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help with non polar extraction...

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Nuniabiz:
well all this time and still a stranger, swin generally feels "read more, pester less" but has come to a point where he has no other choice.
in following swigeez's post rxn workup he has reached a point of confusion as hesay's his immaginary friends usually steam distil but the denser is broke so they dreamed they would have to use naptha. In swigeez write up it says to check the ph of the rxn fluid as the non polar will have no reading per say so after basing and extracting with the napptha he then say's to titrate the np to neutral? but if it has no reading how can you bring it to neautral?
the dream went like this. swin based without the non polar present but added it immediately after and shook let sit them seperated did this three times and has athe naptha seperated but the ph is already below neutral so he is lost in his dream.

could he reacidify the rxn fluid and base with non polar present or should he just evap the NP as is. to his nose he dreams it smells like the amines are still in the rxn fluid but could very well be wrong. anyone who can offer help would be most apreaciated as its dream time and pressing on thanks in advance
stay safe
Nunia
ps rp/i rxn red filtered and washed with xylene and vm&p napptha then based and more naptha added to extract 3x

cthulhujr:
ok...one more time

base the post rxn solution
extract with non polar
   the fb will go into the non polar
rinse the non-polar with clean dH2O
then add some more clean water
titriate with acid so the stuff leaves the non polar and goes into that water you just added.
the water you just added is where the ph is checked until neutral...not the non-polar.

clear as mud now??

Read every post an the Stimulants FAQ 9 times and write "I'll be a good Little Bee and do my homework" on the blackboard 1,143 times

You don't want to end up penniless, clueless and insane like swic do you??

stereoIsomer:
To add one more clarification- your NP should be naturally ATOP the water layer. It is the water layer you want to test PH in.

How do you do this ?

If you DIP a PH strip INTO the NP to get to the water, you will coat your PH strip with NP and it probably will not register PH.

Here's where the use of a Separatory Funnel comes into play. You should already be doing the titration IN a Sep Funnel- but basically, the purpose of the sep funnel, the mechanics of a Separatory Funnel are such that you can DRAIN the lower (ie aqueous, ie water) layer DRIPWISE onto a PH strip and test it's PH.

There are many "ghetto" methods for making a sep funnel including using ziplock baggies in which a trickle-hole gets punched in the bottom, but I'd say the most valuable post rxn piece of glasswear you can own is a SEPARATORY FUNNEL. They enourmously facilitate these last steps- including the shaking, washing of the NP.

peace!

ChemNewbie:
Hey man. These other guys covered most of it, but here it is again anyway.

-Wash post rxn fluid 3 times with xylene or naptha (NP)
-Add fresh NP 1/3 volume of post rxn fluid
-Add saturated (1:1 ratio) NaOH solution until pH ~13-14
-Stir/Swirl vessel for a few minutes. Let layers seperate for at least 15-20 min.
-Remove NP layer from water layer by suctioning with a large syringe (Meat marinade injector)
-Add fresh NP to vessel
-Repeat steps 4, 5 and 6 a total of 3 times.
Combine all NP pulls and wash with cold water, then hot water, then one wash with a 20% NaOH solution.
-**Add dH20 1/3 the volume of NP
-**Add HCl acid dropwise until water layer is pH 6-6.5
-**Remove water layer from the vessel by suctioning it from under the NP layer with a DIFFERENT syringe that has a short piece of tubing attached.
-**Repeat steps 8, 9, and 10 a total of 3 times.
-**Combine 3 lots of dH20 and evaporate over very low heat until surface has skinned over, then quickly pour in a large volume of cold, dry acetone to "flash" the dH20 and crash out any remaining product. Pan the meth to one side of the dish, and decant any liquids into a jar or beaker and place in the freezer for later crystal collection.
-Scrape up the meth after it has dried, and wash well in acetone before using.

**Swic really prefers gassing to titrating for better yields, and at this point, after the wash with 20% NaOH solution, he simply dries the NP well with baked Epsom salts, decants the NP off of the Epsoms into another beaker, and gasses until no more meth precipitates from the NP. After filtering the meth out of the NP, the crystals are rinsed thoroughly with cold dry acetone, and allowed to dry. The cake of meth is then dissolved in a minimal amount of boiling IS0, and acetone is added until just before the solution starts to cloud. Then the beaker is capped off and placed in the freezer for the night. Clean, shiny meth is then harvested from the beaker the following morning, and quickly rinsed with cold acetone and allowed to dry.

This is just one of about 800 million different ways to accomplish the same thing. Do whatever works best for you dude.

Later

CN

SHORTY:
Swic really prefers gassing to titrating for better yields

I disagree with this statement.  If done properly the yeild should be the same whether gassing or titrating.

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