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| Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists. |
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#1
 2003-11-18, 00:54
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DarkSky 
Regular
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I2 Recovery from rxn fluid
Can someone give SWID help with the proper way to extract I2 from used rxn fluid. SWID has read the post at the hive.... Worlock: "Sodium Iodide recovery" (Stimulants), However this post is very vague as quanities of perxoid and bleach that is added abd exactly how the I2 is recovered.
If SWID used 6g of I2 for the rxn what would be the proper way to recover this from the rxn fuid
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#2
 2003-11-18, 03:34
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kneedragger 
Regular
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Re: I2 Recovery from rxn fluid
Here is one from the Hive. SWIM has not tried it.
--kneedragger
SHORTY
(Hive Bee)
07-27-03 05:51
No 450132
Recycling Iodine
(Rated as: excellent)
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.
Chemicals
Dh2O
18% H2O2 Hydogen Peroxide (lower concentrations will require less dh20)
37% 12Mol HCL
Methanol
(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 doesnt have to bee dry and its easier to squirt it than pour it. Any alcohol should suffice.)
Materials
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
rubber bands
Method
Step 1
Pour the basic post rxn solution through 2 coffee filters into the 2 liter soda bottle. This may take a while but if you dont 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.
Step 2
Next add the same amount of dh20 to the 2 liter. If using 3% H2O2 then dont add any dh20. Other concentrations should bee calculated accordingly.
Step 3
Add approximately 50ml of hcl to the soda bottle and cap and shake. Release the pressure between shaking.
Step 4
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.
Step 5
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 doesnt 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.
Step 6
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.
Step 7
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.
Step 8
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.
Notes
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 12 long piece of 4 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 bbs. It changes from blue to pink when it has absorbed its capacity.If you cant get silica gel you use other drying agents but I wouldnt 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 cant 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 doesnt 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.
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#3
 2003-11-18, 18:55
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DarkSky 
Regular
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Re: I2 Recovery from rxn fluid
Thanks kneedragger, this is just what SWID was looking for. Ill let you know how things go once SWID has actually tried it
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#4
 2003-11-18, 20:19
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the meth god 
Regular
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Re: I2 Recovery from rxn fluid
quote:Originally posted by kneedragger:
Here is one from the Hive. SWIM has not tried it.
--kneedragger
SHORTY
(Hive Bee)
07-27-03 05:51
No 450132
Recycling Iodine
(Rated as: excellent)
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.
Chemicals
Dh2O
18% H2O2 Hydogen Peroxide (lower concentrations will require less dh20)
37% 12Mol HCL
Methanol
(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 doesnt have to bee dry and its easier to squirt it than pour it. Any alcohol should suffice.)
Materials
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
rubber bands
Method
Step 1
Pour the basic post rxn solution through 2 coffee filters into the 2 liter soda bottle. This may take a while but if you dont 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.
Step 2
Next add the same amount of dh20 to the 2 liter. If using 3% H2O2 then dont add any dh20. Other concentrations should bee calculated accordingly.
Step 3
Add approximately 50ml of hcl to the soda bottle and cap and shake. Release the pressure between shaking.
Step 4
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.
Step 5
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 doesnt 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.
Step 6
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.
Step 7
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.
Step 8
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.
Notes
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 12 long piece of 4 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 bbs. It changes from blue to pink when it has absorbed its capacity.If you cant get silica gel you use other drying agents but I wouldnt 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 cant 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 doesnt 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.
This works!
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#5
 2003-11-18, 21:58
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kman 
Regular
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Re: I2 Recovery from rxn fluid
Haven't seen anything about I2 recovery on the hive, but there is a method in the crystal creations part of the chem section on rhodium.ws,.
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