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w/h) 1 Copyright ? 2023 Phase Technologies, Inc What to consider for the Freezing Process 冷凍過程中需要考慮的問題 ? Initial shelf surface temperature (formulation, fill volume, stability) 擱板表面的初始溫度(配方,裝料體積,穩(wěn)定性) ? Initial shelf surface temperature (ambient, 4 8 oC, 0 oC) 擱板表面的初始溫度(室溫 , 4 8 oC, 0 oC) ? Shelf cooling rate (supercooling and fill volume) 擱板冷卻速率(過冷河裝料體積) ? Freezing temperature (eutectic or collapse temperature 10 oC lower – mobility of water is zero) 冷凍溫度(共晶和塌陷溫度 10 oC更低 水的移動(dòng)性為零 ? Time (fill volume)/ 時(shí)間(裝料體積) Copyright ? 2023 Phase Technologies, Inc Effect of Freezing on the Product 冷凍對(duì)產(chǎn)品的影響 ? Was there a change in the position of the formulation?/ 配方的成分時(shí)候有變化 ? Any change in turbidity?/混濁度是否有變化 ? Nature of the frozen cake (uniform or crust or glaze) 冷凍餅狀物的性質(zhì)(均一或者硬殼或凍膠層) Copyright ? 2023 Phase Technologies, Inc Example of a Freezing Process 凍干過程舉例 ? Degree of Supercooling = 7 oC 過冷度 = 7 oC ? Collapse temperature (Tc) = 23 oC 塌陷溫度 = 23 oC ? Freezing temperature – 35 oC 冷凍溫度 – 35 oC Copyright ? 2023 Phase Technologies, Inc Key Process Steps 主要工藝步驟 ?Freezing 冷凍 ?Primary Drying 第一次干燥 Copyright ? 2023 Phase Technologies, Inc Primary Drying 第一次干燥 ? Sublimation of ice from the matrix according to the phase diagram of water 根據(jù)水的相圖使水從基質(zhì)中升華 ? Lyophilization – frozen interstitial 凍干 脈間區(qū)凍結(jié) ? Freeze Drying – frozen or not frozen interstitial region. 冷凍干燥 脈間區(qū)凍結(jié)或不凍結(jié) Copyright ? 2023 Phase Technologies, Inc Key Primary Drying Parameters 第一次干燥主要參數(shù) ? Pc Ts Tp ? Pc = Chamber pressure/箱內(nèi)壓力 ? Ts = Shelf surface temperature/擱板表面溫度 ? Tp = Product temperature/產(chǎn)品溫度 Copyright ? 2023 Phase Technologies, Inc Select the Chamber Pressure 選擇箱內(nèi)壓力 ? Determine the vapor pressure of ice at 5 oC below the collapse or eutectic temperature 在低于塌陷溫度或共晶點(diǎn) 5 oC的溫度下確定冰的蒸氣壓 Copyright ? 2023 Phase Technologies, Inc Select the Chamber Pressure 選擇箱內(nèi)壓力 ? Select a lower chamber pressure (Pc ) 選擇較低的箱內(nèi)壓力 (Pc ) ? A pressure that will give a difference in ice interface temperature (Ti ) (defined by the phase diagram of water) and the product temperature (Tp