Barium, 1,4-bis (C13-rich C11-14-isoalkyl) 2-sulfobutanedioate phosphate complex

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Testing was conducted between 08 February 2008 and 11 March 2008.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted in compliance with agreed protocols, with no or minor deviation from standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of relevant results.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2008

Report date:

2008

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

Date of inspection: 21/08/2007 Date of signature: 15/10/2007

Type of method:

other: differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

dibarium(2+) bis(1,5-dioxo-1,5-bis(tridecyloxy)pentane-3-sulfonate) hydrogen phosphate

EC Number:

931-037-9

Molecular formula:

Molecular formula for each combination of chain length. C13,13: (C30H57O7S)2 Ba @ BaHOP4 C11,12: (C27H51O7S)2 Ba @ BaHOP4 C12,12: (C28H53O7S)2 Ba @ BaHOP4 C12,13: (C29H55O7S)2 Ba @ BaHOP4 C13,14: (C31H59O7S)2 Ba @ BaHOP4 C14,14: (C32H61O7S)2 Ba @ BaHOP4

IUPAC Name:

dibarium(2+) bis(1,5-dioxo-1,5-bis(tridecyloxy)pentane-3-sulfonate) hydrogen phosphate

Details on test material:

Sponsor's identification: Barium di(bistridecylsulfosuccinate) in mixture with Barium hydrogen phosphate
Description : pale yellow solid
Batch number : Y-T-1
Storage conditions: room temperature, in the dark

Results and discussion

Melting / freezing point

Decomposition:

yes

Decomp. temp.:

>= 502 K

Remarks on result:

other: The test material decomposed, with melting, from 502 K.

Any other information on results incl. tables

Thermographic Data – Determination 1

Thermal Event	Interpretation	Temperature
		ºC	K
Endotherm	Decomposition, with melting	272.47	546

Thermographic Data – Determination 2

Thermal Event	Interpretation	Temperature
		ºC	K
Endotherm	Decomposition, with melting	273.19	546

Overall result: the test material decomposed, with melting from 546 K

Thermographic Data – Determination 1

Thermal Event	Interpretation	Temperature
		ºC	K
Endotherm	Decomposition, with melting	228.56	502

Thermographic Data – Determination 2

Thermal Event	Interpretation	Temperature
		ºC	K
Endotherm	Decomposition, with melting	229.16	502

Overall result: the test material decomposed, with melting from 502 K.

Discussion:

Assignment of the DSC thermograms was completed using observations recorded during an assessment performed using an amended liquid bath apparatus. The test material was observed to discolour to a light brown/orange solid over the temperature range of approximately 220°C to 230°C. On continuation of the test, the sample melted over a temperature range of 234°C to 237°C to give a dark brown, bubbling liquid, with a large quantity of froth above it.

Similar thermographic profiles were obtained using air and nitrogen atmospheres; this indicated that the observed decomposition in all DSC determinations was probably thermal and not oxidative. As expected with thermal decomposition, the onset temperatures were dependent on the heating rate/temperature program used. That is, on comparison of the preliminary screening test and the definitive test results, the slower heating rate of the definitive test resulted in a lower decomposition temperature. This was attributed to the test material having been exposed to an elevated temperature for an extended period of time, i.e. the decomposition temperature is a combined function of both temperature and exposure period. Of the data available, the definitive test results can be justified as the overall conclusion from the testing completed, as it used the heating rate of 1°C/minute (1 K/minute) as specified by the method guideline. However it is important to also note that the decomposition temperature was sensitive to heating rate.

Applicant's summary and conclusion

Conclusions:

The test material decomposed, with melting, from 502 K. However, the decomposition temperature was determined to be sensitive to heating rate and subsequently increased with an increase in heating rate, as the test material was exposed to elevated temperatures for a shorter time period. The definitive result was determined using a heating rate of 1 K/min, as required by the method guideline.

Executive summary:

Melting/Freezing Temperature. The test material decomposed, with melting, from 502 K, by differential scanning calorimetry, using ASTM E537-86, Method A1 of Commission Directive 92/69/EEC. However, the decomposition temperature was determined to be sensitive to heating rate and subsequently increased with an increase in heating rate, as the test material was exposed to elevated temperatures for a shorter period of time. The definitive result was determined using a heating rate of 1 K/min, as specified by the method guideline.