Hello all. Been lurking for a while before signing up and SWIM took a crack at an STB extraction. Did lots of reading up on different TEKs, materials, labware, Recrystallization, and whatnot so SWIM felt somewhat well read and up to date on techniques. Have read some advanced methods and TEKs but felt to go simple due to popularity, ease, and effectiveness.
Abstract:
SWIM attempted this OZTek 15 Min STB heptane TEK:
https://dmt-nexus.me/forum/default.aspx?g=posts&m=153156 and
http://www.shroomery.org/forums/showflat.php/Cat/0/Number/12738710SWIM followed directions pretty closely...And yields were VERY LOW from 3 pulls. Off the bat, SWIM thinks the root was to blame.
First time half-weight Tek. Second time full weight tek.
SWIM's overall Observations:1. Mixing NaOH solution got in excess of 180°F
2. Nalgene Labware can handle the heat without issues.
3. MHRB Solution sticks to inside walls of nalgene containers making clarity and decanting. Is this Normal? Also did the same in glass container.
4. Clarity of Nalgene O.K..
Very difficult to see line between heptane and MHRB solution.
4a.Seperation of heptane from solution very difficult to do with pipette and also Sep Funnel. Inside walls of sep funnel extremely dirty with MHRB. Making Sep Funnel useless due to contamination.
4b.Something like a graduated cylinder with a smaller diameter seems like it would be easier to pull off.
5. Heptane was very yellow upon seperation. Lemon-lime gatorade
6. Freeze precip(FP) worked, but yeilds were very low and waxy yellowish. Also lots od yellow oily matter. Some little white nodules but all mixed up for re-X
7. Re-X process pretty straight forward. Small initial product makes it difficult overall. Oily yellow matter settled to bottom, Hazy, less yellow solution in pipette when pulling saturated solution from water bath. Hazy was a good sign. Slowly cool to room temp, then room temp for a few hours then FP and strain heptane. Yields were unusable and still yellowish waxy. Using Shot glass method
8. The most that ever came out from a pull was about a pea-sized quantity of light yellow waxy matter.
9. What's the best FP container?
10. DMT seems to be soluble in room temp heptane.
SWIM's expectations/reservations/outcome:1.MHRB solution wouldn't stick to sides of labware/containers. Especially sep funnel. Why?
2.Haven't found use for filtration funnel.
3.Went in with high confidence. Now, total bummer.
Questions:1. Bad MHRB?
2. Why the clumpyness of MHRB solution? Maybe need more NaOH solution to MHRB ratio? More or less concentrated(higher/lower pH) NaOH solution?
3. Improper TEK/technique?
4. Does each pull have it's own FP or is all of the solvent FP'd at once in one container? SWIM did separate.
5. What effect does temperature of the MHRB solution have on the extraction process? Aside from heating the heptane to allow greater solubility.
Any other comments? input? questions for me?
Thanks for reading and I'm looking forward to an engaging discussion on these issues.