[BlueTheCow]

Hello again!

I'm trying to figure out what kind of methods I'm going to use for qualitative and quantitative analysis of fairly unpredictable (at least to me, right now) solid mixtures.

The mixtures I expect to analyze will most probably be mostly or totally inorganic. Particle sizes will be consistently below a certain upper limit (due to controlled crushing/grinding). The number of different compounds in the system could be anywhere from 1 (if I happen to get a pure sample; this is unlikely) to hundreds (also unlikely, but I suppose it's still possible). Usually though, there will be around 2-20 compounds in significant amounts. Water may be present, but I suppose if the analytical method required it's removal, I could implement a process for that.

What I'd like to be able to do is figure out what the mixture is made up of (that is, which compounds are present), and figure out in what specific amounts the component compounds are present.

Sounds simple (in fact I think I may be overthinking it... but maybe not.)

I've been looking through analytical methods (google/wikipedia) and most promising so far seems to be X-ray photoelectron spectroscopy (XPS, aka ESCA, Electron Spectroscopy for Chemical Analysis).
A few of the negatives about it that concern me are (a) the fact that it cannot detect hydrogen (or helium, but I don't expect the presence of helium), according to wikipedia, which could be a bad thing as there may be hydrogen-containing compounds in my mixtures, and I don't know how this will affect the analyses; (b) the fact that it is a "surface chemical analysis technique", which means that the results may not be accurate for the entire sample (I suppose I could take multiple samples throughout the mixture and do some math on the results to estimate the entirety with greater accuracy, but I'm not entirely sure if this is efficient or even possible), and (c) it looks like this method will be fairly expensive, as the technologies are not exactly low-level (and I suspect  at least part of the cost will be in safety measures, due to the high energy of the radiation). Of course, I'm not expecting a cheap solution, and if there isn't one, I'd just have to lay the money down... but I can hope for a cheap solution! 

In any case, I'm not experienced in analytical chemistry, and it is hard for me to find and compare methods. Are there any more methods that you guys can suggest for me to look into?

Thanks!

[nj_bartel]

could you find something they're soluble in and perform HPLC then perform mass spectroscopy on the separated compounds?  NMR would also help your inability to detect hydrogens I believe.