SDS Volume (4206)

Volume 71. Nitromethane with Water or Organic Solvents, p None

Original Measurements

Salvi, M. V.; Van Hook, W. A.; J. Phys. Chem. 94, 7812 (1990).

Variables:

Room Temp: 313 - 316 $\pu{K}$
Pressure: 0.1 - 50 $\pu{kPa}$

Prepared by:

V.P. Sazonov

Method/Apparatus/Procedure:

The synthetic method was used. Measurements were made using techniques and apparatus described in [1] with minor modification. Mixtures of [1] and (2) were prepared gravimetrically. The solutions were degassed with a series of freeze-pump ($\pu{\le 0.1 Pa}$) - thaw cycles. After transfer to the apparatus (previously warmed above the CST) the demixing was determined by allowing the mixture to cool to the transition temperature at a rate of 3 to 5 mK/min while stirring. Temperature was measured by platinum resistance thermometry.

Source and Purity of Materials:

1. Mallinkrodt; analytical grade; dried over anhydrous $\ce{CaCl2}$ and twice distilled in a spinning band column below 343 K.
2. Prepared by refluxing reagent grade 99.8% $\ce{D2O}$/ethanediol = 2.5/1 and removing the water by fractional distillation at reduced pressure; the deuterated glycol fraction was collected, dried again over molecular sieve and redistilled.

Estimated Errors:

Ambient temperature: ±0.3 mK.
Pressure: ±0.01 MPa.

References

¹ Singh, R. R.; Van Hook, W. A.; J. Chem. Phys. 87, 6097 (1987).