1-benzyl-3-carbamoylpyridinium chloride

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key 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:

OECD Guideline 103 (Boiling Point)

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 24 h at 130°.

Key result

Decomposition:

yes

Decomp. temp.:

ca. 257 °C

Remarks on result:

not determinable

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	1	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 boiling point could not be determined as the substance decomposed at 257 °C, after melting at 245 °C. The decomposition was confirmed by an additional experiment with a boiling capillary inside a heated metal block according to Siwoloboff.

Executive summary:

To determine the boiling point of 1-Benzyl-3-carbamoyl-pyridinium, chloride, an analysis was conducted in accordance with OECD test guideline 103 by using a Perkin-Elmer DSC 4000.

To eliminate potential impurities one sub-sample was dried for 24 h at 130 °C. Both 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-pyridiniumchloride with about 245 °C. Both samples decomposed at 257 °C. Hence, the boiling point could not be determined.

Description of key information

The boiling point could not be assigned, due to the substance decomposing at 257 °C, after melting at 245 °C (Kuhlmann, 2017). The experiment was conducted in accordance with the OECD TG 103.