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[UPDATE]Found these pics of a freeze-precip--w/big crystals!

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coAsTal

coAsTal

Rising Star
So I thought I'd post them and ask some questions based off of them. [img:db99c12647]http://img264.imageshack.us/img264/4700/spicefreeze001zh4.th.jpg[/img:db99c12647] [img:db99c12647]http://img123.imageshack.us/img123/6933/spicefreeze002cz7.th.jpg[/img:db99c12647] I'm guessing the solvent (looks like Bestine tin on glass in pic 2) was evaporated down substantially before being put in the shot glasses, and was then heated to super-absorb the spice forming in the bottom of the evap. container. Then, placed in the shot glass and freezer, this is what happened. The impurities and small bit of yellow/brown waxy sludge appears to be separate from the white spice crystals. ---------------------------------------- NOW FOR THE REST OF THE STORY... what did this person do next? The story ends there-- with no impression of the next steps taken. Is this the stage where you remove the glass, and pour it through a coffee filter immediately, and harvest clean spice? Is this the "final stage" ? Or was this just an initial stage of good refinement... Any help and comment would be instructive :) (PS-- what a wonderful forum! )
 
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Hello and welcome. If it were me, I'd have poured the Bestine off through a coffee filter (in case there were any stray crystals) and left the shot glass upended to drip dry for awhile. Then I'd have scraped the crystals and all out onto a piece of smooth, absorbant paper and spread them around to dry completely. Then, using toothpicks, I'd have carefully separated all that was crystal from all that was non-crystal. The non-crystal will still have a lot of spice in it, so it should be saved and worked into the next batch. The crystal could be used as is, or if I thought another round of cleaning was in order (you can get it to just clear shards) I'd put the spice in one shot glass and bestine in another and slowly warm them both up in a water bath. The crystal will melt and when the bestine is warm to the touch, it can be added a little at a time until the solution is clear. Leave the shot glass in the water bath and let it cool, undisturbed, to room temp. Then move the glass to the refrigerator. Then to the freezer. Have fun.
 
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Upon further research, I found another pic online somewhere of what appears to be a post-filtered experiment. It doesn't look like very much-- I'm guessing it was collected from the smaller of the two previous pics. [img:21c569def1]http://img265.imageshack.us/img265/8914/spicefilter001yk8.th.jpg[/img:21c569def1] It is very pale yellow in color--almost white--and powdery consistency, from looking at the pic. [b:21c569def1]I've found out some more info-- Here's a newly discovered pic from the results of the second shot glass... [img:21c569def1]http://img182.imageshack.us/img182/8274/spicefilter2on4.th.jpg[/img:21c569def1] I read that the weight of the full first pull (both shot glasses) was 200mg total-- As I read this I thought this was a very, extremely small amount for the full 1lb. MHRB that was said to be used in the experiment. As you might imagine, the writer of that article was very upset at the tiny, albeit very clean, results of all that work. :( What would you advise a new researcher to do when thinking about this process?[/b:21c569def1]
 
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I heard from my source it was the Lazy man's tek, 1lb . from BBB, not powdered, but hand ripped small, +250g pure lye in 2litres water, soaked for over two days in lye solution. Then, solution placed into 1 gallon glass pickle jar, 550ml Bestine added, and soaked for 1 day. First pull was evap'd down and shown in the pics found online. I read further that the second bestine pull was being cool-frozen-cool-frozen in a quart mason jar after 2-day soak-up to help with good crystal formation before filtering. Then third pull was made using fresh odorless mineral spirits after 1 day soak , which was then heated to exactly 115 degrees for 2 hours (in sealed 1 gallon pickle jar underwater) before being pulled and placed into its own mason jar, where it was being cool-frozen-cool-frozen. The fourth pull would begin when the second bestine pull was filtered of spice and placed back into gallon jar with bark.
 
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Hmmm... My friend in Antarctica is getting suspicious that "high quality inner rootbark" associated with those initials is bunk. He didn't get skunked that hard, but did get significantly lower yields than he should have. He's going to do a long long long A/B on 200g and if he gets less than a gram of good spice, he's going to bitch. In your case (that you're reading about) the culprit could be using heptane as the NP. I don't know, my friend has only recrystalized with it. It might not suck the alks out of solution as readily as naptha. The extreme cleanliness of your product (I thought at first that you were refering to freeze precipitating a recrystalization) certainly seems to indicate that heptane is much more selective in what it takes up. It'll be interesting to see what comes out in your OMS, though they're still suspect in my mind. He's never used them but reports of low yields started coming around when people started using it. I've yet to read a SXS comparison. Anyway, if the basified solution were still around, I sure be interested to hear what came out of a naptha and then a xylene (or toluene) pull.
 
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I've discovered another set of pictures somewhere on the internet: I'll post them here: It appears to be the person's second pull (Bestine) results [img:d296200107]http://img407.imageshack.us/img407/5040/secondpullspice001pk1.th.jpg[/img:d296200107] In the Jar [img:d296200107]http://img267.imageshack.us/img267/8167/secondpullspicefinal002de0.th.jpg[/img:d296200107] Weighed after collection. ___________ I saw a note attached to the original post where the writer said that there was a bit left uncollected in the bottom of the jar after extraction (a hard, gummy textured "smear") that was removed by placing ~50ml bestine into the jar, sealing it, and running hot tap water over the entire jar to heat the glass and solvent, which was swished around the interior, liquefying and catching all the stray spice on the bottom and sides. This was placed into a new, smaller cup, covered, and put into the freezer for later extraction. Then I read that the Bestine from this pull was returned to the gallon jar and the cycle beganeth again. This observer is unsure of what "SXS" means. This observer wonders if VM&P Naptha would be the flavor that is referred to in the final sentence of Noman's post...
 
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[quote:c7af8af7c6="coAsTal"]This observer is unsure of what "SXS" means. This observer wonders if VM&P Naptha would be the flavor that is referred to in the final sentence of Noman's post...[/quote:c7af8af7c6] Side By Side VM+P is best as long as it evaps clean.
 
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I got the impression from reading the original poster of these questions (I think they are from Texas or something-- as they talk about bull shit a lot) that they had some of that around that they were thinking of trying after the current Bestine pull. I'll let you know if I ever hear back from them...
 
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[quote:51825959cf="Noman"]If it were me, I'd have poured the Bestine off through a coffee filter (in case there were any stray crystals) and left the shot glass upended to drip dry for awhile.[/quote:51825959cf] SWIM is on his first extraction using a version of the straight to base method. 100g of quality powdered MHRB netted about 1.3g of oily yellow crystals after three pulls. The first pull was freeze precipitated and ended up at 0.1g, whilst the second was evapped and made 0.9g. SWIM combined all the spice and redissolved in a very small amount of hot naptha for a first re-x, but is concerned about the next stage of the procedure, as it might have been bad technique that lost product on the first pull. After 12 hours in the freezer the naptha is now clear yellow. All the crystals appear to be stuck to the sides, so SWIM is wondering about the next step. Should he simply open the 125ml jam jar, pour off the naptha (for later reuse), quickly re-seal and bring to room temp, then open to evap the remaining naptha; or, scrape the insides with a spoon to get all the crystals mobile and then pour through a coffee filter? SWIM used the former method after the first pull and saw a very small yield. Looking at Noman's photo of a jar upended on a larger jar, is there not a danger that the spice will absorb water from the air whilst it is warming to room temp? Could this occur even when opening the jar for a few seconds to pour off the naptha and re-closing? SWIM would appreciate any advice - the tek seems to have gone reasonably well for a first attempt and it would be a shame to lose all the spice now!
 
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As I dig deeper into the archives, I find further postings by the Texan. It appears that there was essentially [i:eb313371fe][b:eb313371fe]nothing[/b:eb313371fe][/i:eb313371fe] extracted from the third pull using 600ml Odorless Mineral Spirits.... even though the mixture of solvent and lye solution was heated to 115 degrees in the gallon jar for the two hours prior to extraction. According to the collective Teks, this heating alone should have benefited the transfer of the magic alkaloids quite a bit... At the time the poster had written the message, the OMS jar was still in the freezer, after a cool-freeze-cool crystallization cycle (CFC), but only two or three tiny 1-2mm balls of spice were visible on the bottom of the solvent. At a later time, the quart of OMS was to be evaporated down considerably and then CFC'd again... with hope still remaining... The next step would be to repeat 120 degree heating of Bestine mix in the lye solution for two hours... followed by a (final?) pull using VM&P naptha. The Texan noted that the total extract at the time of that post was 1.65 grams of spice (albeit a very high quality, pale yellow/creme colored) plus the bit that was still in the OMS jar, estimated at 5mg or so [i:eb313371fe] This observer notes that that is approximately one third of what might be expected from such an effort with the amounts of materials involved...[/i:eb313371fe]
 
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[quote:671d206643="coAsTal"]This observer notes that that is approximately one third of what might be expected from such an effort with the amounts of materials involved...[/i][/quote:671d206643] More like half. I don't buy into these claims of 1%+ yields from garden variety non-Mexican bark.
 
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Well, I read recently that the third pull (OMS) is still showing nothing, after CFC (Cool-Freeze Cycle) a few times. It gets cloudy, but nothing is separating from the solution... The Fourth pull that the Texan made re-using the Bestine from pull 2, does have some spice collecting in the bottom-- She told me that the fifth, and probably final pull (Using VM&P Naptha) has been soaking in the gallon jar with the lye solution for days now and may be poured out tonight or tomorrow (after heating for 2 hours) for CFC. The researcher still wonders where there are better alternatives for research than bbb.
 
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[quote:3e543472bf="coAsTal"]Well, I read recently that the third pull (OMS) is still showing nothing, after CFC (Cool-Freeze Cycle) a few times. It gets cloudy, but nothing is separating from the solution... The Fourth pull that the Texan made re-using the Bestine from pull 2, does have some spice collecting in the bottom-- [/quote:3e543472bf] Well, that tells me that OMS is fucked as a nonpolar if a bestine pull after it yields more spice. (i knew it) The Antarctican still hasn't done an A/B on his latest bark samples, so he isn't positive that this batch is bunk. He's had the greatest success with European sources, but hates international ordering since LE is starting to become aware of the stuff.
 
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[quote:6ad5c4805d="Noman"]Well, that tells me that OMS is fucked as a nonpolar if a bestine pull after it yields more spice. (i knew it) The Antarctican still hasn't done an A/B on his latest bark samples, so he isn't positive that this batch is bunk. He's had the greatest success with European sources, but hates international ordering since LE is starting to become aware of the stuff.[/quote:6ad5c4805d] Perhaps the OMS is best used just for the re-crystallization stage(s), sticking to naptha for the initial pulls. Clean naptha is hard to find in Europe, the lighter fluids leave a lot of oily residue.
 
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Additional data has made itself known to me: I found pictures of the Odorless Mineral Spirits jar(Klean Strip Brand) post-extraction (pull number three)-- with pics of the fourth pull jar (Bestine) side-by-side for comparison. After repeated CFC, the OMS solvent was poured through a coffee filter, and only a very tiny amount of spice was witnessed in the bottom of the quart jar. Again-- this solvent had been in contact with the lye solution for days before extracting--in addition to being heated to 115 degrees or so for two hours prior to extraction. The fourth pull, consisting of re-used (first-pull) Bestine, was also poured through a coffee filter, with a considerable amount of spice collected in the filter, in addition to a solid amount still clinging to the interior of the quart jar (that was later to be removed with heated bestine, transferred to a smaller container, and recrystallized for ease of collection) It appears to have proven the theory that OMS is a poor alkaloid extractor... the Texan was glad it was not the only thing she had to use in her experiments. Here is the pic that was discovered with the above information: [img:1304c5fb14]http://img295.imageshack.us/img295/5097/omsandbestfourthpulloo3.th.jpg[/img:1304c5fb14] A post script said that the VM&P Naptha (Fifth pull) was also collected from the lye solution in it's own jar, and is beginning the CFC process now. The curious researcher hopes the Texan will tell of the results of that as well...
 
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