Chloro[29H,31H-phthalocyaninato(2-)-N29,N30,N31,N32]aluminium

Adsorption / desorption

Administrative data

Endpoint:

adsorption / desorption: screening

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2019

Materials and methods

Test guideline

Test guideline 1

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))

Test guideline 2

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))

GLP compliance:

yes (incl. QA statement)

Type of method:

HPLC estimation method

Media:

other: soil and sewage sludge

Test material

Test material information

Constituent 1

Reference substance name:

Chloro[29H,31H-phthalocyaninato(2-)-N29,N30,N31,N32]aluminium

EC Number:

237-998-4

EC Name:

Chloro[29H,31H-phthalocyaninato(2-)-N29,N30,N31,N32]aluminium

Cas Number:

14154-42-8

Molecular formula:

C32H16AlClN8

IUPAC Name:

31h-phthalocyaninato(2-)-n29,n39,n31,n32]-chloro[29(sp-5-12)-aluminu; chloro[29H,31H-phthalocyaninato(2-)-N29,N30,N31,N32]-,(SP-5-12)-Aluminum;CHLOROALUMINUM PHTHALOCYANINE;CHLORO(29H,31H-PHTHALOCYANINATO)ALUMINUM; CHLORO(PHTHALOCYANINATO)ALUMINIUM;ALUMINUM PHTHALOCYANINE CHLORIDE;PHTHALOCYANINE CHLOROALUMINUM; chloro[29H,31H-phthalocyaninato(2-)-N29,N30,N31,N32]aluminium

Test material form:

solid: particulate/powder

Study design

Test temperature:

25 ± 0.5 °C

Results and discussion

Adsorption coefficient

Adsorption coefficient 1

Key result

Sample No.:

#1

Type:

log Koc

Value:

-3.07 dimensionless

pH:

4

Temp.:

25 °C

Adsorption coefficient 2

Key result

Sample No.:

#2

Type:

log Koc

Value:

-3.07 dimensionless

pH:

4

Temp.:

25 °C

Adsorption coefficient 3

Key result

Sample No.:

#3

Type:

log Koc

Value:

-3.07 dimensionless

pH:

4

Temp.:

25 °C

Applicant's summary and conclusion

Executive summary:

The study was performed using a HPLC with a cyanopropyl chemical bound resin on a silica basecolumn.Sixreference items with different retention times and sodium nitrate as dead time marker were used to produce a calibration curve, since retention time on cyanopropyl columns and K_OCare correlated. The reference items were chosen on behalf of the pre-test.

Because the test item is ionisable, this study was conducted at pH 4 and pH 10 to ensure the determination of the ionised and of the unionised form.

Therefore, two determinations were performed using mobile phases, adjusted to pH 4.0 resp. pH 10.0 to ensure a defined pH value.

For the determination at pH 4.0,a solvent blank, followed by three injections of a solution of the reference items, were analysed with HPLC. Then, three injections of a solution of the test item; and finally three injections of the solution with the reference items, in total ten runs.

For each reference item, the capacity factor k’ was calculated from the retention time of sodium nitrate and the retention time of the respective reference item. A calibration function was set up using the literature values for K_OCof the reference items and the mean capacity factor of the six determinations. In the graph log k’ versus log K_OC, linear regression was performed,giving r²= 0.9972 and r = 0.9986 for pH 4.

 

The chromatogram of the test item at pH 4.0 gave one small peak at 1.683 min and one large peak at 2.190 min. With the calibration function log k’ versus log K_OC, the corresponding log K_OCcould be calculated as -3.070 ± 0.000 for peak 1 and 0.331±0.00 (mean ± standard deviation) for peak 2. As the test item peaks lay outside the calibrated range, the log K_OCof the test item is stated as < 1.25 (log K_OCof the reference Acetanilide with the lowest log K_OC) at pH 4.

For the determination at pH 10.0, an HPLC program with an isocratic part for substances eluting in the calibrated range. The isocratic part was finished after the retention time of4,4’-DDTas the reference with the highest log K_OC. The isocratic part was followed by a washing step with mobile phase pH 4. The washing step was used to elute the test item from the column and to show detectability of the test item.

A solvent blank, followed by one injection of a solution of the reference items, was analysed with HPLC. Then two injections of a solution of the test item were conducted and finally one injection of the solution with the reference items, in total five runs.

In the graph log k’ versus log K_OC, linear regression was performed,giving r²= 0.9945 and r = 0.9972 for pH 10.

The test item peak showed a retention time of 30.9 min with a very low standard deviation of 0.035 min. The determination was precise. The calculation of the log K_OCof the test item peak is not possible, because the peak eluted not in the isocratic part of the HPLC program. Extrapolation is not possible therefore. Because the retention time of the test item peak is higher than the retention time of4,4’-DDT(14.9 minutes), the log K_OCof the test item at pH 10 is stated as > 5.63 (log K_OCof4,4’-DDTas reference with the highest log K_OC)

Therefore, the log K_OCof the test item is stated as< 1.25 (pH 4) and > 5.63 (pH 10).