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Sample Preparation - High osmium (Os) recoveries for ICH Q3D methods

 
We are working on the analysis of heavy metals as discussed in ICH Q3D, and we are facing a problem with osmium (Os) recovery. I need a sample preparation method for any pharma or food matrix to analyze Osmium (Os) using ICP-OES. I am getting higher recovery while digesting the material in a mixture of nitric acid and hydrochloric acid. I got about 1100-1300% recovery for Osmium. Any suggestions?
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Any digestion method that uses HNO3 can potentially create problems with osmium (Os) analyses, due to the formation of the highly volatile (and deadly) Os tetraoxide (OsO4). The consequence of forming volatile OsO4 is significantly increased signal intensities (high recoveries) due to enhanced nebulization effects in ICP spray chambers. We would recommend avoiding any use of HNO3 (or other oxidizing reagents) during the sample preparation steps. Please seehttps://www.inorganicventures.com/samples-containing-ruthenium-and-osmium for more information.

Posted: 09/06/18 22:08:20

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