I didn't want to start a new thread about this, as this one looks to have gotten some good attention from scientific people.
I recently came across a process detailing a pretty rigorous acid-base extraction of nicotine yielding near-pure nicotine crystals. Obviously the purer the crystals the better, as it gives one a more accurate idea of the nicotine concentration in whatever they choose to use them for. This is NOT taken from a patent, it's from sciencemadness and i'm sure some of you have already seen this.
And mad props to cheapskate, the author and inventor of this tek, where ever he may be. This is >7 years old
[all annotations in square brackets]
OK, to close this off and leave something for others attempting this same item, I finally did it. There were a large (really large) number of problems as detailed previously, but I've found a way of getting the nicotine out of tobacco on a small scale that can be handled at home.
First though, the tobacco chosen is important. For example, good old rolling tobacco you buy in bulk at the discount cigarette store works great. Marlboros have too many additives that mess up the works. Tobacco dust sold in four pound bags works well, but there is actually very little nicotine in it. Something in the processing is removing the nicotine.
So go get the cheap rolling tobacco that has already been ground up. [I believe using dry tobacco is important for this experiment, as it sucks up the lye-water solution while the kerosene sits around and sucks up the freebase nicotine]
The initial extraction is to use around 100 grams of tobacco and 300ml of kerosene. Yes, I know that I swore off this stuff because it left a taint to the nicotine, but I found a way to remove it later. Also add 50ml of 40% sodium hydroxide solution to the mix. This frees the nicotine from the salts in the tobacco and helps break down the cellular walls.
Let this set with occasional stirring for 24 hours. The tobacco will swell some and the mix will increase in viscosity. Filter and squeeze through cloth to get all the liquid you can and put the tobacco back in the container for another kerosene extraction with 200 ml this time. Note that you won't get the 300ml back, you'll be lucky if you get 200ml out of the tobacco and the water will have disapeared. 24 hours later filter and squeeze what you can out of the tobacco and just throw it away. Further extractions are an exercise in futility.
[If you have a buchner funnel setup, it would drastically decrease filter time]
Combine the kerosene fractions and set them aside while you prepare a solution of 20ml 30% hydrochloride and 80 ml of water. Just use the old driveway cleaner from the local building supply. Extract once with 50ml of the acidic water and a LOT of stirring, shaking, whatever. The kerosene layer will be on top and will turn a milky yellow color. The water layer, bottom, will turn an amber color; separate and repeat the extraction with the other 50ml of acidic water.
The kerosene can now be discarded or set aside (just in case). The amber water needs to be washed with a little VM&P naptha. Use about 30ml and mix well so it can take up all the left over kerosene. This is the stage where you get rid of the nasty kerosene. Basify to ph>10 with 40% water solution of NaOH and add enough salt so no more will dissolve.
This is where it gets interesting. [I agree, I haven't seen any lit other then this one tek that uses salt-saturation to drive nicotine out of solution]
The basic salt-saturated solution will cause the nicotine to separate at temperatures over 60C. So, just for fun take the temperature up to around 70C and you'll see the oil separate and rise to the top as a separate (very small)layer. This isn't pure nicotine, but includes all the alkaloids and some other contaminants. But it does give one a good idea what you're going to get.
Cool, filter out the solids, and extract twice with 30ml of naptha. Evaporate the naptha at room temperature and you have a small amount of relatively pure nicotine. There isn't enough here to do much with [not the case for those looking to make e-juice
], so dissolve in acetone [Substitute H2O or grain alcohol] and save. Repeat the entire procedure saving the nicotine in acetone until you have enough to deal with. I use 4 of the full extractions to get enough nicotine to further purify.
[aside] I figure that the utility of this tek for e-cig people pretty much ends here, as we now have a semi-pure batch which could easily be added to homemade e-juice in known concentrations. If anything it's safest to stop here and assume whatever you've pulled is 100% nicotine and use accordingly.
Further purification. The right way to do this is a vacuum distillation under an inert gas, but most of us don't have the equipment to do that so.... First evaporate the acetone at room temperature and dissolve the nicotine in basic water (ph> 11). Extract with pure (distilled) ether. This is important since the ether one can get at the auto parts stores has contaminants in it. You can find instructions on distilling ether on the web, just be sure to keep flames away and use good ventilation. Evaporate most of the ether and use the small amount left to help you pour the fluids into a container for storage. Evaporate the last of the ether from your container by warming slightly and you're done.
If you have the equipment, you can scale this up to larger amounts of tobacco and cut down the effort. One can even arrange a pump to pump the kerosene through the tobacco to extract on a continuing basis and do an acidic water extraction in line by letting the kerosene bubble up through the acidic water before being returned to the tobacco. With a little screening and filtering this could be set up to produce reasonable quantities of high percentage nicotine. The surprising part is how little nicotine there actually is in tobacco. One would think there's 4 or 5 grams in each 100 grams of tobacco, but I just couldn't find it. I did get as much as 3 grams on the first pass, but that was as good as it got and only happened once. So, keep your expectations in check and proceed. [end]
I think ill be trying this, or some form of it, in the next two weeks. I'll post my results in this thread and if all goes well ill start my own advanced xtract tek thread!
Happy vaping people!
...on the one hand I'm so very impressed with this.
