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nice yield (tek included) Options
 
blacklist666
#1 Posted : 11/18/2011 5:33:47 AM
Using This Method, SWIM got 100g MHRB into 2.098% yield from Brazilian inner root bark. (Before re-crystallization) Any recommendations?

Mix of Gir’s 100 Gram Extraction Tek,
Hot Tuna’s Solubility and Temperature Experiment #4,
and Plasmod3smata’s Glass Shard Re-crystallization. =)

* Always use exhaust hood, range hood, exhaust fan, or stove fan when working with solvents or lye.

* Put on plastic goggles, and a face mask, and yellow dish washing gloves where applicable. Use common sense.

{-----------Set Up Base Solution (5 - 15 Minutes) ---------}

1. Add 1500ml filtered water to milk jug using funnel.

Note: Get Vinegar near by to neutralize any lye accidents.

2. Add 100 grams granulated Lye using funnel. (Wash funnel afterwards)

Notes: Make sure it's measured. Add slowly. Do not submerge milk jug in cold water while adding. Wait for heat reaction before adding more. (Do not inhale fumes. Fumes make eyes burn.) (Allow pressure to release, or milk jug might explode) (Bottom of milk jug may burn hands if held) (Just leave it on the table with a hot pad underneath it.)

3. Add 100 grams MHRB powder to the milk jug using funnel.

(Tap funnel to slowly add MHRB so funnel does not clog)

4. Shake the milk jug up and down 20 times violently over the course of 5 seconds (Wait 24 hours for lye to get bark broken down)

{---------Add Naphtha & Prepare Heated Water Bath --------------}

5. Add 60ml naphtha to milk jug.

Note: (Use yellow re-used naphtha from prior freeze precipitation if you have it.)

6. Get a pot large enough to hold the milk jug.

7. Fill pot 3/5 full of tap water.

8. Set stove on “High” until you bring the water temperature to 130F, then turn off the burner.

Note: (The temperature of the water should continue to rise until it gets to 140F, and then slowly go back down to 130F over 10 minutes or so.)

{--------- Mixing the Heated Pull ----------}

9. (With the 130F – 140F water temperature, and after the milk jug sits in the water for 3 minutes) Lift the milk jug out of the water bath, and turn the milk jug end over end slowly for 1 minute. (It should be fast enough to begin hearing a little slurp glush sound, but not too much.)

Note: Look at the milk jug to see if the clear naphtha layer is getting absorbed into the rest of the dark solution. If not, turn end over end a little faster and then wait and see if you’re actually getting the naphtha to stop (momentarily) forming a layer on top. If you got the naphtha layer to go away momentarily, keep the speed you’ve got. Otherwise, increase speed of turning end over end slightly until upon inspection you are actually driving the naphtha through the rest of the solution mixing it well. If the solution sloshes around a little bit as you turn it end over end, this can actually be a good thing. No shaking.

10. Place milk jug in the heat bath for 3 minutes. Check the temperature to make sure it doesn’t go below 125F. If it does, turn the burner on high until the temperature reaches 130F, and then turn it off.

11. Repeat steps 9 & 10 for a second time.

12. Repeat steps 9 & 10 again for a 3rd time.

{--------- Pulling out the Naphtha --------}

13. Sit milk jug on top of 2 paper towels.

14. Set tall jar next to milk jug.

15. Take lid off of milk jug.

16. Carefully slowly squeeze the milk jug until the clear layer at the top moves up to the mouth of the milk jug. (So you can more easily siphon it off with a glass turkey baster)

17. Seal the lid now, to give the layers another 30 seconds or so to separate from the agitation of scrunching down the milk jug.

18. Get a hold of the milk jug (all crushed down) with one hand, and use the other hand to take off the milk jug lid, and pick up the glass turkey baster.

19. Get a comfortable grip on the glass turkey baster's squeezer; squeeze a comfortable amount of air out of the head of the glass turkey baster.

20. Place the tip of the glass turkey baster just deep enough under the naphtha layer so that you will not break surface tension while sucking up naphtha. The object is not to break surface tension with the naphtha layer, but you need the tip a little lower than surface depth while drawing the naphtha up.

21. Slowly evenly release the glass turkey baster's head. Be careful not to draw too fast causing black stuff to shoot up into the glass turkey baster's neck. If this happens, stop drawing, and wait for black chunks to settle back into the milk jug. Reposition your tip just under the surface, squeeze the jug a little so your naphtha is as close to the top of the milk jug as possible, and resume drawing more slowly in order to get more naphtha until you can see the naphtha layer is all but gone & all you’re pulling up is black.

22. When you have drawn about half as much naphtha as you could, perform the next two steps simultaneously.

23. Let go of the yellow ball atop the glass turkey baster.

24. Position the tip of the glass turkey baster over top of the Mason jar.

Note: If all goes well, the suction of air entering the baster should have prevented any naphtha from falling out while you moved the tip over top of the Mason jar.

25. Empty the glass turkey baster all the way into a Mason jar, and go back for more.

26. You should probably only get about 2&1/2–3 or so draws of naphtha from the milk jugs using the glass turkey baster until you run into black stuff. Then it’s time to stop & repeat steps 5 – 26 for another pull. Collect all the naphtha into the same Mason jar in step 25. This combining of pulls will be ok because we let the Water/Lye/MHRB solution sit for a day, so the sum of the solvents from each pull should be saturated enough to precipitate graciously.

27. Perform 3 more of these pulls for 4 pulls total. You should get around 50ml of naphtha out each time, so 200ml of naphtha to freeze precipitate.

{-------- Removing lye / Sodium Carbonate Wash ------}

28. Place your Naphtha (combined from your 4 pulls in the Mason jar) into a (I used a 1000ml) separatory funnel sitting on top of a wine bottle with a large diameter base.

Note: Make sure the separatory funnel itself is propped up against something so it doesn’t accidentally get knocked over.

29. Prepare 30ml of filtered water heated to 140Fin in a mason jar & add a pinch of sodium carbonate.

30. Stir until granules are fully dissolved, and water is a cloudy color.

31. Let solution sit for 5 minutes to make sure it’s fully diluted.

32. Place in freezer until solution is cold as old dish water left overnight.

33. Add this solution into the separatory funnel.

34. At a 45 degree angle, swirl the solution around 10 times in a circular motion, (As hard as you can safely) (Total process should take 3 seconds) and place separatory funnel back into the wine bottle.

Note: The separation of the multiple layers should be literally instant. You may have 2 layers, or 5. Quickly get rid of anything below the top layer including any bubbly layer right below your Naphtha layer at the top.

35. Add 30ml of filtered water to the separatory funnel, swirl same way, and get rid of everything below the top layer just as fast as before.

36. Perform step 35 again just as before. (For a second water wash)

37. Add the naphtha from the separatory funnel to a wide mouthed martini glass. Use Glad Press N’ Seal plastic wrap to create an air tight seal around the top of the glass

38. Being careful not to spill any liquid, place the martini glass closest to the back of the freezer as you can get it, or as close to the place where the cold is coming from. Ideally you are suppose to defrost your unit first, clean it, remove any ice or food, have a dedicated freezer that goes at least -30C, or use Mason jar opposed to martini glasses to conserve space. Ideally you set your mason jar next to ice blocks, dry ice, covered with cold packs, freezer bags full of ice, but no mater what you do, with your freezer compartment on the max coldest setting it has. Leave it alone for 24 hrs. (Write down What time you put it in the freezer.) A freezer capable of -70C supposedly can freeze precipitate in 3 hours; -25C supposedly in 20-24 hours. Your mileage may vary. If you have a mini fridge, it may take 24-36 hours. If your bark is good, then your solution should have plenty of crystal to crash out and stick to the edges of the glass.

{-------Preparation for Removing from fridge (24 hours later) ------}

Depending on which freeze precipitation vessel you chose in the previous step, there will be different ways to handle each step. The process is to remove the vessel, quickly pour the fluid through a coffee filter, (so it collects into another vessel) and get excess naphtha away from the crystal stuck to the inside of the glass; Using gravity to allow the naphtha to drip into a collection dish, and a fan to help evaporate any excess naphtha in the vessel.

For those using a martini glass keep reading. For those using Mason jar skip down past this section.

{--------- For Those Using a "Martini Glass" (Steps 39–55) ------}

39. Prepare a glass jar with a funnel on top, and plug a fan in near by.

40. Place a coffee filter snugly inside the funnel making sure to push it down as if it already had a load bearing weight of fluid draining through it.

41. Crease any lines the filter makes, and gently push then to the side to make sure the creases don’t allow any fluid to get past the filter.

42. Carefully remove martini glass from freezer & set on counter, remove plastic wrap, and pour naphtha through filter fast enough to prevent a spill, but slow enough not to splash.

43. Squeeze the bottom of the coffee filter to get the solvent to pass through it more quickly after 2 minutes if the solvent is having difficulty passing through, otherwise, carefully pick up the coffee filter by it’s edges, (keeping the fluid in the bottom) place a new coffee filter into the funnel, and drop the fluid from the original coffee filter into the new one. The new coffee filter should help it to drain through faster.

44. Remove coffee filter from funnel, set it on Pyrex plate, and place in a cabinet to dry for 15-20 minutes.

45. Turn on the fan to the lowest setting.

46. Place a Pyrex dish in front of the fan.

47. Place a spoon in the Pyrex dish.

48. Face the martini glass towards the fan.

49. Allow the martini glass to drain any excess naphtha onto the Pyrex dish.

50. Once the martini glass has stopped dripping, place it in the Pyrex dish facing the fan.

51. Place the edge of the martini glass into the spoon in order to keep it from blowing around.

52. Tip up the back end of the martini glass in order to assist the naphtha in dripping down into the Pyrex dish.

53. Allow the fan to blow on the martini glass for approximately 10-15 minutes.

54. Check to see if you can smell any naphtha coming from the martini glass. If you can, keep blowing air on it. If you can’t, proceed.

55. Using the spatula that best gets into the bottom of glass, scrape the crystals down, and pour them out into a clean dry mason jar. (Labeled “Unrefined”)

{------- For Those Using a “Mason Jar” (Steps 39–52) ------}

39. Prepare a glass jar place a funnel over top, place a coffee filter in funnel making sure to push it down as if it already had a load bearing weight of fluid draining through it.

40. Crease any lines the filter makes, and gently push then to the side to make sure the creases don’t allow any fluid to get past the filter.

41. Carefully remove the Mason jar from freezer, Unscrew lid, pour Naphtha through coffee filter passing down the funnel into glass jar.

42. Reseal Mason jar and place it upside down in freezer for 2 hours.

43. Squeeze the bottom of the coffee filter to get the solvent to pass through it more quickly after 2 minutes if the solvent is having difficulty passing through, otherwise, carefully pick up the coffee filter by it’s edges, (keeping the fluid in the bottom) place a new coffee filter into the funnel, and drop the fluid from the original coffee filter into the new one. The new coffee filter should help it to drain through faster.

44. Remove coffee filter from funnel, set it on Pyrex plate, and place in a cabinet to dry for 15-20 minutes.

45. Place a Pyrex dish on the kitchen counter.

46. Place a coffee filter on top of it.

47. Flatten out the coffee filter over top of the Pyrex dish.

48. After the 2 hours is up, Remove the upside down mason jar from the freezer and remove the lid over top of the coffee filter carefully allowing liquid to drip onto the coffee filter.

49. Set the jar down (upside down) on top of the filter.

50. In 2-3 minutes, move the jar's orientation slightly.

51. If you see a large wet ring of naphtha/water, reposition it for another 2-3 minutes, otherwise, plug in a fan, set it on low, face the jar at the fan at an angle and slowly turn the jar.

52. Hold the jar in front of the fan for 10-15 minutes.

53. Check at first to see if naphtha is still in the jar rolling around. If so, place back on the coffee filter to let it drip out of the jar.

54. If you can still smell naphtha coming off the jar, go for another 3 minutes or until you can no longer smell naphtha what so ever.

55. Using the spatula that best gets in the corners of the jar, scrape the crystals down to the bottom of the jar, and pour them out into a clean dry mason jar. (Labeled “Unrefined”)


{----Re-crystallization (1 Hour Work, 3 Hour Wait, 20 Minute Work, 24 Hour Wait) ----}

56. Get a deep pot and fill it with hot sink water.

57. Place the strainer in the pot of water.

58. Adjust level so the water comes up enough to cover half of a mason jar.

59. Turn heat on between “medium high” and “high” to bring water to boil.

60. Put 1g of crystal into a clean dry shot glass labeled (Initial).

61. Place 50-60ml of Bestine in a Mason jar.

62. Place Mason jar on top of the strainer so it won’t fall over and let it sit in the boiling water bath until you begin to see tiny little bubbles streaming from the bottom to the top in the Bestine (Or leave it in there for 15 minutes as is called for, I left it for 10-12 minutes.)

Note: If Bestine becomes too hot, it will flow over like champagne up into the air, and you will loose your solvent.

63. Turn off burner.

64. Using hot mittens place Mason jar onto kitchen counter and remove pot from heat.

65. Swirl Mason jar for 10 seconds.

66. Pour 25-30ml hot solvent into the shot glass containing the 1 gram of crystal. The shot glass should be 2/3 to ¾ full of Bestine.

67. Stick eyedropper to the bottom of the shot glass to suck in and squeeze out the Bestine thoroughly to assure all the crystal is fully dissolved.

68. Use eye dropper to fish out any hair\dust chunks that remain in the shot glass placing that into a shot glass labeled (Impurities).

69. Remove strainer from pot.

70. Add ice packs to pot water to reduce temperature until kitchen thermometer reads 150F.

71. Put strainer back into pot.

72. Reduce water level in the pot so the shot glass can sit on the strainer where it’s immersed 3/4 up the glass.

73. Cover the shot glass (Labeled “Initial”) with foil, place rubber band around top to secure tin foil, and set into 150f water bath for 2 hours (or until water is as cold as cold dish water or damn near close.)

74. Remove shot glass from water bath, and remove rubber band and aluminum foil.

Note: You will see white or cloudy Bestine on top (Bestine + DMT), red crap underneath (Impurities/Oils), and water on the bottom.

75. Use eye dropper to suck up (yellow/red/orange) oils and squirt into shot glass. (Labeled Impurities)

Note: In the “Impurities” shot glass, oil & crap will sink, but Bestine containing DMT will float.

76. Tilt the “Impurities” shot glass and suck out the top layer that looks clean and add back to the ”Initial” shot glass. Repeat until you start sucking up oils.

77. Pour the contents of the “Initial” shot glass into another shot glass labeled “Final”.

Note: The crusty (red/yellow/orange) oil remaining in the “Initial” shot glass will stick to the insides of the glass. Save that stuff for every 10-20 re-crystallizations.

78. Cover “Final” shot glass with foil & rubber band.

79. Let it sit for 3-4 hours in room temperature

80. Place the “Final” shot glass in the freezer on coldest setting in the back next to the ice covered with cold packs for 24 hours. (Write down the time you put it in for reference)

81. Take Shot glass out of the freezer and remove aluminum foil and rubber band.

82. Pour the Bestine into another mason jar labeled “Reusable Bestine”.

83. Set shot glass in front of a fan set to low setting for 10-15 minutes. (Or until dry)

84. Use a dental pick to scrape crystal out of the “Final” shot glass onto a coffee filter.

85. Use a razor blade; lightly scrape crystal from coffee filter into a small Mason jar labeled “Pure Crystal”.
I= SWIM = Not Me. The I AM I Does Not Exist, and is Referenced to SWIM Who Is Not A Friend I Never Met, Nor Hallucinated While Imagining The Is-ness of Suchness That Is SWIM Who Is Not Me, Myself, Nor I As The Expression Of Non Dual Aspect of Non-Dual Reality Subjectively Denied By Swim, or accompanying Me-Anti-ness'es. =) All Credit Goes To The ANTI-SWIM'ness of SWIM's cousin's room-mate's uncle's deceased cat's in-law's second removed nephew's aunt WHOM authored SWIM's 2000 Year Old Desert Scribblings from a drunk rabbit in the Serengeti desert found in an insane asylum under water, on Easter eggs, crucified by the on fire pagan music listening christian maniac from India running around believing he was Jesus repenting this bush he called the Acacia tree; So I Heard from a bum who claims to be SWIM, But I Forgot... And Again, "I" Refers To Someone Who Is Not Me.
 
nen888
Acacia expert | Skills: Acacia, Botany, Tryptamines, CounsellingExtraordinary knowledge | Skills: Acacia, Botany, Tryptamines, CounsellingSenior Member | Skills: Acacia, Botany, Tryptamines, Counselling
#2 Posted : 11/18/2011 5:38:48 AM
..thanks Blacklist666, that's one of the most comprehensive teks i've seen..i'm usually an A/B head, but i like the detail of this tek..worth a try..Smile
do you ever measure your pH with strips/metre..?
 
blacklist666
#3 Posted : 11/18/2011 5:55:51 AM
With granulated Lye, I did measure pH the first time using strips. I kept adding too much lye (150-200g per 100g MHRB) & never got it to pH 14. The first time I only waited 2 hours before attempting any pulls. I think that caused some issues. I can only imagine the granulated lye takes some time to work it's magic. Perhaps I should take measurements next time after 24 hours.

I'm hoping the attention to detail will help new members overcome any obstacles in their first extraction, as well as answer some simple questions I keep seeing pop up from time to time.

I'll write a materials list if someone needs it.
I= SWIM = Not Me. The I AM I Does Not Exist, and is Referenced to SWIM Who Is Not A Friend I Never Met, Nor Hallucinated While Imagining The Is-ness of Suchness That Is SWIM Who Is Not Me, Myself, Nor I As The Expression Of Non Dual Aspect of Non-Dual Reality Subjectively Denied By Swim, or accompanying Me-Anti-ness'es. =) All Credit Goes To The ANTI-SWIM'ness of SWIM's cousin's room-mate's uncle's deceased cat's in-law's second removed nephew's aunt WHOM authored SWIM's 2000 Year Old Desert Scribblings from a drunk rabbit in the Serengeti desert found in an insane asylum under water, on Easter eggs, crucified by the on fire pagan music listening christian maniac from India running around believing he was Jesus repenting this bush he called the Acacia tree; So I Heard from a bum who claims to be SWIM, But I Forgot... And Again, "I" Refers To Someone Who Is Not Me.
 
 
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