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New Design of the High-Pressure Optical Cell for Vapor–Liquid Equilibrium Measurements. Supercritical Binary Mixture (Propane/n-Butane) + Acetophenone
Journal of Chemical & Engineering Data ( IF 2.0 ) Pub Date : 2020-06-22 , DOI: 10.1021/acs.jced.0c00104
Vener F. Khairutdinov 1 , Farid M. Gumerov 1 , Farizan R. Gabitov 1 , Zufar I. Zaripov 1 , Ilnar Sh. Khabriev 1 , Talgat R. Akhmetzyanov 1 , Ilmutdin M. Abdulagatov 2, 3
Affiliation  

A new design of the high-pressure and high-temperature optical cell has been developed for precise measurements of the vapor–liquid equilibrium (VLE) properties of multicomponent mixtures at pressures up to 50 MPa and at temperatures from room to 450.15 K. The present design of the VLE optical cell allows avoidance of the separation of the binary system out of the sampler (in the sampling tube) and accurate determination of the concentrations of the coexisting phases without disturbing the phase equilibrium conditions during the high-pressure sampling procedure (thermodynamically consistent PTxy data). A sufficiently large volume (117 cm3) of the measuring cell allows extraction of a relatively large sample volume (about 4.1 cm3) from the liquid and the vapor phase independently without breaking the phase equilibrium (PT) conditions during the sampling procedure from each phase. This allows a considerable increase of the accuracy of the concentration determination of the equilibrium phases using the gravimetric method, especially the vapor phase. The gravimetric sampling method provides a precise analysis of the coexisting phase concentrations without using expensive chromatographic columns, which are not always suitable for the analysis of various complex multicomponent mixtures. The accuracy, reliability, and correct operation of the new design of the high-pressure VLE cell was verified by measuring the phase equilibrium properties of pure (propane) and the binary (propane + n-butane) mixture with well-known VLE properties. Also, the method was applied for the new, previously unexplored, ternary mixture of supercritical solvent (0.527 propane + 0.473 n-butane) + acetophenone. The values of the critical parameters for the ternary mixture have been estimated from the experimental VLE data near the critical point. The combined expanded uncertainty of the temperature, pressure, and concentration measurements at 0.95 confidence level with a coverage factor of k = 2 is estimated to be 0.15 K, 0.0022, and 0.03, respectively.

中文翻译:

用于蒸气-液体平衡测量的高压光学电池的新设计。超临界二元混合物(丙烷/丁烷)+苯乙酮

已经开发出一种高压高温光学电池的新设计,用于在压力高达50 MPa和室温至450.15 K的温度下精确测量多组分混合物的气液平衡(VLE)特性。 VLE光学元件的设计可以避免二元系统从采样器中分离出来(在采样管中),并且可以准确确定共存相的浓度,而不会干扰高压采样过程(热力学)中的相平衡条件一致的PTxy数据)。测量池足够大的体积(117 cm 3)可以提取相对较大的样品体积(约4.1 cm 3))从液相和气相中分离出来,而不会在从每一相进行采样的过程中破坏相平衡(PT)条件。这允许显着提高使用重量分析法尤其是气相的平衡相的浓度确定的准确性。重量采样方法无需使用昂贵的色谱柱即可对共存相浓度进行精确分析,而色谱柱并不总是适合于分析各种复杂的多组分混合物。通过测量纯丙烷(丙烷)和二元丙烷(丙烷+ n)的相平衡特性,验证了高压VLE电池新设计的准确性,可靠性和正确操作。-丁烷)混合物具有众所周知的VLE特性。同样,该方法也适用于以前从未探索过的新的超临界溶剂(0.527丙烷+ 0.473丁烷)+苯乙酮的三元混合物。根据接近临界点的VLE实验数据估算出三元混合物的临界参数值。在0.95置信度下,覆盖因子k = 2时,温度,压力和浓度测量的组合扩展不确定性分别估计为0.15 K,0.0022和0.03。
更新日期:2020-07-09
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