34 replies to this topic

[el_ronhub_bird]

So I just received a kilo of ACRB. Since MHRB is over triple the price it was a couple years ago when I first ordered some, I decided to give ACRB a try. I know it's a bit trickier to extract than MHRB so I'm gonna be depending on you guys for some help. From what I gather, ACRB needs to be defatted similar to mescaline extraction. So I'll start out by asking for any tips or tricks? Info on defatting? Thanks guys!

[Phineas_Carmichael]

Having never worked with ACRB I'm afraid I can't provide any specifics. That said, from what I've read you are absolutely correct; it needs an A/B extraction protocol with a thorough defat during the acid phase.

Defats are best accomplished with a broad-spectrum non-polar solvent that pulls all kinds of stuff. Simple cyclic molecules like xylene or toluene are generally used, with d-limonene being a "green" alternative or a substitute in places where the high VOC solvents are restricted by law. It is said that cooking oil can be used in a pinch but I'm not crazy about that idea.

At least 5 defats of the reduced acidic extract will probably be required. Keep going until no color comes over in the defat solvent. Then evap maybe 30mL of the last pull & check for residue. Rinse & repeat until you are confident that your acidic extract is as clean as you can get it.

As far as extraction goes, for ACRB I would keep the heat low in the acidic phase and extend the time. Just spit-balling, but like 2-4 hours on low in a ceramic slow-cooker (~190°F-200°F) per pull vs 30min at a simmer on the stove (~212°F) might be better. At higher temperatures more gunk comes out, and Acacia spp. are said to have a lot more gunk than MHRB.

ACRB or Phalaris are the rare cases where I might select a very specific targeted non-polar solvent for the basic pulls as well. Pulling with heptane (brand-name Bestine) instead of naphtha at cool room temperature will be expensive, but it will discourage any remaining gunk from coming over.

Freeze precipitation will almost certainly be necessary for white crystalline product right off the throw. Recrystallization is always an option to purify yellow product. One could (and IMO should!) continue to extract the basic phase with progressively less selective non-polar solvents and evap to yield various psychoactive goos and waxes of interesting colors after getting the crystals. Recrystallization "waste" falls into this category as well.

I know you are an accomplished extraction chemist Bird, but I feel compelled to include a note about safety for any newbies who might read this thread years from now...
 

1) Gloves & goggles, a fire extinguisher, and a dedicated lab space are absolute must-haves. The kitchen is fine for heating water-based liquids, but don't do the reactions or solvent-work on your kitchen table where the cat can knock stuff over!
2)Lab-grade glassware & tools are a would-be-nice, but Mason jars and/or thick HDPE (high-density polyethylene) will work for 1 extraction, just don't re-use them or let stuff sit in them for months under the sink.
3) Always check the SDS for any consumer grade solvents or reagents before you buy them.
4) Save everything until the end. The target molecule is in there somewhere; we can't wazzle it out if it was in the defat solvent we threw out 3 days ago...
5) Proper disposal of material (especially non-polar solvents) is ecologically responsible. Returning the spent xylene to the can with a bit of paint and dropping it off at a haz-mat center will ensure that we give our children a slightly less destroyed planet.

Sorry for the delay & for writing a book! Did I touch on most of the things you had questions about? I check in every day and generally answer more specific questions much faster. Please reach out if you have any more questions or if my writing above was unclear in any way. Also, I'm always available via PM if you (or anyone) has a question that you're not comfortable asking on the open boards.

I hate to give you homework again, but I'd love to see what you end up doing with your ACRB. I haven't seen very many extraction write-ups that use it...

Edited by Sidestreet, 01 October 2022 - 03:59 PM.
Requested by Phin :)

[el_ronhub_bird]

@Phineas_Carmichael

Thanks for the "book" I really appreciate your thorough information and instructions. You've certainly given me enough "homework" to get a good start on the extraction. I'll get started on the vinegar washes tonight then hopefully get into the defatting within the next few days. I've always done my vinegar washes with MHRB in the slow cooker so I'll probably just stick to that method here as well. I'll be checking in and will probably have a whole host of questions for you guys along the way. With your help I've processed many very successful (imo) extractions that I wouldn't have been able to pull off without you guys. I'd just like to express my gratitude to you guys once again. The fact that you take the time out of your day to share your knowledge with me or us (all for free I might add) means so much. I could go on and on but I'll stop myself from doing so here.

[el_ronhub_bird]

@Phineas_Carmichael I already fucked up your instructions lol. I left my slow cooker on high (instead of low) overnight and to my surprise I woke up to the contents lightly simmering. I seem to remember that my crockpot doesn't boil let alone simmer on the highest setting but apparently I was wrong. My next 2 washes I'll keep it on low. Hopefully I didn't pull too much gunk per your warning. Anyways I'll finish up my last 2 washes today and get to defatting it. I'll also start posting pics when there's actually something to see. I'm thinking about processing a bit of MHRB while I've got all the supplies out and I'm in extraction mode. As far as the ACRB, I'm processing half a kilo in this extraction, that's just over a pound for my fellow Americans. If I do decide to process some MHRB, it will be a quarter kilo, 250 grams.

A question for you Phineas: I've got quite the selection of solvents but no heptane (or Bestine.) I did a quick Google search and it appears that none of the big box stores near me carry it. So I guess I actually have a few questions:1.Is there some other place that might carry it besides the Wal-Marts and Home Depots? 2.Is there a suitable replacement I could use instead? 3. It seems Amazon carries it, would it be stupid to order it online? I.E. getting red flagged or put on a list or something? Although I don't care too much about those things, I'm pretty sure I'm already on every list. As long as it's not illegal where I live (in which case Amazon wouldn't ship it to me anyway) I'd probably do that as a last resort. I'd prefer to buy it with cash in person but like I said, that's a preference. I'll resort to other things if necessary lol.

[el_ronhub_bird]

Ok, I got all 3 washes done. The first wash is the creamed coffee colored one in the half gallon mason jar. The last 2 washes are combined in the vinegar jug and are a very different color from the first. I hope the color difference is due to something like tannins (or anything like that) coming out in the first wash leaving the second 2 washes a different color. I'm hoping it's from something like that instead of from my fuck-up, leaving the first wash for too long on too high of a temperature. Oh well, the show must go on! I've got quite a bit of sediment removed from the last 2 washes so I'm gonna go ahead and start reducing that overnight. The first wash I'll leave on the counter to allow more sediment to fall out. Then tomorrow I'll add it to the rest and continue reducing. I think I've gotta get more xylene but hopefully I'll at least get the defatting started tomorrow. So that's where we stand ATM

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[Phineas_Carmichael]

Looking good, Bird! Off to a great start. I'm real excited to see an ACRB extraction in real time, thank you for taking us with you on this one!

On most slow cookers (looking at you, Cröck-Pôt) the low setting puts the heating element at 200°F while high puts it at 300°F. Usually the high setting will boil water eventually, but what's in the cooking vessel with the water will affect how long it takes to come to a simmer. I've cooked overnight chili on high that was simmering after 4 hours and I've cooked 48-hour beans that never did. It's a coin-flip on high, but low will almost never simmer under normal conditions.

As far as "fuckups" go, this one is pretty mild lol. You're fine. I suspect you are correct, that the 1st hot extraction pulled more colored impurities than the 2nd & 3rd. You ever make a pot of coffee but don't want to wait for the whole pot to brew so you stick your mug under 1st & get a cup that's way way stronger than the rest of the pot? I think this is a similar phenomenon, but with drugs instead of coffee.

As for Bestine, it's just the brand name of a rubber cement thinner that is 100% heptane. Your best bet for sourcing it locally is actually arts & crafts stores (as much as I hate Høbby Löbby I'll darken their doorstep only for heptane and only if the local Michelle's doesnt carry it) or hobby shops. There's usually a few small cans in the collage/decoupage section or near the model kits. Wherever you can find rubber cement it should be nearby. It's far-and-away the most expensive common solvent though, which is why it's usually used just for re-Xing. If you wanted to get real fancy you could distill heptane (and a bunch of other interesting solvents) out of naphtha, but fractional distillation is more work than we Clandestine Chemists usually like to do...

I used to preach cash & carry purchases for all this stuff or don't use it, but have relaxed that policy over time. I think law enforcement has better things to do than police my Amazon carts. That said, if they were actively looking at me for anything I have no doubt they could get that information, but having made some pretty sketchy purchases from 3rd party sellers I'm fairly confident nothing there sets off an alarm at the local precinct.

Oh crap, Ive written another book! I'll try harder to be more concise in the future

Edited by Phineas_Carmichael, 28 September 2022 - 01:13 AM.

[el_ronhub_bird]

@Phineas_Carmichael keep them books coming and I'll keep reading them. I've gotta question, the Klean Strip Xylene I've used for past extractions doesn't have ingredients listed. Here, I'll quote what it says about ingredients: WARNING:this product can expose you to chemicals including Ethylbenzene and Cumene...if that is an ingredient list then that's a pretty strange way of phrasing it. To my point, I just re-upped on Xylene and it's a brand I've never used before. The very first thing the back label says is: CAUTIONS: CONTAINS XYLENE AND ETHYLBENZENE. So here is my question; is ethylbenzene always an ingredient in Xylene and will this new brand suffice for my purposes? I'll post about the brand and post pics of the container if more info is needed

[el_ronhub_bird]

Ok so the brand of Xylene I bought is Sunnyside. My Google research yielded one reference to Sunnyside Naptha being "unsavory." But I also came across a thread on the Nexus with several people claiming their use of Sunnyside Xylol yielded them great results. Idk, I'm gonna hold off on using this stuff for now. Fortunately I have a bit of Klean Strip Xylene left so I can at least get started on the defat. Worse case scenario I return the Sunnyside Xylol and get my money back to spend on a better brand. Oh and I ordered some Bestine online so I'm well on my way on this particular extraction adventure

[Phineas_Carmichael]

Xylene is just a benzene ring (6-membered flat ring, like a hexagon) with 2 carbons attached to it. It can also be called dimethylbenzene. There are 4 ways you can attach 2 carbons to a benzene ring:

1) Right next to each other on the ring to form ortho-xylene (or 1,2-dimethylbenzene)
2) With 1 ring member between them to form meta-xylene (or 1,3-dimethylbenzene)
3) Directly across the ring from each other to form para-xylene (or 1,4-dimethylbenzene)
4) Both on the same ring member (as an ethyl chain) to form ethylbenzene

Commercial grade xylene is always a mixture of the 1st 3 because their chemical properties are virtually identical as far as painters & varnish makers are concerned. The production method for commercial-grade xylene ensures that there will always be a small amount of ethylbenzene & cumene present, nothing to worry about. And no reason to buy pure lab-grade para-xylene at 10x the price for a defat solvent in the clandestine lab.

I checked the SDS for Sunnyside xylol, it's 60-100% xylene isomers, 10-30% ethylbenzene, and 0.1-1% cumene. Because you aren't evaporating the defat solvent the additional molecules might actually work in your favor, producing a more broadly targeting solvent blend. I think you're golden.

Edited by Phineas_Carmichael, 29 September 2022 - 02:11 AM.

[el_ronhub_bird]

@Phineas_Carmichael thanks a lot man, I appreciate you. Every time I'm getting myself into one of these extractions you're always at the ready to help me out. And I'm sure I'm not the only one. Your knowledge and the time you spend articulating it for us noobs is truly remarkable and is evidence of your passion and selflessness. I look up to you as one of my online mentors. Every little compliment you give me I take as a HUGE honor. And all the advice you've given me has led me to create exceptional products. I hope this doesn't come across as dick riding, I just want to say thank you for all you do here. For all the guidance you've provided me with. I could go on and I'm already rambling so I'll just leave it at this: thanks brother!

[el_ronhub_bird]

Should fat pulls be done heated or at room temperature?

[el_ronhub_bird]

Just to tease you guys a bit, here are a few items I intend to do extractions on in the very near future. What is shown is 250grams of Syrian Rue, 250grams of MHRB, and 250grams of Peruvianus skins. I sure am a lucky guy to have such wonderful botanicals in my possession.

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[Phineas_Carmichael]

Thank you for your kind words, Bird, it warms my heart to read them. I had some excellent mentors myself and remember well how it felt to be complimented by them, so when someone has success or does a good thing I try to make darn sure that they know I'm proud. Honestly, I just like to talk about chemistry & whole-heartedly believe that these molecules improve the quality of life for humanity as a species. So thank you for doing your part by extracting and sharing them, and also for giving me the chance to ramble about molecules occasionally.

Heated defats will accomplish the goal in fewer pulls, but one has to balance speed & efficiency with safety & detection. Xylene doesn't boil until around 140°C, so you can't boil it out of an aqueous solution, but hot xylene *STINKS* and the vapors are probably pretty carcinogenic, especially ethylbenzene. If you have a well-ventilated work space (ideally one that ventilates up through a chimney or something, not at ground level) & are far enough away from nosy neighbors who might call law enforcement because they "smell chemicals," you can go ahead and run heated defats, probably no hotter than 140°F. Running them at room temp is safer, but it'll take more pulls to get the acidic extract totally clean.

That's a mighty fine looking pile of botanicals you've got there! Makes me want to drag my gear out of the attic, for sure. But with only 1100Sqft & 5 cats I unfortunately no longer have a safe dedicated lab space. That just means I have to live vicariously through you and all the other excellent Clandestine Chemists here on Topia! Keep up the good work!

Edited by Phineas_Carmichael, 29 September 2022 - 01:57 AM.

[Phineas_Carmichael]

I checked the SDS for Sunnyside xylol, it's 60-100% xylene isomers, 10-30% ethylbenzene, and 0.1-1% cumene. Because you aren't evaporating the defat solvent the additional molecules might actually work in your favor, producing a more broadly targeting solvent blend. I think you're golden.

In re-reading I realized I should have checked the SDS for Klean-Strip as well...
The SDS for Klean-strip is exactly the same. 60-100% xylene, 10-30% ethylbenzene, and 0.1-1% cumene. The only potential difference is potential "non-hazardous" additives in the various Ronsonol products that cam cause problems. Because you're not evaporating it I'm 98% confident you're good to go with the sunnyside.

[el_ronhub_bird]

Sorry for the slow progression here, just busy plus minor hiccups with the extraction itself. So I had a problem with my sep funnel, it was apparently clogged by sediment and wouldn't drain. Anyway I fixed that. What is shown in the pics are the approximately 1500ml of ACRB vinegar juice and in the quart jar is my first fat pull. So far so good! Onward!

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[el_ronhub_bird]

After 5 or 6 fat pulls, here's what remains: on the right is my (hopefully) defatted ACRB juice. Then on the left is a jar containing the conglomeration of all fat pulls. You can see the fats sink leaving clear xylene on the top of it.

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[el_ronhub_bird]

I was having a minor problem with emulsions but adding a bit of vinegar and doing warmed pulls seems to have fixed it

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[Phineas_Carmichael]

Holy heck! Look at all that gunk you pulled out!

I was going to ask about emulsions on the defat, but it looks like you've been successfuly breaking them.

What's your plan for basification? Adding crystalline lye with stirring in an ice bath or using a concentrated NaOH solution?

Again, I'm loving seeing this extraction in real-time! Keep up the good work!

[el_ronhub_bird]

@Phineas_Carmichael that gunk all collapsed down to a much smaller volume when I ran it through the sep funnel. As far as basifying I hadn't really concocted a plan yet. I guess by default I would do it the way I have before: slowly adding lye to water to make a solution then slowly adding that to the ACRB juice. Unless you had something new to try, I'd certainly do that. I have one question right now: would it be alright to reduce the bark juice at this point before basing? It would be a bit more convenient to handle and process it if it were reduced a bit. But if that's inadvisable, I can just keep going along like I have been. Thanks guys!

[Phineas_Carmichael]

As long as the pH is below 6ish you can reduce further without damaging the target molecule, and definitely should if you'll be increasing the volume again by basifying with a solution. Ideally you want to get it down to where the whole amount will fit in your sep funnel with enough space for solvent pulls. Some people reduce down so far that the aqueous extract takes on a syrupy consistency, just watch (& follow your nose) for scorching as it gets near that point; it will thin out again when you add the NaOH solution.

My buddy Freddie always based with a solution so that sounds like a good plan to me. 40g/L of will get you a pH 14 NaOH solution, some folks go as high as 60g/L but any more than that is just a waste of lye really.

Getting on to the home stretch now, keep up the excellent work!