Tar bases, coal, lutidine fraction

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:

Experimental start date: 15 January 2016, Experimental completion date: 15 January 2016

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995 (Freezing temperature method)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

Commission Regulation (EC) No 440/2008, dated May 30, 2008

Deviations:

no

GLP compliance:

no

Remarks:

However, the study was performed in a test facility which has been certified to be in compliance with the principles of GLP.

Type of method:

method to determine freezing temperature

Melting / freezing pt.:

> -20 °C

Atm. press.:

ca. 101 kPa

Decomposition:

no

Sublimation:

no

Remarks on result:

other: Determination made under ambient pressure

Melting / freezing pt.:

> 253 K

Atm. press.:

ca. 101 kPa

Decomposition:

no

Sublimation:

no

Remarks on result:

other: Determination made under ambient pressure

Cooling data for determinations 1 and 2 are shown in Table 1 and Table 2 respectively.

Graphs of temperature (K) versus time (seconds) for determinations 1 and 2 are shown in the attached Figure 1 and Figure 2 respectively.

Determination 1 result:

Freezing temperature less than -20 °C (<253 K).

Determination 2 result:

Freezing temperature less than -20 °C (<253 K).

Overall result:

Freezing temperature less than -20 °C (<253 K).

The test item showed no change in appearance during cooling.

Table 1: Determination 1, Cooling Data

Time [s]	Temperature [°C]	Time [s]	Temperature [°C]
0	21.0	780	-11.5
30	19.0	810	-12.0
60	18.0	840	-12.5
90	16.0	870	-13.0
120	13.0	900	-13.5
150	10.5	930	-15.0
180	9.0	960	-15.0
210	7.0	990	-15.5
240	6.0	1020	-16.0
270	5.0	1050	-16.5
300	3.0	1080	-17.0
330	2.0	1110	-17.5
360	0.5	1140	-18.0
390	-1.0	1170	-18.5
420	-1.5	1200	-18.5
450	-3.0	1230	-19.0
480	-3.5	1260	-19.0
510	-4.5	1290	-19.5
540	-5.0	1320	-19.5
570	-6.0	1350	-20.0
600	-7.0	1380	-20.0
630	-8.0	1410	-20.0
660	-8.5	1440	-20.0
690	-9.5	1470	-20.5
720	-10.0	1500	-20.5
750	-11.0	1530	-21.0

Table 2: Determination 2, Cooling Data

Time [s]	Temperature [°C]	Time [s]	Temperature [°C]
0	20.5	690	-11.0
30	19.0	720	-12.0
60	17.0	750	-12.0
90	15.0	780	-12.5
120	13.0	810	-13.5
150	11.0	840	-14.5
180	9.0	870	-15.0
210	7.5	900	-15.5
240	6.0	930	-16.0
270	4.5	960	-16.5
300	3.5	990	-17.0
330	2.0	1020	-17.0
360	1.0	1050	-18.0
390	0.0	1080	-18.5
420	-1.0	1110	-18.5
450	-3.0	1140	-19.0
480	-3.5	1170	-20.0
510	-5.0	1200	-20.0
540	-6.0	1230	-20.0
570	-7.0	1260	-20.0
600	-8.0	1290	-20.5
630	-9.0	1320	-21.0
660	-10.0	-	-

 

Conclusions:

In a valid, reliable and conclusive study according to OECD TG 102 (1995) and Method A.1 (EC) No 440/2008, the freezing temperature of the test item has been determined to be less than -20 °C (<253 K).

Executive summary:

The freezing temperature of the test item was investigated in a non-GLP study using the method according to the OECD TG 102 (1995) and EU A.1 (Commission Regulation (EC) No 440/2008) protocols. The experiment is considered relevant, adequate and conclusive.

An aliquot (approximately 15 mL) of test item was placed into a test tube containing a thermometer. A wire loop with which the sample could be agitated was placed inside the tube to ensure sample homogeneity during cooling. The test tube was surrounded by a glass jacket and then placed into a large beaker containing a dry ice/acetone mixture. The temperature and observations of the test item were recorded approximately every 30 seconds. The dry ice/acetone bath was maintained until the temperature had reached approximately 20 °C or until the test item solidified. The determination was carried out in duplicate. The test item showed no change in appearance during cooling. In conclusion the freezing temperature of the test item has been determined to be less than -20 °C (<253 K).

Description of key information

In a valid, reliable and conclusive study according to OECD TG 102 (1995) and Method A.1 (EC) No 440/2008, the freezing temperature of the test item has been determined to be less than -20 °C (<253 K).