Rapid Determination of Vial Heat Transfer Parameters Using Tunable Diode Laser Absorption Spectroscopy (TDLAS) in Response to Step-Changes in Pressure Set-Point During Freeze-Drying
Rapid Determination of Vial Heat Transfer Parameters Using Tunable Diode Laser Absorption Spectroscopy (TDLAS) in Response to Step-Changes in Pressure Set-Point During Freeze-Drying
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DOI：
10.1002/jps.21478
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发表时间：
2009-03-01
影响因子：
3.8
通讯作者：
Sacha, Gregory
中科院分区：
文献类型：
--
作者：
Kuu, Wei Y.;Nail, Steven L.;Sacha, Gregory
本研究的目的是利用可调谐半导体激光吸收光谱(TDLAS)测量的升华速率分布，快速确定小瓶的换热参数，即接触参数K-ES和分离距离L(V)。在这项研究中，将每个大小的瓶子装入纯水，然后使用LyoStar II干燥机(FTS Systems)进行冷冻干燥循环，将室内压力设定值逐级改变为25、50、100、200、300和400mTorr。用在25mTorr压力设定点测量的升华速率进行非线性参数估计，独立地确定了K-Es。在获得K-Es后，利用在25到400mTorr处获得的汇集升华速率曲线，通过非线性参数估计确定每个小瓶大小的L(V)值。利用得到的K-Es和L(V)值，可以很容易地计算出小瓶换热系数K-v随压力的变化。有趣的是，注意到两个类似类型的10毫升肖特油管瓶的K-v有显著差异，主要是由于瓶底的几何形状，如瓶底接触面积的图像所示。(C)2008 Wiley-Liss，Inc.和美国药剂师协会药学杂志98：1136-1154,2009
The purpose of this study was to perform a rapid determination of vial heat transfer parameters, that is, the contact parameter K-es and the separation distance l(v) using the sublimation rate profiles measured by tunable diode laser absorption spectroscopy (TDLAS). In this study, each size of vial was filled with pure water followed by a freeze-drying cycle using a LyoStar II dryer (FTS Systems) with step-changes of the chamber pressure set-point at to 25, 50, 100, 200, 300, and 400 mTorr. K-es was independently determined by nonlinear parameter estimation using the sublimation rates measured at the pressure set-point of 25 mTorr. After obtaining K-es the l(v) value for each vial size was determined by nonlinear parameter estimation using the pooled sublimation rate profiles obtained at 25 to 400 mTorr. The vial heat transfer coefficient K-v as a function of the chamber pressure, was readily calculated, using the obtained K-es and l(v) values. It is interesting to note the significant difference in K-v of two similar types of 10 mL Schott tubing vials, primary due to the geometry of the vial-bottom, as demonstrated by the images of the contact areas of the vial-bottom. (C) 2008 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 98:1136-1154, 2009