4-hydroxy-2,5-dimethylfuran-2(3H)-one

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

experimental dates: 05 to 26 Oct. 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

The study was conducted according to an internationally recognised method, and under GLP. Deviation was considered not significant. The substance is adequately characterised. Therefore full validation applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

27 Jul. 1995

Deviations:

yes

Remarks:

design of the vessel

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

Regulation (EC) 440/2008

Deviations:

yes

Remarks:

design of the vessel

GLP compliance:

yes (incl. QA statement)

Remarks:

Landesamt für Umwelt, Wasserwirtschaft und Gewerbeaufsicht (inspected on 13 & 14 October 2014, 2010 / signed on 08 April 2015)

Type of method:

dynamic method

Specific details on test material used for the study:

A fresh sample of the test item appearing as a powder was first ground. But during grinding it could be already observed that the test item became muddy. Therefore a fresh sample of the test item was dried overnight in an exsiccator. After drying the test item appeared as a paste. With this sample the Pre-Test and two determinations with the dynamic method were performed. The results of the performance of the dynamic method were not repeatable. Therefore a fresh sample of the test item without drying and grinding was used for the determination of the boiling point.

Key result

Boiling pt.:

230 °C

Atm. press.:

ca. 1 013 hPa

Decomposition:

yes

Decomp. temp.:

ca. 200 °C

The pre-test was performed with the Siwoloboff method. The Siwoloboff method was found not applicable because the test item turned to strong dark colour (decomposition suspected). Therefore the main test following dynamic method was performed.

Determination	Observations	Temperature Cottrell pump	Temperature test item (observed boiling)
1	At 100 °C melted to yellow liquid. At 140 °C Colour orange. At 170 °C colour redbrown, the colour was from time to time darker.	182.8 °C (456.0 K)	205.0 °C (478.2 K)
2	At 120 °C melted to yellow-orange liquid. At 200 °C colour orange. At 220 °C colour red-brown, the colour was from time to time darker.	206.8 °C (480.0 K)	230.0 °C (503.2 K)
3	At 140 °C melted to yellow liquid. At 200 °C colour orange. At 215 °C colour red-brown, the colour was from time to time darker.	219.3 °C (492.5 K)	230.0 °C (503.2 K)
4	At 140 °C melted to yellow liquid. At 200 °C colour orange. At 215 °C colour red-brown, the colour was from time to time darker.	218.9 °C (492.1 K)	230.0 °C (503.2 K)

Determinations 1 and 2 were performed with test item dried in an exsiccator.

Determinations 3 and 4 were performed with the fresh test item without drying and grinding.

All observation temperatures are the test item temperatures. After cooling down, the test item was dark red-brown viscous liquid. Decomposition of the test item was considered during experiment indicated by colour change and temperature difference at approx. 200°C.

For the calculation of the value of the mean and the evaluation, the results of the first and the second determinations were discarded.

At 230.0 °C (503.2 K), the test item boils with signs of decomposition. Boiling was indicated by pumping Cottrell pump producing a mixture of vapour and liquid.

As the test item showed decomposition, the calculation following the equation of Sidney-Young for correction to normal atmospheric pressure was not necessary.

Executive summary:

The boiling point of the test substance was determined under GLP according to OECD 103/EU A2 guideline, with the dynamic method.

The determination was performed in duplicate with untreated sample, as results on dried sample was not repeatable.

The experiment showed decomposition from ca 200°C, indicated by colour change, and temperature difference between the test item and the vessel, followed by boiling at ca 230°C.

Description of key information

The test item decomposes from ca 200°C (colour change) before boiling at ca 230°C.

Additional information

A fully reliable experimental study, conducted according to a recognized OECD/EC method and under GLP, is available. Therefore, it is considered as a key study. As the substance decomposes prior to boiling, no value is retained as key data.