Swip heard about a bee who had tried another approach to the degakification of feedstock, that in his opinion looked promising. At first he was considering sharing only with a few who have been especially helful, but then he read a bit of Geez's "making me sick" thread and reallized that others are probably having similar problems. SWIP was. So he decided to share what is thus far an unperfected technique, in hopes that others may improve on it.
However his decision to share didn't come before he had already contacted the fist bee on his list, and this was another reason he decided to tell me to post the information now. He heard nothing for several days after sending the PM. Finally it dawned on him how he might react if the situation had been reversed--especially considering the kind of questions he was asking. (Sorry, Shorty. SWIP was feeling enthusiastic and didn't think it through.)
As a final preface, SWIP wants to again emphasize that this procedure has not been perfected, it just seems better than the presently available alternatives, and has been working moderately well for SWIM for several weeks.
Here's what SWIM's acquaintance said to do:
Grind up some 120's as fine as possible and put them in a beaker or a glass that will hold them without being more than about 1/3 full. Run out to the grocery store and buy a bottle of ammonium hydroxide, or as it's usually labeled, household ammonia. (Don't get sudsy ammonia!) Also pick up a box of washing soda if you don't have any. Poor some [edit]ammonium hydroxide [/edit] into the glass with the GUPS--not too much, just enough to turn them into what looks like smooth marshmallow cream.
Pause a moment to laugh maniacally as the GUPS turn to slime--a pitiful attempt to thwart your intentions.
Next take your jar of washing soda and add a volume approximately equal to the marshmallow creme. The amount isn't critical but it's better to have too much than too little. Stir well, pressing the washing soda into the creme as thoroughly as possible. Now add xylene. Again, be generous, but not so much that you will have trouble getting the pfed back out of it. Stir this mixture and right away you may notice the volume decrease as the freebase disolves. Let it sit for at least fifteen minutes. Leave it overnight if you wish, or continue on immediately. Decant off the xylene into a funnel with a moderately compacted cotton ball in the barrel and a coffee filter. Gass the pfed to extract. Be patient during the gassing. SWIP says he was used to having the pfed fall right out, but that it took much longer than usual. (Maybe his HCl generator wasn't working well?)
After capturing the product in the coffee filter, rinse off the xylene with some acetone, and allow it to dry.
Now go back and do it again for better yeild, beginning by pouring the xylene back in with the GUPS. The second time through you might want to add a little dH2O*. No more than 5ml for two 20 count boxes of feedstock. Swim hasn't yet determined the optimum amount, just be conservative. When you finish, pull again and again until you're happy with your yeild. SWIP doesn't think heat helps at all, and in fact may cause you to pull some gak. If the last pull you made is sparse but you're nowhere near the theoretical yeild, add a bit more dH2O.
When this is all finished, combine the fruits of your labors in a beaker and add enough concentrated NaOH solution to thoroughly wet the product. Stir well until it's all been converted to free base. Add a little more NaOH if you aren't sure. Then add dH2O in about the same quantity as the liquid already in the beaker. Swirl and filter through two coffee filters. Rinse again 2-3 times with cold dH2O, and don't discard the rinse water. [When you have saved enough of the rinse water to make it worthwhile, add a layer of xylene to pull, separate then gas to recover more pfed.) Spread out on a plate to dry, but don't use heat. Remember, pfed freebase turns to vapor at a reletively low temperature, and even warming it will cost you yeild.
While you're waiting, take an ehrlenmeyer flask and match it up with a test tube with a diameter nearly the same as the mouth of the flask. If what you have is too small, cut rubber strips from an inner tube about 3/4 inch wide. Wrap this around the top of the test tube, stretching it snug as you go. Keep at this until it makes a nice snug fit with the mouth of the flask. Now cover all of the rubber with several layers of teflon tape pulled snug.
Crush some ice and fill the test tube, dump your dry freebase into the flask and insert the test tube. It should fit snuggly enough that you have to push with moderate pressure to seat it in the flask. Not so much you rusk breaking it, but enough that you don't have to worry that it might fall inside. If it's too loose add more rubber and teflon. If it's too tight, take some off.
Now place the (borosilicate) flask on a hotplate or a burner covered with a flat metal plate. Don't try to substitute anything else. Cups and jars can't take it and may break explosively. (Also, don't ever put your glassware directly on heating coils!)
It's a little tedious the first time through this because you've got to find just the right setting for your hotplate. Turn it on but keep the heat very low. Wait five minutes and if the freebase isn't melting, turn up the heat just a little. Keep at this until you find the setting that will just cause the freebase to melt and subsequently vaporize. If you mark the spot on the hotplate you won't have to go through this again. Having found the right temperature you might want to watch it for a few minutes to make sure it isn't going to get lots hotter as soon as you turn your back, and once you're satisfied set up a fan to blow on the outside of the beaker and go do something else for 1/2 hour. If you think of it, come back after fifteen minutes and suck out the now melted ice from the test tube with an eyedropper, and replace it with fresh. Try not to distrube the beaker though, because the crystals will fall back to the bottom and melt again. Not a big deal, just another few minutes wait.
After 1/2 hour take a look, and you should see the sides of the beaker are now coated with freebase crystals, and there will likely be some gak at the bottom that hasn't done much of anything. Remove the flask from heat and set aside to cool, being as gentle as you can so as not to disturb the fragile crystals. When completely coooled turn off the fan, and carefully pull out the test tube. Holding it over a container, scrape the crystlas from it's sides. Invert the beaker over teh container and shake out the loose crystals. Finally, reach a scraper into the beaker and scrape the remaining crystals off of the sides and into the container. The clean crystals will be found on the side down to just above the bottom of the flask, and it will be easy to see where you want to stop scraping. Be careful not to scrape loose any of the gak at the bottom.
*On dH2O, listen to what everyone has been saying lately. If you don't believe it makes a difference, the next time you need to mix up some NaOH, mix two batches. In one use dH2O and in the other use tap water. It may not be immediately obvious, but after a few days the batch made with tap water will have particles floating around in it--a really visible contamination. SWIP used to think it was because his drain cleaner NaOH was poor quality but he was wrong!
Looking forward to hearing of improvements and other comments.
PP