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Melting point / freezing point

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Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2018-05-04 to 2018-09-19
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose for cross-reference:
reference to same study
Reason / purpose for cross-reference:
reference to same study
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: Thermal Stability (OECD 113)
Version / remarks:
1981
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
signed 2017-02-28
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Storage Conditions: -15 °C to 40 °C
Atm. press.:
>= 1 004 - <= 1 017 hPa
Decomposition:
yes
Decomp. temp.:
> 120 °C

          

Melting and Boiling Point (DSC)

Six endothermic effects were detected in the temperature ranges of -10 °C to 10 °C (melting of water (impurity)), 60 °C – 180 °C (decomposition under boiling) and 190 °C – 280 °C, 380 °C – 450 °C, 450 °C – 500 °C and 500 °C – 590 °C (possible phase transition, decomposition).

Results of the DSC-measurements

No.

Sample weight / mg

Onset of Effect / °C

Range of effect / °C

Weight loss / mg

Atmospheric pressure / hPa

PN15771

10.02

-1.73
147.52
231.83
398.21
454.42
508.76

-10 to 10 (endo)
60 – 170 (endo)
200 – 280 (endo)
380 – 450 (endo)
450 – 490 (endo)
500 – 570 (endo)

8.07
81 %

1000.0

PN15794

8.01

-4.37
151.12
212.26
405.01
475.16
510.67

-10 to 10 (endo)
90 – 180 (endo)
190 – 280 (endo)

380 – 450 (endo)
460 – 500 (endo)
500 – 590 (endo)

6.29
79 %

999.2

It is not possible to assign any of the observed endothermic effects definitely to a melting of the test item.

There is no boiling of the test item observed. However, a mass loss of approx. 80 % was observed during measurement. This may due to the decomposition and boiling of decomposition products of 2-ethylhexanoate. The iron decomposition products are still remain as residue in the test crucible.

Measurements by the Test Tube

For verification of the DSC resultsthe test item was additionally tested in a test tube.In the temperature range of -80 to approx. -60 °C the test item was solid. The appearance of the test item during warming up was between -50 °C and -15 °C very stringy mass and at 25 °C black viscous liquid. The test item shows a softening in the temperature range of approx. -55 °C to -50 °C.

Measurements by the Capillary Method

For verificationof the DSC results the test item was additionally tested with the capillary method. At 120 °C the colour of the test item changed to brown. At approx. 128 °C bubbles, formation of gas and rise of the test item were observed. Above 150 °C strong bubbles were detected. In the temperature range of 250 °C to ~330 °C the colour of the test item was changed to grey/brown and turbid. The measurement was stopped at 350 °C with a dark grey residue remaining in the capillary. Neither a melting nor a boiling of the test item could be observed. It is assumed, that the test item decomposes at temperatures >120 °C. Results correlate with the DSC measurement in an open crucible.

Thermal Stability (DSC)

In the DSC run PN15599 three endothermic effects were observed in the temperature ranges of 120 °C to 160 °C, 160 °C to 190 °C and 300 °C to 330 °C. In the DSC run PN15600 one endothermic effect was observed in the temperature range of 180 °C to 200 °C. In the DSC run PN15665 two endothermic effects were observed in the temperature range of 100 °C to 150 °C and 170 °C to 200 °C. No exothermic effects were detected until the maximum test temperature of 600 °C, only a pressure rise at approx. 350 °C was observed.

 Results of the DSC-measurements

No.

Sample weight / mg

Start of effect / °C

Energy*/ (J/g)

PN15599

9.87

120
160
310

+10 (endothermic)
+10 (endothermic)
+40 (endothermic)

PN15600

17.54

180

+10 (endothermic)

PN15665

11.19

100
170

+25 (endothermic)
+20 (endothermic)

*Negative energy for exothermic processes, positive energy for endothermic processes

Conclusions:
Melting and Boiling Point
No definitive signs of melting/boiling of the test item 2-ethylhexanoic acid, iron salt were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under nitrogen, up to 600 °C, heating rate of 10 K/min) and by the capillary method (up to 350 °C, heating rate of 10 K/min). The measurements were performed according to Regulation EC No. 440/2008 Method A.1./A.2. and OECD Test Guidelines 102/103 (1995) at atmospheric pressure (994 – 1006 hPa). It is assumed that the test item decomposes with a mass loss of ~80 % at temperatures >120 °C.

Thermal Stability
In the temperature range of 100 °C to 340 °C different endothermic effects were observed. No exothermic effects were detected until the maximum test temperature of 600 °C, only a pressure rise at approx. 350 °C was observed.

Description of key information

It is assumed that the test item 2-ethylhexanoic acid, iron salt decomposes with a mass loss of ~80 % at temperatures >120 °C, at atmospheric pressure (994 – 1006 hPa) and under nitrogen .

Key value for chemical safety assessment

Additional information

Melting and Boiling Point

No definitive signs of melting/boiling of the test item 2-ethylhexanoic acid, iron salt were observed by differential scanning calorimetry (DSC) measurements (open glass crucible under nitrogen, up to 600 °C, heating rate of 10 K/min) and by the capillary method (up to 350 °C, heating rate of 10 K/min). The measurements were performed according to Regulation EC No. 440/2008 Method A.1./A.2. and OECD Test Guidelines 102/103 (1995) at atmospheric pressure (994 – 1006 hPa). It is assumed that the test item decomposes with a mass loss of ~80 % at temperatures >120 °C.

Thermal Stability

In the temperature range of 100 °C to 340 °C different endothermic effects were observed. No exothermic effects were detected until the maximum test temperature of 600 °C, only a pressure rise at approx. 350 °C was observed.