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Author Topic:   Mercury contamination during CaO/ KOH safrole Isosafrole conversion
dajale
Member
posted 05-11-99 02:50 PM     Click Here to See the Profile for dajale     

I dreamt that my stir bar broke my thermometer while I was boiling up some Isosafrole. I said forget it and went ahead and tried to distill over the Isosafrole under vacuum. The oil came over as usual but the condenser was filled with gray cake and the distilled oil has a gray ting to it (urrr nasty). I'm thinking that every thing will be okay if I run the oil through vacuum filtration and distill over again, what does the Hive Mind think? If I were to really do this would this work or would I have to dispose of the oil?

Rhodium
Administrator
posted 05-11-99 07:58 PM     Click Here to See the Profile for Rhodium     
Dispose of it. Mercury vapor is voilatile.

dajale
Member
posted 05-12-99 12:56 PM     Click Here to See the Profile for dajale     
I dreamt that I passed the distillate through my vacuum filter, got the translucent liquorice smelling oil I was used too, and disposed of the gray filter cake. I thought of using that to make MDP-2-P via the TS 2 method 2. If I did and the operation was happening as usual, would you still advise I throw it away?

Thanks for the help

Osmium
Member
posted 05-12-99 12:57 PM     Click Here to See the Profile for Osmium     
Distill ALL the products in the following synthesis, and try to filter your iso through some celite or something else. Might also help to let the Hg react with another metal to form some amalgam (Cu powder, Al foil etc.).

Fan of Shulgin
Member
posted 05-12-99 07:18 PM     Click Here to See the Profile for Fan of Shulgin     
I concur with Osmium......

With a slight change.... i recommend you actually add some Hg to the reactions vessel - just enough so as to produce a discernable lump! Hg tends to aggregate, so once you have a sizeable lump in the vessel add shit loads of Al foil (gradually and way in excess) to allow it to amalgamate. Leave this for about a week (if you want to be safe and you have patience) and then decant the organic liquor from the vessel. Id defintely follow this up with a organic extraction and celite filtration just to be on the safe side.

Peace, love and empathy

Fan of Shulgin

Stik E. Fingers
Member
posted 05-13-99 10:40 AM     Click Here to See the Profile for Stik E. Fingers     
Can activated carbon & plain sulfphur (both in Hg clean up packs)be used?

This is probably unwanted, but I'm horrified at the prevelence of Hg methods - particularly given the high doses of the products (& attendant general contamination mass). Bear in mind that one will be dead long before consuming 200mg of organic Hg over a year (ref Selinger, Chemistry in the Market place, 1986, p.437). Very long residences in body parts too: I'd question the prevalent attitude to low dose organic Hg - even from dental fillings. A (0.5mg/kg)fish helping gives about 100 ug (absorbed). Some believe brain damage begins at about 3 ug/g brain tissue - had in 50 single-fish-meal-days. Less in reality, as all sources contribute.
I beleive that if one retained any possibly Hg contaminated product (including regular pruduction employing Hg) it should be analysed for Hg species before release (& don't equate toxicity of high 1/2 life organic Hg with inorganic Hg or even elemental Hg).

Sorry to sound off but worried.

Semtex Enigma
Member
posted 05-13-99 04:48 PM     Click Here to See the Profile for Semtex Enigma     
How many GALLONS were contaminated? Cause if this is some small amount (<100g), dispose of it, and start over. Sas can't be THAT hard to get, even if it is listed...

Osmium
Member
posted 05-14-99 01:26 PM     Click Here to See the Profile for Osmium     
People have made Hg-free honey via the Al/Hg method, so please, get real. There's a little elemental Hg in there. What's the problem? It's not readily soluble, so decant it, filter it and treat it with some Al foil to remove the very last traces. It's that easy.

All times are CT (US)

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