Thanks again entropymaster! I suspected as much... And thanks for the recrystallization 101. Sounds simple enough. So I'll hunt down some bestine/heptane (doesn't Coleman's contain a significant quantity of heptane? I guess it has to be pure, like all good things...). Question: would I be better off just switching to bestine/heptane as a primary solvent (assuming I can find it in Canada)? Now that I have been directed to the nursery I will brush up on my chemistry and write a couple of tryp (sic) reports and extraction/precip/recrystallization follow-ups with the view to graduating to: whatever's after the nursery! Then I'll be able to contribute to some of the fascinating threads I have been eavesdropping on... I'm itching, I'll be honest!
cheers,
JBA

Yeah, most naphtha contains a good amount of heptane... pure heptane is ideal for recrystallizing, but any clean naphtha will do.

For extracting, clean naphtha works just fine and is a whole lot cheaper than heptane. Most people only use heptane to recrystallize for that reason.

how do I get a hold of clean naptha then?

Buy a kind that isn't Coleman fuel. Evaporate a portion of it to see if it leaves a residue. If it does, chuck it. If it doesn't, it's clean.

I'm not familiar with what brands are good in canada, but I'm sure you can find that info on this site if you look. Or maybe a canadian can chime in and let you know what brands are good.

Yeah, shellite as far as I know isn't available here - nor are any of the brands I have come across on this site (any Canadians want to chime in and correct me?) I'll poke around and see what I can dig up. Thanks,
JBA

After much research I tracked down some Bestine (aka Best Test). Apparently the ministry of health and welfare canada have temporarily prohibited the sale of it here, so all the major centers don't sell it. Strangely, they carry it, but won't SELL it until they get the new health and welfare approved stickers! They have stockpiles of it, but won't let it out the door! I managed to find a tiny blueprinting store that sells it (probably off the government warning radar - they probably aren't aware they are selling it illegally (although maybe they are...)) I will pick some up this afternoon.
cheers,
JBA

Quick update and question:

located and bought some bestine; evaporated my 2 quantities (mason jars transferred to Pyrex dishes) to a third of original volume and placed in a freezer at -18 C. What I have read here is that I should wait 72 hours after placing in a freezer - is this necessary if the freezer is significantly colder than a standard fridge freezer? I need to clean and recrystallize after, and I have a window of opportunity (I will be alone) for the next three days and while a patient man, would love to finish and try my spice before this time elapses...
Any thoughts?
cheers
JBA

If in a hurry, freeze for 12-24 hours and strain, saving the bestine for when you have more time, and just recrystalize what you get at first. Working with naptha, since she just repeats pulls with the same solvent, SWIM's typical freezing time would be about 16 hours.

Update: After 24 hrs at -18 C there were some very small crystals visible in each Pyrex dish, and now after 36 hrs it seems to have stabilized, or is precipitating extremely slowly. I initially used 133G pre-powdered MHRB, and at the purported 0.57% this quantity should yield an average of about 750 mg of spice. Granted its hard to eyeball, but what I have doesn't look anywhere close to this. Should I have evaporated more before freezing (I got down to 1/3 of original quantity)? Should I cull what I have and evaporate some more and refreeze? Should I endeavour to pull again from the basified liquid? and mix longer? Also, there is a small floating green oily spot in each of the pyrex dishes that doesn't look unlike a drop of olive oil. I went through three defatting phases following QT's tech, despite reading a consensus that MHRB doesn't need it (I like to follow techs/recipes/instructions to the letter for the first time - makes troubleshooting easier). So what are these yellow/green droplets and are they normal?
Any advice to help salvage my yield on this batch or allay my fears would be greatly appreciated (I have kept everything except the MHRB once it was filtered out...). It's been a lot of work (outdated and complex tech...) and while I am grateful that i have some spice snowing out of solvent, I want to make sure I maximize my yield before chucking anything (as well as honing my skills and acknowledging my errors for next time!)
thanks,
JBA

Hey JBA -
Cannot comment on the green oily spot, perhaps if you shared a picture that might help. With the time constraints you mentioned earlier, perhaps culling the product you do have and then pulling again with your naptha would reward the most?

Newbie question: how do I attach photos? When I checked the attach files box I expected a dialogue box to select source for images, but got nothing...
cheers,
JBA

Newbie question: how do I attach photos? When I checked the attach files box I expected a dialogue box to select source for images, but got nothing...
cheers,
JBA

oops, guess I figured it out... the first one (if you've been following this thread) is my acid extraction; #2 is filtering the MHRB out of the acidic solution; #3 is the bubbly non-separating basified "juice" that was what initiated this thread; #4 is my successful separation (after help from all of you!);#5 is the naptha collected from the jars (which hopefully contains the spice of my labours!; #6 and on are the shots of the freezing pecipitate and the little oily spot in question (in response to ragabr's response to my question; I also included a shot in this post of a little cocktail: I kept my 5th pull separate and am evaporating to see if anything is there and to see what evaporated spice looks like in comparison to precipitate; it should also tell me if a 6th pull is warranted...
thanks again (and sorry for the newbie multiple posts...)
JBA

sorry, photos loaded out of order as well... Newbie, newbie, newbie! Anyway, they should be sort of self explanatory.

Here are the 2 pyrex dishes (drip drying upside down)with my first pull out of the Coleman's. I guess there was more than I thought! I don't have a sensitive enough scale to know how much I'll have, though... I guess I'll look around on e-bay unless anyone has any suggestions (or recommendations for brand). The shop where I buy my MHRB (and spores!)has a "my weigh" scale, but its over two hundred bucks...
I have kept the solvent and will evaporate a little more and refreeze to see if I got it all (I left it in the freezer for 46 hours). I removed the green oily drop when I decanted the solvent (see previous posts and photos). Curious that it was yellowish/green coming from MHRB. Anyone know what that could be?
cheers,
JBA

Very nice whiteness!! o_O The oily spot looks very much like SWIM's pulls when she uses heated naptha. Here's a couple pictures of the product, think it looks more powdering than yours since she didn't re-x. If you wanted extra assurance, and you hadn't already done so, you could dissolve the oil spot in some solvent, wash with sodium carbonate and dry it out again.

Surprisingly, these shots are before recrystallization! And theyre already crystals. Given that it's so white should i bother with the re-x? Incidentally, the fifth pull that i evaporated is now a pile of blue gunk. Somehow the precip seems to have (at least partially) purified the spice. Should bestine the whie spice?

SWIM feels very hesitant providing advice on the white spice. She just doesn't know enough about the initial solvent used.

I guess i'll recrystallize using the bestine just in case , unless someone else pipes up and tells me i don't need to. I am looking forward to checking out your photos ragabr - my phone won't open them. Thanks again. It's really exciting and somewhat magical to see those crystals finally!!
Jba

Ragabr - I thought it was my phone, but even on my desktop my browser says it can't find the server...

jbark - sorry! I continue having trouble linking within the nexus :S

I believe I fixed it.