4,8-Cyclododecadien-1-one

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:

14-02-2015 to 17-04-2015

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:

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)

Remarks:

inspected: June 2013; signature: November 2013

Type of method:

HPLC estimation method

Media:

other: soil and sediment

Radiolabelling:

no

Details on study design: HPLC method:

EQUIPMENT
- Instrument: HPLC Agilent 1100
- Detector: Diode Array Detector (DAD)
- Column: YMC-Pack Cyano, 250 x 4.0 mm, S-5 IJm, 12nm, batch 11334
- Detection system: UV-diode array detection, 210 nm for the test item sample solution, 210 to 250 nm (range) for the reference items and 210 nm deadtime solutions

MOBILE PHASES
- Type: Methanol: HPLC water (55 : 45 v/v); Flow-rate 0.8 mL per minute.
- Experiments with additives carried out on separate columns: No
- pH: mobile phase: pH = ca. 7.0
- Column temperature: 20-25°C
- Solutes for dissolving test and reference substances: None.

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

REFERENCE SUBSTANCES
Acetanilide, CAS 103-84-4, log Koc (soil) 1.26, log Koc (sewage sludge) 1.52 (OECD Guideline 121); concentration 5 mg/L
Atrazine, CAS 1912-24-9, log Koc (soil) 1.81, log Koc (sewage sludge) 1.66 (OECD Guideline 121); concentration 5 mg/L
Monuron, CAS 150-68-5, log Koc (soil) 1.99, log Koc (sewage sludge) 1.46 (OECD Guideline 121); concentration 5 mg/L
Linuron, CAS 330-55-2, log Koc (soil) 2.59, log Koc (sewage sludge) 2.43 (OECD Guideline 121); concentration 5 mg/L
Phenyl benzoate, CAS 93-99-2, log Koc (soil) 2.87, log Koc (sewage sludge) 3.26 (OECD Guideline 121); concentration 5 mg/L
Fenthion, CAS 55-38-9, log Koc (soil) 3.31, log Koc (sewage sludge) 3.75 (OECD Guideline 121); concentration 5 mg/L
Phenanthrene, CAS 85-01-8, log Koc (soil) 4.09, log Koc (sewage sludge) 4.35 (OECD Guideline 121); concentration 5 mg/L

DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: 10μL per injection; an aliquot of test item (200 mg/L) was diluted to with methanol and then a test concentration of 110 mg/L sample was prepared using methanol/HPLC water to mobile phase ratio (methanol/HPLC water 55:45 v/v). Injected in triplicate,
- Quantity of reference substances: 10μL per injection; the concentration of each reference substance is indicated above injected in duplicate. Dead time was determined at 5 mg/L in triplcate.

REPETITIONS
- Number of determinations: three

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

Remarks:

in soil

Value:

2.4 dimensionless

pH:

7

Temp.:

23.6 °C

Remarks on result:

other: Mean temperature: 23.6 °C (min: 23.5 °C ; max: 23.7 °C)

Type:

Koc

Remarks:

in soil

Value:

251 L/kg

pH:

7

Temp.:

23.6 °C

Remarks on result:

other: Mean temperature: 23.6 °C (min: 23.5 °C ; max: 23.7 °C)

Type:

log Koc

Remarks:

in sewage sludge

Value:

2.5 dimensionless

pH:

7

Temp.:

23.6 °C

Remarks on result:

other: Mean temperature: 23.6 °C (min: 23.5 °C ; max: 23.7 °C)

Type:

Koc

Remarks:

in sewage sludge

Value:

316 L/kg

pH:

7

Temp.:

23.6 °C

Remarks on result:

other: Mean temperature: 23.6 °C (min: 23.5 °C ; max: 23.7 °C)

Details on results (HPLC method):

- Retention times of reference substances used for calibration: See table 1.
- Details of fitted regression line (log k' vs. log Koc): Calibration 1: r = 0.9550 and r2 = 0.9120 and Calibration 2: r = 0.9605 and r2 = 0.9225
- Average retention data for test substance: See table 2

Table 1. Capacity Factors (k’) of the reference substances and for soil and sewage sludge

Reference Item	Log Koc Soil	Log Koc sewage sludge	1^stcalibration			2^ndcalibration
			tr2 / min	k'	log k’	tr2 / min	k'	log k’
Acetanilide	1.26	1.52	4.073	1.536	0.186	4.076	1.538	0.187
Atrazine	1.81	1.66	4.743	1.953	0.291	4.749	1.957	0.292
Monuron	1.99	1.46	5.073	2.159	0.334	5.078	2.162	0.335
Linuron (1)	2.59	2.43	7.951	3.951	0.597	7.968	3.961	0.598
Benzoic acid phenyl ester	2.87	3.26	7.671	3.776	0.577	7.689	3.788	0.578
Fenthion	3.31	3.75	13.068	7.137	0.854	13.100	7.157	0.855
Phenanthrene	4.09	4.35	12.302	6.660	0.823	12.322	6.672	0.824

tr1 = Retention time injection 1

tr2 = Retention time injection 2

k’ = Capacity Factor

Koc = Adsorption Coefficient

(1) = not used for tr sewage sludge determination

 

Table 2. Capacity Factors (k’) of the reference substances and for soil and sewage sludge

	Log Koc Soil	Log Koc sewage sludge	tr2 / min	k'	log k’
Test Item			6.317	2.933	0.4673
			6.320	2.935	0.4676
			6.318	2.934	0.4675
Mean	2.4 ± 0.1	2.5 ± 0.2	6.318	2.934	0.4675
95% C.I.	2.1 to 2.7	2.0 to 2.9

tr = Retention time

C.I. = Confidence Interval

Validity criteria fulfilled:

yes

Conclusions:

The test item adsorption coefficient (log Koc) according to OECD Guideline 121 was estimated by HPLC analysis to be for soil: log Koc 2.4 at 23.6 °C and for sewage sludge Koc = 2.5 at 23.6 °C.

Executive summary:

The study was performed to OECD TG 121 and EU Method C.19 to assess the adsorption coefficient (Koc) of the test substance in accordance with GLP using a high performance chromatography system. The retention times of the test substance 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 pH ca. 7.0 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 substance adsorption coefficient (log Koc) for soil/sewage sludge was estimated to be for soil: log Koc 2.4 and for sewage sludge Koc = 2.5 at 23.6 °C and pH ca. 7.0 by HPLC analysis.

Description of key information

log Koc (soil) = 2.4 (Koc 251) and log Koc (sewage sludge) = 2.5 (Koc 316) at 23.6 °C, pH ca. 7.0 and 1 atm, OECD TG 121, 2014

Additional information

The study was performed to OECD TG 121 and EU Method C.19 to assess the adsorption coefficient (Koc) of the test substance in accordance with GLP using a high performance chromatography system. The retention times of the test substance 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 pH ca. 7.0 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 substance adsorption coefficient (log Koc) for soil/sewage sludge was estimated to be for soil: log Koc 2.4 and for sewage sludge Koc = 2.5 at 23.6 °C and pH ca. 7.0 by HPLC analysis.