Nickel, 5-[2-(2-hydroxy-3,7-disulfo-1-naphthalenyl)diazenyl]-1H-1,2,4-triazole-3-carboxylate sodium complexes

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Study initiation 30th October 2002, experimental phase 6-18th November

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Meets the criteria for classification as Reliable without restriction according to Klimisch et al (1997)

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2003

Report date:

2003

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

GLP compliance:

yes

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

-

EC Number:

443-510-2

EC Name:

-

Cas Number:

738587-10-5

Molecular formula:

C26H14N10Ni2O18S4 as free acid

IUPAC Name:

dinickel(2+) sodium 3-carboxy-5-[(1E)-2-(7-oxido-2,6-disulfonaphthalen-1-yl)diazen-1-yl]-1H-1,2,4-triazol-1-ide 3-carboxy-5-[(1E)-2-(7-oxido-2-sulfo-6-sulfonatonaphthalen-1-yl)diazen-1-yl]-1H-1,2,4-triazol-1-ide

Results and discussion

Boiling point

Boiling pt.:

> 420 °C

Atm. press.:

101.3 kPa

Any other information on results incl. tables

Two samples of approximately 10 - 11 mg of test material, sealed in aluminium crucibles with a micro pin hole in the lid, were heated at 10 K.min-1 in a Mettler DSC821e from 25 - 450°C under a nitrogen purge (75 ml.min-1).

In both scans, a broad endothermic peak was observed at a peak temperature of ca. 135°C, followed by a large and vigorous exotherm at a peak temperature of ca. 420°C. It is known from information provided by the Sponsor that the endothermic peak is not associated with melting, as the test substance has been shown not to melt below 310°C. The exothermic peak

suggests that decomposition has occurred, which was confirmed by examination of the samples after cooling, revealing the presence of a residue of 61 - 62% of the original mass. No endothermic peak indicative of boiling was observed.

Applicant's summary and conclusion

Conclusions:

The test substance decomposes without boiling.

Executive summary:

Introduction

The boiling point was measured by DSC, which is an approved method for Test A2.

The heat flow to the sample is measured as it is heated at a constant rate in a sealed crucible which, for a boiling point determination, must have a very small pin hole in the lid. As the boiling point is approached, the heat flow begins to increase as the sample evaporates through the pin hole. Once the sample boils, its temperature remains constant and the furnace temperature moves ahead of that of the sample at a constant rate, causing the heat flow profile to have a linear portion before it again subsides once the sample has boiled away. The temperature at the linear portion of the DSC thermogram is the boiling point.

Results and conclusion

Two samples of approximately 10 - 11 mg of test material, sealed in aluminium crucibles with a micro pin hole in the lid, were heated at 10 K.min-1 in a Mettler DSC821e from 25 - 450°C under a nitrogenpurge (75 ml.min-1).

In both scans, a broad endothermic peak was observed at a peak temperature of ca. 135°C, followed by a large and vigorous exotherm at a peak temperature of ca. 420°C. It is known from information provided by the Sponsor that the endothermic peak is not associated with melting, as the test substance has been shown not to melt below 310°C. The exothermic peak

suggests that decomposition has occurred, which was confirmed by examination of the samples after cooling, revealing the presence of a residue of 61 - 62% of the original mass. No endothermic peak indicative of boiling was observed.

A typical Thermogram is shown in figure 1 and can be found in the 'Attached bckground material' under 'DSC Thermograph from Physical and Chemical properties Report HT02 -405B'

The test substance decomposes without boiling.