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Topic: Analysis for triphenylphosphine  (Read 12131 times)

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Offline limpet chicken

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Analysis for triphenylphosphine
« on: April 17, 2005, 08:39:21 PM »
Does anyone know of a way to test for triphenylphosphine?

I had a rather unpleasant incident just the other day with a product ordered from the netherlands, containing 3,4-methylenedioxymethcathinone "methylone" for short, to cut a long story short, I was poisoned by it, quite badly.

There was a related product, containing methylone also sold, which for reasons unknown was made illegal (in the netherlands) just recently, at the time, I was unaware that that was the case, and for what reason, as I am still unaware of the latter, however, somebody ended up testing the first product, and it is likely that it contained dangerous quantities of triphenylphosphine, which is a nasty corrosive poison, which fits in neatly with the symptoms of poisoning, namely severe haemoptysis, if TPP was present in the first product, then it might possibly also be present in the one that poisoned me.

Does anyone know how I could test a given sample, by chemical means for triphenylphosphine? because I am thinking of testing a vial of the current product for it, as people need to know if this shyte is floating around on the net, before more people are poisoned by it.

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hemispheredancer

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Re:Analysis for triphenylphosphine
« Reply #1 on: April 20, 2005, 01:40:35 PM »
First off, be careful with chemicals that you buy from unknown suppliers.  And ingesting those said chemicals.  Most of the sites selling "explosion" tell you not to INGEST the stuff.  But considering that its not a controlled substance anywhere that I am aware (though closely related to amphetamines), I'll try to help answer your question.  You say that there was triphenyl phosphine (TPP) found in an other sample of a similar purchase.  How are you sure that it was TPP.  In most cases TPP will convert to TPP oxide with any exposure to air/water.  I have yet to find a synthesis of methylone that uses TPP in any step.  This is one reagent that is usually avoided if the desired product has and possibilty of making it into humans.  TPP tends to drag along with the product from step to step.  But alas I'm not sonvinced that it was used in the synthesis of methylone.  All that aside, its generally easy to co-spot the sample versus known samples of TPP and TPP oxide using TLC.  There are many other methods but this would be the easiet.

Offline Mitch

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Re:Analysis for triphenylphosphine
« Reply #2 on: April 20, 2005, 03:57:56 PM »
We have TPP in lab, and doesn't seem to be "that" reactive to ambient air and moisture.

And stop ingesting chemicals...  ::)
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Offline limpet chicken

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Re:Analysis for triphenylphosphine
« Reply #3 on: April 20, 2005, 05:02:17 PM »
Mitch, I didn't INTENTIONALLY ingest TPP, I just believe the product I had (and everybody knows full well, that explosion and the other brand I had are intended for ingestion, the "do not ingest" is merely legal boilerplate, why else would they flavour it ;))

(And WHY, decide to randomly put a centrally active cathinone compound, in something to scent one's room ::))

"Explosion" I believe, is possibly contamianted with TPP, as I say, because someone on bluelight.nu (registered there under the same name as here) did a GC/MS on it, and found it to have a peak for TPP, as well as the intended methylone.

I am almost entirely better now, I just want to be able to chemically test another vial of this stuff, for TPP, to confirm or deny my suspicions that this also, is contaminated.
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Offline Mitch

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Re:Analysis for triphenylphosphine
« Reply #4 on: April 20, 2005, 06:10:18 PM »
Once TPP is used in a reaction it becomes very difficult to get out. It can stay with a compound for several more steps.
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Offline limpet chicken

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Re:Analysis for triphenylphosphine
« Reply #5 on: April 20, 2005, 06:29:17 PM »
Mitch, why is that? why does TPP follow on after a rxn?

Surely an acid/base extraction of any alkaloidal type of matter would free if from triphenylphosphine, unless of course, it dissolves in both polar AND nonpolar solvents.

Aaakk! nasty, pervasive throat-burning stuff :-X
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Offline Mitch

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Re:Analysis for triphenylphosphine
« Reply #6 on: April 20, 2005, 08:54:02 PM »
It's just a fact of nature. When I've used it and had to isolate my compounds, I could still see it's aromatic proton peaks in NMR. To be honest, its usually gone after the next step for me, but others may not be as careful in removing impurities.

It's just one of those extremely useful reagents that just end up being a hassle to use. If you run a mass spec. of a compound that has trace TPP in it, and then you run other samples that have no chance of having TPP in it, the trace TPP from the original sample will give false-positives for TPP, because TPP loves to stick to columns/silicon. Its an annoying but flexible reagent.
« Last Edit: April 20, 2005, 08:56:45 PM by Mitch »
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