A new method for the determination of the unfrozen matrix concentration and the maximal freeze-concentration
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A new method for the determination of the unfrozen matrix concentration and the maximal freeze-concentration. / Liesebach, Jens; Rades, Thomas; Lim, Miang.
In: Thermochimica Acta, Vol. 401, No. 2, 19.05.2003, p. 159-168.Research output: Contribution to journal › Journal article › Research › peer-review
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TY - JOUR
T1 - A new method for the determination of the unfrozen matrix concentration and the maximal freeze-concentration
AU - Liesebach, Jens
AU - Rades, Thomas
AU - Lim, Miang
PY - 2003/5/19
Y1 - 2003/5/19
N2 - During the freezing process, water is partially separated as ice and the solutes are concentrated in the unfrozen matrix (UFM). With further lowering of the temperature, the UFM becomes highly viscous. The high viscosity of the UFM prolongs ice formation and makes it difficult to accurately determine the glass transition (Tg′) and the concentration (Cg′) of the maximally freeze-concentrated matrix. In this study, a new method for the determination of the concentration of the UFM was developed using differential scanning calorimetry (DSC). Sugar solutions were frozen, annealed at temperatures slightly above the expected Tg′, rapidly cooled and then heated to 20°C. The UFM concentrations of the annealed samples were obtained by estimating the solute concentration corresponding to the Tg at the respective annealing temperature. The dependence of the Tg on experimental conditions such as the annealing time, annealing temperature and cooling rate was studied in detail. Values for Cg′ and Tg′ were obtained by linear and quadratic extrapolations of the experimental data over a short temperature and solute concentration range. The maximal freeze-concentrations of glucose, sucrose and maltose were determined to be 79.9, 80.9 and 80.3% (w/w), respectively. Results of this study were in good agreement to previously published data.
AB - During the freezing process, water is partially separated as ice and the solutes are concentrated in the unfrozen matrix (UFM). With further lowering of the temperature, the UFM becomes highly viscous. The high viscosity of the UFM prolongs ice formation and makes it difficult to accurately determine the glass transition (Tg′) and the concentration (Cg′) of the maximally freeze-concentrated matrix. In this study, a new method for the determination of the concentration of the UFM was developed using differential scanning calorimetry (DSC). Sugar solutions were frozen, annealed at temperatures slightly above the expected Tg′, rapidly cooled and then heated to 20°C. The UFM concentrations of the annealed samples were obtained by estimating the solute concentration corresponding to the Tg at the respective annealing temperature. The dependence of the Tg on experimental conditions such as the annealing time, annealing temperature and cooling rate was studied in detail. Values for Cg′ and Tg′ were obtained by linear and quadratic extrapolations of the experimental data over a short temperature and solute concentration range. The maximal freeze-concentrations of glucose, sucrose and maltose were determined to be 79.9, 80.9 and 80.3% (w/w), respectively. Results of this study were in good agreement to previously published data.
KW - DSC
KW - Glass transition
KW - Maximal freeze-concentration
KW - Phase diagram
KW - Sugar
UR - http://www.scopus.com/inward/record.url?scp=0038351941&partnerID=8YFLogxK
U2 - 10.1016/S0040-6031(02)00546-4
DO - 10.1016/S0040-6031(02)00546-4
M3 - Journal article
AN - SCOPUS:0038351941
VL - 401
SP - 159
EP - 168
JO - Thermochimica Acta
JF - Thermochimica Acta
SN - 0040-6031
IS - 2
ER -
ID: 299429679