4,4'-bis(dimethylamino)-4''-(methylamino)trityl alcohol

Adsorption / desorption

Link to relevant study record(s)

Reference

Endpoint:

adsorption / desorption: screening

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study

Justification for type of information:

Experimental test result performed using standard OECD test guidelines

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))

GLP compliance:

no

Type of method:

HPLC estimation method

Media:

soil/sewage sludge

Specific details on test material used for the study:

- Batch Number: KCP/FS/199/21
- Physical Apperance: Violet Powder

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Recommended storage conditions: Keep containers tightly closed in a dry and well ventilated place.

Radiolabelling:

no

Test temperature:

25°C

Details on study design: HPLC method:

EQUIPMENT
- Apparatus: HPLC
- Type: HPLC Model No. : Agilent Technologies,1260 Infinity II
- Type, material and dimension of analytical (guard) column: Cynopropyl gaurd column, 4.6*250 mm, 5 Âμm
- Detection system: Chem Station Open lab Control Panel at a wavelength of 210 nm

MOBILE PHASES
- Type: Methanol : water (55:45)
- Experiments with additives carried out on separate columns: no

DETERMINATION OF DEAD TIME
- Method: by means of homologous series / by inert substances which are not retained by the column

REFERENCE SUBSTANCES
- Identity: The reference substances 4-Chloroaniline, Toluene, 2,5-Dichloroaniline, 1-naphthol, Naphthalene, Phenanthrene and 1,2,3-Trichlorobenzene having Koc value ranging from 4.166 to 10.006.

DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: 20μl
- Quantity of reference substances: 20μl

REPETITIONS
- Number of determinations: Duplicates

EVALUATION
Retention time tR were measured, averaged and the decimal logarithms of the capacity factors k' were calculated. The graph was plotted between log Koc versus log k'. The linear regression parameter of the relationship log Koc vs log k' were also calculated from the data obtained with calibration samples and therewith, log Koc of the test substance was determined from its measured capacity factor.

Additional information:
HPLC Procedure:
The solutions of the test substance and reference substances were prepared in acetonitrile. Each of the reference substance and test substance were analysed by HPLC at 210 nm. After equilibration of the HPLC system, Urea was injected first, the reference substances were injected in duplicate, followed by the test chemical solution in duplicate. Reference substances were injected again after test sample, no change in retention time of reference substances was observed. Retention time tR were measured, averaged and the decimal logarithms of the capacity factors k' were calculated. The graph was plotted between log Koc versus log k'. The linear regression parameter of the relationship log Koc vs log k' were also calculated from the data obtained with calibration samples and therewith, log Koc of the test substance was determined from its measured capacity factor.

Operating Conditions:
HPLC Model No. : Agilent Technologies,1260 Infinity II
Flow Rate : 1.0ml/min
Column : Cyanoprpyl (CN), 4.6*250 mm, 5 Âμm
Guard columns : Cynopropyl gaurd column
Mobile phase : Methanol : water (55:45)
Temperature : 25°C
Detector : Variable wavelength detector @210nm
Injector : Autosampler
Injector volume : 20μl
Data Acquisition software : Chem Station Open lab Control Panel

Details on sampling:
- Concentrations: 2000 mg/l
- Preparation of Test chemical: A test item solution was prepared by accurately weighing 20 mg of test item and diluted with methanol up to 10 ml. Thus, the test solution concentration was 2000 mg/l. The sample was sonicated for 5 minutes and filtered through a 0.22 µm syringe filter. The pH of the sample was found to be 7.9.

Analytical monitoring:

not required

Details on matrix:

Not applicable

Details on test conditions:

Not applicable

Key result

Type:

log Koc

Value:

4.386 dimensionless

pH:

7.9

Temp.:

25 °C

Remarks on result:

other: logKoc was reported to be 4.386±0.010

Details on results (HPLC method):

The Adsorption coefficient (KOC) on soil and on sewage sludge of the test chemical was determined to be 4.386±0.010 at 25°C.

Adsorption and desorption constants:

Not applicable

Recovery of test material:

Not applicable

Concentration of test substance at end of adsorption equilibration period:

Not applicable

Concentration of test substance at end of desorption equilibration period:

Not applicable

Transformation products:

not specified

Details on results (Batch equilibrium method):

Not applicable

Table 1:

Reference substances	tR1	tR2	Mean tR± S.D.	k'	Log k'	Log Koc
Sodium nitrate	3.159	3.124	3.142±0.025	NA	NA	NA
4-Chloroaniline	4.166	4.184	4.175±0.013	0.329	-0.483	1.7
Toluene	4.418	4.421	4.420±0.002	0.407	-0.391	2.1
2,5-Dichloroaniline	6.188	6.162	6.175±0.018	0.966	-0.015	3.7
1-naphthol	6.34	6.127	6.234±0.151	0.984	-0.007	3.7
Naphthalene	7.022	7.03	7.026±0.006	1.237	0.092	4.1
Phenanthrene	9.016	9.004	9.010±0.008	1.868	0.271	4.8
1,2,3- Trichlorobenzene	10.006	9.923	9.965±0.059	2.172	0.337	5.2

Table 1- The above table indicates, eight reference substances were taken according to structural similarity with the test chemical to prepare calibration graph. Individual reference substances were allowed to pass through the column on fixed operating conditions in order to obtain the values of t_Rand SD.  These values are then used to determine k' which is then converted to log k' value (applying equation no. 1). This log k' was then plotted on the calibration curve to determined log Koc value of each.

Table 2:

Test chemical		k’	Log k’	Log Koc	Mean of Log Koc± S.D
tR1	7.611	1.423	0.153	4.379	4.386±0.010
tR2	7.645	1.434	0.156	4.393

Validity criteria fulfilled:

yes

Conclusions:

The Adsorption Coefficient of test chemical was determined as per the HPLC method (OECD Guideline-121). The Log Koc value was determined to be 4.386±0.010 at 25°C.

Executive summary:

The adsorption coefficient Koc in soil and in sewage sludge of test chemical was determined by the Reverse Phase High Performance Liquid Chromatographic method according to OECD Guideline No. 121 for testing of Chemicals. A test item solution was prepared by accurately weighing 20 mg of test item and diluted with methanol up to 10 ml. Thus, the test solution concentration was 2000 mg/l. The sample was sonicated for 5 minutes and filtered through a 0.22 µm syringe filter. The pH of the sample was found to be 7.9. Each of the reference substance and test substance were analysed by HPLC at 210 nm. For the HPLC method, HPLC model no. Agilent Technologies,1260 Infinity II was used. Column used was Cyanoprpyl (CN), 4.6*250 mm, 5 Âμm. Methanol : water (55:45) was used as a mobile phase. During the study, flow rate was 1.0ml/min. Study was performed at a temperature of 25°C. Injector volume was 20μl. Chem Station Open lab Control Panel was used as a data Acquisition software and detector wavelength taken for the study was 210 nm. After equilibration of the HPLC system, Urea was injected first, the reference substances were injected in duplicate, followed by the test chemical solution in duplicate. Reference substances were injected again after test sample, no change in retention time of reference substances was observed. Retention time tR were measured, averaged and the decimal logarithms of the capacity factors k' were calculated. The graph was plotted between log Koc versus log k'. The linear regression parameter of the relationship log Koc vs log k' were also calculated from the data obtained with calibration samples and therewith, log Koc of the test substance was determined from its measured capacity factor. The reference substances were chosen according to estimated Koc range of the test substance and generalized calibration graph was prepared. The reference substances 4-Chloroaniline, Toluene, 2,5-Dichloroaniline, 1-naphtol, Naphthalene, Phenanthrenea and 1,2,3-Trichlorobenzene were chosen having log Koc range from 4.166 to 10.006. The Log Koc value of test chemical was determined to be 4.386±0.010 at 25°C.This log Koc value indicates that the test chemical has a strong sorption to soil and sediment and therefore have negligible to slow migration potential to ground water.

Description of key information

The adsorption coefficient Koc in soil and in sewage sludge of test chemical was determined by the Reverse Phase High Performance Liquid Chromatographic method according to OECD Guideline No. 121 for testing of Chemicals. A test item solution was prepared by accurately weighing 20 mg of test item and diluted with methanol up to 10 ml. Thus, the test solution concentration was 2000 mg/l. The sample was sonicated for 5 minutes and filtered through a 0.22 µm syringe filter. The pH of the sample was found to be 7.9. Each of the reference substance and test substance were analysed by HPLC at 210 nm. For the HPLC method, HPLC model no. Agilent Technologies,1260 Infinity II was used. Column used was Cyanoprpyl (CN), 4.6*250 mm, 5 Âμm. Methanol : water (55:45) was used as a mobile phase. During the study, flow rate was 1.0ml/min. Study was performed at a temperature of 25°C. Injector volume was 20μl. Chem Station Open lab Control Panel was used as a data Acquisition software and detector wavelength taken for the study was 210 nm. After equilibration of the HPLC system, Urea was injected first, the reference substances were injected in duplicate, followed by the test chemical solution in duplicate. Reference substances were injected again after test sample, no change in retention time of reference substances was observed. Retention time tR were measured, averaged and the decimal logarithms of the capacity factors k' were calculated. The graph was plotted between log Koc versus log k'. The linear regression parameter of the relationship log Koc vs log k' were also calculated from the data obtained with calibration samples and therewith, log Koc of the test substance was determined from its measured capacity factor. The reference substances were chosen according to estimated Koc range of the test substance and generalized calibration graph was prepared. The reference substances 4-Chloroaniline, Toluene, 2,5-Dichloroaniline, 1-naphtol, Naphthalene, Phenanthrenea and 1,2,3-Trichlorobenzene were chosen having log Koc range from 4.166 to 10.006. The Log Koc value of test chemical was determined to be 4.386±0.010 at 25°C.This log Koc value indicates that the test chemical has a strong sorption to soil and sediment and therefore have negligible to slow migration potential to ground water.

Key value for chemical safety assessment

Koc at 20 °C:

24 322

Additional information

The adsorption coefficient Koc in soil and in sewage sludge of test chemical was determined by the Reverse Phase High Performance Liquid Chromatographic method according to OECD Guideline No. 121 for testing of Chemicals. A test item solution was prepared by accurately weighing 20 mg of test item and diluted with methanol up to 10 ml. Thus, the test solution concentration was 2000 mg/l. The sample was sonicated for 5 minutes and filtered through a 0.22 µm syringe filter. The pH of the sample was found to be 7.9. Each of the reference substance and test substance were analysed by HPLC at 210 nm. For the HPLC method, HPLC model no. Agilent Technologies,1260 Infinity II was used. Column used was Cyanoprpyl (CN), 4.6*250 mm, 5 Âμm. Methanol : water (55:45) was used as a mobile phase. During the study, flow rate was 1.0ml/min. Study was performed at a temperature of 25°C. Injector volume was 20μl. Chem Station Open lab Control Panel was used as a data Acquisition software and detector wavelength taken for the study was 210 nm. After equilibration of the HPLC system, Urea was injected first, the reference substances were injected in duplicate, followed by the test chemical solution in duplicate. Reference substances were injected again after test sample, no change in retention time of reference substances was observed. Retention time tR were measured, averaged and the decimal logarithms of the capacity factors k' were calculated. The graph was plotted between log Koc versus log k'. The linear regression parameter of the relationship log Koc vs log k' were also calculated from the data obtained with calibration samples and therewith, log Koc of the test substance was determined from its measured capacity factor. The reference substances were chosen according to estimated Koc range of the test substance and generalized calibration graph was prepared. The reference substances 4-Chloroaniline, Toluene, 2,5-Dichloroaniline, 1-naphtol, Naphthalene, Phenanthrenea and 1,2,3-Trichlorobenzene were chosen having log Koc range from 4.166 to 10.006. The Log Koc value of test chemical was determined to be 4.386±0.010 at 25°C.This log Koc value indicates that the test chemical has a strong sorption to soil and sediment and therefore have negligible to slow migration potential to ground water.