Hello everyone! This is SWIMs second attempt at Vovin's TEK. The first time it having made mistakes along the way, but it was over all a fun learning process. SWIM thought he should share how the second time went. One thing that SWIM seems to not see in many extraction TEKs is the temperature at which the naphtha should be warmed to and how cold the freeze precipitation was. SWIM got himself a laser thermometer from Harbor Freight for about $38. SWIM recorded the temp. along the way for each pull with naphtha. SWIM isn't saying these are the temperatures you need to use, just that these are the temp. that SWIM had success with on this extraction. SWIM however didn't have the laser thermometer for measuring the acid baths when he did them. SWIM will have to do that on his next extraction a report back to you guys. So here we go...
DAY 1
- Simmering 1200mL of distilled water to be added to 100g of pre-powdered Mimosa root bark.
- Add a very small drop of hydrochloric acid to simmering distilled water, to bring pH to about 4.
- Added the just enough acidified water to the root bark to cover it in a flask. Let it sit in a warm bath for 45mins, occasionally stirred.
- Then filtered with a Buchner Filter Flask
- Placed first bath in a separate flask and put the root bark in another for the next bath.
- Did the above x3 times.
- The final resulting three liquids now in one flask is placed over night for decanting in the fridge.
DAY 2
- Liquid has separated into the two distinct layers. Very fine sediments at the bottom with the acidified liquid on top.
- Filtered the liquid with the Buchner Filter Flask again very carefully to not disturb the fine sediment. Then placed liquid in fridge again for a night.
DAY 3
-There was still some even finer sediment left so one more filtration.
- Filtered the liquid with the Buchner Filter Flask again very carefully to not disturb the fine sediment.
DEFAT x3
- Now the acidified extract is about 550mL.
- Began warming Klean Strip VM&P naphtha to be added to acidified liquid for defatting.
- Naphtha was approx. 120 degrees F.
- Placed the acidified liquid in a separatory funnel. Then added the warmed naphtha to it.
- Turned the funnel end over end for 5 mins. Venting ever so often by turning upside down and opening the release valve.
- Place a small piece of plastic wrap over the top of the funnel with hole for venting while sitting. Then placed funnel on a stand and the stand in to a trash can form hardware store filled with hot water at Approx. 120-130 degrees F to help separate the naphtha and acidified liquid into two layer. This also helps dissipate the bubbles from the agitation. Let sit until there was a distinct separation. Approx 1hr the first time, 25 mins second time, and 15 mins the third time. Maintained water temp by removing some of the water and adding new hot water.
NOTE: The reason for the change in times was that SWIM agitated the it too much the first time. Was more careful the next time. The naphtha has to come in contact with all the acidified liquid but doesn't need to be aggressively shaken.
BASIFIYING
- Cleaned seperatory funnel out and placed defatted extract back into the funnel on stand.
- Warmed 300mL of distilled water to 100-120 degrees F and brought the pH to 12.5 with Lye crystals.
- Added small amounts of lye and water solution to the defatted extract until pH was 12.32 and the liquid was a black tar like color.
EXTRACTION x3
- Warmed naphtha in a hot bath to approx. 140-150 degrees F.
- Added naphtha to basified extract and turned end over end until SWIM felt the naphtha had came in contact with all the basified extract. Venting often.
- Then let sit in trash can hot bath at 135-140 degrees F. until a distinct separation of naphtha and extract was seen.
- Then using a glass pipette pulled off the naphtha at the top and placed in a flask.
- Repeated two more times the final pull with only 50mL of warm naphtha.
WASHING
- Took the naphtha and placed it into a clean seperatory funnel. Approx. 350mL of naphtha.
- Took 50mL of distilled water and added a pinch of sodium carbonate.
- Then added 25mL of the sodium carbonate water to the naphtha and shook the hell out of it.
- The separation was immediate and funneled off the water which was at the bottom.
- Did this again two more times but with 25mL of only distilled water.
FREEZE PRECIPITATION
- Placed the DMT containing naphtha into the freezer in a Pyrex casserole dish with cover on at -8 degrees F for a night.
- Next day success! Going to leave it for another whole day then going to pour off the naphtha into a separate glass an place back in the freezer. Then took dish with DMT and turned upside down on another bigger dish to allow the remaining naphtha to run off. Place in freezer at -8 degrees F.
- After a couple of hours tried to scrape up some of the DMT, but was still wet with naphtha. Decided to let evaporate off remaining naphtha by placing coffee filters taped together over the dish and place in a cool dark room.
SIDE NOTE:
Decided to try one more extraction on the basified liquid before SWIM discarded it. Placed these three pulls in another dish and covered it. Then put in a bowl of ice and into -8 degrees F. Within hours big crystals forming. Thinks ice may have helped speed up freeze precipitation. Going to allow to sit for a couple of days.
So there you have it folks! SWIM is going to recrystallize the DMT with lab grade Heptane and then again with lab grade Hexane as soon as SWIM gets them. Which should be around Jan. 7th. It will be SWIM's first time doing a recrystallization. So excited!