TmC47
Nice guy
So, when doing a Zn-reduction an A/B extraction would be required, which I never do. However, there was some dirty spice from STB lying around, which I assumed had oxidized to a certain degree. So, the 7 dwarfs entered the lab and:
1- split the batch in 3x 500mg, X,Y,Z. Z-portion set aside.
2- dissolved X,Y 2x 500 mg in 40 ml vinigar each in seperate containers.
3- defatted both with naphta.
4- Y portion Zn reduced, filtrated.
5- X,Y basification.
6- X,Y extraction.
7- X,Y freeze precip. X: 150 mg, Y: 195 mg
8- leftovers evapped to 8 ml.
9- Freeze again. X: 15 mg, Y: 20 mg
Notes:
2) Not all dissovlves. Stays murky. Most part dissolves, part sinks, part floats, part sits in-between. Solution yellow.
3) Sep funnel 100ml, 20ml Naphta, shake 1min, settle 5mins, repeated 3 times, slightly yellow naphta, even less yellow vinigar. NB: Emulsions were put with the naphta fractions and discarded.
4) 550 mg Zn-powder was added. Because the Acetic acid was not 100% naphta-free, reaction proceeded slow due to passifcation of the Zn. Color changed to a slight greenish hue, with a nasty, fattish smell. Stirred every half hour for 5 mins for 4 hours total. 430 mg of Zn was recovered.
5) 2,5 g of Na2CO3 added for neutrality, 1 g extra. Strong crashing-out, xtals growing on stirring-rod.
6) For X and y both, 40 ml of naphta each in total was needed to dissolve the muck. Emulsion formed (sighs). Glassware dirty from carbonates and spice. cleaned with 10ml+10ml of H2O+naphta. Some stuff remained. Adding water dissolved more, but separation proceeded worse. Result: X,Y both 60 ml naphta-fractions and 80 ml watery fractions. Washed Naphta fraction AGAIN with 40 ml H2o basified with 0,5 g of Na2CO3. Naphta fraction still contained a few micro-droplets of water, which were absorbed with a dash of Na2CO3 straight into the beakers and decanted.
7) evapped 'till half volume, freeze for 24 hrs, decant, dry
9) end results:
X: 165 mg of pretty good looking spice, slightly yellow, medium size (1mm avg.) xtals. Very active and clear. Good taste when 30 mg smoked. Normal DMT visuals. Over 300 mg of what I thought was spice was lost, either way.
Y: 215 mg of very white, very small xtals (grains of sand, really) spice. Effingly strong. Very clearheaded, crisp, abstract visuals. Neutral taste when 30 mg smoked. Over 250 mg of what I thought was spice was lost, either way.
Z: large chunks of yellow/browish spice. Not as strong as the others though. Normal visuals, nothing really special. Rather strong taste when 30 mg smoked.
Oh, did a cleanup with Florisil and evapped all naphta leftovers together for an additional 50 mgs of grayish stuff of unknown composition and potency.
Conclusion:
The original spice contained about 35% of n,n-dmt and 65% unknowns. Of the unknowns, about 20% was recovered as n,n-dmt. Surely a lot of spice was also lost in the copious use of vinegar, naphta, Na2CO3 and many cleanup steps, each resulting in a percentile loss of product.
Although this experiment has been executed far from perfectly, I think it pays to do a Zn reduction step: Batch Y was favorite and quality over quantity is to be preferred. Indeed, one moves to a more laboratory-grade spice, gaining yield over not doing a reduction. But the end result does not look as nice as STB spice. Next project: crystal growing, sothat this problem can be adressed!
1- split the batch in 3x 500mg, X,Y,Z. Z-portion set aside.
2- dissolved X,Y 2x 500 mg in 40 ml vinigar each in seperate containers.
3- defatted both with naphta.
4- Y portion Zn reduced, filtrated.
5- X,Y basification.
6- X,Y extraction.
7- X,Y freeze precip. X: 150 mg, Y: 195 mg
8- leftovers evapped to 8 ml.
9- Freeze again. X: 15 mg, Y: 20 mg
Notes:
2) Not all dissovlves. Stays murky. Most part dissolves, part sinks, part floats, part sits in-between. Solution yellow.
3) Sep funnel 100ml, 20ml Naphta, shake 1min, settle 5mins, repeated 3 times, slightly yellow naphta, even less yellow vinigar. NB: Emulsions were put with the naphta fractions and discarded.
4) 550 mg Zn-powder was added. Because the Acetic acid was not 100% naphta-free, reaction proceeded slow due to passifcation of the Zn. Color changed to a slight greenish hue, with a nasty, fattish smell. Stirred every half hour for 5 mins for 4 hours total. 430 mg of Zn was recovered.
5) 2,5 g of Na2CO3 added for neutrality, 1 g extra. Strong crashing-out, xtals growing on stirring-rod.
6) For X and y both, 40 ml of naphta each in total was needed to dissolve the muck. Emulsion formed (sighs). Glassware dirty from carbonates and spice. cleaned with 10ml+10ml of H2O+naphta. Some stuff remained. Adding water dissolved more, but separation proceeded worse. Result: X,Y both 60 ml naphta-fractions and 80 ml watery fractions. Washed Naphta fraction AGAIN with 40 ml H2o basified with 0,5 g of Na2CO3. Naphta fraction still contained a few micro-droplets of water, which were absorbed with a dash of Na2CO3 straight into the beakers and decanted.
7) evapped 'till half volume, freeze for 24 hrs, decant, dry
9) end results:
X: 165 mg of pretty good looking spice, slightly yellow, medium size (1mm avg.) xtals. Very active and clear. Good taste when 30 mg smoked. Normal DMT visuals. Over 300 mg of what I thought was spice was lost, either way.
Y: 215 mg of very white, very small xtals (grains of sand, really) spice. Effingly strong. Very clearheaded, crisp, abstract visuals. Neutral taste when 30 mg smoked. Over 250 mg of what I thought was spice was lost, either way.
Z: large chunks of yellow/browish spice. Not as strong as the others though. Normal visuals, nothing really special. Rather strong taste when 30 mg smoked.
Oh, did a cleanup with Florisil and evapped all naphta leftovers together for an additional 50 mgs of grayish stuff of unknown composition and potency.
Conclusion:
The original spice contained about 35% of n,n-dmt and 65% unknowns. Of the unknowns, about 20% was recovered as n,n-dmt. Surely a lot of spice was also lost in the copious use of vinegar, naphta, Na2CO3 and many cleanup steps, each resulting in a percentile loss of product.
Although this experiment has been executed far from perfectly, I think it pays to do a Zn reduction step: Batch Y was favorite and quality over quantity is to be preferred. Indeed, one moves to a more laboratory-grade spice, gaining yield over not doing a reduction. But the end result does not look as nice as STB spice. Next project: crystal growing, sothat this problem can be adressed!
