Reaction mass of benzoyl chloride, toluoyl chloride and 2-methyl resorcinol

Water solubility

Administrative data

Endpoint:

water solubility

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

Report date:

2022

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Version / remarks:

27 July 1995

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

No. 440/2008 of 30 May 2008

Deviations:

no

Principles of method if other than guideline:

Twelve timepoints for both systems showed some variability in dissolved test item amount. Due to this, not all of the samples considered to be on a solubility plateau fell within ± 30% of the mean as specified in the test guidelines. There was, however, no obvious issues with the chromatography (e.g., contamination) which would account for the variability, and therefore all of the samples considered to be on a solubility plateau were included in the overall result.
Also, the two vessels gave different results with the higher flow rate showing higher solubility. Therefore, the result from System A has been reported as the overall result to represent the higher limit of solubility shown during testing.

GLP compliance:

yes

Type of method:

column elution method

Test material

Test material information

Constituent 1

Reference substance name:

Reaction mass of benzoyl chloride, toluoyl chloride and 2-methyl resorcinol

Molecular formula:

not applicable

IUPAC Name:

Reaction mass of benzoyl chloride, toluoyl chloride and 2-methyl resorcinol

Test material form:

solid: particulate/powder

Details on test material:

Appearance: beige powder

Results and discussion

Water solubility

Key result

Water solubility:

<= 0 g/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

ca. 7

Any other information on results incl. tables

Preliminary Test

The preliminary estimate of the water solubility at 20.0 ± 0.5 °C was less than 1.0 x 10^-4 g/L. The solution had a pH of 7.2.

Definitive Test

The mean peak areas relating to the standard and sample solutions are shown in the following table:

Table 2

Solution	Mean Total Peak Area
Standard 1.01 mg/L	1.9767 x 10^6
Standard 2.02 mg/L	3.8934 x 10^6
Standard 2.52 mg/L	4.8789 x 10^6
Standard 3.02 mg/L	5.9257 x 10^6
Standard 4.03 mg/L	7.7955 x 10^6
Standard 5.04 mg/L	9.7716 x 10^6
Standard 2.03 mg/L	3.9695 x 10^6
Matrix blank	None detected
System A, Sample 1	9.9793 x 10^7
System B, Sample 1	1.0227 x 10^8
System A, Sample 2	3.5883 x 10^7
System B, Sample 2	9.8551 x 10^7
System A, Sample 3	5.5124 x 10^6
System B, Sample 3	4.7658 x 10^7
System A, Sample 4	1.8924 x 10^7
System B, Sample 4	1.0253 x 10^7
System A, Sample 5	2.4982 x 10^7
System B, Sample 5	1.0138 x 10^6
System A, Sample 6	1.5631 x 10^8
System B, Sample 6	4.2422 x 10^6
Standard 1.01 mg/L	1.9602 x 10^6
Standard 2.02 mg/L	3.8617 x 10^6
Standard 2.52 mg/L	4.8156 x 10^6
Standard 3.02 mg/L	5.8497 x 10^6
Standard 4.03 mg/L	7.7766 x 10^6
Standard 5.04 mg/L	9.7295 x 10^6
Standard 10.1 mg/L	1.9420 x 10^7
Standard 25.2 mg/L	4.8254 x 10^7
Standard 50.4 mg/L	9.6216 x 10^7
Standard 101 mg/L	1.9276 x 10^8
Standard 2.03 mg/L	3.9000 x 10^6
System A, Sample 7	2.4012 x 10^6
System B, Sample 7	6.1089 x 10^6
System A, Sample 8	8.7650 x 10^5
System B, Sample 8	2.1776 x 10^6

Table 2 (continued)

Solution	Mean Total Peak Area
System A, Sample 9	8.5610 x 10^3
System B, Sample 9	1.1745 x 10^4
System A, Sample 10	5.1417 x 10^6
System B, Sample 10	2.5756 x 10^6
System A, Sample 11	2.3735 x 10^8
System B, Sample 11	4.6831 x 10^5
System A, Sample 12	1.2275 x 10^7
System B, Sample 12	7.1594 x 10^5

The calibration curves from which the sample concentrations were calculated are shown in the figures below.

The concentration (mg/L) of test item in the sample solutions is shown in the following table:

Table 3

Sample Number	Sampling Time (hour)		Concentration (mg/L)		Solution pH
	System A	System B	System A	System B	System A	System B
1*	165	164	2.58	2.65	7.3	7.4
2*	170	169	0.927	2.55	6.9	6.9
3*	187	186	0.142	1.23	7.2	7.4
4*	192	191	0.489	0.265	7.3	7.1
5*	211	210	0.646	0.025	7.4	7.4
6*	216	215	4.04	0.109	7.7	6.7
7	453	452	0.062	0.159	7.5	6.6
8	459	458	0.022	0.056	7.5	6.6
9	477	476	< 0.01	< 0.01	7.1	7.1
10	483	482	0.133	0.066	7.2	7.2
11	500	499	6.21^*	0.011	7.2	7.2
12	506	505	0.320	0.017	7.2	7.2

* These samples were considered to not be on the solubility plateau; therefore, these samples were not
used in any subsequent calculations.

The overall results are shown in the following table:

Table 4

System	Mean Concentration (mg/L)	Standard Deviation
A	0.134	0.132
B	0.062	0.059

Overall result: Less than or equal to 1.34 x 10^-4 g/L at 20.0 ± 0.5 °C

Validation
Assessment of the sample recovery procedure was performed and proved adequate for the test as shown in the following table:

Table 5

Nominal Concentration (mg/L)	Recovery Range (%)	Mean Recovery (%)
0.10	99.2 to 99.4	99.3
0.05	93.8 to 94.3	93.9

Test sample concentrations have not been corrected for the recovery of analysis.

Applicant's summary and conclusion

Conclusions:

The water solubility of the test item has been determined to be less than or equal to 1.34 x 10^-4 g/L of solution at 20.0 ± 0.5 °C.