Yes, but probably more efficient. I'm thinking that it would still contain some constituent of the turpentine. I'll explain why below.
Here are the rest of my first run results:
Note: Most chemicals used are from the hardware store, photo lab, etc. This is for the sake of an easily written OTC procedure, should this experiment pan out.
Upon standing overnight in the dark, the water layer completely cleared, except for some odd clear globules stuck to the sides of the glass separatory funnel. Due to these globules, the water layer was gravity filtered through a Whatman qualitative filter paper into a clean beaker. The turpentine layer remained in the separatory funnel.
Using the calculated theoretical maximum amount of HI now in solution in the water layer, an equimolar amount of strong base (NaOH) solution was prepared with a volume of 30mL to make the upcoming titration volume a little easier to gauge.
Entire water layer remaining was neutralized with the weak NaOH solution. It took about one-third of calculated maximum, leading one to believe that only one-third of HI possible had been produced and/or had entered the water layer. Bear in mind that I'm not using a precision balance chamber here, only a 0.1g accuracy scale.
At a pH of 7.0, mixture had a slight terpene-like odor, but not nauseatingly so like pure turpentine. Approximately half of the volume was removed and dried to produce a yellowish gummy substance (pine resin perhaps?). A cold acetone rinse revealed whitish to yellowish crystals, presumably NaI.
To the remaining aliquot was added 5 mL muriatic acid (31.45%). As I don't titrate my own Iodine anymore, the exact ratios escape my memory. Volume was doubled with 3% H2O2, upon addition of which the solution turned immediately brownish orange, with no noticeable heat release. Since no noticeable Iodine precipitated (pretty dilute solution here, no surprise) my favorite chem-hack method was used to test for iodine. A small portion was dripped onto a bleached paper towel. Instant purple success (residual chlorine knocking the iodine out of its comfortable home?).
Of course, one experiment doesn't prove success, and the method will need to be refined. The water layer apparently had some residual terpene-like product in it. However, it was postulated above that this might actually recycle iodine during the HI reduction reaction of ephedrine (jump that gun, elementary).
Distillation is the way to try to get a more pure HI(aq), and would eliminate any concentration questions, provided that no terpenes were present in the HI(aq). Or, as Foxy2 stated, bubbling the produced HI into a massed quantity of H2O until a desired mass was reached would help with this. As I have a gun-shyness about distilling acids, this is a good method for me, if it proves to pan out.
I never have liked turpentine due to the odor. I'm starting to fall in love with it, though.
I just noticed that the patent seeker stated that upon standing, the HI breaks off causing condensation of the terpene (organic not my forte, did the halogen attack the double bond on the alpha- or beta- pinene? If so, can some organic genius determine the nature and name of the formed condensation product? The structure of terpene is easily found). That may explain why the turpentine layer went from orangish-brown to yellow spontaneously and rapidly upon standing.
Preliminary findings (subject to more experimental data):
Yes, one can combine turpentine with iodine crystals and produce an acidic solution containing the I- ion, likely to indicate HI. The residual terpenes in the HI (if any) may not hinder the reduction of ephedrine, and may actually help to recycle iodine. Why was my water layer clear, and not brownish like most people think of HI(aq)? Because it didn't get the chance to oxidize any iodine back. The pure appearance of 57% HI is clear and water-like. I may expose some of the next test run to UV light to try to get the gradual browning expected.
Coming soon, larger scale experiment, producing about 100mL of HI(aq). I will try to get a stronger concentration, and titrate precisely to determine HI concentration. If this run proves out, HI(aq) will be passed on to the man who knows this guy who might have a use for HI(aq) to, uh, clean silver or something, and reduction results will be posted.
Any questions, tips, advice, etc.? All feedback is appreciated here! This seems amazing to me, glad for the push-off in this direction Elementary , PolySam, and terbium.
Normally, I’d kill for some redP. If this works, I may be smoking pole for turps (kidding, just kidding).
"Wyatt, I am rolling."
