Because the stainless steel large volume pans required for DSC
of water-containing samples at temperatures >100 C have a smaller
diameter at the top than at the bottom, it was impossible to remove
the samples from the pans without damage to the sample.
Fitting the pans with a thermally inert silicon rubber insert gave
satisfactory results: the insert could be easily removed from the
pan with tweezers, which allowed a trouble-free transfer of the
heated starch sample to a screw-cap tube for further characterization.
With insert, the sample mass at complete filling was 20–
25 mg, whilst in conventional DSC without insert it was 50 mg.
Preparative DSC was compared to conventional DSC in order to
establish the effect of the insert and the reduced sample mass. For
potato starch the M1 and M2 transitions were comparable in both
types of experiment, but a small shift in the HT endotherm was observed,
which was considered acceptable. The homogeneity of potato
starch heated to the completion of M1 was checked by
Because the stainless steel large volume pans required for DSCof water-containing samples at temperatures >100 C have a smallerdiameter at the top than at the bottom, it was impossible to removethe samples from the pans without damage to the sample.Fitting the pans with a thermally inert silicon rubber insert gavesatisfactory results: the insert could be easily removed from thepan with tweezers, which allowed a trouble-free transfer of theheated starch sample to a screw-cap tube for further characterization.With insert, the sample mass at complete filling was 20–25 mg, whilst in conventional DSC without insert it was 50 mg.Preparative DSC was compared to conventional DSC in order toestablish the effect of the insert and the reduced sample mass. Forpotato starch the M1 and M2 transitions were comparable in bothtypes of experiment, but a small shift in the HT endotherm was observed,which was considered acceptable. The homogeneity of potatostarch heated to the completion of M1 was checked by
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