50 grams MHRB AB presently in 1 liter odorless mineral spirits. The freezer is so cold my rum is frozen. Is that too much NP solvent? More white specks are forming in the bottom with flat flakes floating in the spirits...

[quote:fb8c734f05="Jumpy"]50 grams MHRB AB presently in 1 liter odorless mineral Is that too much NP solvent? [/quote:fb8c734f05] Way too much. You'll need to evap like QB said. Here's the best A/B tek with freeze precip out there: http://www.drugs-forum.c...um/showthread.php?t=6627

There are crystals... Should I leave alone and evap or filter and then evap, freeze?? Thanks Man!

don't bother filtering small amounts,just evap it at room temperature till the np starts getting cloudy,then put it in the freezer.If your rum is freezing it must be cold eh?

is it good to freeze as soon as it's cloudy, or should you evap a little further just to be sure you get it all or will this make a difference?

No,when it's cloudy is good to freeze it.you can always evap what naptha you have left after filtering out crystals too see if there was anything left behind.there is always a little left behind.I save those dirty leftovers till I have quite a bit from many extractions and then re crystalize the sum of them .

From Noman's quick tek: [quote:41bc9a518e]2) Combine the lye and the water in the mixing jar. Use 15 ml water and 1 gram of lye for every gram of powdered root- bark that will later be added into the mixing jar.[/quote:41bc9a518e] [quote:41bc9a518e]4) Now add to the mixing jar 1 ml of naptha for each 10 ml of water used to create the lye solution.[/quote:41bc9a518e] Use 75ml of non-polar solvent per extraction. If you repeat the extraction 4 times (recommended) you should end up with about 300ml, not a liter. It's too much solvent, as quantumbrujo already said.

Great info! Thank you all! This morning I look and there are maybe 25 - 30 ~1-2mm size crystals clinging to the sides and bottom of the container and the NP is cloudy. I'll do as suggested and room temp evap to to 500ml (or cloudy) and freeze again. Anyone used dry ice for rapid freeze precip?

[quote:590e90b6ac="Jumpy"]Anyone used dry ice for rapid freeze precip?[/quote:590e90b6ac] I quote from Wikipedia: [quote:590e90b6ac]Single-solvent recrystallization Typically the mixture of "compound A" and "impurity B" are dissolved in the minimum amount of solvent to fully dissolve the mixture i.e. a saturated solution. The solution is then allowed to cool. As the solution cools the solubility of compounds in solution drops. This results in the desired compound dropping (recrystallizing) from solution. [b:590e90b6ac]The slower the rate of cooling the bigger the crystals formed will be.[/b:590e90b6ac][/quote:590e90b6ac] So it depends. We usually want large crystals, but it's up to you. I read somewhere else that a very rapid freeze can cause the crystals to enclose some of the solvent, which makes the crystals impure. Some people recommend to switch the solvent between refrigerator and freezer every few hours. This should increase the size of the crystals. I haven't tried this myself, I usually first cool the solvent down in the refrigerator and then put it in the freezer for a few hours. I hope this helps.

I usually don't worry too much about crystal size during the initial precipitation and just do a quick recrystalization later. In retrospect, I think that the NP ratio could be even lower - 2/3 to 1/2 the 1:10 figure I use. Especially for the last couple of pulls when the concentrations are lower. If Astral had just read a little further, he could have nailed my ass for that.

[quote:995338e5b1="Noman"]In retrospect, I think that the NP ratio could be even lower - 2/3 to 1/2 the 1:10 figure I use.[/quote:995338e5b1] You totally lost me in that sentence. Maybe because my English is not as good as the native speakers here, but could you explain that sentence one more time?

My tek calls for 1ml of NP per 10ml lye/bark/H2O solution, so the ratio is 1:10. Using 1/2 to 2/3 that amount works better, so .5ml or .66ml of NP per 10ml solution - for a ratio of 1:20 or so.

[quote:977f7f4d2e="Noman"]My tek calls for 1ml of NP per 10ml lye/bark/H2O solution, so the ratio is 1:10. Using 1/2 to 2/3 that amount works better, so .5ml or .66ml of NP per 10ml solution - for a ratio of 1:20 or so.[/quote:977f7f4d2e] Ok, thanks. Will try.

When my friend extracts from various Acacias (some are pure expirements) he always gets oil. Some crystals do form eventually sometimes, but when collected turn back into oil, which he smokes and gets an effect from. He defats 4 or 5 times, but the fat just never ends and also someone with alot of expirience told him there is no need to defat anyway ? Could it be something to do with the 98% Lye he is using (no such thing as 100% here) ? The solvent "Shellite' evaps clean. Maybe just use the freezer tech to grow crystals ? Also why do you bother to filter the juice from the bark before going from acid the base or before using solvent to pull from the base ? Seems to me that some goodness could be lost and left behind in the bark. Couldn't you just basify the entire acid + bark and then use solvent to pull out of the bark + base ? No bits would get into the solvent so why bother filtering ? thanks.

Rightangle is right about the filtering bit.there is absolutely no need to filter as none of the sludge ever ends up floating in the non polar layer.and tha naptha might grab some goodness still in the plant material when upending too.

SWIM used 98% lye with no problem. SWIM also had the crystals which then turned to goo but then got that goo and added a small amount of warm shellite. The goo was stirred around in the bottom of the container and then the shellite poured off leaving the goo behind. Shellite was then put into freezer again and crystals formed which didnt turn to goo this time. Hope this helps.

thanks for the help. Everytime he does a freezer precip in a large glass pan he gets some crystals, but as the condensation layer on the bottom of the dish thaws out it melts the crystals and he never sees them again, just a little residue once it is all dry He will try a sealed jar next time rather than a glass baking dish.

[quote:74562c2a3a="rightangle"]thanks for the help. Everytime he does a freezer precip in a large glass pan he gets some crystals, but as the condensation layer on the bottom of the dish thaws out it melts the crystals and he never sees them again, just a little residue once it is all dry He will try a sealed jar next time rather than a glass baking dish.[/quote:74562c2a3a] You definately have to use a sealed jar.The best I found is those little urine sample containers that you can buy at the pharmacy.as long as you use HDPE(high density polyethyline) plastic you're OK cause it doesn't react to base and doesn't dissolve in naptha.Mason jars work just as well.By the way if you're gonna be storing a base solution for long periods of time you can't use glass and you're better off using HDPE plastic.the lye solution weakens the glass and it cracks for no reason and you will be left with a caustic spill.

[quote:6c6a1e8de3="quantumbrujo"] By the way if you're gonna be storing a base solution for long periods of time you can't use glass and you're better off using HDPE plastic.the lye solution weakens the glass and it cracks for no reason and you will be left with a caustic spill.[/quote:6c6a1e8de3] I didn't know that. I thought base didn't react with glass in any way. So what do you mean by long periods of time? I really don't want an accident like that to happen

so im going to buigin an extraction on some MHRB soon. i have 1/2 pound. im thinking of taking 24 grams and making some jurema with a cold water infusion and using the rest as two 100gram batches. i realy dont want any part of this to go wrong so even though i have hundreds of hours of research on the topic im going to go through this step by step and ask you to tell me any tips that you could give me while you were doing YOUR extraction, and if i should change my method. ive got the bark, im going to get some jars and pans then some naptha, xylene, lye, and bestine (just to see which works better). my method is going to be basification with lye. my question there is how much per liter is good for ph 13.5?. second question is how much watter for 100 grams would be good? then im going to wait an hour or so stiring it. add the naptha or bestine, not too sure which. shake it up and put it in a warm water bath to kill emusion. after that im gonna use a turkey baster to draw off all the liquid, i asume a container with a small diamiter would be better for drawing it off. while thats evaporating a little bit im gonna do it again, this time with some warmer solvent. after the first one evaps some im gona put it in a fridge. question--how many hours would be best for CLEAN spice in the fridge/ freezer/fridge and so forth. then i plan on just pouring off the solvent and leting that dry off and keeping the crystals each time. after im all done with the naptha and stuff im gonna run an extraction using xylene to try and pull some jungle dmt, will this be posible after the pulls with naptha?