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HELP! MARSOFOLD TEK GONE HORRIBLY WRONG! Budding chemist :(

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tejas

Rising Star
HELP!!!! My freinds cats’ dogs’ boyfreind (who is a budding chemist) realllllly messed up! SWIM recently embarked(mimosa bark that is) on a massive DMT marsofold extraction tek, however he managed to not get a single gram of god-spice! SWIM is quite proficient in chemistry and was wondering if someone could explain the chemistry of the marsofold tek to him so he can try and figure out what went wrong. SWIM lives in the uk and some supplies are unavailble. He did do a few things differently, i.e in the polar extraction; after slow-cooking the white vinegar-water solution he left the bark fibre in the pot as it settled. He didn’t think this would make a difference. When siphoning off the fluid (using mcdonald straws and accidently swallowing some of the naptha :/ ) he did accidently mix the lower dark layer with the naptha layer leaving some hydrophillic bubbles in a hydophobic enviroment  . The only real thing that he thinks that could have made this go monumentally wrong was not using naptha, or using what he thought was naptha but what wasnt. Whatever it was, it smelt like white spirit. http://www.agwoodcare.co.uk/show_product.php?id=50 So swim was wondering what other chemical alternatives to naptha could be used, and the chemical reasons for using naptha. PLEASE HELP!
 
sounds like you used solvent that didn't work very well, lol. see if you can find bestine over there in the UK. I think i've read a few people using that. May want to wait for someone to back me up on that though, lol
 
Swim followed the intructions exactly, but for reiteration ill point out the main changes and possible errors. Swim was wondering what the use of white vinegar is for, and whether it is purely just because it is an easily available acid. The white vinegar solution is meant to mix up to pH 2 and possibly lower is this correct? Swim used white vinegar cleaner to make this solution, tasting it it was very acidic but still unsure of the overall pH of the solution he made. Swim also used this caustic soda: Choiceful It said 98% solid NaOH and swim added 5 tablespoons. Again swim was unsure of the pH, and was wondering if someone could clarify the opitmun alkali level for the extraction. Swim added 5 tblspoons,(they are however a different size in the uk so it may have not been enough) . The alkali solution however was enough to crack the measuring jug it went in after a few hours (it wasnt pyrex) Swim then seperated the solution into 3 1.5L wine bottles as swim didnt have a big ole jug. Swim used a little more naptha then 250, using isntead 300 and splitting it evenly into the wine jugs. The naptha was not warmed. Swim then left the naptha solution in the freezer for 4-5 days instead of 3 for extra precip time. But to no avail! Zero precipitate! Main concern for swim is whether leaving the bark fibres in overnight made a difference. Very strange how swim manged to not get a single gram! not even a milligram! Muchos gracies for any help!
 
How much MHRB did you use? Are you sure you got the right kind? Maybe your source is not so good? "He did do a few things differently, i.e in the polar extraction; after slow-cooking the white vinegar-water solution he left the bark fibre in the pot as it settled. He didn’t think this would make a difference." -Sounds like you followed proper procedure here. You want to cook the bark-mash 3 or more times, saving the liquid and reusing the bark on each cook. "When siphoning off the fluid (using mcdonald straws and accidently swallowing some of the naptha :/ ) he did accidently mix the lower dark layer with the naptha layer leaving some hydrophillic bubbles in a hydophobic enviroment." -This is wrong on multiple levels. You really need proper tools, using a drinking straw is pretty stupid idea in my book. A turkey baster, or even eye droppers would have been a much better choice. You need to be extra careful not to get any of the dark crap into the naphtha that you siphon off. "Swim used white vinegar cleaner to make this solution" -I don't know what white vinegar cleaner is or whether it's got extra stuff in it besides distilled white vinegar and water. Could be a potential problem if it's not pure though I suppose. Distilled White Vinegar is used because it is cheap, widely available and relatively pure. There are alternatives, "Swim also used this caustic soda: Choiceful It said 98% solid NaOH and swim added 5 tablespoons." -You really want 100% pure NaOH, anything else and you will be dealing with some nasty toxic crap like heavy metals and fragrance and who knows what else. "Again swim was unsure of the pH, and was wondering if someone could clarify the opitmun alkali level for the extraction." -Ideal PH is somewhere between 11 - 13.5 afaik "The alkali solution however was enough to crack the measuring jug it went in after a few hours (it wasnt pyrex)" -Why was the basified solution sitting in the jug for so long? For STB teks I can understand the long alkali soak but when doing an A/B there is no reason to let it sit that long that I can think of. "Swim used a little more naptha then 250, using isntead 300 and splitting it evenly into the wine jugs. The naptha was not warmed." - Was that the total amount of Naphtha you used or was that amount used per pull? Heating the Naphtha in a warm water bath is a good idea as long as you take safety precautions. "Swim then left the naptha solution in the freezer for 4-5 days instead of 3 for extra precip time." If you used too much Naphtha, the concentration of DMT in the solvent will not be high enough to crash out during freeze precip. You can try to evaporate a good portion of the Naphtha and then freeze again, you may have better results.
 
after re-reading the post, and laughing at the budding chemist using mcdonalds drinking straws, I think too much solvent is probably the issue as posted above. Take your solvent, and just evaporate it at room temperature. You should get your spice out of it. You can then take this, and recrystallize it or freeze precipitate it properly by re-dissolving it in a proper amount of solvent.
 
Yes, don't panic !... it's in the solvent - just evaporate the naphtha and you'll be amazed - at the smell and sight ! Set up a fan to gently blow over the glass tray, and as the last 20% remains, turn off the fan and let it evap' slowly. The slower it evaporates, the nicer shaped the crystals grow !... The basifying step is easy to do without pH meter; add the lye-solution until the purple extract goes jet-black, 'slippy' jet black. But STOP adding lye when it goes black ! Don't add solid lye but make a hot-water solution of lye first, and use [b:e51c968426]100%[/b:e51c968426] NaOH. Use glass ware that's rated for the task ! Get glass turkey Basters, and a thick-walled, clear gallon-sized wine jug for the acid bath. Quart-size pickling jars work well for the basifying steps - split the filtered, purple acid extract into multiple jars. I feel that there is little gained from heating the naphtha - in 2 pulls you get >95% of the dmt-freebase out when the naphtha is at Room temp', for max 30 min each pull. Make the naphtha pulls as quick as possible, 20 - 30 min each, and you'll avoid any lye contamination.
 
Cheers guys, luckily swim kept the naptha, but its been a good 2 weeks now and nothing has happened to it though(it hasnt evapped either) Swim used 300ml in [i:37cc95ae34]total[/i:37cc95ae34] so that would be 100ml of naptha per bottle. The solvent did turn jet black though so up and to that point, swim thought he was doing well. (The lye solution was only in the jug for a few minutes before adding it , swim thinks this was enough to cause microfractures in the jug however which proliferated after into large cracks after a few hours) Swim realised that straws was a bad idea but hadn't anything else to hand and had to leave very quickly. Also swim was wondering where to get 100% NaOH from? Anybody in the uk know? Swim will try to evap the naptha, but still marvels that 50ml in extra naptha would result in zero crystals! Thanks again!
 
You can get 99% Naoh from a soap making place but honestly I wouldn't worry about it, your 98% should work just fine.Over time Naoh gradualy turns to sodium carbonate, the 98/99 thing doesn't mean there are impurities, its just a labeling thing to comply with sale of goods act, accurate labelling etc :)
 
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