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Boiling point

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Reference
Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From 12 to 23 April 2012
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/boiling range)
Deviations:
not specified
Qualifier:
according to guideline
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
not specified
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7220 (Boiling Point / Boiling Range)
Deviations:
not specified
Qualifier:
according to guideline
Guideline:
other: SOP-LO-113 Thermal Stabilitiy via DSC
Deviations:
not specified
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry
Remarks:
Measurements by the capillary method to verifty the results of DSC
Key result
Decomposition:
yes
Remarks:
The test item decomposes firstly at a temperature of > 200 °C.
Decomp. temp.:
> 200 °C

Results:

The test itemzincmethacrylateshowed an exothermal effect in the temperature range 220 – 310 °C with a decomposition energy of ‑250 J/g. In the temperature range of 390 – 430 °C an endothermic effect could be observed.

Table1: Results of the DSC-measurements on thermal stability

No.

Sample weight / mg

Start of effect / °C

Energy / J/g

 Remaks

PN3640

10.15

220

390

-250 (exothermal)
80 (endothermic)

 Figure 1

Melting and Boiling point:

The DSC runs PN3647, PN3651 and PN3653 are shown in figures 2, 3 and 4

In the temperature range of 5 – 70 °C an endothermic effect was detected. In the temperature range of approx. 120 – 190 °C an exothermal effect could be measured, with a decomposition energy of ‑30 J/g. Up to 200 °C no mass loss could be measured.

Table 2: Results of the first test series on melting and boiling point

No.

Sample weight / mg

Start of effect / °C

Energy /
J/g
R

Remarks

PN3647

10.12

5

20 (endothermic)

 Figure 2

PN3651

9.86

--

--

 Figure 3

PN3653

11.71

--

--

 Figure 4

Measurements by the capillary method:

To verify the results of the DSC-measurement six additional measurements with the capillary method (Apparatus: Büchi melting Point B-540) was performed.

Table 3: Observations during the capillary method (Heating rate: 10 K/min from 26 °C to 410 °C)

 

Sample 1-3

Sample 4-6

Filling height (each)

6 mm

5 mm

Start (26 °C)

white solid

white solid

197 °C

slight change of the colour from white to light brown, still solid

slight change of the colour from white to light brown, still solid

230 °C

change of the colour to brown, still solid (see figure 5)

change of the colour to brown, still solid

350 °C

change of the colour to dark brown, still solid

change of the colour to dark brown, still solid

At the end of the measurements the test item was still solid. The measurement with the capillary method confirmed the results of the DSC-measurements concerning the melting and boiling behavior.

Conclusions:
The test item zinc methacrylate has no melting and boiling point at atmospheric pressure (1013 hPa). The test item decomposes firstly at a temperature of > 200 °C. The measurement with the capillary method confirmed the results of the DSC-measurements concerning the melting and boiling behavior.
Executive summary:

This study was performed in order to determine the thermal stability as well as the melting/boiling point of Zinc methacrylate according to the EU Method A.2 and OECD 103 and 113. In this test, the thermal stability and the melting/boiling temperature of the test item were investigated by DSC (differential scanning calorimetry). With this method the difference in energy input into the test item and a reference material as a function of temperature was recorded, while the substance and reference material were subjected to the same temperature program. The prepared crucibles (crucible with test item and reference crucible) were placed in the DSC apparatus. To verify the results of the DSC-measurement six additional measurements with the capillary method (Apparatus: Büchi melting Point B-540) was performed. The test item zinc methacrylate has no melting and boiling point at atmospheric pressure (1013 hPa). The test item decomposes firstly at a temperature of > 200 °C. The measurement with the capillary method confirmed the results of the DSC-measurements concerning the melting and boiling behavior. The result has been considered as reliable without restriction because the test was performed in compliance with OECD and EU guidelines giving scientifically valid results (Moller, 2012).

Description of key information

The test item zinc methacrylate has no melting and boiling point at atmospheric pressure (1013 hPa). The test item decomposes firstly at a temperature of > 200 °C. The measurement with the capillary method confirmed the results of the DSC-measurements concerning the melting and boiling behavior.

Key value for chemical safety assessment

Additional information

Key study was performed in order to determine the thermal stability as well as the melting/boiling point of Zinc methacrylate according to the EUMethod A.2 and OECD 103 and 113.In this test, the thermal stability and the boiling temperature of the test item were investigated by DSC (differential scanning calorimetry). To verify the results of the DSC-measurement six additional measurements with the capillary method (Apparatus: Büchi melting Point B-540) were performed. The test item zinc methacrylate has no melting and boiling point at atmospheric pressure (1013 hPa). The test item decomposes firstly at a temperature of > 200 °C. The measurement with the capillary method confirmed the results of the DSC-measurements concerning the melting and boiling behavior (Moller, 2012).