The sample is in flour shape (with known MC). With 2 mg sample, 7 micro liter di-ionized water seemed to be very insufficient. I am suspicious about the results. Is it possible to increase the water amount?
I think you are talking about DSC (differential scanning calorimetry) of flour sample.
Yes, thermal analysis of flour can be done by DSC and you can increase the moisture content for proper hydration of flour. As you mentioned, it seems that after hydration your sample is like a thick paste, in this case, increase the amount of water for hydration and also give some resting period to your hydrated sample
I still cannot acquire a good peak for my samples compared to literature. The ratio of water:flour is 3 to 1, but still gelatinization temperature, onset temperature, and final temp. together with enthalpy value are not satisfactory.
In this case, you have to standardise your method first.
It is very common during thermal analysis of some kind of sample. So don't worry and run your experiment with different water flour ratio e.g. you can take this in 2:1 or 1:1 ratio. I hope you gave some resting period to your hydrated sample.
There are several factors which contribute in attaining sharp peak e.g water flour ratio, heating rate, gas flow rate etc.
So, also keep all these pont in consideration. I hope you will get your result by this.
The aluminum pans were swelling with increasing in temperature. As the methods indicated on hermetically sealed pans, I think evaporation of water might be the reason I don't get any peak.
I do appreciate your response. This is the method I've been using:
About 2 mg dried flour were weighed on an aluminium pan and 7 μL of distilled water were added. The pan was sealed tightly and was kept still for 1 h before the analysis. An empty aluminium pan was used as reference. The sample was submitted to a heating program over a range of temperature from 10 to 120 °C at heating rate of 10 °C min-1.