Propylphosphonic dichloride

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

1 (reliable without restriction)

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Test guideline 3

Qualifier:

according to guideline

Guideline:

other: DIN ISO 3016

GLP compliance:

yes (incl. QA statement)

Type of method:

other: thermal analysis and pour point

Test material

Test material information

Constituent 1

Reference substance name:

Propylphosphonic dichloride

EC Number:

225-195-1

EC Name:

Propylphosphonic dichloride

Cas Number:

4708-04-7

Molecular formula:

C3H7Cl2OP

IUPAC Name:

propylphosphonoyl dichloride

Details on test material:

Chemical Name (IUPAC): Propylphosphonic dichloride
Molecular Formula: C3H7Cl2OP
CAS-No.: 4708-04-7
Molecular Weight: 160.966 g/mol
Batch No.: DALA082836
Purity: 98.4 % (31P-NMR)
Date of expiry: 31.10.2012
Certificate of analysis: No AZ-006-2011, 31.10.2011

Results and discussion

Melting / freezing point

Melting / freezing pt.:

-21 °C

Any other information on results incl. tables

DSC RESULTS AND DISCUSSION

In none of the DSC tests (1 - 5, 7) with the test item an endothermic or exothermic peak could be observed. Therefore no melting or freezing temperature was detected in the temperature range of 25°C (298 K) to – 50°C (223 K).

Test 6 was performed with water and the found onset temperature of each peak are summarized in the following table:

Test No. 6

Peak type       Onset Temp. 1st cycle Onset Temp. 2nd cycle       mean Onset Temp.

[#]                                   [°C]                                   [°C]                   [°C]

endothermic - 0.40                                 - 0.60                - 0.50

exothermic                  - 11.09                             - 15.27               - 13.18

The detected average melting temperature (endothermic peak) of water was found to be – 0.50°C that is in good agreement with the expected value of 0.0 +/- 0.5°C. Furthermore the freezing temperature (exothermic peak) was found to be in the range between -11°C and -15°C. Theoretically the melting and freezing temperature should be the same value, but the sample act like a supercooled liquid.

Due to these experiments it was decided to check for the Pour Point of the test item and to feature another method to test for the freezing/melting temperature.

RESULTS OF THE POUR POINT TEST

All temperature values for both tests were rounded to integer values (no decimals) due to the fluctuations during the thermometer readings.

Test #1

Temp. Sample

[°C] Solidified ?[yes|no] Temp. Fr. Mixture [°C] Comment

-11       no                      -63                         No solids visible; sample is liquid

-14       no                      -62                      No solids visible; sample is liquid

-17       no                      -64                      No solids visible; sample is liquid

-20       no                      -60                     No solids visible; sample is liquid

Test #1.: Sample temperature was checked with a calibrated Hg-thermometer. The temperature of the freezing mixture was measured with the Pt100 thermometer.

Test #2/3

Temp. Sample[°C] Solidified ?[yes|no] Temp. Mixture[°C] Comment

-11                     no                            -51       No solids visible; sample is liquid

-14                                 no                            ---       No solids visible; sample is liquid

-17                     no                            ---       No solids visible; sample is liquid

-20                     no                            ---       No solids visible; sample is liquid

-44                     no                            ---       initial solids visible; sample is liquid

-22                     yes                            ---       test item completely solidified

-20.90                     yes                            ---       Mixture of liquid and solids

Test #2/3: Sample temperature and the temperature of the freezing mixture was checked with the same Pt100 thermometer.

After the first solids were visible at -44°C, the test item was continuously going to solidify, simultaneously the temperature of the sample was rising during this process. At -22°C the test item was completely solidified. Now the centrifuge tube was removed from the cooled glass beaker. The test item was stored at room temperature (test #3) until an equilibrium of the solid and the liquid phase was achieved. At this point the temperature in the centrifuge tube was -20.90°C. This temperature is the melting point of the test item.