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Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2014
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Qualifier:
equivalent or similar to guideline
Guideline:
other: SAV.421: Messungen im Differentiakalorimeter Mettler Toledo (R) System und TAI 2910/2920
GLP compliance:
no
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
- Lot/batch No.: 407940
Key result
Melting / freezing pt.:
ca. 66 °C
Decomposition:
yes
Decomp. temp.:
> 188 °C

Results (scan with 4°C/min)

Sample

Run

Thermal Signal

Range [°C], Peak-Temperature [°C]

Energy [kJ/kg]

919210.14.0472.02

LIMS Nr : 23215

N° 1

Endo : 55 -77, 66

Exo : 199-263, 240

-12

204

919210.14.0472.02

LIMS Nr : 23215

N° 2

Endo : 55 -75, 66

Exo : 190 -281, 258

-12

210

Conclusions:
The test item shows a melting point at 66°C and starts decompositing at 188-190°C.
Executive summary:

A double determination of the thermal stability of the test item by DSC (Differential Scanning Calorimetry) was performed with a DSC 820e Mettler, with closed crucibles.

At the end of the measurement, the crucibles were tight and no losses was registered.

The results show an endothermic reaction between 55°C to 75-77°C, with a peak of -12 kJ/kg at 66°C. Then, an exothermic phase appears between ca. 188 -190°C, with a peak of 204-210 kJ/kg at 258°C.

It seems that the Sepisol Fast Yellow MG-F has a melting point at around 66°C, and starts decomposing at ca. 188 -190°C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2014-05-21
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Qualifier:
no guideline followed
Principles of method if other than guideline:
Determination of the melting point by the thermoanalytical technique DSC
GLP compliance:
no
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
- Lot/batch No.: 407940
Key result
Melting / freezing pt.:
ca. 70 °C
Decomposition:
yes
Decomp. temp.:
ca. 230 °C
Conclusions:
The test item has a melting point according the DSC of 70°C.
Executive summary:

A determination of the thermal stability of the test item by DSC (Differential Scanning Calorimetry) was performed with a DSC Mettler TOLEDO DSC 1, using a perforated crucible.

The result shows an endothermic reaction between 52 and 79°C, with a peak of -8.79 kJ/kg at 70°C.

Then an exothermic phase starts at 230°C, consistent with the beginning of the decomposition of the test item.

It seems that the Sepisol Fast Yellow MG-F has a melting point at around 66°C, and starts decomposing at ca. 230°C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
2014-02-13
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Qualifier:
equivalent or similar to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
similar to Kofler hot bar
Deviations:
yes
Remarks:
: hot bar PROLABO, temperature is homogenous on the hot bar
Principles of method if other than guideline:
Technic similar to the Kofler Hot bar.
Apparatus PROLABO: temperature is homegenous at every point of the hot bar
GLP compliance:
no
Type of method:
hot stages
Remarks:
similar to Kofler hot bar
Specific details on test material used for the study:
- batch: 407940
Key result
Decomposition:
yes
Decomp. temp.:
ca. 230 °C
Remarks on result:
other: The test item decompose before melting

Calibration of the hot bar Prolabo: A dividing line is observed and a fluid phase is appearing. There was a temperature lag between the theoretical melting and the measured one, but the order of magnitude is correct.

 

Test item: With the increase temperature, the test item became darker and stickier. At 163°C (non corrected value), the test item is liquefied.

 

Product

Readed T°C at which the product becomes sticky

Measured Testo's T°C of the « apparent melting »

Corrected T°C according to the « standard »

Remarks

Potassium thiocyanate

Theoretical MP = 173 °C

 

174°C

176°C

Around 170°C the correction is estimated at -3°C

Ammonium dihydrogen phosphate

Theoretical MP= 190 °C

At 194°C, crystals becomes colorless

200°C

Around 200°C the correction is estimated at -10°C

Melting point difficult to measured

Test Item

Lot 316576

106°C

(became darker)

138°C

(liquid appearance)

Around 137°C

(minus 1°C)

230°C : liquid darkens

270°C : smoke + carbonization

300°C : test stopped

Conclusions:
Under normal conditions of pressure, Sepisol Fast Yellow MG-F has no melting point.
Executive summary:

Under normal conditions of pressure, Sepisol Fast Yellow MG-F seems to have a softening point at 130°c but no melting point. The test material starts to decompose around 230°C becomes darker and at 280°C the test item is carbonized with smoke. The assay was stopped after reaching 300°C with the hot bar.

Description of key information

3 tests were performed to determine the melting of the test item:

- one hot bar test

- two DSC with open and close crucible

The substance has no melting point and starts decomposing at temperature > 200°C.

Key value for chemical safety assessment

Additional information

3 tests were performed to determine the melting of the test item:

- one hot bar test

- two DSC with open and close crucible

Method used

Melting point temperature

Decomposition temperature

Hot bar method

no melting point (softening point at 130°C)

Starts at 230°C

DSC n°1 with close crucible

66°C

Starts at 188 -190°C

DSC n°2 with open crucible

70°C

Starts at 230°C

The 2 DSC, which give a close result, have both been performed with a Mettler-Toledo apparatus.

An endothermic peak in a DSC heating curve, performed with a Mettler Toledo apparatus is a melting peak if:

- the sample weight does not decrease significantly over the course of the peak, and

- the sample appears to have visibly melted after the measurement, and

- the surface area of the peak is between about 120 Jg-1 to 170 Jg-1 for non-polyleric organic substances, and

- the half-width of the peak is significantly less than 10 K (i.e. 10°C).

The surface area of the peaks is very low (-12 and -8.79 kJ/kg), which is << of the 120 kJ/kg cut off value.

No data is provided concerning the half-width of the peaks.

Therefore, the endothermic peak observed at 66 -70°C does not fulfill all the criteria of a melting peak.

Conclusion: The substance has no melting point and starts decomposing at temperature > 200°C.