Allyltributylphosphonium chloride

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Study plan dated : 13 Jun 2018 and experimental completion date 06 Aug 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2019

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

capillary method

Remarks:

Melting Point meter MPM-HV2 with Capillary Tubes Glass tubes, closed on one side, with thin walls, inner diameter 1 mm, length 60 to 100 mm, clean and dry. Usage followed the corresponding SOP 11400377 in the current edition

Test material

Test material information

Constituent 1

Reference substance name:

Allyltributylphosphonium chloride

EC Number:

216-231-7

EC Name:

Allyltributylphosphonium chloride

Cas Number:

1530-48-9

Molecular formula:

C15H32P.Cl

IUPAC Name:

tributyl(prop-2-en-1-yl)phosphanium chloride

impurity 1

Reference substance name:

Tetrahydrothiophene 1,1-dioxide

EC Number:

204-783-1

EC Name:

Tetrahydrothiophene 1,1-dioxide

Cas Number:

126-33-0

Molecular formula:

C4H8O2S

IUPAC Name:

tetrahydrothiophene 1,1-dioxide

impurity 2

Reference substance name:

Tributyl-1-propen-1-yl-phosphonium chloride

Molecular formula:

C15H32P.Cl

IUPAC Name:

Tributyl-1-propen-1-yl-phosphonium chloride

Test material form:

other: solid : wax like

Details on test material:

Homogeneity : homogeneous if totally melted
Note: For every use the test item was completely melted and the melted test item
was used for the test.

Specific details on test material used for the study:

Specification
The following information concerning identity and composition of the test item was provided
by the sponsor.
Name Allyltributylphosphonium chloride
Batch no. INT 18 192
Appearance Beige crystallised mass
Homogeneity homogeneous if totally melted
Vapour pressure <0.1 hPa at 30 °C
Stability in solvents H2O: unknown; EtOH: unknown; acetone: unknown;
CH3CN: unknown; DMSO: unknown
Solubility in solvents H2O: > 1 g/L; EtOH: unknown; acetone: unknown;
CH3CN: unknown; DMSO: unknown
Expiry date 17. Oct. 2019
Storage Room Temperature (20 ± 5°C)
Note: For every use the test item must be completely melted and the melted test item
was used for the test

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

>= 72.8 - <= 80 °C

Atm. press.:

ca. 1 atm

Decomposition:

yes

Decomp. temp.:

ca. 300 °C

Sublimation:

no

Any other information on results incl. tables

Observations	Temperatures
The test item began to melt	85 °C
The test item completely melted to a slightly yellowish clear liquid	105 °C
Individual bubble with long interval, the colour getting slightly greenish	Since 300 °C
Often bubbles were visible	Since 300 °C
The test item boiled with lots of bubbles but not developed bubble chain	333 °C
Performing of heating	Up to 338 °C
No more bubbles were observed	290 °C

After cooling down the test item stayed as a clear greenish gel like mass, decomposition was considered

Applicant's summary and conclusion

Conclusions:

The determination of the melting point and boiling point of the test item
Allyltributylphosphonium chloride should have been determined via DSC (differential scanning
calorimetry)
As in the Pre-test for boiling point following Siwoloboff the test item showed signs of decomposition
(indicating by colour change and physical state change) and strong contamination
was observed after the security pre-test for the DSC instrument after consulting with
the sponsor only the determination of melting point was performed using DSC.
However, the DSC measurements yielded no satisfactory results. Therefore, the measurements
for the melting point were repeated using the Melting point meter MPM-HV2.
The melting range was determined as: 72.9 °C to 80.1 °C (346.1 to 353.3 K)
These values are the means of two independent determinations.
The boiling point of the test item Allyltributylphosphonium chloride ist technically not
feasible as the test item decomposed before boiling.
No observations were made which might cause doubts on the validity of the study outcome.
Therefore, the result of the study is considered valid.