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Chemical Stability and Compatibility - Digesting an organic with Os Spike

 
Alternative to oxidizing-acid digestion
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Daniel Veit Total posts: 1

   I am developing a method for a 24 ICH metal analysis of Hydroxypropyl Methylcellulose.  I cannot get Os spikes to recover and I understand it is because we are microwave digesting the sample in HNO3.  From everything I've read on your site and others, the problem is osmium tetroxide formation.  However, the only thing that's going to digest the sample is an oxidizing acid (as far as I know).  I'm sure HClO4 or H2SO4 will be just as detrimental.  I can't get it into solution with just HCl.  Everyone says use an HCl matrix with Os but how do you reconcile that with a need to spike and then digest?  I can't digest in nitric and then dilute in HCl because the sample must be spiked before any preparation steps.  Thanks for any assitance!

 

Dan

Posted: 09/13/19 08:59:10

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