Diallyl hexahydrophthalate

Adsorption / desorption

Link to relevant study record(s)

Reference

Endpoint:

adsorption / desorption, other

Remarks:

Estimation of the Adsorption Coefficient (Koc) of MDAC

Type of information:

experimental study

Adequacy of study:

key study

Study period:

16 April 2018 to 18 April 2018 (Experimental start to experimental completion)

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline 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

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)

Type of method:

HPLC estimation method

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL

- Test item : MDAC (Diallyl hexahydrophthalate)
- Source.of test material: Osaka Soda Co., Ltd. Japan
- Lot/batch No.of test material: 40201
- Expiration date of the lot/batch:26 January 2019
- Purity test date: 26 September 2017

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: Controlled room temperature, protected from light
- Stability under test conditions: Assumed stable for the duration of the test
- Solubility and stability of the test substance in the solvent/vehicle: Not relevant
- Reactivity of the test substance with the solvent/vehicle of the cell culture medium: not relevant

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing: Not relavent

Radiolabelling:

no

Test temperature:

HPLC Conditions: Temperature 25°C

Details on study design: HPLC method:

EQUIPMENT
- Apparatus: HPLC system: Knauer Azura HPLC-UV
Balance: Sartorius BP221S
Ultrasonic bath: ELMA Elmasonic S300
Water purification system: Millipore, Direct-Q 8 UV
Refrigerator: Zanussi

- HPLC Conditions (type, material and dimension of analytical column):
Column: ACE 5 CN 250 × 4.6 mm, 5 μm
Mobil Phase: Acetonitrile : ultrapure water (ASTM Type I, prepared by Direct-Q 8 UV system, Millipore) . Ratio 6 : 4
Flow: 1 mL/min
Detector (UV): 210 nm
Injection volume: 20 μL
Temperature: 25°C

- Detection system: High performance liquid chromatography (HPLC), method applicable for substances,which have log Koc value ranging from about 0 to 6.

MOBILE PHASES
- Type: Acetonitrile (Super gradient, VWR, Batch No.: 17L121524) : ultrapure water = 6 : 4
- Experiments with additives carried out on separate columns: no
- pH: Not specified
- Solutes for dissolving test and reference substances: Sodium nitrate (Cas# 7631-99-4) dissolved with eluent at ca. 1 mg/mL. Reference substance and test item dissolved in Acetnitrile at ca. 1 mg/mL. The reference stock solutions were diluted with eluent resulting about 10μg/mL solution, the sodium nitrate and the test item solution were diluted with eluent to about 100 μg/mL.

DETERMINATION OF DEAD TIME
- Method: Dead time, t0 was determined by the injection of sodium nitrate solution.

REFERENCE SUBSTANCES
- Identity:
Chemical name CAS number log Koc Purity (%) Batch No.

Sodium nitrate 7631-99-4 t0 100.1 17H114112
Acetanilide 103-84-4 1.25 99.9 S6921344
Methyl benzoate 93-58-3 1.80 99.7 S6046630
Isoproturon 34123-59-6 1.86 99.8 SZBD221XV
Linuron 330-55-2 2.59 99.7 SZBD038XV
Naphthalene 91-20-3 2.75 99.8 10187351
α-Endosulfan 959-98-8 4.09 99.8 BCBS8631
DDT 50-29-3 5.63 98.7 SZBE057XV

DETERMINATION OF RETENTION TIMES
Three series of the above reference solutions and the test item solution were measured alternately, with two replicate injections.
For the determination of t0 (t0 = retention time of the unretarded component) sodium nitrate solution was injected.
The retention times were determined.

- Quantity of test substance introduced in the column: Not specified
- Quantity of reference substances: Not specified
- Intervals of calibration:

REPETITIONS
- Number of determinations: Three series of the above reference solutions and the test item solution were measuredalternately, with two replicate injections.

EVALUATION
- Calculation of capacity factors k': The capacity factors, k were calculated from the retention times (tR) of the selected
reference substances and the dead time (t0):
k = tR − t0
------------
t0
A calibration plot of log k versus log Koc was prepared. (See Figure 1.) The calibrationequation was determined by linear regression using the least squares method.
Repeatability is the difference of maximum and minimum values of log Koc derived from individual measurements.
Accuracy is the difference between the estimated log Koc and the log Koc value determined by the batch equilibrium method.

- Calculation of retention times:
Three series of the above reference solutions and the test item solution were measured alternately, with two replicate injections. For the determination of t0 (t0 = retention time of the unretarded component) sodium nitrate solution was injected.
The retention times were determined.

- Determination of the log Koc value:
The three calibration series and three test item series were measured alternately. The adsorption coefficient Koc was determined based on a calibration curve using 7 reference items. The capacity factors were calculated from the dead time and retention times of the reference substances. The log k data of the reference substances were plotted against their log Koc values. The equation of the curve fitted to the calibration points.

Analytical monitoring:

no

Key result

Type:

log Koc

Value:

2.89 dimensionless

Temp.:

25 °C

Details on results (HPLC method):

- Retention times of reference substances used for calibration: See below
- Details of fitted regression line (log k' vs. log Koc):
The three calibration series and three test item series were measured alternately. The adsorption coefficient Koc was determined based on a calibration curve using 7 reference items.
The capacity factors were calculated from the dead time and retention times of the reference substances. The log k data of the reference substances were plotted against their log Koc values. The equation of the curve fitted to the calibration points is as follows: log k = 0.1016 × log Koc – 0.1481 (R2= 0.9800)

- Graph of regression line attached: No
- Average retention data for test substance: See below.

Chemical log Koc from OECD 121 Retention time (min) log k Calc) log Koc (Calc) Repeatability ΔlogKoc Accuracy log unit

Sodium nitrate - Mean 1.83 ---------- for determination of dead time ---------

Acetanilide 1.25 Mean 3.44 -0.054 0.92 0.03 0.33

Methyl benzoate 1.80 Mean 3.87 0.048 1.93 0.04 0.13

Isoproturon 1.86 Mean 3.84 0.042 1.87 0.02 0.01

Linuron 2.59 Mean 4.19 0.111 2.55 0.02 0.04

Naphthalene 2.75 Mean 4.44 0.155 2.98 0.03 0.23

α-Endosulfan 4.09 Mean 5.40 0.291 4.32 0.02 0.23

DDT 5.63 Mean 6.42 0.400 5.40 0.01 0.23


MDAC (test item) - Mean 4.39 0.146 2.89 0.017

Validity criteria fulfilled:

yes

Conclusions:

Based on the chromatograms, one peak was detected from the test item at 4.39 min retention time. Based on the calibration, the log Koc of MDAC is to estimated 2.89 ± 0.010
(with 95% confidence interval).

Description of key information

Based on the calibration, the log Koc of MDAC is to estimated 2.89 ± 0.010 (with 95% confidence interval).

Key value for chemical safety assessment

Koc at 20 °C:

776