Phenol, 4-(9H-carbazol-3-ylamino)-, reaction products with sodium sulfide (Na2(Sx)) and sulfur, leuco deriv.

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:

2017-03-01 - 2017-05-18

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

2008

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Remarks:

including capillary method for verfication

Key result

Melting / freezing pt.:

> 500 °C

Atm. press.:

1 006.1 hPa

Decomposition:

no

Remarks on result:

other: no melting point up to a temperature of 500 °C

Results

The test item showed an endothermic effect in the temperature range of 50 – 150 °C, which was followed by an exothermic effect in the temperature rang 130 – 260 °C, with a mean decomposition energy of approx. 30 J/g. No further thermal effects could be observed up to the maximum test temperature of 500 °C.

Table 1:    Results of the DSC-measurements

No.	Sample weight / mg	Onset of Effect / °C	Range of effect / °C	Weight loss / mg	Remark
PN12982	14.90	64.92 ---	60 – 130 (endo) 180 – 250 (exo)	3.89	Figure 1
PN12983	17.00	61.44 ---	50 – 150 (endo) 160 – 260 (exo)	5.53	Figure 2

During the heating phase a endothermic effect was detected the temperature range of 50 – 150 °C, which cannot be clearly assigned to the melting of the test item.

Since no further endothermic effects could observed be up to the maximum test temperature of 500 °C, it can be stated that the test item has no boiling point up to 500 °C.

Measurements by the capillary method:

To verify the results of the DSC measurement, an additional measurement with the capillary method (Apparatus: Stuart Melting Point SMP30) was performed in the temperature range of 50 – 400 °C with a heating rate of 10 K/min. The observations during the test with the capillary method are summarized in Table 2.

Table 2:    Observations during the test with the capillary method (Heating rate: 10 K/min)

Temperature	Observation	Temperature	Observation
Start (50 °C)	Blueish black solid	250 °C	Blueish black solid
75 °C	Blueish black solid	275 °C	Blueish black solid
100 °C	Blueish black solid	300 °C	Blueish black solid
125 °C	Blueish black solid	325 °C	Blueish black solid
150 °C	Blueish black solid	350 °C	Blueish black solid
175 °C	Blueish black solid	375 °C	Blueish black solid
200 °C	Blueish black solid	End (400 °C)	Blueish black solid
225 °C	Blueish black solid

According to the observations during the test with the capillary method, the endothermic effect in the temperature range of 50 – 150°C in the DSC measurements cannot be assigned to the melting of the test item. Since the test item contains 2.7 % water, it can be assumed, that the endothermic effect is caused by the drying of the test item.

As the test item showed no significant change in its appearance up to a temperature of 400 °C in the capillary method and no distinct endothermic effects could be observed in the DSC measurements, it can be stated that the test item has no melting and boiling point up to a temperature of 500 °C.

Conclusions:

Final Results:
The test item Leuco Sulfur Blue 20 has no melting point up to a temperature of 500 °C at atmospheric pressure (1006.1 hPa) as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).

Executive summary:

 Summary

The test item Leuco Sulfur Blue 20 has no melting point up to a temperature of 500 °C at atmospheric pressure (1006.1 hPa) as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).

Description of key information

The test item Leuco Sulfur Blue 20 has no melting point up to a temperature of 500 °C at atmospheric pressure (1006.1 hPa) as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).