IUPAC-NIST Solubilities Database

IUPAC-NIST Solubility Database
NIST Standard Reference Database 106

Solubility System: Acetonitrile-d3 with Water

Components:
   (1) Water; H2O; [7732-18-5]  NIST Chemistry WebBook for detail
   (2) Acetonitrile-d₃; C2D3N; [2206-26-0]  NIST Chemistry WebBook for detail

Original Measurements:
   Szydlowski, J.; Szykula, M., Fluid Phase Equilib. 154, 79 (1999).

Variables:
   Temperature = 256 K to 273 K

Prepared By:
   Valerii P. Sazonov

Experimental Remarks:

   UCST was reported at 272.961 ± 0.005 K at x_1c = 0.365 ± 0.002 (100 w₁ = 58.4, compiler).

Experimental Data:   (Notes on the Nomenclature)

Mutual solubility of acetonitrile-d₃ (1) and water (2)
t/°C	T/K	10² * Mass Fraction w₁ (compiler)	Mole Fraction x₁	Comment(s)
-16.861	256.289	-	-	Water-rich phase
-12.653	260.497	-	-	Water-rich phase
-8.217	264.933	34.0	0.174	Water-rich phase
-7.653	265.497	-	-	Water-rich phase
-5.062	268.088	-	-	Water-rich phase
-4.660	268.490	38.4	0.203	Water-rich phase
-2.825	270.325	-	-	Water-rich phase
-1.475	271.675	-	-	Water-rich phase
-1.428	271.722	45.3	0.253	Water-rich phase
-0.552	272.598	-	-	Water-rich phase
-0.410	272.740	51.2	0.300	Water-rich phase
-0.189	272.961	58.1	0.362	Water-rich phase
-16.861	256.289	87.5	0.742	Acetonitrile-d3-rich phase
-12.653	260.497	85.1	0.701	Acetonitrile-d3-rich phase
-8.217	264.933	-	-	Acetonitrile-d3-rich phase
-7.653	265.497	81.4	0.642	Acetonitrile-d3-rich phase
-5.062	268.088	78.6	0.600	Acetonitrile-d3-rich phase
-4.660	268.490	-	-	Acetonitrile-d3-rich phase
-2.825	270.325	74.9	0.550	Acetonitrile-d3-rich phase
-1.475	271.675	71.0	0.500	Acetonitrile-d3-rich phase
-1.428	271.722	-	-	Acetonitrile-d3-rich phase
-0.552	272.598	66.8	0.451	Acetonitrile-d3-rich phase
-0.410	272.740	-	-	Acetonitrile-d3-rich phase
-0.189	272.961	-	-	Acetonitrile-d3-rich phase

Method/Apparatus/Procedure:
   The synthetic method was used with a simplified version of the apparatus described in work.¹ Temperature was changed at the rate < 0.01 K/min; there was no visible influence of the rate on the transition temperature up to the rate 0.1 K/min. Due to the very weak turbidity a long capillary cell was employed. A 5-mW Polythec HeNe laser was used as a probe for detecting the phase separation.

Source and Purity of Materials:
   (1) Sigma; 99.5 % D; carefully dried over 5 Å molecular sieves; not purified.
   (2) Millipore Mili-Q; quality.

Estimated Errors:

   Temperature: ± 5 mK

References:
   1. J. Szydlowski, L. P. Rebelo, and W. A. Van Hook, Rev. Sci. Instrum. 63, 1717 (1992).