Soybean meal, protein extn. residue

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:

04 January 2018 to 30 March 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline 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

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

>= 30 - <= 120 °C

Atm. press.:

>= 100.2 - <= 102.1 kPa

Thermal Analysis

- Determination 1: Loss on heating: 65 %

- Determination 2: Loss on heating: 12 %

- Determination 3: Loss on heating: 9 %

- Determination 4: Loss on heating: 20 %

- Determination 5: Loss on heating: 72 %

- Determination 6: Loss on heating: 72 %

- Atmospheric pressure:

Determination 1: 100.2 kPa

Determination 2 to 6: 102.1 kPa

 

Modified Capillary / Liquid Bath Method

- Significant sample observations and temperatures are summarised in the following tables:

Table 2: Visual Evaluation on Heating – Determination 1

Temperature (°C)	Observations
21	Fine, beige, dry powder, at the start of the test.
98	The test material appears to be shrinking away from the walls of the tube, leaving some frond-like projections reaching out to the glass tube.
118	The central part of the test material now appears to be a block of waxy, beige material, some frond-like projections remain.
122	Liquid (beige, contains bubbles) appeared around the test material and above it, rapidly covering half of the test material, fronds are now absent.
137	The test material is mostly very viscous, foaming liquid, beige with an orange/dark beige section (~ 10 %) at the top. The test material has expanded to cover ~ 5 cm of the tube.
152	The test material is now wholly foam, covering entire tube, beige/ light brown in colour, darkest near the surface, bottom of tube almost empty due to large bubbles. The test material near the top has much denser bubbles. The top of the test material is now above the level of the silicone fluid.
170	The foam is becoming darker in colour, now a pale brown colour with many large bubbles near the top, above the level of the silicone fluid.
183	The foam is now dark brown in colour beneath the level of the silicone fluid, large bubbles present. Above the level of the silicone fluid, the test material is still a pale brown foam with smaller bubbles. Test halted.

 

Table 3: Visual Evaluation on Heating – Determination 2

Temperature (°C)	Observations
30	Fine, beige, dry powder, at the start of the test.
75	Gaps are appearing in between the grains of powder, at least they are now more evident.
90	Shrinkage is beginning, test material is pulling away from the glass, fronds are connecting glass tube to the test material main block.
105	Moistening of the test material, including the fronds.
125	The fronds have mostly collapsed, becoming part of the main test material block, which now has an appearance of mostly liquid, foam (beige), with some dry patches (also beige).
135	The dry patches are now absent, leaving a denser foam in the centre, upper part of the test material, slowly expanding upwards leaving behind a very bubbly foam beneath it. Now covers ~ 2.5 cm of the tube
143	Central denser foam is still moving up the tube, leaving less dense-appearing foam beneath it, now covers ~ 5 cm of the tube.
152	The test material foam now covers the entire tube, larger bubbles formed near the base. Test halted.

 

- Overall result: Melted/softened from approximately 30 to 120 °C (303 to 393 K).

 

Discussion

- As the DSC thermogram did not show any definitive indications of melting and boiling, it was considered that an additional, capillary / modified liquid bath method would give more definitive results as to how the test material changes physically on heating. As both procedures gave useful information, the modified liquid bath procedure results were taken alongside the DSC thermograms to give a better understanding of how the test material acts on heating.

- As a result of the initial low rate of enthalpy change during melting / softening and partial boiling / decomposition, the onset temperatures could only be approximated.

- Similar thermographic profiles were obtained using air and nitrogen atmospheres. This indicated that the decomposition was probably thermal and not oxidative.

Conclusions:

Under the conditions of this study, the test material was determined to melt/soften from approximately 30 to 120 °C at 100.2 to 102.1 kPa.

Executive summary:

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102 and EU Method A.1, under GLP conditions.

As the DSC thermogram did not show any definitive indications of melting and boiling, it was considered that an additional, capillary / modified liquid bath method would give more definitive results as to how the test material changes physically on heating. As both procedures gave useful information, the modified liquid bath procedure results were taken alongside the DSC thermograms to give a better understanding of how the test material acts on heating.

As a result of the initial low rate of enthalpy change during melting / softening and partial boiling / decomposition, the onset temperatures could only be approximated. Similar thermographic profiles were obtained using air and nitrogen atmospheres. This indicated that the decomposition was probably thermal and not oxidative.

Under the conditions of this study, the test material was determined to melt/soften from approximately 30 to 120 °C at 100.2 to 102.1 kPa.

Description of key information

Under the conditions of this study, the test material was determined to melt/soften from approximately 30 to 120 °C at 100.2 to 102.1 kPa.

Additional information

The melting point of the test material was investigated in accordance with the standardised guidelines OECD 102 and EU Method A.1, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

As the DSC thermogram did not show any definitive indications of melting and boiling, it was considered that an additional, capillary / modified liquid bath method would give more definitive results as to how the test material changes physically on heating. As both procedures gave useful information, the modified liquid bath procedure results were taken alongside the DSC thermograms to give a better understanding of how the test material acts on heating.

As a result of the initial low rate of enthalpy change during melting / softening and partial boiling / decomposition, the onset temperatures could only be approximated. Similar thermographic profiles were obtained using air and nitrogen atmospheres. This indicated that the decomposition was probably thermal and not oxidative.

Under the conditions of this study, the test material was determined to melt/soften from approximately 30 to 120 °C at 100.2 to 102.1 kPa.