This is the 1st time I post, so my apologies if I am posting in the wrong place/way. I am a self-professed newbie having a lot of problems separating Naptha. I have read extensively on this site from the FAQ & troubleshooting sections to forum posts concerning separation « anxiety » (couldn’t resist…) I am using « QT’s Extraction for students » (from erowid - I know, I know, but I am already in neck deep and just want to get out so I can start a simpler tech…), with muriatic acid, naptha (Coleman camp fuel) for a solvent and NaOH (lye acquired in a soap-making shop) as a base. I used 133 g pre-powdered MHRB split into 4 large mason jars.
Followed the tech as closely as possible (but a vague tech leads to vague technique…). Here is an abreviated version of my lab notes (sorry for the length and the details, but I really have no idea where I went wrong):

Day 1 acidified demineralized water to ph 2. Poured to cover MHRB in 4 jars and shook till mixed. Heated under 50 degrees C (122F) then let sit.
Day 2 48 hours later – filtered all through coffee filters 2 X.

Repeated day 1 & 2 twice more then discarded MHRB.

Day 7 defatted with about 100 ml naptha in each jar. Shook vigorously for 20 mins.
Day 8 24 hours later : removed naptha and pink cloudy guck. Filtered through coffee filters 2 X (still some mhrb residue.)

Repeated day 7 & 8 twice more. No more visible MHRB residue.

Day 13 Mixed NaOH to ph 12 in tap water (ran out of demineralized water – is this where I went wrong ?) This is where things get a little sloppy; Added teaspoon after teaspoon of base to defatted jars (tech called for about 10, but when I got to 30 in each jar (containing an extraction from an initial 33g MHRB in each) there was still no heat or change of colour or consistency. I added 2 tsp NaOH to my remaining (approx) 500ml of base. And added tsp after tsp – at 8 a reaction started (grey to black sludge, but curiously no temperature change…) and by 12 tsp I reached target ph (11 in my case – although very difficult to tell ph differences between 10 and 13 : green grey to grey green to grey, so I can’t really be sure of the exact ph…) Oh yeah, shook vigorously all the while (what can I say – I’m a noob! I won’t shake next time I promise…)

Day 14 Now things get strange: 24 hours later and the mixture seems to have separated into 3 distinct layers : a 2mm band of burgundy liquid sandwiched between two layers of grey sludge ! I remixed (this time by slowly overending jars for 10 mins each to avoid bubbles & emulsion…) then let sit for 48 hrs.

Day 15 Same 3 layers. Following the troubleshooting guide on this site, I added 25 ml naptha & remixed slowly and waited 5 hours . No change. Added 4 tsp of same NaOH preparation as before.

Day 16 24 hrs later. Some change : mixture has now separated into 2 layers -
the liquid has settled to deep burgundy (a grey silt like sediment has accumulated on the bottom) and the solvent has sort of separated into a distinct layer, although seems to be emulsified if I understand the term correctly (bubbles, not translucent and pinkish in colour). There is however, a thin film of clear solvent on the top (roughly ½ mm…). Added 5 tsp of NaOH mixture, mixed end over end, put in warm water, cooled and waited :

Day 17 no change… Added 2 tsp of salt into one jar as a test, then overended to mix (curiously, it thickened up, turned to black sludge and despite my efforts to the contrary, formed thick bubbles on the surface). 10 hours later, full circle : a thin burgundy layer sandwiched between 2 thick grey layers !

At a loss as to what to do next… only thing i haven’t tried is filtering through cotton. Doesn’t sound like it’ll work and I am dreading it, but if I’m told to, I’ll buckle up and hit it. Current status is 3 jars in 2 lyers as per day 16 and one in grey sandwich hell as per day 17.
I can send pictures if it’ll help, but my camera battery is charging at the moment. I have 2 (obvious) questions : What did I do wrong and what do I do next? thanks in advance, guys.

forgot to mention : NaCL added was iodized table salt...

Did the water ever turn opaque black when you add lye? If not, add more lye. Hell, add some more lye anyway. Also add a load of rock salt and some more water.

Also, Coleman fuel has a toxic antirust additive, so you'll need to recrystallize at least twice with a clean solvent after you get your spice... and definitely don't collect the spice by evaporation, do a freeze precip.

Water turned opaque gray and sludgy... never really black though. You think even more lye? To the one I added salt to, the others, or to all four of them? I was wondering how I came full circle with the salt one... This morning the 3 layers are still there, although the middle burgundy one is now about 2-3cm (1 inch) thick.

add more lye, definitely

Yes, MORE LYE!!!

Seriously, I basify the crap outta my extractions. Dont ask me how many grams of lye to bark, cuz I don't know. I just dump a ton of lye into my acidified mhrb solution. I use so much lye that even though I shake the hell out of my wine jug, any emulsion clears in under 10 minutes. It's a beautiful beautiful thing and makes extracting so much easier. As entropymancer said, your water should be opaque black. It's so black that it will visibly darken from that dark, deep purple it starts as.

peace
SB

More lye it is then!! What should I do to the jar I added salt to? Same thing? Lye, lye, lye till the truth will out...
thanks, I'll keep you posted.
JBA

Added some fresh mixed lye, and one of the jars separated (although the other 2 were only part way there). Added more lye to all jars (including salted one) and am going to wait and see. I am more hopeful now though. thanks again and I'll keep you all posted.
cheers,
jba

You want a jet black mixture that you can shake the crap out of without foam forming on the surface before you add your solvent, then you can't go wrong.

Jet black... it seems to be separating now, but the bottom liquid is still a dark burgundy. I guess I'll add even more. Wow was I way off!! Time to switch techs (and to pay more attention!)
JBA

Yeah, QT's tek is absolutely awful. I've told erowid that if they don't want to take it down, they should at least put a warning at the top; it's been the downfall of many first-time extractors.

The bottom layer is the mimosa-lye-water... if it's still burgundy, you probably need to keep adding more lye.

yeah - it's still burgundy (VERY dark, though). The separation looks clean, although there seems to be less solvent than what I put in. Any suggestions for a second timer's tech, preferably shorter than QT - but I don't mind the labour if it's a longer one that works. For now I'll add more base and try and get it black, then (hopefully) skim the solvent off and move on to the next step. Should I freeze precip? How many pulls should I do? I was planning 5...
thanks,
JBA

There's a lot of good extraction teks out there, and they're pretty much all shorter than QT's. Rather than taking a week or two, most of the current teks can be completed in a day or two. Check out the extraction teks section of the Nexus wiki and see which teks suit you. There's even some teks that only require foodsafe chemicals.

Five pulls should be plenty; chances are you'll have pulled the majority of the spice in the first three.

Definitely freeze-precip. Like I said earlier, Coleman camp fuel has an antirust compound that will end up in your DMT turning it blue or green... you don't want that! If very little DMT precipitates in the freezer, evaporate the solvent to about 1/3 of the original volume and then put it back in the freezer. Even with freeze-precipitation though, I'd still strongly recommend you recrystallize the DMT at least once or twice with a clean solvent (like bestine) after you initially collect it.

So now the layers are separating quite fast - about 15 mins! I have been remixing a couple of times (necessary?) just to make sure its pulling its quota, but was wondering if there is a correlation between the amount of time separating and yield per pull. Thanks again everyone, and thanks entropymancer for the heads up about Coleman's... I had read that elsewhere as well, and I will hunt down a recrystallize tech once I have freeze precipped and gathered the spice.
cheers,
JBA

Sorry to repost, but I think I posted when most were asleep, so I'll try again (but maybe I was just being ignored! :~} . If i am breaking any forum guidelines, just let me know. Thanks:

So now the layers are separating quite fast - about 15 mins! I have been remixing a couple of times (necessary?) just to make sure its pulling its quota, but was wondering if there is a correlation between the amount of time separating and yield per pull. Thanks again everyone, and thanks entropymancer for the heads up about Coleman's... I had read that elsewhere as well, and I will hunt down a recrystallize tech once I have freeze precipped and gathered the spice.
cheers,
JBA

SWIM says she hasn't noticed a correlation between the amount of time separating (after stirring, whatever is done) and yield. She has noticed a *huge* relationship between amount of time stirring and yield.

Thanks for the reply ragabr. For stirring I turn end over end briskly but not vigorously 100 times, wait 5-10 mins, then repeat once; I hope that's enough! I am also about to cull my fifth pull, so hopefully I'll have got everything! Any recommendations for a precip/recrystallization tech? I have perused the nexus tech section, but noman's and lazy man's and the tech in the DMT handbook all seem a little vague and hard to apply to my situation... (for example, one thing I am told I will need to separate in a purification is the rust proofing blue gunk in Colemean's. If I use Coleman's solvent to purify, presumably it won't remove the blue that the original Coleman's imparted to my spice... (or will it? my chemistry knowledge is of an educated layman, but no better, so i might be completely wrong.))

On another topic, which are the nursery forums where a newbie like me can post? Is there a list or do I need to go to each topic and look at the bottom to see whether I can post or not? And when (and how) do I graduate from the nursery? I am very patient, just wondering as I haven't been able to track this info down on the site. Thanks again for being a great resource and a friendly community!
cheers,
JBA

SWIM has never tried recrystalization; perhaps Phlux's guide for mescaline would help?

The list of nursery forums appears at the bottom, of the Forum main page, right above "Active Discussions".

Best of luck with everything!

Thanks again ragbr - found the nursery and the lists of topics!
Can anyone else answer the other questions in my previous post?
cheers,
JBA

No, you can't use colemans for recrystallizing, that defeats the purpose. You need a clean solvent... heptane is best (at least in the US it's sold as Bestine, I don't know about Canada).

I'm sure you could find some recrystallization teks and pictorials if you search the site (or even search through google). I'm not really familiar with any because it's such a simple process: Dissolve the spice in a minimal amount of hot solvent (heated safely, away from spark sources), pipette out any gunk that doesn't dissolve, and cool the solution slowly. Voila, cleaner crystals precipitate. Maybe someone else could help you out with a link to a particular tek or pictorial.

You graduate from the nursery whenever the mods see fit. In general, they look for good contributions and thoughtful discussion