Bismuth tris(2-ethylhexanoate)

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018-05-17 to 2018-09-19

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: Thermal Stability (OECD 113)

Version / remarks:

1981

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

signed 2017-02-28

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

Storage conditions: -15 °C to 40 °C

Melting / freezing pt.:

>= -60 - <= 20 °C

Atm. press.:

>= 1 007 - <= 1 017 hPa

Decomposition:

yes

Decomp. temp.:

>= 230 °C

Remarks on result:

other: melting range: softening: -60 °C to -55 °C; very pasty: -55 °C to -40 °C; viscous paste: -10 °C; viscous liquid: 20 °C

Melting and Boiling Point (DSC)

Two endothermic signals in the temperature ranges of -70 °C to -30 °C and 220 °C – 370 °C were detected.

Results of the DSC-measurements

No.	Sample weight [mg]	Onset of Effect [°C]	Range of effect [°C]	Weight loss [mg]	Atmospheric pressure [hPa]
PN15727	19.49	-63.03 324.9	-65 to -40 (endo) 250 – 370 (endo)	12.49 64 %	1017.2
PN15728	13.71	-63.36 311.6	-70 to -30 (endo) 220 –360 (endo)	7.58 55 %	1017.2

During the cooling phase, no thermal effects were observed, which can be assigned to the freezing of the test item.

During the heating phase the test item showed two endothermic signals in the temperature range of -70 °C to -30 °C and 220 °C – 370 °C which cannot be definitely assigned to the boiling of the test item.

In view of the fact that the measured weight loss of each sample was only between 55 % and 64 % of the respective initial sample weight, the observed endothermic effects cannot be definitely assigned to the boiling of bismuth tris(2-ethylhexanoate).

Measurements by the Test Tube

Due to the fact that a very small peak at approx. -50 °C in the DSC was observed, the melting of the test item was verified in a test tube. For this purpose approx. 6.5 g of the test item in a test tube were cooled down with liquid nitrogen to approx. -70 °C. In the temperature range of -70 °C to -60 °C the test item was solid. The test item shows a softening in the temperature range of approx. -60 °C to -55 °C. The appearance of the test item during warming up was at approx. -55 °C to -40 °C very pasty, at -10 °C viscous paste and at 20 °C viscous liquid.

Measurements by the capillary method

For verification of the results the test item was additionally tested with the capillary method. At approx. 230 °C separate bubbles were observed. At approx. 250 °C solid part fell out. The test item started to change the colour at 260 °C from brown to dark brown, at approx. 265 °C to light brown, at 285 °C to grey/brown and became turbid at 300 °C, like a suspension. Above 320 °C developed bubbles faster, the test item turned grey. At a temperature of 326 °C the continuous and fast formation of bubbles (boiling) was observed. At 336 °C to 360 °C a grey/turbid, residue suspension was observed witch remained in the capillary.

The visual inspection of the measurement showed a boiling at 326 °C, accompanied by the release of volatile decomposition products of the test item in the temperature range of the endothermic effect detected in the DSC.

Thermal Stability (DSC)

In the temperature range from ambient temperature to 600 °C no thermal effects were observed.

Results of the DSC-measurements

No.	Sample weight [mg]	Start of effect [°C]	Energy [J/g]
PN15674	9.74	---	---
PN15675	8.93	---	---

No thermal effects of the test item were observed up to a temperature of 600 °C, only a pressure rise at approx. 380 °C was observed.

Conclusions:

Melting and Boiling Point
No definitive signs of melting of the test item bismuth tris(2-ethylhexanoate) were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, from -90 °C up to 600 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995) at atmospheric pressure (1017 hPa).
Based on the visual inspection in a test tube, the study monitor defined a melting range of -60 °C to 20 °C. From -70 °C to -60 °C the test item is a solid, a softening appeared from -60 °C to -55 °C, from -55 °C to -40 °C the test item is very pasty, at -10 °C it is a viscous paste and at 20 °C a viscous liquid.
No definitive signs of boiling of the test item bismuth tris(2-ethylhexanoate) were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, up to 600 °C, heating rate of 10 K/min) and by the capillary method (up to 360 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.2. and OECD Test Guideline 103 (1995) at atmospheric pressure (1007 – 1017 hPa). It is assumed that the test item boiled under decomposition at temperatures >230 °C.

Thermal Stability
In DSC measurements (closed glass crucible under air, from room temperature up to 600 °C, heating rate of 3 K/min) according to OECD guideline 113 (1981) the test item bismuth tris(2-ethylhexanoate) showed no thermal effects, only a pressure rise starting at approx. 380 °C was observed.

Description of key information

Melting and Boiling Point

Based on the visual inspection in a test tube, the study monitor defined a melting range for bismuth tris(2-ethylhexanoate) of -60 °C to 20 °C. The test item boiled under decomposition at temperatures >230 °C.

Additional information

Melting and Boiling Point

No definitive signs of melting of the test item bismuth tris(2-ethylhexanoate) were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, from -90 °C up to 600 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995) at atmospheric pressure (1017 hPa).

Based on the visual inspection in a test tube, the study monitor defined a melting range of -60 °C to 20 °C. From -70 °C to -60 °C the test item is a solid, a softening appeared from -60 °C to -55 °C, from -55 °C to -40 °C the test item is very pasty, at -10 °C it is a viscous paste and at 20 °C a viscous liquid.

No definitive signs of boiling of the test item bismuth tris(2-ethylhexanoate) were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air, up to 600 °C, heating rate of 10 K/min) and by the capillary method (up to 360 °C, heating rate of 10 K/min). The measurements were performed according to Regulation (EC) No. 440/2008 Method A.2. and OECD Test Guideline 103 (1995) at atmospheric pressure (1007 – 1017 hPa). It is assumed that the test item boiled under decomposition at temperatures >230 °C.

Thermal Stability

In DSC measurements (closed glass crucible under air, from room temperature up to 600 °C, heating rate of 3 K/min) according to OECD guideline 113 (1981) the test item bismuth tris(2-ethylhexanoate) showed no thermal effects, only a pressure rise starting at approx. 380 °C was observed.