Rambhatla Shailaja, Pikal Michael J
School of Pharmacy, University of Connecticut, Storrs, CT 06269, USA.
AAPS PharmSciTech. 2003;4(2):E14. doi: 10.1208/pt040214.
The aim of this study is to determine whether radiation heat transfer is responsible for the position dependence of heat transfer known as the edge vial effect. Freeze drying was performed on a laboratory-scale freeze dryer using pure water with vials that were fully stoppered but had precision cut metal tubes inserted in them to ensure uniformity in resistance to vapor flow. Sublimation rates were determined gravimetrically. Vials were sputter-coated with gold and placed at selected positions on the shelf. Average sublimation rates were determined for vials located at the front, side, and center of an array of vials. Sublimation rates were also determined with and without the use of aluminum foil as a radiation shield. The effect of the guardrail material and its contribution to the edge vial effect by conduction heat transfer was studied by replacing the stainless steel band with a low-thermal conductivity material (styrofoam). The emissivities (epsilon) of relevant surfaces were measured using an infrared thermometer. Sublimation rate experiments were also conducted with vials suspended off the shelf to study the role of convection heat transfer. It was found that sublimation rates were significantly higher for vials located in the front compared to vials in the center. Additional radiation shields in the form of aluminum foil on the inside door resulted in a decrease in sublimation rates for the front vials and to a lesser extent, the center vials. There was a significant decrease in sublimation rate for gold-coated vials (epsilon approximately 0.4) placed at the front of an array when compared to that of clear vials (epsilon approximately 0.9). In the case of experiments with vials suspended off the shelf, the heat transfer coefficient was found to be independent of chamber pressure, indicating that pure convection plays no significant role in heat transfer. Higher sublimation rates were observed when the steel band was used instead of Styrofoam while the highest sublimation rates were obtained in the absence of the guardrail, indicating that the metal band can act as a thermal shield but also transmits some heat from the shelf via conduction and radiation. Atypical radiation heat transfer is responsible for higher sublimation rates for vials located at the front and side of an array. However, the guardrail contributes a little to heat transfer by conduction.
本研究的目的是确定辐射热传递是否是导致被称为边缘瓶效应的热传递位置依赖性的原因。在实验室规模的冻干机上使用纯水进行冷冻干燥,所用小瓶完全密封,但插入了精密切割的金属管,以确保蒸汽流动阻力的均匀性。通过重量法测定升华速率。小瓶用金进行溅射镀膜,并放置在搁板上的选定位置。测定了位于一排小瓶的前部、侧面和中心的小瓶的平均升华速率。还分别在使用和不使用铝箔作为辐射屏蔽的情况下测定升华速率。通过用低导热率材料(聚苯乙烯泡沫塑料)替换不锈钢带,研究了护栏材料的影响及其通过传导热传递对边缘瓶效应的贡献。使用红外温度计测量相关表面的发射率(ε)。还对悬置于搁板上方的小瓶进行了升华速率实验,以研究对流热传递的作用。结果发现,位于前部的小瓶的升华速率明显高于位于中心的小瓶。内门上以铝箔形式设置的额外辐射屏蔽导致前部小瓶的升华速率降低,对中心小瓶的影响较小。与透明小瓶(ε约为0.9)相比,放置在阵列前部的镀金小瓶(ε约为0.4)的升华速率显著降低。在小瓶悬置于搁板上方的实验中,发现传热系数与腔室压力无关,这表明纯对流在热传递中不起重要作用。当使用钢带而非聚苯乙烯泡沫塑料时,观察到升华速率更高,而在没有护栏的情况下获得了最高的升华速率,这表明金属带可以起到热屏蔽的作用,但也会通过传导和辐射从搁板传递一些热量。非典型辐射热传递是导致位于阵列前部和侧面的小瓶升华速率较高的原因。然而,护栏对传导热传递的贡献较小。