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Microtek
National Hazard
Posts: 869
Registered: 23-9-2002
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Instead of purifying your nitrate esters "blind" you should invest in some indicator strip. Then you test the pH of the acetone solution of ETN or
PETN and if it is acid you add a little base such as dilute ammonia or solid bicarbonate. You only just go to neutral, or VERY SLIGHTLY above because
the esterification is an equilibrium reaction that will react with water to produce dilute nitric acid and erythritol or PE. This reverse reaction is
so slow that you can wash your product with as much clean water as you want, but it is catalysed by both acid and base. That is why you shouldn't use
NaOH (the hydroxide ion is too strong a base), and also why you shouldn't use too much ammonia (higher concentration means more catalytic activity).
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ManyInterests
National Hazard
Posts: 930
Registered: 19-5-2019
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Yes. I learned that a while ago. I didn't bother with pH strips before, but this is not the case anymore. I use pH strips also when washing my
material and during recrystalization now.
The PETN that I made was done a long time ago and before I learned how to properly recrystalize things (and realize that multiple recrystalizations is
essential). I have learned much since then and I will salvage what PETN I did make and also make sure that the next batch or two that I make will not
only be prepared properly, but also purified properly.
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