Hello. As a first time extractor I am struggling a bit. Maybe just too many variables at this point but maybe someone can offer me some insight.

First try: 50g MHRB powder and un-named solvent whose msds reads: "Solvent Naphtha Heavy Aromatic 95%/Med Aliphatic 5%". Its a clear yellow liquid. I start with Noman's Tek. I kept the solvent in a warm crockpot bath win between mixes and pulls. Pulls are slightly cloudy but not too much, more clear. Sometimes the gaps were substantial (like an hour or so). Nevertheless, it all seems to go well, bit tricky after the freezer as the first filter paper I tried was too dense, naphtha pooled. Quickly changed to cooking oil filter and the naphtha went through. After drying everything I got about .38g crystals - white, tinged with yellow and some golden brown goo. OK. Not too bad I think. Lost a bit in the filters and probably re-dissolving in solvent etc. Coulda been more dilligent and careful. But maybe I can get more yield?

(Not sure how to attach pics but if successful -> pics 1-11)

Try #2: Cyb's Max Ion Tek. Same MHRB, but now a different solvent. Another name product whose MSDS says exactly the same as before. Except its clear, not yellow. Didn't think too much of that. But now I follow the tek and I'm not too sure about how much to heat the bottle of basified. I read that maybe too much heat is pulling too much other stuff and hence the color/goo. OK so just heat the solvent this time. From very first pull it is very cloudy opaque yellow? Haven't seen this before. Maybe its the salt? No worries, I continue with this. Until I pull the jars out of the freezer. They're frozen! Not very hard though. When I open the jar I cant pour anything off. Its solid to slushy?! I put it back and wait another day and a half. Same thing. As it melts I see soupy white stuff floating around inside. like satuated dumpling dough. I try to pour it through a filter, it all goes through. The dumpling lookiung stuff too. Its gone back into the soupy liquid solvent. The little stuff that remains on the bottom of the jars liquified within a minute or three. No use in front of the fan it just liquified. Now what? Well, try evaporation. That took forever. Days and days. The opaque fluid became clear in about an hour but in the end there is just thick yellow oil. Out of six pulls. Most disappointing. I put it down to the naphtha not necessarily being what the MSDS said it was. Oh well, I'll figure out later what to do with the oil.

(Pics 12-14)

I get some lighter fluid to use as the solvent and start again with Cyb Max Ion and another 50g MHRB. This time the pulls aren't cloudy at all. No heating of the basified, just the solvent. Do six pulls and into the freezer in dishes this time. Now this works a lot better than last time but there's much less yield - about .2g but much more yellow than via Noman's on my first attempt. WTF? Cyb's is supposed to give more yield than Noman? Okay, must be me again. The thing is, this time it was easier to decant the solvent and dry what crystals there were. Pretty much like the pics I see how but just not so much crystal. Well, better than last time but way worse than first time.

(Pics 15-16)

Maybe there's still some left in the basified that the lighter fluid didn't pull? Did 2 x 50ml of my yellow heavy Naptha. Again it's extremely cloudy. But slowly cooled and in a jar and into the freezer. Two days. I pull it out and joy! There's all sorts of white stuff floating in it like the first time! I decant, but this time only had a coffee filter. Its too dense and most of the stuff evaporates in front of me back into solvent liquid and that into the filter. Oh well, there's a nice layer of white on the bottom (last pic - moments before it melted). I rush to get the fan going but no go, it melts and becomes a milky solvent mess again. I put all solvent I can gather, heat and soak the filter with fresh hot solvent in hopes of leaching whatever's in there and put it all into a dish rather than bottle this time. Its evaporating now to reduce a bit and then it'll go back into the freezer. I know there's spice in there! Hopefully I'll get it.

tl,dr;

My heavy "naphtha" solvent seems to be far more successful at pulling than the lighter fluid. But the last phase of out the freezer is just failing badly. There is no time to get dry crystals. It all liquifies very fast. And if I evaporate, well, then I get yellow oil.

I don't really know what to do about this? I have some other solvents to try but then I'm introducing even more forks and variables. If the heavy naphtha evaporated like the lighter fluid it would be perfect it seems. Maybe its just not compatible with Cyb's tek and I should go back to Noman? That wasn't perfect but it wasn't this milky solvent and it was easier to filter at least the bulk of spice obtained. Or do I try other solvents and stick with Cyb's tek?

I'm really unsure about how to proceed from here. I still have some MHRB and willing to fail more if I learn along the way, but maybe someone has some pointers or can point to some issues? I know theres not a lot of detail as I don't want to make this sooo long!

Right now I'm hoping the spice sticks to the dish better than the bottle. And if successfull I will mine the basified for more.

But maybe I should use some process like mini-a/b on the cloudy naphtha and then re-pull with the lighter one?

Anyone?

tia

Hey mate.
About the first one. You could also evaporate about 50% of your solvent before freezing. And when the floor is covered with crystals you simply let the rest evaporate. If your solvent is fine with an evaporation test before the extraction. ..It will leave nothing behind.

Did you do an evap.test with the second solvent?
Could also be that some of your lye-bark mix came across. You can clean your yield with a sodium carbonate wash. It's explained in the Noman's Tek

https://wiki.dmt-nexus.me/Noman%27s_tek




Cheers mate

Yes, evaporation tests were done. All good, just took forever (over two days) for around a teaspoonfull to evaporate!

I did evaporate 50% before freezing. Its after freezing and decanting where everything gets lost. Whatever is floating around in the jar just disappears. The solvent does not clear and redissolves the crystals. Did it twice to see if I could do it faster. But it seems to be the solvent's propensity to hang around that is the problem with that. Even after being upside down over 24hrs its still exactly the same. Back to liquid with a couple of minutes. Hence the resort to full evaporation.

I have never got to any crystals via evaporation. Never. Always oil. Even the goo, which hardened, only came from scraping the jars I used the very first time and from which I got some crystals.

The cloudy versions go clear again at some point and if evaporated they will always end up as yellow oil. They didn't precipitate anything. The only time there were crystals was the very first time, and then after using lighter fluid as a solvent. Just not as much with the lighter fluid.

At the moment I have two pulls done (after the 6 lighter fluid pulls on same basified) with the original solvent which again came out v cloudy. It is evaporating (very very slowly even with fan) and has gone clear yellow again.

I don't think there has been any lye brought in. I have been very careful with that, decanting three times to leave behind any darker stuff and erring on the side of caution.

Will 'cleaning' make it more likely to crystallise or is that something different. My big problem now is that anything that appears in the freezer disappears into liquid almost immediately and certainly cannot be fan dried at all. I thought this had a lot to do with the solvent hanging around. It didn't happen with the lighter fuel which evaporates very fast. In that case it went just as per cyb's tek and crystals were the result.

Maybe there is a method to first extract the spice into this solvent, then remove it again, then extract it a second time with the lighter fluid to get the benefit of the higher yield from the solvent? Is this a backsalt or mini-a/b? Is that thinking sensible?

In terms of colour I would read this thread

The reason you are being left with goo after evaporating could be because it is becoming oxidised during the process. This is why freeze precipitation is preferred.

I say don't overcomplicate it too much and stick with lighter distillates, as heavy naphtha does not aid in freeze precipitation and is a nightmare to evaporate. Make sure to check the MSDS of your lighter fluid too.

Good luck!

I am in a similar situation.
New to extracting and using cybs salt tek. The freezer part is the most difficult for me as I see crystals begining to form on the glass pans and dissolve/become invisible when i am taking it out of the freezer and the naphtha is moving around some. my last two pulls I am splitting the naptha into 2 glass pans so its a thinner layer of naphtha and perhaps will let the crystals form better, and hopefully make it easier to remove the naphtha as well. Before it looks like theres all kinds of stuff going away with the naphtha thats is being poured out. Ive been getting about 50/50 crystals on top of an oily layer.

gonna be reading through a lot of stuff on the site in the weeks to come in hopes to getting better results.

good luck!

Hi guys sorry if this is not the right place to post this
I was wondering if anyone has tried using CLIPPER lighter fluid instead of naphtha as the non polar solvent? I did an evap rest with a few drops and there is no oily residue but u can see the spot that it evaped from, anyone know if this would be okay to use ?

Heavy naphtha is ok if it's aliphatic, although medium naphtha is preferable. Aromatics hinder freeze precipitation, and heavy naphtha, as observed, takes ages to evaporate. I'd recommend recrystallising from light naphtha or heptane if heavy or medium naphtha was used for freeze precipitation.


Clipper? Sounds like it leaves a residue, some brands contain rust prevention agents. It's technically possible to clean these up by distilling them straight out of the can, but you'd need to know what you're doing before attempting that. Mistakes could lead to injury/death/legal trouble.

UPDATE:

Somewhat later. I had to take a break from my chemistry work and have recently come back to it. Things have been going a little bit better now but I am still having the same issues, namely solvents, and getting the crystals out of the solvent before they seem to disappear back in again and re-emerge as goo weeks later.

My very first extract (see yellow naphtha bit above) yielded distinct crystals and powder. Just not much. 280-300mg from 50g. Seemed okay, but when I tried to re-x with n-Heptane (wanted to be pro out of the box) I never saw it again! Gone spice. gone Heptane. (swore never to clean again) Next try I used my 'clear heavy naphtha' cos no-one else's pics showed yellow 'naphtha'. And Max Ion Tek (greedy - want more yield). Another 50g MHRB. Heat bath, heating solvent, everything cloudy etc looks brilliant. Im so positive. And then disaster in the freezer. Its frozen! Naptha doesnt freeze! This one just did. No way decanting did anything good and all became liquid again very fast. Dejected, I evaporated yet again. Yellow oil and goo. A lot! Damn, I have a bunch of that now.

3 more 50g tries (all Max Ion), same new MHRB shipment. After try #1 I rejected the 3rd solvent (also clear heavy 'naphtha' from another source) I was using as it half froze by itself in the freezer. Definitely that was the cause of the 'slush puppy' issue. Evaporated - browny yellow oily grunge. OK, dissolved in IPA as it was as 'dry' as it was going to get. Maybe for leaf later?

OK. Next, #2 - Used Newton lighter fluid as solvent 6 pulls no heat bath - nothing precipitated. Evaporated - still nothing nothing!

Using the same salted/basified mixture, I tried 3 other 'heavy aliphatic naphtha's". Nothing, not even goo on evaporation.

Pretty much failure from my point of view. Granted I haven't tried anything with the goo, but that's not what I'm trying to achieve right now, which is getting what everyone else is getting.

Now I'm doubting the MHRB. Its new, not what I used "successfully" before but it came all the way from source. Direct from an individual, not a store, and it cost a lot. Especially the shipping. I found him through Google Google/Translate and he seemed like a really nice guy! We whatsapped. How could it be bad? It just had to be something else, Right? (Denial?)

Starting to lose hope now, source mullein, thinking of just doing the goo/leaf thang. But it seemed like I was too close to ditch now. So,I started again and to minimise the variables I went back to what I did first. Except this time I promised to be satisfied with my yellowy white powder (if I got some again) and no more cleaning etc:

1. Same MHRB powder, Noman's Tek not Max Ion (but I did the freezer bit since that didn't involve chess and shouldn't hurt), same yellow 'naphtha I used to get my original 300 odd mg of ever so slightly yellow crystals/powder.

2. I heat bathed the basified all night, heated the solvent all the time and kept the whole thing warm...I shook and rested, much longer times.

3. I got one naphtha pull out and bottled. I shook the bottle new 50ml added. The bottle slipped and... basified mess all over the kitchen. @#$!

4. Put the first pull in the freezer anyway.

Forgot it was in there and after four days (work intervened) I saw my little pull in the freezer. I gently picked it up and SNOW GLOBE! More than I had ever seen before! Wow. I put it back and got filters - coffee, whatman, cooking oil. Decanted through whitman but it didn't let naphtha through. Tried others and rushing now finally managed to get some powder before it all went liquid again. But when the powder was dry after a few days and I couldn't smell naphtha there was almost 700mg. One pull. The bark was good! I knew he was a good guy! Awesome.

Now I'm going again, same thing, but skipping the drop-the-schott-bottle-step. Other than my heavy yellow naphtha (of which only 500ml left and no way to re-source) I hope to get some more crystals. The difference between ones I saw in the snow globe vs what got rescued was huge. There is obviously a lot of spice in this MHRB for sure.

later:

Still the freeze precip to dry crystals is the stumbling block. Its not working. I did 6 pulls but I am losing more than half of it back into 'naphtha'. BUT I have already 1.1g DRY after four days. And a lot disappeared into filter papers etc.

I really don't want to evaporate the naphtha I rescued (decanted) because 'Im pretty sure I know that will make goo.

So what now? I still have a solvent problem. The naphtha works, but is limited and problematic at the end. What else can I use? Lab chems all obtainable, PE, -anes, etc. - its just that 'naphtha' is not a name anyone knows in this country (even though it appears in MSDS and CAS numbers) How the hek do I get all those crystal clumps I see out of the yellow slush puppy snow globe as it comes out the freezer and into the plate dry like the ones I got. Am I too greedy? I really feel I am losing more than half. It sure looks that way.

Things I did different I will do again: Take my time. Soak, shake, settle, keep it warm, one pull a day max. Lots of shake and settle. Also, leave in freezer more than 3 days. After peeping every day I saw a HUGE difference in crystally cloud on fourth day. Seriously huge.

I am now the proud owner of total 1.4g yellow tinged spice and a whole lot of goo.

BUT

How can I get this thing better? I think its all in the solvent for me - high BoilPoint or low or mix or this or that? Can anyone help (who managed to read all this) - I am a total noob at this chemistry thing but I really think I'm pretty close to my goal of getting the max out of what I got...

Anyone?

Thanx

PS here a couple pics of current status from two pulls of 50ml naptha: not to shabby right? But seemed like more than that got lost on the way

Hey Merkin -

First let me say that I am new here and have never used plant matter for extractions before. But I have done extractions and have used the same chems and tek folks around here use. Still, consider carefully before following any of my advice.

One thing I can offer that I know will help you out is to do filtration throught a 1000ml flask (sound about right for the pulls you're doing?) and a Buchner filter & hand pump to go with it *and* use the #5 Quality filter paper. Your product will be cleaner , filter faster and much less likely to join back up with your solvent when filtering. They aren't really expensive. Looks like you probably already have the flask. My flask has an arm where the hand pump attaches but you can use a regular flask - just make sure you get a Buchner funnel that has an arm attached to it for the suction.

I should probably shut up at this point but I'll live dangerously... Naptha is a really shitty solvent - except when it's hot. The A/B tek around here turns what would otherwise be a shortcoming into an advantage. You extract hot and as soon as it starts cooling down, you get the precipitate. The best of both worlds as long as you know the limitations. Even reading DMT threads on other websites, I hear comments like "Use naptha in your zippo. Use toluene in your extractions." and "Naptha is only good if you want to use it to extract junk from your acid solution prior to making it basic". Nobody around here crabs too much about it but there is a healthy amount of debate on the efficacy of NAPTHA in A/B in general and even in the DMT-related world.

I'll stop here before I get clobbered by a more experienced user. I really don't know the answer for these type of extractions. And by "these types" I not only mean plant matter, I'm also talking about the fact that your end product is a freebase rather than a salt which is still making my head spin.

Best of luck.

Okay, well I think I have the solvent thang sorted now. My issues were definitely related to this aspect of the process. I have 'sacrificed'* about 400g of MHRB in testing various options (50g per shot) and am now able to get a consistent result of slightly yellow crystals around 1.5%-1.8% using Cyb Max Ion tek. The best for me has been a mix of Petroleum Ether 60-80+80-100+100-120, equally mixed. Adding in the 30-60 or 40-60 really doesn't seem to add much to the party. I have not 'washed' or re-x'ed anything lately for fear of losing it all but I will sample before deciding if that's at all necessary.

For the first time I got a dish-full of those little shardy clumps like so many of the pics I've seen here. Chalk up almost all my hassles to one basic thing: the damn confusion about this thing called "naphtha" and what name its known by everywhere other than in the USA!

Quite coincidentally I recently met and chatted to a chemistry teacher at a braai (bbq) and mentioned my confusion about "naphtha" (carefully avoiding any why's) and he laughed and said very simply that here it's called 'Benzine' or 'Cleaning Benzine' and the "heavy" naphtha is called 'Mineral Turpentine' (aka paint brush cleaner). Sure enough on checking MSDS's of some common brands he seems to be spot on. As these are hardware store items I grabbed two brands of Benzine which list on MSDS:
Brand #1: "Solvent naphtha (petroleum), light aliph. 85% 64742-89-8, n-hexane 15% 110-54-3"
Brand #2: "n-Hexane, Heptane, Pentane, n-Butane" but does not list percentages

I think it's worth sacrificing another 50gx2 to compare yields - main reason: they are a LOT cheaper than the Petroleum Ether (Chem Supply co). Then I can decide on the way forward and which solvent(s) I will use in future.

All in all its been quite a frustrating and confusing (but ultimately satisfying) learning experience and now that the fog is clearing somewhat I have more than enough spice to move on to the next phase. Especially since my GVG recently arrived safely all the way from the US My end results have varied from slightly tinted white, to light yellow to crunchy orange (plus of course a bunch of oily goo!) All waiting patiently in their own little polytops. I look forward to sampling them all.

Oh, and one tip for beginners: a 25ml pipette with a red plastic "pi-pump" on top is far and away the best method to extract the solvent layer. No question. Definitely no turkey baster (totally useless!) and syringes (better but solvent damages rubber - I went through over 40 x 20ml syringes!). That setup should be listed as an essential tool and I'm not sure why not - it's a no-brainer! I guess glass pipettes might not be easily obtainable elsewhere? But they're really cheap and so is the pump.

Lesson: The right solvent = smooth, simple ride. Not quite the right one = much confusion, weird results, disappointment and desperate begging posts!

Thanks everyone who gave me useful advice directly and all those nexian threads my head is still spinning with...

---
*Although tbh, getting just under a g out of 50g powder can't really be called a 'sacrifice' now, can it?

Thanks mikeAtHome - you're right, I do have a buchner funnel (with a tap aspirator). Never used it before but I defintely will now. The last few extractions I did have not had that same problem I had with the "heavy" naphtha, it all decanted perfectly - and the spice stuck to evap dish as desired and wasn't in suspension so I didn't need any filters! Solve one thing, other issues disappear... I'm kinda new to this all but really keen to learn how that thing works youtube here we come...

As a non-chemistry person I really love the aesthetic of lab glassware. It's made so precisely, is so delicate and yet so practical and looks really beautiful. I bought a philips beaker (I have absolutely no idea what its used for) just for its looks! And I am totally in love with Schott You-tility bottles. Exquisite! I have always loved their lab bottles - and the way they all have the same cap size - (my kitchen is full of them since I hate plastic) but with this product their designers hit it out the park! Who woulda thunk it

OK, through many experimental extractions later and with over a kilo of bark expended on trials, I have tried all sorts of available solvents and I am pretty happy with the following. I am posting now to give this thread a definite conclusion and also in case there are any of my fellow countrymen (Saffas) who may have the same problem. These solvents work pretty much equally well and are all easily and locally available:

For freeze precipitation:
1. Zippo (Black) and or Newport Lighter Fluid - most expensive, not necessary imo
2. nHeptane, Hexane, Pentane 1-1-1 mix. Works well. Moderate price, lab supply stores. The mix works about 20% better than any one component by itself.
3. Benzine ( "Benzine for Cleaning" ) with an "i" not an "e" - by far the cheapest, easily available and works well. I reckon this is the closest to vm&p naphtha if not the same? Just evap test different brands before using).
4. Petroleum Ether (mix of 30-120°BP) - relatively expensive (to make a 30-120 mix you need to buy 4 different bottles (30-60,60-80,80-100,100-120)! Least offensive smell but not as good (only minutely though). Evaporates fast and super clean. Not worth the cost imo.

All will deliver pretty much exactly the same yields and very clean freeze precip results (slight yellow tint) if you watch the heating temps. The easiest - Benzine from your local hardware store. Start here. Brands vary though so evap test essential.

RE-X:
nHeptane (quite easily available here) no question.

FASA:
Toluene and Xylene AR Grade easily available for FASA pulls and final pull on all extractions.

AVOID:
White Spirits, Parafin -- crap to zero results.

UNTRIED ??
d-Limonene - kinda rare and quite expensive compared to all of the above.
"Genuine" Turpentine -- Couldnt find a conclusion to using this as per phlux's thread on nexus, and many dissenting posts so didn't go there. Bought a bottle though so maybe I will try sometime.
"Mineral" Turpentine -- Not too keen to try. But who knows...


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