I collected solid samples from a plugged tube-side of a heat exchanger. These deposits include compounds such as hexachlorodisilane, hexachlorodisiloxane, pentachlorodisilane, graphite dust and amorphous/polycrystalline silicon dust. In the process of collection, the sample has been exposed to moisture, and hence the disilanes should have hydrolyzed to silica/HCl, siloxanes, etc. and the graphite and silicon should remain unaltered.

How do I go about quantifying each component? I am expecting this will be a multi-step analysis with separation/extraction followed by a combination of analytical techniques.

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    $\begingroup$ It is always beneficial to state what instruments you have access to. $\endgroup$
    – M. Farooq
    Oct 4 '21 at 21:14

I would recommend sending a sample to a company or lab that can run a Raman spectrum, an ATR infrared spectrum and an SEM-EDAX. The companies will probably run samples for free if you can convince them you want to buy an instrument[or are very nice]. Careful preparation of standards should give reasonable quantitative data from at least one of the methods for each component. I do recommend that much more care be exercised in sample collection and preservation.


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