I'm not sure I follow what you did. You were doing a big STE extraction of white sixties, and caught the alcohol/naptha solution on fire while you were boiling off the alcohol to precipitate the pseudo?
You must have burned off the alcohol and some of the xylene and naptha to have burned pseudo in the pan. If you put the fire out and there was no pseudo in the pan, you still had the pseudo dissolved in alcohol and should have let it cool, then resumed the extraction method with safety equipment in place and cleaned the pseudo after finishing the extraction.
Sounds like you were lucky you didn't burn the place down. A liter of boiling naptha is an angry monster to deal with. Two gallons is putting the monster on steroids. You are lucky to be alive, much less worried about the pills.
I assume you were boiling off the alcohol in the naptha/xylene solution when it caught on fire. The fire burned long enough to burn off or boil off the rest of the alcohol in the solution and some of the pseudo may have precipitated. You burned off some of the naptha/xylene solution.
You filtered this solution. If the pseudo had precipitated, you would have pseudo in the filter. What did you filter out of the solution? If there was pseudo in this mix, you should dissolve it in alcohol and recrystallize it a couple of times.
I take it that you washed the STE naptha/xylene solution with a gallon of water, separated the water out, added xylene, and based the water layer with straight NaOH in an aluminum pan. Not all of the NaOH dissolved and a lot of it settled to the bottom of the pan, and began reacting with the aluminum. When you discovered this you poured off the water/NaOH layer.
It would have been very helpful here to have washed the xylene with water. You sound as though you washed it with a very small amount of water... and you should have done several water washes and a brine wash at this point, or even a wash with NaOH solution.
You titrated the xylene, evaporated the acidic water to get a brown powder with white flakes mixed in it.
What a nightmare. This wasn't a bad day, it was a bad month.
The brown powder should contain a lot of the pseudo. I don't know what all else it may contain. I don't know if the white crystals are pseudo or not, since you don't describe them. They may be, but they may be several other thngs as well.
Dissolve all of the brown powder in alcohol. I suggest methanol, but denatured is fine. Filter the alcohol through a sand filter. You could use a charmin plug, but I suspect you need a better filter here. Take a two liter soda bottle and cut the bottom off, put a few cotton balls in the neck of the bottle to hold the sand in, add a bout an inch of activated carbon, then add about four inches of sand. Pour out a measured quantity of alcohol, pour it in the filter and let it drain. Measure how much alcohol drains out, subtract from the amount you started with, and write the number down somewhere you can find it in a little while. This is the amount of alcohol to use to rinse the filter after you pour the pseudo solution through it.
Filter the alcohol/pseudo solution through the sand filter. Yes, it will take a long time. Don't hurry it. You can stir the top of the sand to make sure the filter isn't clogged up. When the alcohol finishes filtering, pour the amount of alcohol you calculated earlier through the filter and collect it and add it to the other alcohol/pseudo solution you filtered. (I assume you don't have a vacuum or a buchner funnel. If you do, you don't need me to explain how to use them in this juncture.)
With a fan blowing across the container you have the alcohol in, slowly reduce the volume on low heat until the solution is saturated; add acetone and stir well, allow the solution to cool to room temp, then move it to the refrigerator and let it form crystals. If you aren't familiar with dual solvent recrystallization, read up on it before you start. Check the Newbee forum sticky threads, and the stim forum digest thread for posts on the subject.
If you get pseudo crystals, you will need to do the process again--- dissolve in alcohol, filter out any solids, reduce the alcohol to saturation, add acetone, cool and allow crystals to grow.
If you don't get any crystals to grow and the solution is now very cold: Heat the solution up slowly, stirring, watching for any precipitants to form. If you have precipitants form as you heat the solution up, filter them out and continue heating the solution. Look for them around 50-55C and again around 70C. As the solution thickens, flash with acetone, pan the acetone around well, let more of it evap, flash again, pan, let the pseudo settle and pour off the acetone (save it). Rinse with fresh acetone. Add that rinse to the first acetone. Put it in the refrigerator. Some pseudo may form in it as it cools.
The pseudo should recrystallize now if you repeat the crystallization process. If it does not make crystals this time, you probably have polymers in the mix that your extraction method did not deal with. (I assume the pills you used are the cleaner type white 60's; if not, you need to read the recent extraction threads in the stim forum. I don't want to address those extraction issues here.)
If you still can't grown crystals, you can evaporate the solution, flash with acetone, then do another a/b. You could also dissolve the pseudo in alcohol and precipitate the pseudo in xylene to help clean it, but I am leery of recommending this particular method to you. I suspect you are a little skittish about boiling solvents right now, and you should be.
I don't know what the sparklies in the brown powder are. They could be several things. One of them is pseudo. Several others are not. The ones you don't want in the mix mostly won't dissolve in alcohol. The crystallization method will do a lot of cleaning. If they dissolve in alcohol, chances are you want them. If they don't dissolve in alcohol, chances are you don't.
You can substitute water for the alcohol in the crystallization process, given the quantity you are working with. I do not recommend water on the first attempt at crystallization. Alcohol will not dissolve a lot of impurites that could be in the mix; water will. Get them out as early as you can. Done with growing crystals?
NOW---Go back to the naptha/xylene solution. Heat it up to 105C and see if anything precipitates. If you have a white precipitant, filter while the solvent is still hot and rinse with MEK immediately. Recrystallize this with alcohol and acetone.
Do an additional pull or two with xylene on the lye water. Do put it in a non-reactive pan to do this. You may have additional pseudo in the water layer. Titrate the first portion of naptha again. It may yeild more pseudo.
Be careful with boiling solvents. The safety information is there for a reason. I've had fires myself, and more than one. I've burned myself several times, and burned myself seriously on one of those occasions. I know you have a real problem trying to recover the pseudo, and I hope my comments help you.
I do suggest that you take the time to read the material available in the stim forum and on Rhodium's site before you go any further. Do go over the dual solvent recrysallization material if you are not familiar with it, and do it before you attempt to recrystallize the pseudo.
And good luck. You have to have some, or you wouldn't have been around to ask the questions you asked.
