Amines, N-tallow alkyltrimethylenedi-, reaction products with epichlorohydrin

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

14.09.2018 - 29.09.2018

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

study well documented, meets generally accepted scientific principles, acceptable for assessment

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Principles of method if other than guideline:

The water solubility of a test item was determined in two sequential steps Viz.,
• Qualitative analysis: Preliminary test to determine the range of test item solubility whether solubility was greater or lesser than 10-2g/L, the results was used to define the method for definitive test
• Quantitative analysis: Definitive test to determine the actual solubility in g/L either by Shake flask method (test item solubility greater than 10-2g/L) or by Column elution method (test item solubility lesser than 10-2g/L)
The preliminary test was conducted with 0.1g and 0.01g of test item with incremental addition of distilled water up to 1.0L with extended time of 96 hours. The results on preliminary solubility of test item at a concentration of 10-1g/L revealed that small portion adhered to the walls of the glass container/flask, small portion formed white color dispersion in liquid and remaining portion coagulates as white precipitate above the liquid layer. However the results on preliminary solubility of test item at a concentration of 10-2g/L revealed that fine traces adhered to the walls of the glass container/flask with clear solution and without any coagulation. Since the results on preliminary test results confirm the solubility of test item was less than 10-2g/L, column elution method was preferred.
In order to quantify the test item solubility by instrumentation technique, initial method development phase was conducted with HPLC using PDA detector (wavelength 200nm) and GC using mass spectral detector. The method suitability results revealed that in both the methods good separation of peaks was achieved. But the peak identification pertaining to test item was found to be critical for the following reasons.
• Multiple peaks resolved in HPLC (PDA detector) and GC (MSD) instrumentation techniques.
• Mass spectral analysis provides same fragmentation pattern for the good response peaks resolved at retention time of 7.7, 8.7, 8.9 and 9.8 minutes. However the fragmentation pattern differed for equally good response peaks resolved at 5.8, 9.5 and 11.5 minutes.
• Moreover the absorbance pattern was different for the peaks resolved with HPLC reverse phase conditions.

GLP compliance:

yes

Type of method:

column elution method

Specific details on test material used for the study:

Chemical Name Amines, N-tallow alkyl trimethylenedi-reaction products with epichlorohydrin
CAS Number 93821-29-5
Batch Number 93821-29-5
Molecular weight Not available
Molecular Formula Not available
Purity % Not available
Manufacturing date March 2018
Expiry date February 2019

Key result

Water solubility:

ca. 0.02 g/L

Conc. based on:

test mat.

Temp.:

20 °C

pH:

7

Conclusions:

The hypothetical value on water solubility of the liquid test item was ≤ 10-2g/L.

Executive summary:

The water solubility of test item, poly flow 130 cannot be precisely and accurately quantified. The test item in distilled water of 100.04 mg/L, upon incremental addition of distilled water from 0.1mL to 1L was found to be insoluble, rather it flocculated at the top of water layer partially, part adhered to the glass vessel and remaining part of the test item was found to be in dispersive state.

Additionally the preliminary test was conducted using the test item at a concentration of 10.34mg/L as per the procedure mentioned above, the results revealed that the test item in 1000mL of distilled water was found to be clear solution with fine traces of oily layer adhering to the sides of the glass vessel.

The initial experimentation on test item solubilization reveals that n-Hexane and n-Octanol were the suitable choice of solvent. Hence it has been decided to use solvent n-Hexane as diluent for test item evaluation with gas chromatograph and n-Octanol as diluent for test item evaluation with liquid chromatograph.

The method development phase was carried out prior to method validation. The results from GC-MS and HPLC-PDA instrumentation technique revealed that the test item was a multi - component chemical, since the test item resolved in to multiple peaks. The different fragmentation pattern from GC-MS and different absorbance pattern from HPLC-PDA, substantiates that the test item is an UVCB substance. This property hinders the refining of analytical reference standard to compare with the resolved peaks. Thus, the solubility of the test item cannot be precisely and accurately defined.

However based on preliminary investigation on the whole of the liquid test item poly flow 130, the solubility can be approximately defined as around 10-2g/L or lesser than that.

Description of key information

PolyFlo130 (OECD 105): ≤ 0.02 g/L

Key value for chemical safety assessment

Water solubility:

0.02 g/L

at the temperature of:

20 °C

Additional information

The water solubility of test item, poly flow 130 cannot be precisely and accurately quantified. The test item in distilled water of 100.04 mg/L, upon incremental addition of distilled water from 0.1mL to 1L was found to be insoluble, rather it flocculated at the top of water layer partially, part adhered to the glass vessel and remaining part of the test item was found to be in dispersive state.

Additionally the preliminary test was conducted using the test item at a concentration of 10.34mg/L as per the procedure mentioned above, the results revealed that the test item in 1000mL of distilled water was found to be clear solution with fine traces of oily layer adhering to the sides of the glass vessel.

The initial experimentation on test item solubilization reveals that n-Hexane and n-Octanol were the suitable choice of solvent. Hence it has been decided to use solvent n-Hexane as diluent for test item evaluation with gas chromatograph and n-Octanol as diluent for test item evaluation with liquid chromatograph.

The method development phase was carried out prior to method validation. The results from GC-MS and HPLC-PDA instrumentation technique revealed that the test item was a multi - component chemical, since the test item resolved in to multiple peaks. The different fragmentation pattern from GC-MS and different absorbance pattern from HPLC-PDA, substantiates that the test item is an UVCB substance. This property hinders the refining of analytical reference standard to compare with the resolved peaks. Thus, the solubility of the test item cannot be precisely and accurately defined.

However based on preliminary investigation on the whole of the liquid test item poly flow 130, the solubility can be approximately defined as around 10-2g/L or lesser than that.