iodine wont go away

[WHO_ME]

swims last few dreams have been nasty with iodine everywhere......swim does his usual dream only now he uses tincture instead of the usual feed store I...and each time there has been i left over after the dream....could this be from lack of cleaning or is swim just not cooking long enough....the quality of product has suffered the last dream...but was still alright...what is causing the excess iodine?

[unionpacific]

what are you talking about .. tincture comes from the feed store.

are you washing your rxn fluid with NP x3?
how long are you cooking?

[WHO_ME]

down this way we used to get the I pellets from the feed store...but now all they carry is the tincture...and i cooked the last time for bout 2 and a half hours using a push pull setup..

[SHORTY]

Two and a half hours isn't long enough for a rp/i synth.  What are your ratios i/e/rp/dh20?  How can you expect to get a decent answer if you don't provide more details?

[WHO_ME]

the rario was 140g of e and 145g I...and 48g of rp...the rp was lab grade and the I was tint...second time using the tincture.....in prior runs i always used similiar ratios and never had any trouble until i switched to the tint...im trying another run....will allow more reaction time and see how it comes out..

[unionpacific]

When you use I from tinc make sure it's dry or it will contain water

[LukkyDMethod]

If I ever get so lazy and impatient that I try to waste that weight of precursors with a 2.5 hour cook, please just shoot me. 

Why not go way longer and get yourself a heavy duty liebug condensor?

That's just way too much good product to hear about going down the drain.  SWIL has never even seen lab-grade RP, and if he did, he would probably treat every gram like gold!  Quit taking your shit for granted, and put some effort into this reaction. 

Lukky D

[xboXer]

take a few to make your own RP. for a scant 3 weeks, a month at the most, you have a kilo min. for the cost of running a 220 tombstone welder on a boneash/charcoal/silica mix. Then heating the WP under vac, or in an argon aptmosphere for a couple days on the barby (gas, not kingsford)
Just flood the argon well while allowing the H2O to evap. and dump back into a bucket of H2O (warm/hot) to rinse out any unconverted P when finished. Rinse 3/4 times, VIOLA' RP

For lab grade, ya gotta do some work, but hey, only once if you make enuff...

clear head and a set of common sense/wits/sobriety is req.

[SHORTY]

the rario was 140g of e and 145g I...and 48g of rp...

How much dh20 was added?  If you were to use these same ratios along with at least 120ml of dh20 and used a condenser to reflux for at least 24 hours you would be rewarded with a high yeild of very potent meth.  I would think that with that much it would be well worth the "weight".

[wareami]

of the iodine source, iodo-sides will always be present in shorter cooks. Even fullblown long wet refluxes if the ratios aren't just right.
Get some sodium thiosulfate from the photo store.
Use a small crystal or 2 to oxdize the free iodine from the yellow honeywater.

[geezmeister]

The fact that the I2 is from tincture is not of any particular significance, nor is the ratio of I2 added, which is acceptable in this size reaction but edging toward the low side. The low ratio would not give you excess free iodine in the reaction fluid. It is there because it has not be recycled into HI. Why not? Problem is not the iodine. The problem is likely the phosphorous. It may have been lab grade, but I  suspect it has been used a couple of times, and probably got coated with something that got through with the pseudo. A longer cook time would do wonders for the product and the yield, if the red phosphorous were cleaned before use. Soak it first in some some MeOH, then rinse it with acetone. See if there is any waxy trash that comes out of the red phos or if the acetone comes of yellowish and thick. If so, your red phos got gakked. That coated red phos was not available to recycle the I2 to HI and you had excess  I2 available in the reaction fluid.

My guess, any way. You really provide to few details of the reaction to do much more than guess.

[wareami]

This is why Ibee felt the excess free iodo's might be present as well.

Even fullblown long wet refluxes if the ratios aren't just right.

Not the iodine but the lack of HI created as evidenced by the ratio's stated
almost a two to one ratio of I2 to RP.
That doesn't cut it if a full reduction is to bee expected.

Peace of the reaction

Have FUN-Bee SAFE