Amorphous forms are meta-stable they have the tendency to recrystallize when they are exposed to the temperature, pressure and humidity.
Take time points from the solid and record XRPD. You will not be able to identify below 5-10% amorphous by this techniques. Also you need reference standards (pure crystalline and amorphous material) for quantitation. If you have access to isothermal titration calorimetry you might be able to reach 2% limit of quantitation (LOQ).
I agree with dr. Ahmed Najim, change from crystal to amorphous can be detected by X ray diffraction and DSC, also in amorphous statement show increased in both solubility and dissolution rate of drug as compare with crystal form of drug
During dissolution and solubility studies, if drug is precipitating out then only these techniques are valid. The identification may be started carried out using optical microscopy, and finalized on the basis of powder XRD, DSC, and Tetrahertz-Time Domain Spectroscopy.
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