Nuniabiz (Stranger)
06-14-03 19:14
No 440063
      help with non polar extraction...  Bookmark   

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
(Hive Bee)
06-14-03 19:47
No 440067
      ok...one more time base the post rxn solution...  Bookmark   

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??

I-R'lyeh! Cthulhu fhtagn! I I!
 
 
 
 
    stereoIsomer
(Stranger)
06-15-03 04:09
No 440130
      The purpose of a Sep Funnel  Bookmark   

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
(Newbee)
06-15-03 06:47
No 440146
      Wuddup Nunia?  Bookmark   

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

Just fuckin'do it already
 
 
 
 
    SHORTY
(Hive Bee)
06-15-03 11:02
No 440170
      Better Yields?  Bookmark   

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.

It wasn't Me!
 
 
 
 
    Coitus
(Hive Bee)
06-15-03 11:26
No 440175
      Yields  Bookmark   

I have also noticed better yields with gassing. It's probably due to my always going overboard on adding the acid when titrating.

You don't have to worry about ph when gassing, which makes it quicker and easier in my book. No boiling off H20 or evaping!!

COITUS
 
 
 
 
    ChemNewbie
(Newbee)
06-15-03 11:47
No 440179
      Theoretically, yields should be the same....  Bookmark   

And if everything went perfectly, there's no reason yields shoud be any less for the titrators. But, there are a lot more opportunities for little mistakes here and there with titration. There are several more steps involved, with chances to lose just a tiny bit of product with each one. I think Geez once referred to this as "Mechanical losses". (ie more liquids being transferred to more pieces of labware = more residuals left behind that may contain product).  But I will say that pH is still important in gassing to a degree, because Swic has definately managed to over gas a batch here and there, and caused himself more work during the cleanup process than should be neccessary.

Just fuckin'do it already
 
 
 
 
    SHORTY
(Hive Bee)
06-16-03 17:11
No 440389
      More steps?  Bookmark   

Im not sure what extra steps would be taken but i just add a little dh2o after washing the np, then add my hcl shake, check ph, shake, check ph, shake, check ph and drain into visionware pan.  I sometimes get the ph after the second shake and have managed to hit it on the first try a couple times.  But it usually takes three.  Anyways, when i gas i add a drying agent to the np after washing, a small amount of yeild may be lost in the drying agent.  By this time i have went from the sep to another vessel with drying agent then filter into yet another vessel and then gas.  So actually i do more transferring when gassing than i do when titrating.  Which is probably why i prefer titrating.  I hate washing glassware.

It wasn't Me!
 
 
 
 
    geezmeister
(Of Counsel)
06-17-03 08:00
No 440539
      humidity  Bookmark   

If you live in a humid climate, there will be times that titration will serve you better than gassing. Under very humid conditions, gassing can become difficult to do successfully. There is no real reason for the yields to be different except for lab technique and those "mechanical losses" to the sides of the glassware, filters, etc.

I know of lot of folks who gas and filter through coffee filters. This is a poor way to do it. Get some filter paper. You can wash a large amount of meth out of those coffee filters, which are absorbent filters. You can rinse most of it out, but it will be mixed with paper fiber and the oils, waxes, and trash the filter catches. You can titrate and never use a filter at all. Pan the acetone wash to a corner, then out of the pan, and let it all air dry.
No losses to filters. No paper filters in the trash. Less expense, evidence, loss.

Jacked told us that a long time ago. As ususal, he was completely correct.

Mostly harmless
 
 
 
 
    SHORTY
(Hive Bee)
06-17-03 22:07
No 440674
      Tropical Climate  Bookmark   

Your are 100% right geez!  I live in a tropical climate, which is of course always very humid.  On top ot that i have no A/C in my lab.  I never use filters for meth, i just decant the acetone wash into a empty acetone bottle and cap it then into the freezer for a rainy day.  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.  I then realized that i was wasting time and effort trying to gas and just started titrating.  It was a bit frustrating in the beginning trying to test the ph and shit but after doing it for a while its quite simple.

It wasn't Me!
 
 
 
 
    LukkyDMethod
(Newbee)
06-17-03 23:44
No 440712
      A/B problems?  Bookmark   

Nunia:

Almost there dude, but keep reading and replaying every step in that dream.  Down to every last detail, such as how your hand will pour the liquid!  Once one can do this successfully and understand it, they will begin to master the process of the A/B.

SWIL usually titrates.  And like everybody has been saying, the yields(in theory) should be the same.  SWIL realizes that in his reality, they aren't always the same.  See, SWIL has no seperatory funnel, so he is doomed low yields due to titration failure with the turkey baster and eye dropper technique!

Nunia, SWIN has come along way.  Tell him to keep reading, and maybe rather than beat him back under the stairs for his mistakes, reward him for his positive progress.

The art of the A/B is a crucial step.  Learn it, the time spent will pay in diamonds and $$$

Lukky D
 
 
 
 
    Nuniabiz
(Stranger)
06-20-03 06:43
No 441305
      thank you one and all...  Bookmark   

thanx all much apreaciated and all excellent advice. the problem was that my friends friend dreamed this dream with out any consultation and callled swin in to try to rescue his callamity.

a post rxn a/b and then steam distillation and titration was attempted on part of the rxn fluid which was in swin's eyes obviously contaminated with peg at least. bright yellow but it was swihis gig and swin was just to attempt to save what was salvagable.

he has decided where he went wrong.... if there was a complete rxn at all that is swin wasn't even in the neighborhood so??? can say. but when the washes were complete and basing was started swin unfortunately had not added the new NP and just based the rxn fluid alone in swin's mind though this should have only created a layer of freebase oil which should then have been picked up by the NP when added. is this not true? the whole thing has been put on hold while other dreams have been dreamed without peobem but waswte not want not as swin's pops used to say .
again many thanx for the responses and great info
stay safe
Nunia
 
 
 
 
    wareami
(Hive Addict)
06-20-03 10:37
No 441345
      Haste Makes Waste :  Bookmark   


waswte not want not



How true!
All of the answers were provided Nunia.
The initial conception of acid/base titration is ware SWIN got trapped under the stairs!
With the two newest Gaak's to hit the market, if they aren't removed prior to rxn, the post rxn workup is severely hindered by pH climates. Before with the one Poo-Tang, just the basing side was affected! Now a darker reddish orange substance has reared it's ugly head which in Ibee's eye's, reeks havoc on the acidity side.
Both will lock UP the Amine! You can titrate or gas your ass off and still come UP empty handed if you GO one Toke over the line either way!
SWIN: When basing the postrxn solution, always use an NP buffer on top of the Honey water! Basing straight will screw ya because of the pH testing and the time needed for the amine to move UP! Since SWIN is learning this newer strange A/B method, might as well do it right by including visuals, that rarely fail! Regardless of how bad they fuck with the pH to prevent amine mining!
Base with a 50% dilute lye solution...IN SPLASHES. Look for the ribbons to move UP into the NP. BASE NO MORE! Pull the amine loaded NP. Check the pH of the basified solution after pulling NP. Add fresh NP. Check pH again. If under 12.5pH, Add a splash of dilute NAOH.
You should notice a difference in pH....before and after adding fresh NP.
For some reason, this new shit (Gaak) is that sensitive to pH and locks the amine if overshot. And based on findings at Camp P2M, locking UP is occuring on the gassing side as well! Ibee could bee wrong, but he blames the redder orange Poo-Tang, not the peach colored Poo-tang! They must be working hand in hand!
Now that a few NP pulls have been collected and contain amines, add 25ml dh2o to NP/Honey! Add dropwise 9 drops of hcl and shake. Check pH of dh2o/honey. Should be under 7pH! Bee careful not to overshoot and go below 3pH.
It hasn't been tested yet by UP-AWE-NITE labs on the titration end, but Ibee seems to think that adding more NP/Amine to the over-acidified mix, if it happens to go below 3pH, will re-release the amine into the dh2o layer!
In any case, stay glued to the newest UPdates from the worker bees on how to cirumvent disaster concerning these newer gaak's!
Ibee feels the time has cum to explore the new avenues to obtaining starter feed! The writing is on the Wall!
Good Luck Friend
Terminal Velocity
Peacecool


Empty the prisons: make room for Congress!
https://www.chemhead.org
 
 
 
 
    mickyfinn
(Newbee)
06-20-03 14:53
No 441395
      Ker Plunk - seemingly contrary information  Bookmark   


add 25ml dh2o to NP/Honey! Add dropwise 9 drops of hcl and shake. Check pH of dh2o/honey. Should be under 7pH!




There is a thread by geez that indicates 10 drops Muriatic/HCI to 75ml DH20 is the ratio? Is this due to differences in available rxn fluid used or?

SWIM has serious questions about the ker plunk as well but will post separately in own thread. Thinks he got it last night but the volume was so small and the verbage seemingly contrary that he's not sure it was done correctly. SWIM needs to be sure with the current completed "Frankenstein Alchemy" rxn that he uses the best methodology available for the current prevailing conditions. There is thick yellow fluid in somebody's flask...

[Frankenstein alchemy]
"yes, Igor, we know this reflux has been opened, nearly rinsed through, refined with additions, stopped and refined again, refired, and refired again...just fire it up again please, thank you."


so we kept the good ol' vices, and labored to invent a few...
 
 
 
 
    wareami
(Hive Addict)
06-20-03 16:19
No 441417
      Absorbtion!  Bookmark   

Mickey: The amount of amine present will determine the initial pH of the honeywater solution!
The Kidz have never been one to question the GeezMonster or his directives regarding amounts.
They just give amounts based on what works for them! Not that the amounts geez quoted won't work!

Is this due to differences in available rxn fluid used or?



A heavily saturated solution will still contain the maximum available amine if the pH was basic enough to send the amine into the NP and enough room allows for the amine to occupy it. Therefore, if 2g of amine is taken into 250ml NP and then salted with 9drops hcl into 75ml dh2o the pH should be the same as if the amine saturated 25ml dh2o were used and 9drops hcl were added.
Jacked always suggested that the more dh2o the merrier when titrating postrxn workUPs!
The Kidz don't always have the patience to wait on 75ml of dh2o to evap so they force a saturation situation in 25ml and it requires the same amount of hcl!
If'n that makes sense!
Then they will add another 25ml dh2o to the NP/Honey and add 6drops hcl and shake! Pull the h2o and evap.
It helps to check the pH at this stage!
They repeat until all amine is pulled from the NP!
Geez is right though...as it is better to use more dh2o because patience always pays in the end. All bees know that!
smile
Peacecool


Empty the prisons: make room for Congress!
https://www.chemhead.org
 
 
 
 
    mickyfinn
(Newbee)
06-20-03 17:47
No 441442
      more fluid in titration = safety layer in case  Bookmark   

SWIM wasn't attempting to cause division, or infer anything...just attempting to understand.


A heavily saturated solution will still contain the maximum available amine if the pH was basic enough to send the amine into the NP and enough room allows for the amine to occupy it. Therefore, if 2g of amine is taken into 250ml NP and then salted with 9drops hcl into 75ml dh2o the pH should be the same as if the amine saturated 25ml dh2o were used and 9drops hcl were added.




okay, SWIM sees the hasty saturated minimal volume as a future experiment. smile



Jacked always suggested that the more dh2o the merrier when titrating postrxn workUPs!




Safety in numbers (or volume in this case.)


The Kidz don't always have the patience to wait on 75ml of dh2o to evap so they force a saturation situation in 25ml and it requires the same amount of hcl!
If'n that makes sense!




Okay, so a 2g nano is the subject at hand. To the rxn solution is added an NP (VM&P) layer of at least 120% volume of rxn solution.
*This is then based in whichever manner chosen (ker plunk)and the first pull of 50ml NP layer is washed with one cold dh20, one hot dh20, and one cold dh20.
*This then has 2ml of DH20 added(1ml per potential gram of yield) and HCI is added dropwise, shaken and repeated if neccessary until a ph of 6.5-7 is obtained. Theoretically if SWIM had 1G or 100G it's still about 9-10 drops to freedom or the correct ph of honey?
*This is then pulled and evapped and worked up further to clean.

Since SWIM still not sure what the rabbits look like:
If additional amount of dh20 were to be titrated with HCI to ph 6-7 then would the honey be a substance that appears like "oil in water" if the solution were thinly spread out on the evap plate? Theoretically then SWIM could use medicine dropper to separate the extra h20 from the "oil" to speed up the evap process?

SWIM has had various versions of what appears to be oil in the dh20 that ended up evaping to some nasty stuff., lately they've been red for some reason although not initially. Some of them gradually became reddish while still residing in the NP after HCI was added and then shaken and some became so upon evaping...




Then they will add another 25ml dh2o to the NP/Honey and add 6drops hcl and shake! Pull the h2o and evap.
It helps to check the pH at this stage!
They repeat until all amine is pulled from the NP!




So if SWIM adds a drop to the NP pull and it turns red(1ph)
then SWIM is done...SWIM doesn't recall reading about sign of final pull, just that >3 is probably not a good function of time.


with cake and vulgar surplus, you can have it and eat it too...
 
 
 
 
    johndee
(Hive Bee)
06-20-03 18:46
No 441458
      rethink  Bookmark   


Theoretically if SWIM had 1G or 100G it's still about 9-10 drops to freedom or the correct ph of honey?




No.

The acid molecule and the free base molecule "want" to find each other at which time they will migrate to the water layer as the HCL salt.  So as one titrates the PH is somewhat dynamic, and takes some time of inactivity beefore it stabilizes, that is why so many have trouble overshooting PH.

Relax, take your time. Understanding what you are doing should bee more important than your short-term success, right now...

Beelieve it or Not.

 
 
 
 
    mickyfinn
(Hive Bee)
06-20-03 19:32
No 441476
      re-determine  Bookmark   

It didn't sound like that should be correct...so what determines the amount of HCI to dh20/NP (laymans terms?) or what write up is clear in indicating this? Don't remember it geez or Osmium post workup threads but those are printed out and about to be re-read...

Based on what SWIJD indicates it seems that adding the HCI in 1/3 increments of what one estimates is correct ratio for that situation and then waiting 5 minutes to test would be good rule of thumb in order to keep from overshooting? What determines the waiting time before the molecules merge...concentration of N/P/honey?

Probably gonna get a UTFSE but if so, how do you effectively search for this info...this 28.8-56K modem CRAP is killing SWIM...

Agreed, understanding is more important than final product, at all times. SWIM still newbee and eager to get full process finished, of course. Plus, SWIM is learning much from reading after having been though some stages.
"Aha! That's what went wrong" or "Yeah, that was cool, just like that"...SWIM always been man of action, need hands on experience to grokk in fullness most times.

someone said the Big Man may joining us soon....
 
 
 
 
    johndee
(Hive Bee)
06-20-03 20:15
No 441482
      attempting to be precise, but am oh sooo stooned..  Bookmark   


so what determines the amount of HCI to dh20/NP (laymans terms?)




The estimated yield determines the amount of DH2O/ and NP.

The amount of NP, or water DOES NOT directly determine the amount of acid. The amount of NP or water is a variable linked to the variable of degree of saturation of these media.

The amount of acid is determined by observation, and if properly done, by observation of the STABILIZED PH level ALONE!, as the molecules link, one-to-one for the HCL salt as SwiJD recalls, sulfate on the other hand would require 2 acids per freebase molecule - now, we are NOT making sulfate so that is just an example.

As I recall, the example given originally in a post by geez or jacked...(75 ml with 10 drops HCL, mixed then combined into NP) was simply a method to pull a  saturated water/product mix from a reaction KNOWN to be large enough to produce X+ amount.

The feed amounts, nor any other predetermined figure, can never accurately be used to determine the amount of acid. Only the molecule count, when the rxn is done, And the molecules have successfully migrated to NP, and are qeued up to become...

HCL salt, soluble in the water layer and "wanting" to migrate to the same.

This amount WILL include unconverted pfed/efed and any iodofed as well.

"Broken" molecules will not usually link.

Clear as MUD, yet?, lol?


The Great Work is within
 
 
 
 
    geezmeister
(Of Counsel)
06-20-03 20:37
No 441486
      re read  Bookmark   

MickeyFinn: Go back and re read the whole post on titrating in the post-reaction workup writeup. You either missed part of it or didn't read it all. The part you are quoting related to pulling some cream off the top of the reaction to have some meth to fuel you up to do the rest of it patiently and carefully. It is not meant, nor was it ever meant, to tell you how much acid to use with how much water...seriously.

Its how to get the cream right off the top. Read the whole post.

Mostly harmless
 
 
 
 
    mickyfinn
(Hive Bee)
06-20-03 21:17
No 441491
      retention  Bookmark   

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.

so I hope that someone saves a seat for me on the last plane out...
 
 
 
 
    ChemNewbie
(Hive Bee)
06-20-03 23:47
No 441506
      Yeah Swic does the same thing  Bookmark   


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.


Just fuckin'do it already
 
 
 
 
    SHORTY
(Hive Bee)
06-21-03 07:12
No 441549
      Also, in my experiences i have found...  Bookmark   

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.

It wasn't Me!
 
 
 
 
    wareami
(Hive Addict)
06-21-03 08:07
No 441556
      Strippers cost more...  Bookmark   

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 (wareami: "SweetBee", Chemicals & Equipment)

Empty the prisons: make room for Congress!
https://www.chemhead.org
 
 
 
 
    SHORTY
(Hive Bee)
06-21-03 12:36
No 441578
      Wonder what the difference is  Bookmark   

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.

It wasn't Me!
 
 
 
 
    wareami
(Hive Addict)
06-21-03 22:27
No 441638
      Revelations  Bookmark   

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


Empty the prisons: make room for Congress!
https://www.chemhead.org
 
 
 
 
    ChemNewbie
(Hive Bee)
06-22-03 02:16
No 441665
      Wuzzup Ware  Bookmark   

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

Just fuckin'do it already
 
 
 
 
    SHORTY
(Hive Bee)
06-22-03 03:22
No 441669
      Thats interesting  Bookmark   

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.

It wasn't Me!
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
06-22-03 11:30
No 441728
      bubbles  Bookmark   

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....

Tighten Up!  (UH)
 
 
 
 
    ChemNewbie
(Hive Bee)
06-22-03 13:16
No 441748
      Yeah same here...  Bookmark   

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

Just fuckin'do it already