post reaction workup problems

[zorilla]

[DarkSky]

zorilla, It's hard to tell from your post so I guess Ill ask, exactly which layer did you "collect", to use your words? The Top or bottom layer? It sounds to SWID like you "collected" the bottom layer, else why would you add more naptha to it before you attempted to titrate?

[zorilla]

i collected the bottom layer.it was the clear liquid ..i posted wrong i didn't add more naptha.i'm so tired trying to figure this out i can't even think.

[Osmium]

Then go to bed and continue tomorrow.

[zorilla]

i've searched the search engine here for at least 6 hrs.i cannot find any information about not having 2 layers after adding muratic acid .i've also searched the rhodium archives.
   up to this point swim thinks he has done everything right.

[ChemoSabe]

Once you've again had your fill of sleep read this post carefully to see what you might have missed.

Post 485240

(ChemoSabe: "Post Rxn", Stimulants)

Also you need to give much more detail of exactly what you've done for each step of this process for anyone to really know exactly where you are and what you may have neglected.

If you are dealing with muriatic I would assume that you are trying to salt out or titrate the freebase from your NonPolar solvent. If you really do have your NP sovent isolated and water washed then you might actually be ready fo this step. If you added muriatic and no layers are apparent it's logical to assume that before you added muriatic you neglected to add 20ml of dH20. Or, if you premixed the muriatic into a dilute solution first and then added it to the NP then you must have accidently used something other than dH2O which is miscible (won't form a layer with) with your NP. I think acetone might behave similar to this if used in this manner.

That's the best guess I can make with the info you gave but if something prior to this was done substandardly you might still be a ways from truly being at the titration stage.

Sleep 1st. then double check your procedure with the post accesible throught the red linked post above.

[zorilla]

yes i am trying to titrate the freebase out of the NonPolar solvent.i premixed muratic with dh20 and i'm sure it was distilled.
  after adding the cooled lye and dh2o mixture to get the dead fish smell my liquid was on the bottom.maybe this is the problem.

[ChemoSabe]

Adding the lye is what pushes the freebase into your NP which optimally will be warm or hot naphtha. If you have not completed adding the lye (basing up) then the freebase has not yet fully migrated and you are not ready for titration.

If you happen to titrate the lye water you end up synthing sodium chloride. Otherwise referred to as common table salt.

Did you go over the post I linked to previously? IT covers everything you should be double checking now to know if you're ready to titrate.

I still think you should sleep some and then compare what you've done so far with that post I linked. The info up to titration is all there in (relatively) no uncertain terms.

[DarkSky]

zorilla, I’m going to try and be as clear as I can here. After you finish your rxn you take your honey and dilute with 5 times it’s volume of DH2O, I assume you did this. Now, you should your honey first this but I’m not going there right now because that’s not where your immediate problem lies. After cleaning the honey you add 200ml of your NP of choice, then you add a lye base solution to this mixture raising the PH to 13. You said you did this so you are with me so far, right??

Anyway, you stir this up gently and let it set for 15 to 30 minutes then….now listen very carefully to what I’m about to say, you take the TOP LAYER, THE ONE WITH THE NAPTHA and use that for your titration. Now SWID has never used Naphtha but, unless he is mistaken, it floats on TOP of water, not on the bottom. The product in the honey/based solution moves to the top layer, into the NP, when you get the PH above 13. From your reply to my question you stated you collected the BOTTOM layer which happens to be the layer with the freebase in it! Of course you not going to get any separation of layers, you added water with acid to water with lye….guess what water and water DON’T separate! I hope you kept the naphtha that you removed from the base solution, you can take that and citrate it to recover some of your product.

However, all is not lost! Take the aqueous solution, you know the water/lye with water stuff you just made, and add more lye solution to it to raise the PH above 13 again. Understand this, you have added acid to this solution so it will take a little doing to get the PH up but you can do it. Also, you should be prepared, because of this total brain fart on your part you are going to lose some of the product you could have otherwise recovered if this had not happened. Don’t be surprised if you only get 30%, maybe 40% back if you are lucky on the E you invested.

Here’s a link for something I think you should read, it will save you a lot of heartache in the future. Copy the link and post it in your browser address bar and it will take you there. Good Luck!

Post 428410

(geezmeister: "The post-reaction workup: a cook's summary", Stimulants)

[zorilla]

well swims dream got better.added more lye and water solution.now my liquid was on top.decanted the liquid.added dh2o and muratic acid shook like hell;evaporated the good stuff and cleaned with acetone.yields were low but what i got in this dream was superb.thanks for all the help.geezmeister's post reaction is what i was following.guess i just didn't digest the info right.