Registration Dossier

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
15 May 2019 - 24 July 2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry

Test material

Constituent 1
Chemical structure
Reference substance name:
Reference substance 001
Cas Number:
67-47-0
Molecular formula:
C6H6O3
impurity 1
Chemical structure
Reference substance name:
Fructose
EC Number:
200-333-3
EC Name:
Fructose
Cas Number:
57-48-7
Molecular formula:
C6H12O6
IUPAC Name:
D-fructose
impurity 2
Chemical structure
Reference substance name:
1-(furan-2-yl)-2-hydroxyethanone
Cas Number:
17678-19-2
Molecular formula:
C6H6O3
IUPAC Name:
1-(furan-2-yl)-2-hydroxyethanone
impurity 3
Reference substance name:
Water
EC Number:
231-791-2
EC Name:
Water
Cas Number:
7732-18-5
Molecular formula:
H2O
IUPAC Name:
water
impurity 4
Chemical structure
Reference substance name:
Sodium formate
EC Number:
205-488-0
EC Name:
Sodium formate
Cas Number:
141-53-7
Molecular formula:
CH2O2.Na
IUPAC Name:
sodium formate
impurity 5
Chemical structure
Reference substance name:
Sodium nitrate
EC Number:
231-554-3
EC Name:
Sodium nitrate
Cas Number:
7631-99-4
Molecular formula:
HNO3.Na
IUPAC Name:
sodium nitrate
impurity 6
Chemical structure
Reference substance name:
Glucose
EC Number:
200-075-1
EC Name:
Glucose
Cas Number:
50-99-7
Molecular formula:
C6H12O6
IUPAC Name:
D-glucose
impurity 7
Chemical structure
Reference substance name:
Sodium acetate
EC Number:
204-823-8
EC Name:
Sodium acetate
Cas Number:
127-09-3
Molecular formula:
C2H4O2.Na
IUPAC Name:
sodium acetate
impurity 8
Chemical structure
Reference substance name:
2-furaldehyde
EC Number:
202-627-7
EC Name:
2-furaldehyde
Cas Number:
98-01-1
Molecular formula:
C5H4O2
IUPAC Name:
2-furaldehyde
impurity 9
Chemical structure
Reference substance name:
Sodium 4-oxovalerate
EC Number:
243-378-4
EC Name:
Sodium 4-oxovalerate
Cas Number:
19856-23-6
Molecular formula:
C5H8O3.Na
IUPAC Name:
sodium 4-oxopentanoate
impurity 10
Chemical structure
Reference substance name:
Formaldehyde
EC Number:
200-001-8
EC Name:
Formaldehyde
Cas Number:
50-00-0
Molecular formula:
CH2O
IUPAC Name:
formaldehyde
Test material form:
solid: crystalline
Details on test material:
freeze-dried material
Batch: 1808A-RO-C-I1-FD-Chg#3
Appearance Crystal / brown
Storage: Refrigerator (2 - 8 °C)
Expiring date: 31 December 2019
Specific details on test material used for the study:
Storage Conditions: Dry, dark and cooled (2 °C to 8 °C)
Expiry Date: 2019-12-31

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
ca. 25 °C

Any other information on results incl. tables

Melting Point

During the cooling phase no thermal effects could be observed down to a temperature of -90 °C. In the subsequent heating phase an endothermic effect was observed in the temperature range of -70 °C to -40 °C. Since the test item does not seem to be completely solid, more like a sticky mass, at the storage temperature between 2 °C to 8 °C, the measured endothermic effect may be assigned to the start of the liquification process, which spans over a large temperature range up to room temperature. Due to the wide range, the DSC measurements cannot be used for an evaluation of a specific melting point. The results of the DSC-measurements are summarized in the following table:

Results of the DSC-measurement

No.

Sample weight / mg

 

Onset of Effect / °C

 

Range of effect / °C

 

Weight loss / mg

 

Atmospheric pressure / hPa

PN17787

13.18

-62.65

--

-70 to -40 (endo) 120 to 500 (exo)

 

8.32

1013.0

PN17808

10.78

-64.09

--

-70 to -40 (endo) 120 to 500 (exo)

 

6.92

992.2

PN17822

11.85

---

120 to 500 (exo)

7.60

1006.4

Optical verification using the capillary method and the visual melting test in a test tube

To verify the results of the DSC measurement, an additional measurement in a boiling capillary was performed in the temperature range of 30 °C to 200 °C with a heating rate of 10 K/min. The test item immediately started to liquify at room temperature (25°C).

The visual melting test in a test tube was started at a temperature of 1.4 °C. During the slow heating process up to room temperature the test item started to melt at a temperature of approx. 20 °C. At a temperature of 25.3 °C the test item was completely molten. Due to the result of the visual verification of the melting behaviour in the test tube and observations in the capillary method, it can be stated that the test item has a melting point of approx. 25 °C.

Applicant's summary and conclusion

Conclusions:
The test item 5-(Hydroxymethyl)furfural has a melting point of approximately 25 °C as determined by the capillary method and in the visual melting test in a test tube according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).
Executive summary:

The test item 5-(Hydroxymethyl)furfural has a melting point of approximately 25 °C as determined by the capillary method and in the visual melting test in a test tube according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).