This is my first attempt using 50 g. finely shredded/powdered MHRB. Custom STB tek based on Lazyman and Entropymaster's guide
-Mixed about 50+ g. lye with 750 mL of water in an empty olive oil g. the bottle had been thoroughly washed of oil.
-Added MHRB - 50 g. of MHRB. Ordered 1 Kilo from online vendor for $80; only used 50 g. here due to small bottle size and to test out my tek
-Shook vigorously, let sit for 2.5 hours. The water looked typically black and watery (not jelly-like).
-1st pull: added 50 mL of HOT naphtha (boiled water with pyrex container flouting in it - turned off heat - added naphtha to pyrex container - let sit 2 minutes until Naphtha felt hot to touch)
-Turned end over end until well mixed. I found that the two layers separated quickly And without emulsions quite easily and later on in the tek I mixed the solvent in quite vigorously with no ill effect.
-Gave closed bottle a "hot shower" in the sink for 10 minutes. Once the bottle was hot I found that the layers stayed mixed together but when r
emoved form the sink the layers separated easily. I used the hot water bath to increase the interaction, so to speak, of the solvent and the lye water.
-Removed naphtha into a pyrex baking dish with a turkey baster. I think this was where the majority of my problems were, as I didn't really know what I was doing and did get a few tiny blobs/dots of black lye water in my naphtha.
-Set in sun to reduce volume while doing other pulls.
-2nd Pull- Same as first, but before heating up Naphtha I mixed 200 mL of water and 25 g. of lye in a separate container and then added it to the root bark water. Shook bottle vigorously, let sit for 10 minutes, then repeated Naphtha pull.
-3rd pull - same but used less Naphtha, maybe 30 mL
-4th pull - added a "dash" (20-30 mL) of Naphtha to bottle; shook vigorously; stored; will let sit for a week or so then pull Naphtha.
-Meanwhile all 3 first pulls were sitting combined, spread out in a pyrex baking sheet, in order to reduce volume. They sat another hour. By this time I noticed that while the Naphtha was a pale translucent yellow/white, there was a definite "blob" of orangey fluid sticking together at the bottom of the dish. When poured out into a smaller container with a lid, the orangey stuff collected in the corner and eventually went into the container and was frozen.
-The total first three pulls, collected (estimated volume of 75-100 mL) went in a rubbed-lidded, sealed, glass pyrex container (half-pint) into the back of a 'very cold' standard freezer. First however, 200 or so mL of water with a pinch of washing soda (sodium carbonate, grocery store) was added; layers were stirred, allowed to seperate; lower water layer was discarded. After this wash was complete the Naphtha was placed in the freezer.
-I just took it out to look, about 4 hours into the freezing. Opened it up, took a peek, put in fridge for 20 minutes and returned to freezer. here are my observations:
-Naphtha is milky. Definite 'mountains' of something, either mushy crystals or gooey stuff, is at the bottom. I suspect a combination of yellowy DMT crystals, and little pin-points of maroon-colored... impurities? jungle? fat? Also, below both of these I think is a layer of yello-orange goo. However, the freezing is by no means over and I don't know yet how it will look when it fully crystalizes and I pour off the Naphtha and let the crystals dry to a crisp. For all I know the goo might resolve into yellowy crystals.
My questions:
-Is it possible/reasonable that the semi-pure (pale yellow) DMT crystals separate themselves from the worthless (maroon-colored) impurities/whatever the hell it is? Or would one expect them to be combined simply in one orange-red impure-DMT crystal? If they are separate, is there any chance of me 'picking out' the good stuff with like tweezers or something and discarding everything else?
-How can I avoid all these colors in the future - from that orangey liquid in the naphtha too the orange goo and maroon dots?
Part of it is just that it was the first time and you learn much from experience. By the end I was an expert at removing Naphtha without getting lye water. etc.
Also, what purification steps do you recommend at this point? Residual lye has already (hopefully) been taken care of with Na2CO3 wash. I'm thinking recrystalization in warm Naphtha; that's easy enough. Is activated charcoal worth it?
Thanks for the help everyone
Will post results tomorrow
-Mixed about 50+ g. lye with 750 mL of water in an empty olive oil g. the bottle had been thoroughly washed of oil.
-Added MHRB - 50 g. of MHRB. Ordered 1 Kilo from online vendor for $80; only used 50 g. here due to small bottle size and to test out my tek
-Shook vigorously, let sit for 2.5 hours. The water looked typically black and watery (not jelly-like).
-1st pull: added 50 mL of HOT naphtha (boiled water with pyrex container flouting in it - turned off heat - added naphtha to pyrex container - let sit 2 minutes until Naphtha felt hot to touch)
-Turned end over end until well mixed. I found that the two layers separated quickly And without emulsions quite easily and later on in the tek I mixed the solvent in quite vigorously with no ill effect.
-Gave closed bottle a "hot shower" in the sink for 10 minutes. Once the bottle was hot I found that the layers stayed mixed together but when r
emoved form the sink the layers separated easily. I used the hot water bath to increase the interaction, so to speak, of the solvent and the lye water.
-Removed naphtha into a pyrex baking dish with a turkey baster. I think this was where the majority of my problems were, as I didn't really know what I was doing and did get a few tiny blobs/dots of black lye water in my naphtha.
-Set in sun to reduce volume while doing other pulls.
-2nd Pull- Same as first, but before heating up Naphtha I mixed 200 mL of water and 25 g. of lye in a separate container and then added it to the root bark water. Shook bottle vigorously, let sit for 10 minutes, then repeated Naphtha pull.
-3rd pull - same but used less Naphtha, maybe 30 mL
-4th pull - added a "dash" (20-30 mL) of Naphtha to bottle; shook vigorously; stored; will let sit for a week or so then pull Naphtha.
-Meanwhile all 3 first pulls were sitting combined, spread out in a pyrex baking sheet, in order to reduce volume. They sat another hour. By this time I noticed that while the Naphtha was a pale translucent yellow/white, there was a definite "blob" of orangey fluid sticking together at the bottom of the dish. When poured out into a smaller container with a lid, the orangey stuff collected in the corner and eventually went into the container and was frozen.
-The total first three pulls, collected (estimated volume of 75-100 mL) went in a rubbed-lidded, sealed, glass pyrex container (half-pint) into the back of a 'very cold' standard freezer. First however, 200 or so mL of water with a pinch of washing soda (sodium carbonate, grocery store) was added; layers were stirred, allowed to seperate; lower water layer was discarded. After this wash was complete the Naphtha was placed in the freezer.
-I just took it out to look, about 4 hours into the freezing. Opened it up, took a peek, put in fridge for 20 minutes and returned to freezer. here are my observations:
-Naphtha is milky. Definite 'mountains' of something, either mushy crystals or gooey stuff, is at the bottom. I suspect a combination of yellowy DMT crystals, and little pin-points of maroon-colored... impurities? jungle? fat? Also, below both of these I think is a layer of yello-orange goo. However, the freezing is by no means over and I don't know yet how it will look when it fully crystalizes and I pour off the Naphtha and let the crystals dry to a crisp. For all I know the goo might resolve into yellowy crystals.
My questions:
-Is it possible/reasonable that the semi-pure (pale yellow) DMT crystals separate themselves from the worthless (maroon-colored) impurities/whatever the hell it is? Or would one expect them to be combined simply in one orange-red impure-DMT crystal? If they are separate, is there any chance of me 'picking out' the good stuff with like tweezers or something and discarding everything else?
-How can I avoid all these colors in the future - from that orangey liquid in the naphtha too the orange goo and maroon dots?
Part of it is just that it was the first time and you learn much from experience. By the end I was an expert at removing Naphtha without getting lye water. etc.
Also, what purification steps do you recommend at this point? Residual lye has already (hopefully) been taken care of with Na2CO3 wash. I'm thinking recrystalization in warm Naphtha; that's easy enough. Is activated charcoal worth it?
Thanks for the help everyone
Will post results tomorrow
