the known column dead time.
- Determination of the log Koc value: Capacity factors (log k') for reference substances were plotted against absorption coefficients (log Koc). The log Koc for the test item was then calculated using the resultant equation for the calibration curve and the experimentally determined log k'.
- Retention times of reference substances used for calibration: Reference sample injections completed in duplicate.
- Identity: Acetanilide, Retention time average: 3.893 minutes
- Identity: Atrazine, Retention time average: 4.067 minutes
- Identity: Isoproturon, Retention time average: 4.281 minutes
- Identity: Triadimenol, Retention time average: 4.340 minutes
- Identity: Linuron, Retention time average: 4.577 minutes
- Identity: Naphthalene, Retention time average: 4.796 minutes
- Identity: Fenthion, Retention time average: 5.187 minutes
- Identity: alpha-Endosulfan, Retention time average: 5.393 minutes
- Identity: Diclofop-methyl, Retention time average: 5.405 minutes
- Identity: Phenanthrene, Retention time average: 5.717 minutes
- Identity: DDT, Retention time average: 7.168 minutes

- Dead-Time: 3.456 minutes
- Details of fitted regression line (log k' vs. log Koc): Linear regression of all reference substances; A = - 1.056 , B = 0.203 and R = 0.972
- Retention data for test item: Single peak. The average retention time; peak 1: 4.358 minutes (Log Koc = 2.33)

Validity criteria fulfilled:

yes

Conclusions:

The test item adsorption coefficient (log Koc) for soil/sewage sludge according to OECD Guideline 121 was estimated to be log Koc = 2.33 at 30°C and ca. pH 2.33 by HPLC analysis.

Executive summary:

The study was performed to OECD TG 121 guideline under GLP to assess the adsorption coefficient (Koc) of the test item in accordance with GLP using a high-performance chromatography system. The retention times of the test item and selected reference items were accurately measured using HPLC fitted with a cyanopropyl column. The retention times were consistent over the course of the study. The dead time of the instrument was also measured, and capacity factors were calculated for each substance. Calibration curves were constructed by plotting the capacity factor (log k') for the reference substances against their adsorption coefficients (log Koc). Linear regression analysis was performed, and this showed a reasonable relationship between the capacity factors and the adsorption coefficients. The test was performed at a singular approximately neutral pH (pH 7) as the test item does not possess ionisable moieties in an environmentally relevant pH range. The adsorption coefficient of the test item was estimated using the calibration curve constructed from all reference items. Under the conditions of this study, the test item adsorption coefficient (log Koc) for soil/sewage sludge was estimated to be log Koc 2.33 at 30°C and ca. pH 7 by HPLC analysis.

Description of key information

log Koc = 2.33, 40 °C, ca. pH 7 and 1 atm, OECD TG 121, 2001

Additional information

Key study: OECD TG 121, 2001 : The study was performed to OECD TG 121 guideline under GLP to assess the adsorption coefficient (Koc) of the test item in accordance with GLP using a high-performance chromatography system. The retention times of the test item and selected reference items were accurately measured using HPLC fitted with a cyanopropyl column. The retention times were consistent over the course of the study. The dead time of the instrument was also measured, and capacity factors were calculated for each substance. Calibration curves were constructed by plotting the capacity factor (log k') for the reference substances against their adsorption coefficients (log Koc). Linear regression analysis was performed, and this showed a reasonable relationship between the capacity factors and the adsorption coefficients. The test was performed at a singular approximately neutral pH (pH 7) as the test item does not possess ionisable moieties in an environmentally relevant pH range. The adsorption coefficient of the test item was estimated using the calibration curve constructed from all reference items. Under the conditions of this study, the test item adsorption coefficient (log Koc) for soil/sewage sludge was estimated to be log Koc 2.33 at 30°C and ca. pH 7 by HPLC analysis.