Bismuth(3+) neodecanoate

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:

2018-01-17 to 2018-09-10

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

Remarks:

capillary method, test tube

Specific details on test material used for the study:

Storage conditions: Room temperature tightly closed

Melting / freezing pt.:

>= -50 - <= 0 °C

Atm. press.:

>= 1 002 - <= 1 022 hPa

Decomposition:

ambiguous

Remarks:

boiling under decomposition

Decomp. temp.:

>= 320 - <= 410 °C

Sublimation:

no

Melting and Boiling Point (DSC)

The thermograms of the DSC runs PN16195, PN16196 and PN16258 in open glass crucibles under air detected in the temperature range of -50 °C to 0 °C, an endothermic effect followed by an exothermic effect in the temperature range of 10 °C – 240 °C with a mean energy of -120 J/g. A second endothermic effect was observed in the temperature range of 320 °C – 410 °C.

The DSC run PN16195 in open glass crucibles under nitrogen detected in the temperature range of -40 °C to 20 °C an endothermic effect followed by an exothermic effect in the temperature range of 60 °C – 190 °C with a mean energy of -20 J/g. Two further endothermic effects were observed in the temperature range of 300 °C – 400 °C and 460 °C - 600 °C. The exothermic effect is possibly caused by reaction of atmospheric oxygen with the test item.

Results of the DSC-measurements

No.	Sample weight [mg]	Onset of Effect [°C]	Range of effect [°C]	Weight loss [mg]	Atmospheric pressure [hPa]
PN16195	10.42	-41.58 --- 352.32	-50 to -20 (endo) 30 – 230 (exo) 340 – 410 (endo)	8.41 81 %	1007.6
PN16196	11.35	-35.89 --- 337.17	-40 to 0 (endo) 20 – 240 (exo) 320 – 390 (endo)	8.72 77 %	1007.6
PN16258	9.71	-41.39 --- 357.43	-50 to -10 (endo) 10 – 230 (exo) 320 – 410 (endo)	7.90 81 %	1001.9
PN16330	23.35	-35.43 --- 346.99	-40 to 20 (endo) 60 – 190 (exo) 300 – 400 (endo) 460 – 600 (endo)	17.73 76 %	1022.0

*Negative energy for exothermic processes, positive energy for endothermic processes

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 an endothermic signal in the temperature range of -50 °C to 0 °C which is caused by a softening of the test item, confirmed by the measurement in a test tube.

The second endothermic signal in the temperature range of 320 °C to 410 °C can be assigned to a boiling under decomposition of the test item, confirmed by the capillary method (colour change from yellowish to light brown at approx. 300 °C).

In view of the fact that the measured weight loss of each sample was only between 76 % and 81 % of the respective initial sample weight, none of the observed endothermic effects can be definitively assigned to boiling of bismuth (3+) neodecanoate.

Measurements by the Test Tube

Due to the fact that a small melting peak in the DSC was observed, the melting of the test item was verified in a test tube.In the temperature range of -60to approx. -45 °C the test item was a very viscous yellow paste. The test item shows a softening in the temperature range of approx. -40 °C to -32 °C. The appearance of the test item during warming up wasin the temperature range of -32 °C to approx. 0 °C very viscous and at 10 °C viscous liquid.

Measurements by the Capillary Method

The test item was tested with the capillary method in the temperature range 30 °C to 400 °C with a heating rate of 10 K/min. In the temperature range of 30 – 270 °C no change of the test item was observed. The test item changed the colour from yellowish to light brown at approx. 300 °C and slowly bubbles were observed. At approx. 310 °C the test item was light brown and cloudy. At approx. 350 °C faster bubbles and a grey/brown/cloudy appearance of the test item were observed. The visual inspection of the measurement showed boiling accompanied with the release of volatile decomposition products of the test item in the temperature range of the endothermic effect detected in the DSC. It is assumed that the test item decomposes at temperatures >300 °C.

Thermal Stability (DSC)

In the temperature range of 25 °C to 600 °C no thermal effects were observed.

Results of the DSC-measurements

No.	Sample weight [mg]	Start of effect [°C]	Energy [J/g]
PN14968	11.46	---	---
PN14969	8.55	---	---

No decomposition of the test item was observed up to a temperature of 600 °C.

Conclusions:

Melting and Boiling Point
No definitive signs of melting/boiling of the test item bismuth (3+) neodecanoate were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air and nitrogen, up to 600 °C, heating rate of 10 K/min). The DSC measurements were performed according to Regulation (EC) No. 440/2008 Method A.1/A2 and OECD Test Guideline 102/103 (1995) at atmospheric pressure (1002 – 1022 hPa). During the heating phase the test item showed an endothermic signal in the temperature range of -50 °C to 0 °C. In addition, testing was performed in a test tube that showed a softening in the temperature range of approx. -40 °C to -32 °C at atmospheric pressure (1008 hPa).
Based on the results and the visual inspection in a test tube, the study monitor defined a melting range of -50 °C to 0 °C
The second endothermic signal (DSC) in the temperature range of 320 °C to 410 °C may be assigned to boiling of the substance under decomposition, that can be confirmed by the capillary method (change of the appearance from yellowish liquid to grey/brown/cloudy).

Thermal Stability
In the DSC no decomposition of the test item bismuth (3+) neodecanoate was observed up to a temperature of 600 °C.

Description of key information

The test item bismuth (3+) neodecanoate has a melting range of -50 °C to -0 °C and boils under decomposition in the temperature range of 320 °C to 410 °C.

Additional information

Melting and Boiling Point

No definitive signs of melting/boiling of thetest item bismuth (3+) neodecanoatewere observed by differential scanning calorimetry (DSC) measurements (open glass crucible under air and nitrogen, up to 600 °C, heating rate of 10 K/min). The DSC measurements were performed according to Regulation (EC) No. 440/2008 Method A.1/A2 and OECD Test Guideline 102/103 (1995) at atmospheric pressure (1002 – 1022 hPa). During the heating phase the test item showed an endothermic signal in the temperature range of -50 °C to 0 °C. In addition, testing was performed in a test tube that showed a softening in the temperature range of approx. -40 °C to -32 °C at atmospheric pressure (1008 hPa). Based on the results and the visual inspection in a test tube, the study monitor defined a melting range of -50 °C to 0 °C.

The second endothermic signal (DSC) in the temperature range of 320 °C to 410 °C may be assigned to boiling of the substance under decomposition, that can be confirmed by the capillary method (change of the appearance from yellowish liquid to grey/brown/cloudy).

Thermal Stability

In the DSC no decomposition of the test item bismuth (3+) neodecanoatewas observed up to a temperature of 600 °C.