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As we know, the based water portion of the post rxn solution contains a considerable amount of iodides. The ratio of the i2 used at the start of the rxn and the amount which can be recycled differs greatly with the type of rxn. I have found that the wet reflux tends to keep up to 75% of the iodine which can then bee reclaimed for future use. The dryer rxns contain much less unless a p/p unit was used as the p/p unit contains a large portion. I have tried several methods to recycle the iodine and have finally been able to consistently recycle my iodine. Although I prefer doing things using exact amounts, concentrations, etc. This particular method is one where visual signs are prominent. Since the concentrations of iodides differs with each rxn and the amount of water added when pulling the meth make it nearly impossible to calculate the amount of iodides that are dissolved in the solution.
I steam distill my post rxn solution and after basing and distilling off the meth I pour the remaining solution in a big glass chemical bottle. Whenever I have time or am running out of iodine I then will process some if not all of what I have accumulated. Here are the materials needed as well as the steps I use to reclaim i2.
18% H2O2 Hydogen Peroxide (lower concentrations will require less dh20)
37% 12Mol HCL
(I have kept methanol in a old dishwashing liquid bottle, for various cleaning, since before I even thought of making meth. This works great for this method cause it doesnít have to bee dry and its easier to squirt it than pour it. Any alcohol should suffice.)
1 2 liter soda bottle or equivalent.
1 large funnel fitted to a large bottle or any container
1 Clean, thin cotton towel or piece of a t-shirt
2 coffee filters
Pour the basic post rxn solution through 2 coffee filters into the 2 liter soda bottle. This may take a while but if you donít filter out the solids then your i2 is gonna bee very dirty. If only 1 filter is used it will most likely break towards the end dumping all the shit back into the solution and then you will bee back where you started. Fill the 2 liter with no more than 1/3 full.
Next add the same amount of dh20 to the 2 liter. If using 3% H2O2 then donít add any dh20. Other concentrations should bee calculated accordingly.
Add approximately 50ml of hcl to the soda bottle and cap and shake. Release the pressure between shaking.
Next add about 30ml of 18% H2o2 or the same amount of dh20 that would have been used in the step 2. Shake again while venting between shakes.
Let this set for at least an hour and then shake again as before. The top 2 liter bottle is hard to see through due to iodine, take your methanol and squirt a small amount into it to wash down the iodine. Shake again. Repeat 3 or 4 times until iodine crystals are sitting on top of the solution. If this doesnít happen then add a small amount of hcl and a little more h202 shake and repeat with the methanol as before. (After shaking the upper part of the 2 liter should be fairly clear if it is still getting darker with iodine rinse with dashes of methanol until it no longer appears after shaking.
Take the cloth and put it over the funnel and secure with a rubber band around the rim. Push it down a little to create a cavity. Pour the contents of the 2 liter through the funnel while shaking between pours. When all has been poured add some clean dh20 to the bottle and rinse into the funnel as well.
Rinse the crystals with cool dh20 several times. Put on some rubber gloves and remove the rubber band. Carefully, fold the cloth over the crystals and twist both ends to squeeze out the liquid.
Place the ball in a glass jar and break it apart. Put a clean piece of cloth over the opening of the jar and pour in some silica gel and then screw on the lid so that it holds the cloth in place over the crystals. Store in a cool, dark location. Change the silica gel in when necessary.
I got the idea of using alcohol cause tincture seemed so much easier to get crystals from and tincture contains alcohol. It seems to assist in the cleaning as well as crystal formation.
I use a cloth for filtering the crystal is because coffee filters and lab filter paper are both to fine. The cloth allows more to get through and faster with the end result being cleaner. Of course the other reason is so that the crystals can be wrung out. I took an old clean white t-shirt and cut it into 200mm squares.
I made a funnel out of a 12Ē long piece of 4Ē pvc pipe with a reducer on one end and a few holes drilled into the side for venting. I put the cloth over the open end and put a couple rubberhands to hold it in place. This way its not touching anything on the bottom so it drains faster.
I have also found that using more dh20 is sometimes helpful and a lot of shaking produces cleaner crystals. You want to see a sort of foam of crystals on top of the solution, with craters in it. That is a sign that it is pretty clean.
If you really want to get almost all the water out you can clamp a pair of vice grips on each end of the cloth and then twist as tight as you can without tearing it. Then keeping it tight hit it a few times with a compressed air gun to remove any remaining water.
The silica gel I use is in the form of small spheres like little bbís. It changes from blue to pink when it has absorbed its capacity.If you canít get silica gel you use other drying agents but I wouldnít use the cloth cause it may leak. Use a small plastic container w/ a lid. Drill a small hole through the center of the plastic lid and also the center of the jar lid. Secure the small lid with a screw or whatever on the inside of the jar lid. Take the small container and drill or melt holes around the upper half and fill with calcium chloride flakes or dririte. Then screw the container onto its lid and put the lid on the jar. Be careful when you remove the lid because there will probably bee standing liquid in the plastic container which could splash out if not careful.
Due to the many variables involved in the rxn process the concentration of iodides or reclaimable iodine will vary considerably. Therefore each bee will have to tweak their own ratios of mainly h202. You canít really put too much acid in although you can put too little in and no crystals will form. Excess hcl will rinse off when washing and even if it doesnít it will not hinder the rxn anyway. Too much water is not a problem but again too little is. The alcohol should be used sparingly as it will dissolve some iodine.
It wasn't Me!
for those bees not refluxing.... you can recycle iodine by building a P/P tank. not too hard, only an hour work or so...
then when your reaction is done, tip out your P/P fluid into a container and add 10% sodium hypochlorite in small increments.
2HI + 2Cl -----> I2 + 2HCl
So keep adding till little iodine bits fall out of your liquid. Then filter them out, and save em. Wash many times with H2O to remove any HCl.
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Shorty mentioned this method in another thread and I am pleased that he did a write up on it. This is very useful information. I tried the procedure as I understood it from the other post and recovered 70% of the I2 I added to the reaction. This I2 seems clean.
I added HCl until the solution was acidic; as it was already pretty dilute I did not add additional water I added half a liter of 70% IPA to about a liter of filtered, dilute based reaction fluid, added 3% peroxide until the soution went UPS brown; in an hour a layer of fine I2 crystals had settled to the bottom of the jar. These were rinsed in the same way I would rinse I2 from tincture, compressed, and dried.
The alcohol does seem to help clean the I2. I once took some recovered I2 and dissolved it in IPA to make tincture of iodine. I let this sit for a day, filtered out the solids that settled out, then extracted the I2 from it as I would extract from tincture. The I2 I obtained was a good deal cleaner than what I started with, but still required resubliming. Shorty thought to add the alcohol before extracting the crystals. My impression was the I2 I collected was far cleaner that what I have ever obtained recovering I2 from reaction fluid.
I recovered seventy percent of the I2 I added to start the reaction. I was pleased by the process. If you are not recycling your iodine from your reaction fluid, you need to start. There is no reason not to.
Shorty---once again, thanks for sharing another of your successful ideas with the Hive. I suspect the stronger peroxide was the reason your I2 "floated" rather than settling to the bottom. It may be cleaner, but I suspect you risk damage by using peroxide that concentrated.
SWIS has always recycled I2 from completed reactions and reused. The recycled I2 works just fine at reducing product, but I'm just wondering...has anyone else noticed this about their recycled I2: Whenever SWIS does a reaction using recycled I2, it's always a very calm reaction. In other words, there is no violent reaction at all when the RP is added to the mix, as is usually the case when SWIS uses brand spanking new I2. Doesn't affect the quality of the finished product, just makes for a very calm reaction.
You notice this, geez?
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Stoni-- I have noticed that a few times when I was using only recovered I2, and none from tincture. I just chalked it up to not doing a good enough job resubliming the I2. I'm the only person I have ever seen do it, which means I learned how by reading about it here, and can't say for sure I do it the right since I've never seen anyone else do it. My method does work...so I guess I got the idea. But I wonder if it leaves some trash in.
Since I became a devotee of the long wet reflux, all my reactions seem calm, boring, and not worth watching. Good thing that they don't need to be watched. The recycled I2 has never been a problem except the time I tried using it without resubliming it. Nope. Not a good idea at all. I learned NOT to do that--but at least I learned something that day.
I have never seen anyone extract I2 from an iodide soup with bleach either...and I obviously have not figured that one out, since I always wind up adding too much bleach and lose it. I noted the comments in this thread about the push pull tank water, and the suggestion to extract it with bleach alone. The bleach and iodides react and form I2 and HCl. Is the HCl manufactured fouling the process if I previously added enough acid to make the reaction fluid slightly acidic. I would think one would not want to use H2SO4 to drop the pH if the planned addition of bleach was going to produce HCl. That would produce some gas would it not? Any suggestions for a search and siezure man who can't get the goods with bleach?
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Geez: A good rule of thumb for 2% iodine tincture that Ibee follows when using bleach and sulfuric versus the hydrogen peroxide/hcl is to use half the amount of bleach.
Anymore than that will clear the solution in a jiffy!
Too much H2SO4 will result in the goodz disappearing as well.
But beeing the daredevil that Ibee is, he always eyeballs the sulfuric acid until the purple balls show their asses!
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