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冷凍干燥中升華界面的臨界溫度實(shí)驗(yàn)
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of Sublimation Interface in Freeze-drying
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    摘要:

    利用凍干顯微鏡(FDM)研究了二元水溶液冷凍干燥過程中升華界面的臨界溫度,采用差示掃描量熱法(DSC)測(cè)量了溶液的共晶熔融溫度和最大凍結(jié)濃縮溶液的玻璃化轉(zhuǎn)變溫度。實(shí)驗(yàn)結(jié)果表明,對(duì)于降溫時(shí)發(fā)生共晶的溶液,臨界溫度為共晶熔融溫度,否則將發(fā)生融化;對(duì)于降溫時(shí)發(fā)生玻璃化轉(zhuǎn)變的溶液,臨界溫度為塌陷溫度,否則將發(fā)生塌陷。對(duì)于質(zhì)量分?jǐn)?shù)為5%蔗糖、10%葡萄糖、10%麥芽糖、10%聚乙烯吡咯烷酮(PVP)二元水溶液,微塌陷溫度與塌陷溫度的差值在2℃以內(nèi),微塌陷溫度比玻璃化轉(zhuǎn)變溫度高

    Abstract:

    1~3℃。Freeze-drying microscopy (FDM) was used to investigate the critical temperature (Tcr) of sublimation interface during freeze-drying of binary aqueous solutions, and differential scanning calorimetry (DSC) was used to investigate the eutectic melting temperature (Tem) and the glass transition temperature of the maximally freeze concentrated solution (T′g). The experimental results showed that if a solute crystallized from solution during freezing step, the critical temperature was the eutectic melting temperature, or else a meltback would occur. If the solute remained amorphous during the freezing process, the critical temperature was the collapse temperature, or else the amorphous phase would undergo viscous flow. For 5% Sucrose, 10% glucose, 10% maltose, 10% PVP binary aqueous solutions, the microcollapse temperature (Tmc) and the collapse temperature (Tc) differed by less than 2℃, and Tmc was 1~3℃ above T′g.

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左建國(guó),李維仲,翁林崠.冷凍干燥中升華界面的臨界溫度實(shí)驗(yàn)[J].農(nóng)業(yè)機(jī)械學(xué)報(bào),2010,41(10):126-128. of Sublimation Interface in Freeze-drying[J]. Transactions of the Chinese Society for Agricultural Machinery,2010,41(10):126-128.

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