2-Propenoic acid, 2-methyl-, tris(1-methylethyl)silyl ester

Adsorption / desorption

Administrative data

Endpoint:

adsorption / desorption: screening

Type of information:

experimental study

Adequacy of study:

key study

Study period:

26 May to 27 May 2010

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Recent study conducted by a GLP certified laboratory in accordance with a suitable study guideline.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2010

Report date:

2010

Materials and methods

Test guideline

Test guideline 1

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

Test guideline 2

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

Test material

Test material information

Constituent 1

Reference substance name:

Tripropan-2-ylsilyl 2-methylprop-2-enoate

EC Number:

700-182-8

Cas Number:

134652-60-1

Molecular formula:

C13 H26 O2 Si

IUPAC Name:

Tripropan-2-ylsilyl 2-methylprop-2-enoate

Details on test material:

- Name of test material: TIS-M
- Lot/batch No.: 9925
- Expiration date of the lot/batch: 2 December 2010
- Storage condition of test material: Under nitrogen at room temperature, continuously protected form all light.

Specific details on test material used for the study:

Details on properties of test surrogate or analogue material (migrated information):
None

Radiolabelling:

no

Study design

Test temperature:

25 deg C (column temperature)

HPLC method

Details on study design: HPLC method:

APPARATUS

Stationary Phase LiChrospher 100 CN 250 x 4 mm, 5μm HPLC Column
No.: 841404
HPLC system: Merck-Hitachi LaChrom HPLC system:
D-7000 Interface, No.: 0811-181
L-7100 HPLC pump, No.: 0823-059
L-7200 Autosampler, No.: 0606-021
L-7400 UV Detector, No.: 0928-058
Hitachi 655A-52 Column Oven, No: 6211-016
L 7612 Degasser, No.: 012-05
Balance: BP221S Sartorius, No.: 11809117
Water purification system: MILLIPORE, DIRECT Q3, FOMNO 7334I
Ultrasonic bath: Elmasonic S300H, ELMA, No.: 010890105

HPLC Conditions:

Mobil Phase: ACN : Water ( 60 : 40 )
Flow: 0.5 ml/min.
Injection volume: 10 μl
Detector: UV at 218 nm
Column temperature: 25 °C

DETERMINATION OF DEAD TIME
- Method: Sodium nitrate used to calculate dead time.

REFERENCE SUBSTANCES
- Identity: Sodium nitrate, Acetanilide, Methyl benzoate, Linuron, Naphthalene, Fenthion, Phenantrene and DDT.

DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: TIS-M was dissolved in acetonitrile. The concentration of this solution was 1 mg/ml. This stock solution was diluted with ACN (1 to 100 dilution).
- Quantity of reference substances: Reference substances were dissolved in ACN. Concentration of these stock solutions was about 1 mg/ml.
These stock solutions were diluted with the mobile phase resulting in about 10 μg/ml solutions.
- Intervals of calibration: Various.

REPETITIONS
- Number of determinations: 6

EVALUATION
- Calculation of capacity factors k': k' = (tr-t0)/t0 where tR is the retention time of the selected reference substance and t0 is the dead time.
- 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.
- Determination of the log Koc value: log k' = 0.1016 * log Koc + 0.0607. The calibration equation was determined by linear regression using the least squares method.

Batch equilibrium or other method

Analytical monitoring:

not specified

Details on sampling:

Not applicable

Details on matrix:

Not applicable

Details on test conditions:

Not applicable

Computational methods:

Not applicable

Results and discussion

Adsorption coefficient

Adsorption coefficient 1

Type:

Koc

Value:

17 259

Temp.:

25 °C

Adsorption coefficient 2

Type:

log Koc

Value:

4.24

Temp.:

25 °C

Results: HPLC method

Details on results (HPLC method):

- Mean Retention times of reference substances used for calibration: Sodium Nitrate: 2.40, Acetanilide: 5.82, Methyl Benzoate: 6.71, Linuron: 7.42, Naphthalene: 8.07, Fenthion: 8.88, Phenantrene: 9.13, DDT: 12.53.
- Details of fitted regression line (log k' vs. log Koc):
- Graph of regression line attached
- Average retention data for test substance: 9.85 minutes.

Results: Batch equilibrium or other method

Transformation products:

not specified

Any other information on results incl. tables

Table 2: Measured and calculated data of the reference substances and test item.

Chemical name	Log Koc	Retention Time (min)	Log k’	Log Koc	Accuracy	Repeatability
	From OECD 121		calculated	calculated	Log unit	ΔlogKoc, log unit
Sodium Nitrate	-	2.41	For determination of dead time.
		2.41
		2.40
		2.40
		2.40
		2.40
	Mean	2.40
	CV%	0.2
Acetanilide	1.25	5.81	0.152	0.89	0.34	0.03
		5.82	0.153	0.91
		5.83	0.154	0.92
		5.83	0.154	0.92
		5.82	0.153	0.91
		5.82	0.153	0.91
	Mean	5.82	0.153	0.91
	CV%	0.1	-	-
Methyl- benzoate	1.80	6.69	0.251	1.88	0.10	0.04
		6.69	0.251	1.88
		6.73	0.255	1.92
		6.73	0.255	1.92
		6.72	0.254	1.91
		6.71	0.253	1.90
	Mean	6.71	0.253	1.90
	CV%	0.3	-	-
Linuron	2.59	7.39	0.317	2.52	0.04	0.04
		7.40	0.318	2.53
		7.44	0.321	2.57
		7.42	0.320	2.55
		7.43	0.320	2.56
		7.42	0.320	2.55
	Mean	7.42	0.319	2.55
	CV%	0.3	-	-
Naphthalene	2.75	8.04	0.370	3.05	0.32	0.05
		8.05	0.371	3.05
		8.10	0.375	3.09
		8.07	0.373	3.07
		8.08	0.373	3.08
		8.08	0.373	3.08
	Mean	8.07	0.373	3.07
	CV%	0.3	-	-
Fenthion	3.31	8.86	0.429	3.63	0.33	0.03
		8.86	0.429	3.63
		8.90	0.432	3.65
		8.90	0.432	3.65
		8.88	0.431	3.64
		8.88	0.431	3.64
	Mean	8.88	0.431	3.64
	CV%	0.2	-	-
Phenantrene	4.09	9.12	0.446	3.80	0.29	0.01
		9.13	0.447	3.80
		9.14	0.448	3.81
		9.14	0.448	3.81
		9.13	0.447	3.80
		9.13	0.447	3.80
	Mean	9.13	0.447	3.80
	CV%	0.1	-	-
DDT	5.63	12.55	0.626	5.56	0.08	0.03
		12.56	0.626	5.56
		12.54	0.625	5.56
		12.53	0.625	5.55
		12.49	0.623	5.54
		12.49	0.623	5.54
	Mean	12.53	0.625	5.55
	CV%	0.2	-	-
TIS-M	-	9.88	0.493	4.26	-	-
		9.87	0.492	4.25
		9.85	0.491	4.24
		9.85	0.491	4.24
		9.83	0.490	4.23
		9.81	0.489	4.21
	Mean	9.85	0.491	4.24
	CV%	0.3	-	-

A calibration plot of log k' versus log Koc was prepared.The calibration equation 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.

Retention time of TIS-M (9.85 min) is within the calibrated range, so it was possible to estimate a log Koc value.

Applicant's summary and conclusion

Validity criteria fulfilled:

yes

Conclusions:

The log Koc of the registered substance was estimated to be 4.24 and the adsorption coefficient (Koc) was estimated to be 17 259.

Executive summary:

The adsorption coefficient (Koc) of the registered substance was assessed according to EC C.19 using a HPLC method. It was calibrated using the following reference substances: Sodium Nitrate, Acetanilide, Methyl Benzoate, Linuron, Naphthalene, Fenthion, Phenantrene and DDT. The log Koc of the registered substance was estimated to be 4.24 and the adsorption coefficient (Koc) was estimated to be 17 259.