I am looking for information on relative merits and demerits of different methods (x-ray rietveld analysis based, microscopic, FTIR etc). The crystalline phases shows so much variability in chemistry, how can rietveld analysis be used.
QXRD Rietveld will provide only the average bulk composition of the glassy phase. Despite this drawback this information can be used in mix design of alkali-activated fly ash. This recent article provides an overview:
For a more profund characterization one would need scanning SEM/BSE on polished sections combined with EDX mapping. Multiple images would need to be taken, which allows the classification of the difefrent glass compositions present in fly ash. More information is given in this recent article:
Article A New Quantification Method Based on SEM-EDS to Assess Fly A...
please note that geopolymers aren’t alkali activated materials. Technologies aren’t the same while are really very different. If you want to understand better why geopolymers aren’t alkali activated materials have a look on geopolymer.org , the site of Geopolymer Institute where Prof. Davidovits explains during 4 videos all differences very clearly.
Have you tried HighScore Plus from Malvern Panalytical? It has various features to account for profile shape fitting and Rietveld analysis. You can request a demo version which works for 2 weeks from website: