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Complete Temperature Profiles in Ultra-High-Pressure Liquid Chromatography Columns

机译:超高压液相色谱柱中的完整温度曲线

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The temperature profiles were calculated along and across seven packed columns (lengths 30, 50, 100, and 150 mm, i.d., 1 and 2.1 mm, all packed with Acquity UPLC, BEH-C_(18) particles, average d_(p) approx= 1.7 (mu)m) and their stainless steel tubes (o.d. 4.53 and 6.35 mm). These columns were kept horizontal and sheltered from forced air convection (i.e., under still air conditions), at room temperature. They were all percolated with pure acetonitrile, either under the maximum pressure drop (1034 bar) or at the maximum flow rate (2 mL/min) permitted by the chromatograph. The heat balance equation of chromatographic columns was discretized and solved numerically with minimum approximation. Both the compressibility and the thermal expansion of the eluent were taken into account. The boundary conditions were determined from the experimental measurements of the column inlet pressure and of the temperature profile along the column wall, which were made with a precision better than +-0.1 K. These calculation results provide the 3-D temperature profiles along and across the columns. The axial and radial temperature gradients are discussed in relationship with the experimental conditions used. The temperature map obtained permits a prediction of the chromatographic data obtained under a very high pressure gradient.
机译:沿七个填充柱(长度分别为30、50、100和150 mm,内径分别为1和2.1 mm)填充了Acquity UPLC,BEH-C_(18)颗粒,平均d_(p)约为7 =1.7μm)和它们的不锈钢管(外径4.53和6.35mm)。这些立柱保持水平,并在室温下避开强制空气对流(即在静止空气条件下)。在色谱仪允许的最大压降(1034 bar)或最大流速(2 mL / min)的条件下,均用纯乙腈进行渗滤。离散化色谱柱的热平衡方程,并用最小近似值对其进行数值求解。洗脱液的可压缩性和热膨胀都考虑在内。边界条件是根据对色谱柱入口压力和沿色谱柱壁的温度分布的实验测量结果确定的,这些测量结果的精度优于+ -0.1K。这些计算结果提供了沿3D温度和沿3D温度分布的3D温度分布图。列。讨论了轴向和径向温度梯度与所用实验条件的关系。所获得的温度图允许预测在非常高的压力梯度下获得的色谱数据。

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