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Two ideas on Hasenfratz/Manske NaCl percipitation Options
 
Crystalito
#1 Posted : 7/25/2009 6:22:51 PM
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Lately i have been running a Hasenfratz extraction of the fruits (literally) of my labor, some Peganum harmalas i have planted.

I deviated a bit from the protocol, grinding the seedpods whole ,filtering and evaporating down to a "tar/film" which i re-dissolved in brine.

Upon doing the Manske procedure two modifications have sprung into mind which im currently testing although the conditions are less than ideal*.

1)Follow the manske up to where the alkaloids have percipitated out of the solution. Improvise a waterbath ,where a volume of water is heated in a pan,a towel put in and the jar holding the solution and percipitate can rest on it without touching the metal bottom of the pan. Heat it ,but without disturbing it or mixing. Personally i heat it till the water in the pan starts emanating vapor. Then turn down the heat and let it cool there as it is,prefferably overnight. Next, transfer in fridge and let there so crystals reappear.

The idea behind it is this : By heating the liquid we redissolve some or all of the alkaloids back in solution but because they have percipitated chances are that we are going to have concentration differences in the solution of harmala alkaloids ,being more concentrated at the bottom (some diffusion might occur though).By letting it cool gradualy, in the improvised waterbath (water has better heat capacity than air) and then transfering it to fridge we aid theoretically the solution in developing bigger crystals,easier to filter.Think of it along the lines of "recrystalisation".

2)A crystal or another object could be added at the bottom of the percipitation vessel to give nucleation sites for the crystals to form. I do not know if this will work resulting in bigger crystals but it is worth a try. The object could be anything ,given that it doesnt have a totally smooth surface.

I hope the above can be tried by people more capable than me . * Due to my method of whole seedpods ,the filtering is very very difficult and i think im quite stuck at the moment. I do not have a vacuum pump to filter the solution so i cant get the percipitate.

 

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endlessness
#2 Posted : 7/26/2009 12:08:37 AM

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forget filtering

always decant on the fridge overnight instead. Redissolve in fresh water and repeat everything again.. doing this several times will clean the product and one doesnt have to filter. Then redissolve again in fresh water, and precipitate with a base like sodium carbonate to get freebase, if wanted (will also clean it a bit more.. but dont repeat this step or you get a loss of product).

As for the ideas on crystal growing, I guess that the usual techniques of crystal seeding or temperature change for crystal growth could work, but never felt too bothered to try.

But note that its a different situation than the usual dmt/naphtha story, because in that case dmt is soluble in warm naphtha but insoluble in cold naphtha. In this case its a salt saturated solution, which the harmalas are insoluble in and precipitate as hcl. I think the temperature change of the 'solvent' (water) in this case doesnt affect enough the water-salt solubility to make the water un-saturated and lead to a significant amount of the harmalas redissolving in the water.

Maybe some more chemically oriented members can give a more informed opinion


by the way, one can make an improvised vacuum filtering system with some hdpe jugs/containers, a funnel, filters and a vacuum cleaner
 
Crystalito
#3 Posted : 7/26/2009 3:06:50 PM
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Endlessness,thank you for your quick and kind reply. Your comments make sense and i will put them into practice, thank you also for focusing on the filtering issue.

It is true that crystals are not needed,that is for most people the percipitate is crude enough to be isolated easily.I wonder thoughof the results of such a procedure. In my case i have not seen yet bigger crystals,but keep in mind that my case might differ : i have got way too much "junk" in my isolation vessel and apart from limiting visibility it also limits crystalysation attemps. Lesson learned, next time i will be more careful."He who does not think ahead, better be equiped with enormous patience" Razz
 
endlessness
#4 Posted : 7/26/2009 4:06:58 PM

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if you redissolve your crude stuff in clean water with bit of vinegar, then let it sit overnight in the fridge and throw away the decanted part, this will help you, as the water should still have the alkaloids and the decanted stuff should be only impurities. Then proceed to manske and as I mentioned before, repeat the manske step a few times by adding fresh water to the decanted stuff.. This will help you even now at the current step you are in Smile
 
 
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