I am having some trouble in finding a percentange of amorphous in TiO2 nanopowder 3/5 nm in size. I have already run a XRD experiment which has shown a high match with anatase phase. In my diffractogram there is a slight baseline shift which suggested some amorphous content is present. Morover there are some peaks relative to small percentages of rutile and brookite phases. The only possible way (as I far as know) to quantify my amorphous content is a TGA/DSC measurement that I have been doing by STA 6000 provided from perkin elmer. About the weight losses I have seen that there's a percentage of water , namely physically adbsorbed, and some more interacting with the -OH groups on the external surface of my nanoparticles which leaves my sample at higher temperature, roughly 250-300 Celsius degrees. However my simultaneous DSC scan doen't allow me to understand properly about my amorphous content.

After reading through papers and documents related to this technique I found something to tune my experiment.

1) scan rate at 20 °C/min from 30 to 800 °C

2) heating and cooling stages on the same sample

3) isothermal steps around 400 and 800 °C

None of them seems to work so far, so my question is :

Has anyone faced my some problem during his research , and if so could you give some suggesttions?

Thanks