Blowing on cold saturated nalpha

[Phyrexian Spicenaut]

Hello, Swims been using a stb with nalpha and freeze precip. however after a few days swim poured off the nalpha and collected crystals. However the nalpha is a clear yellow until blown upon, then it begins to swirl and cloud. does this mean there is still a lot of spice yet to settle out? Does swim need to let the nalpha sit out of the freezer for a while, get all cloudy and then continue freeze precip or is it good to heat up for the next extraction? Swim wants to be a efficient as possible with the spice. thanks

 

[gammagore]

Sounds like there is still spice in the naphtha.

Your freezer might not be cold enough to get all the goodies out. Have you checked the temp of the freezer? What is the yield you are getting?

 

[Samadhi-Sukha-Upekkha]

Are you saying that after you remove all the solids from the freeze-precipitated naphtha, and then blow on the resulting clear naphtha, it becomes cloudy? That would be kind of odd.

During any freeze precipitation, there is some spice still left in the naphtha. However, it should only have the maximum amount of spice soluble in freezer-temperature naphtha. When it returns to room temperature, or is gently heated (perhaps to 100-110 degrees fahrenheit), it becomes able to hold more spice. So if there is still spice in your plant material, you can let your naphtha return to room temperature (or gently warm it and the plant material up) and you'll keep pulling alkaloids. Then you put that in the freezer, and all of the extra spice precipitates back out as solids, but the naphtha again holds on to a certain amount of spice which is soluble even in very cold naphtha.

It's hard to tell how much spice is left in the naphtha -- depends on the temperature of your freezer, the brand of the solvent, etc. The only way to get all of the spice out of the naphtha is to completely evaporate the naphtha away. Given that you didn't just evaporate in the first place, I assume you're more concerned with purity than with amount of spice yielded where those two goals conflict.

With that note in mind, it's possible to get pure spice from evaporated naphtha if you dissolve the impure spice in acetone and add FASA to salt it out of solution. I won't provide all the details here because the information is on the forum and wiki, but basically you dissolve the impure spice in acetone, and in a separate container, you dissolve fumaric acid in acetone. Then you mix the two solutions together, and pure spice (as the fumarate salt, not the freebase) precipitates out as a solid. Decant off the acetone (which should contain the undesirable contaminants) and you ought to have rather pure spice fumarate. But that requires time and money to acquire another solvent and another reagent.

 

[Phyrexian Spicenaut]

thank you for the fast response, Indeed the freezer may not be cold enough, Swim has lots of bags of ice covering the jars that have the nalpha, the temp seems as cold as it can get. This nalpha was left in the freezer for 40ish hours will little spice accumulating until swim took it out and let it get cloudy. a couple of hours later swim placed it back in the freezer and the next day there was quite a bit of spice at the bottom. Swim has been trying to get a freebased smokable form of spice so swim decanted the nalpha and placed the yellow solids in the dehydrator. But the yield was small for a kilo (bout 5 grams ofter 5 hot pulls) Swim knows that all bark alk content is different, but swim remains hopeful.
Also, swim already has quite a bit of fumerates, has failed multiple times to freebase it
(wasted a whole can of acetone) and has no interest in buying more fumeric acid, or acetone unless it is used to recrystallize what yellow spice swim has now. belive me swim has been reading the nexus for more than a month and can follow directions very well, just feels that fumerate approach is not for swim yet..

Query- spice swim has is yellow and gummy How long will it take to fully dry to a solid? will it without further recrystallization?

Query#2- does hot nalpha pulls more oils, hence the gummyness?



Thank you for your help.

 

[Samadhi-Sukha-Upekkha]

Query 1: It might or might not ever fully dry. If you scrape it up into a mound then spread that over a surface into a thin layer, and repeat that every day or so, that might help it dry quicker. However, enough contaminants will prevent it from ever becoming solid.

Query 2: Hot naphtha definitely pulls more oils and waxes than cold naphtha, all other conditions being the same, and can be a definite contributor to gumminess. In the future, it can help to avoid the gumminess if you put MHRB into an acidified solution and defat with hot naphtha pulls until no more yellow comes through, then basify up to your desired pH and start pulling with naphtha at whatever temperature you desire. This is still noticeably quicker than doing a full A/B extraction tek, and reduces the tendency of STB teks to yield lots of gummy waxes and oils.

The existing gummy stuff, if it won't dry, probably does need a recrystallization. The problem with naphtha is that both the oils and the alkaloids tend to be more soluble at higher temperatures than at lower temperatures. That's why the FASA tek gives better purity -- but you already said that you didn't want to do it. Luckily, recrystallization with naphtha will probably still be pretty helpful because the oils seem to stay in solution better at lower temperatures.

Perhaps the solubility of the oils does not significantly increase with the warming of the naphtha, but rather the heat causes the oils to more quickly reach the equilibrium of their max solubility in naphtha. This would explain how recrystallization can still help you remove the oils from the alkaloids -- cooling wouldn't make the oils fall back out of solution. It would also explain how vigorous shaking (the kind that makes emulsions even at pH 13.5 or above) of room temperature naphtha/MHRB water solutions can put a lot of oils/waxes in the naphtha.

Do any chemists have any comments about that?

 

[Phyrexian Spicenaut]

interesting, thank you for the info, Swims yellow spice is a bit more dry today, however it is still a bit gummy, will try to post a pic today. Swim has also seen of the defat with a nps prior to extraction in volvins tek and others. this watchas tek said to use room temp nalpha, but does not mention a defat for slightly yellow spice. does one belive there is a way to recrystallize and bet the fats/oils to drop to the bottom of lets say, a shot glass?
Also since the jars were placed in the freezer yesterday, today there is a bit more spice at the bottom of them. Swim will try to gather this and get it into the dehydrator today, however it appears that a recrystallization is in order for the lot of it.

uh sorry for the confusing post, swim was up late last night..

 

[Samadhi-Sukha-Upekkha]

I'm the king of incoherent sleep-deprived writing, so no worries.

I can tell you something helpful my friend does. After removing the naphtha from the MHRB water, washing the naphtha with NaHCO3 water, and evaporating it down until it's just slightly cloudy, he warms the naphtha up in a hot water bath. He uses boiling water for this, but water at around 60 Celsius would probably work just as well. Warming the naphtha causes insoluble contaminants to fall out of emulsion or suspension.

Then, with a bit of practice and a container with a raised middle (shaped like a tupperware) it's possible to tilt the container so all the insolubles collect at one corner, then tilt the container in the opposite direction so the naphtha runs to the other side but leaves the insolubles in that corner. If you touch the insolubles with the tip of a rolled up paper towel, the paper towel soaks them up. As long as the naphtha isn't supersaturated with spice (in other words, any cloudiness from the evaporation step disappeared upon adding heat and perhaps more naphtha), this shouldn't remove any of the spice. Just the insoluble impurities which would have been mixed into the spice upon freeze precipitation or total evaporation.

Even though my friend usually does that before freezing, it can be done any time you want to try and purify some spice. Especially if thorough mixing of the naphtha and the MHRB water has yielded a product with lots of tan/brown/yellow contaminants. The insolubles tend to be yellowish brown, and they're really easy to recognize even underneath a layer of yellow naphtha.

If you do this step, and then evaporate the naphtha down until it gets cloudy and freeze it, you should have a pretty clean product. Maybe you'll require one more recrystallization, but since you've already freeze precipitated and gotten a gooey product, it may help more to try this before you freeze again.

 

[Phyrexian Spicenaut]

interesting... Update- swim checked one of the jars more closely and noticed a handful of scattered crystaline formations, around the inside of a jar. then swim collected these and placed in a petri dish and into the dehydrator. These were almost white with a hint of yellow, looked authentic as well. When Swim checked on them later, to swims dismay they had melted. But alas the puddle was solid, and once scraped up turned out to be some crystalline spice. perhaps 1 recrystallization away from being "glass Spice". This has tickled swim to pieces. they hope it is not a fluke
the other dish with the yellow fatty earwax stuff was mushed up together in hopes of a manual crystallization. After an hour of effort swim would rather wait until later his week when swim gets bestine. Swim decided to make a few more pulls off the jugs, to swims pleasure 7 hours later it is beginning to snow Sim just assumes that yield is still present in the jugs after all and perhaps the first few pulls will be fattier than the current and future ones being preformed.
Swim is ready to graduate from spice 101..

 

[Phyrexian Spicenaut]

Since the topic of the thread is blowing on cold nalpha, swim thought they would share a possible but premature discovery. Swim took a look at the current snowing jars and niticed a floatinf layer of mica like crystal formations. then blowing on the solution to get it to fog and then gently stirring. Swim heard something about "seeding" saturated nalpha with preformed crystals to speed the growth of more crystals.. Swim will check the results in 14 hours time to see if a 25 to 30 hour wait could be sped up lets say 14 to 20 hr.Swim left a variable in the mix by not seeding some of the jars.. Swims will wait and see...