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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:
key study
Study period:
20.05.2008
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
guideline study without detailed documentation
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
DSC Method
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
- Powder
- Substance description: "LK 1404"
Key result
Melting / freezing pt.:
ca. 240 °C
Atm. press.:
101.325 kPa

DSC method:

Rate of temperature increase: 20 K / min

Temperature range: 25 -270 °C

Conclusions:
The analysis shows for both samples a peak at 188.5 °C (arithmetic mean) and 237.9 (arithmetic mean). As the area of the peak is larger at 237.9 °C the melting point is determined for 237.9 °C, rounded up as 240 °C.
Executive summary:

According to the OECD test guideline 102, the melting point for 1-Benzyl-3-carbamoyl-pyridinium,chloride was determined with about 240 °C at 101.325 kPa.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
21. - 23. Nov. 2016
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:
other: OECD Boiling Point TG 103
Version / remarks:
DSC method
GLP compliance:
no
Other quality assurance:
ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories)
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
White powder.

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing: Two different sample preparations: native and dried. The dried sample was was stored in a drying cabinet for 24h at 130°.
Key result
Melting / freezing pt.:
ca. 245 °C
Decomposition:
yes
Decomp. temp.:
ca. 257 °C

The boiling point can be calculated from the onset, whereby impure samples are characterised by their peak maximum. The peak maxima of the analysed sample are given in the following table and are shown graphically in the illustration part.

As can be seen in the DSC curves, the test item shows up to three peaks. The peak at 209 °C (peak no. 1) occurs only in the native sample (measurement 1) and indicates an impurity in the sample material with a relatively low boiling point. This assumption is justified due to several reasons: The impurity is not present in the dried sample material. Furthermore, the certificate of analysis of the sample declares the presence of nicotinamide with a content of 3-4 % and this value was verified in a specific separate experiment by determination of nicotinamide. The verification was conducted for both, the native and dried sample material and hereby, in contrast to the native material, no nicotinamide could be found after temperature treatment. Likewise, this peak could not be found with DSC (measurement 2).

Peak no. 2 and 3 occur in both measurements. Peak no. 2 resp. 4 at approx. 245 °C seem to be the melting point of the test item, whereas peak no. 3 resp. 5 at approx. 257 °C indicate the decomposition of the analysed sample material.

Consequently, the boiling point of the test item could not be determined, since it decomposes at approx. 257 °C. The decomposition could also be confirmed visually in an additional test using a boiling capillary inside a heated metal block according to Siwoloboff.

Table 1: Results

               
 Measurement  Sample Weigh-in [mg]   Peak number [-]  Onset [°C] Peak maximum [°C]   Peak area [mJ] Weight loss [%] 
 1 native  12.49  204.9  209.4  107.4  57.6 
       2 240.9  242.5  236.0   
       3 247.5  255.0  652.2   
 2 dried  14.68 
       4 245.2  246.6  1175  74.0 
       5 252.5 258.7  702.0   

The DSC curves including indvidual peaks no. 1 to 5 are illustrated in the attachment to this IUCLID entry.

Conclusions:
The melting point of the dried and thereby purified test sample as determined by DSC measurements, which where conducted within the scope of measurements in accordance with OECD 103 (Boiling Point), is approximately 245 °C.
Executive summary:

In the context of an experiment to determine the boiling point of 1-Benzyl-3-carbamoyl-pyridinium, chloride, the melting point was additionally established. The analysis was conducted in accordance with OECD Guideline 103.

To eliminate potential impurities one sub-sample was dried for 24 h at 130 °C. The native and the dried sample were applied in the experiment. The melting point for both samples is similar and is determined for 1-Benzyl-3-carbamoyl-pyridinium, chloride to be approximately 245 °C.

Description of key information

The melting point was experimentally determined to be 240 °C (Braun, 2008) according to the OECD TG 102. Likewise the melting point of 245 °C was confirmed within the scope of a test conducted to determine the boiling point following the OECD TG 103 (Kuhlmann, 2017). Both values are very similar.

The value which was determined in accordance with OECD Guideline 102 (Melting Point) is considered the key value. The second measurement according to OECD 103 (Boiling Point) supports the initial finding.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
240 °C

Additional information