help with non polar extraction...

[mickyfinn]

Apologies fellow bees,

Retention has been problematic due to lack of medication and all the review, research, and trying to apply lately.

SWIM took a left turn and after following it forgot it wasn't actually a main road but a shortcut. For whatever reason, SWIM  takes a little longer to understand or retain some things, even with excellent write-ups a guide. SWIM has read that post workup article 3 times and is about to go through it in the lab step by step...he will be taking copious notes in hopes of refraining from making further erroneous assumptions in the future. He will do his best...

Note to self: PM the question to someone next time instead of taking the thread on a tangient, if they don't reply - no worries.

Once again SWIMFINN apologizes for any inconvenience and will now return you to your previously scheduled dreams..already in progress.

[ChemNewbie]

In the past, when i did use the gassing method, i would add dh20 to the np after gassing and seperate the dh20 and evap.

Swic does the same thing, to make sure he gets every little bit of product out of the NP. He even takes it a step further, by evapping the NP sometimes, and recrystalizing the resulting nasty looking gooey shit in ISO, and tone in the freezer. You'd be surprised just how much product gets left half dissolved in the NP layer from not getting the pH quite low enough.

[SHORTY]

When titrating there is a visual indication when the ph is 7 or below.  If you do a wash with saltwater and after shaking the saltwater and flipping over the sep funnel, observe the upper part of the sep.  It will look like it is dry and will not have any drops of water on it. Well i noticed that the same thing happens when you reach the ph at which the salt is formed.  Sometimes there will also be small drops of water on the sep in the np layer.  These droplets will not be there when the ph is 7 or below.  Using this as a indicator has saved me alot of time which would have been spent checking the ph.

[wareami]

The kidz did away with pH testing long ago when they took Jacked's advice about relying on visuals.
Since their experimentation only allowed for small batch testing, getting the maximum return required more observation than they initially started seeing when they began.
SHORTY makes an interesting point about the dh2o that collects, stuck on glass style.
Ibee was amazed how much product he was leaving behind by not forcing those droplets down into the acidic pool.
Ibee's experience also slightly differs from shorty's in that pH 7 and less is when the amine is in the water, those droplets of honey infused dh2o will always be stuck on glass if not washed down with a pipette or other sucker UPper device.
The shape of those bubbles also has a story to tell in most cases!
Here's a link to what Ibee discovered early on about stuck on glass bubbles and what to do with them. Just force them off the sides with Ibee's re-patented cleareyes pipette!

Post 370666 (missing)

(wareami: "SweetBee", Chemicals & Equipment)

[SHORTY]

For some reason when i see the bubbles on the side of the sep in the np section the ph is between 8-11.  Sometimes they are not there at all.  When i hit 7 or below they are never there and the the upper part lools completely dry.  Do you think humidity or ambient temp might be a factor causing the difference between my findings and yours?  My lab is very hot and humid most of the time.  I just figured that the same thing was happening as when doing a saltwater wash of the np.  Only instead of adding salt the salt was the meth.  If that makes any sense.

[wareami]

One of the most interesting bubble observations occurred during the extensive full conversion testing. The Kidz were able to associate the dh2o bubble sizes and shapes with the amount of unreacted.
This will take some fancy descriptive footwork on Ibee's part and some imagining on the part of the reader.
Let's say that a tall spice jar is used to collect the honey laden NP(175ml) To that 50ml dh2o is added along with
9 drops HCL. This is shaken. The area above the NP/dh2o will contain dh2o/amine stuck to the glass. Most pure water droplets will either be  round or teardrop shaped.
A fully reduced product will cause some of the stuck on glass droplets to appear horizonally and bee bigger in size.
NP that contains some unreacted will be very small bubbles and grainy looking or sandy looking.
Ibee has always maintained that short of having a reliable analysis instrument...he uses many less accurate determining factors, that when combined account for accuracy. And then there is always the Bioassay for concrete confirmation.
Many things can be looked for that are often overlooked or dismissed as having little value.
Those stuck on glass bubbles account for missing yield in most cases, regardless of how small!
Peace of the _REaction
Have FUN-Bee SAFE

[ChemNewbie]

Good ta see ya. 
Those missing yields are the biggest reason Swic switched from titrating to gssing. That, and the fact that he hated standing over the fucking stove for an hour evaporating water. The final product has a different taste to it too. The gassed meth had very little if any taste. The titated goodies always tasted burned, or something, even after multiple recrystalizations. And no Swic didn't burn the stuff, as he uses very little heat. Plus gassing is just easier. And quicker. And more forgiving.

CN

[SHORTY]

I have found the exact opposite to be true.  It must be the humidity.  But then again if one uses the same method over a long period of time then he will eventually be better at it.  I know that when i first started i had all types of problems that i never encounter now.  If i ever get an a/c in my lab i will try my hand at gassing but until then i have to stick with titrating.  I can do the post rxn workup via steam distillation and titrating and bee finished in less than 1 1/2 hours.  It used to be an all day project.

[Jacked]

Ever noticed when the np is rich with Fb when acid is added when it comes through the interface it looks like wrinkled water swirling about, When the ph is around 8 or so when acid is added it comes through the interface as bubbles heading to the bottom of the sepfunnle and then back up again...In amounts of h2o to use, thats simple, the more material the acidified FB molecule has to move to the more that will move there during ph adjustment, meaning more Honey on first pull than if less was used.. Turning a three pull event into a two pull event with the last only needing a few drops of acid to bring the ph to 7 or below..Swim Tries to hit 5 on the first pull and in most cases a second pull only yields maybe 10% of expected outcome maxmum. The excess acid when at a 5+ on the ph scale evaps off the finished product towards the end, just be careful not to xtalize by rapid evaping of the H20 this will trap an acid molecule inside a crystal formation of meth. Hard to clean with acetone because acetone wont come into contact with any entrapped substance..  The same idea of "more is better" is employed in the post rxn workup with Np solvent.. Basifying the rxn mixture. With enough room for FB to move to, more gets there on the first attempt leaving a second pull only for shits and giggles.(Not realy)... Swim uses his second pull in standby while pushing his dope from the non-polar to the polar, when or if the ph is over shot you can add the second pull and bring the ph back up without making table salt and sometimes saving your ass from an acid smelling evap that yields dirty xtals....

[ChemNewbie]

Swic has noticed the exact same thing on the rare occasion that he does titrate. He uses quite a bit of water compared to most, and doesn't shake the sep vessel at all (Started doing that after he figured out that all the good stuff was sticking to the sides of the damn sep vessel). At best he will stir it gently with a bamboo skewer for 30 seconds or so, and then sit back and watch as the ribbons of FB spiral down into the polar layer and dissapear, sending bubbles up through the NP layer. The ribbons usually reappear a few minutes later in the water layerin a saturated solution of Meth HCl. The appearance of the saturated H20 layer is the signal to Swic that it's just about time to drain off the water.    That's about the only thing Swic really likes about titrating; The fact that you can actually see some of the chemical changes taking place while they're happening, and know exactly what's going on at that very moment.
As far as humidity goes, it doesn't play very well with gassing. Swic lives in a very humid climate (during the spring and summer months) and had problems for a while with moisture hampering the whole process. He overcame this problem by building a 3x4 foot dry/clean room in the corner of his work area. Originally he had a small de-humidifier, and several large containers of CaCl2 sitting around in certain areas. This seemed to work pretty well, but it got hot as fuck in there sometimes. And now that Swic has started spending more time in there experimenting with NH3 generators he needed to cool it down some. So he went to the local thrift store and got a small non-functional A/C window unit for free. All it needed was a new relay (2 bucks at electronics store) and a freon recharge, and it was good as new. Now Swic's little clean room stays in the low 60's all the time. And no more gassing problems.

CN