Author Topic: pulled salt ? no goods ?  (Read 10259 times)

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lovintweety

  • Guest
pulled salt ? no goods ?
« on: October 28, 2004, 11:53:00 AM »
last 5 dreams got nothing but salt. looks good ,tittrates good and then when almost done drying salt forms on bottom of pan while water is on top still? what am i doing wrong. Have been a honey making bee for 7 years had it happen 2 times ever in the beg.Now the last 5 please help

geezmeister

  • Guest
what are you doing?
« Reply #1 on: October 28, 2004, 01:56:00 PM »
To know what you are doing wrong requires that we at least know what you are, in fact, doing. All we can assume is that you are pursuing an HI type reaction for meth and getting a plate of salt. This suggests a failed reaction (as you tell us you have been having successful ones for years) but in the absence of detail about your reactions, how can we guess what is going wrong?


tina_craig

  • Guest
Swit_c had the same thing happen recently, but
« Reply #2 on: October 28, 2004, 02:26:00 PM »
Swit_c had the same thing happen recently, but was due to a failed rxn and tried to pull unreacted pseudo, fucked up somewhere panicked, based & salted rxn fluid prior to panic, after several container switches, gassings and a bunch of other bullshit found 4 out of 6 grams of missing pseudo in a water layer and evapped this to give salty pseudo and tried reacting only to give salt, no product, but it seems to be a little more obvious where swit_c's problem was, panic, impatience, stupidity and transferral of goods way too many times and the meth gods angry with swit_c's rashness :) .  Was pissed but over it now, got anxious and pulled 1st attempt too soon and added too much water.  Fuck up found and soon to be corrected.  But, yeah, ended up with salt that probably was from salting first rxn attempt fluid to reclaim pseudo.  If such a thing, meth gods forbid were to happen again, does salting rxn fluid work the same for pseudo as it does for meth?  Don't know if this has anything in it that will help with swiy's problem but sounded similar. ;)


lovintweety

  • Guest
here's the details
« Reply #3 on: October 29, 2004, 06:23:00 AM »
sorry i didn't give  dream details. 25pse,50 I2,25mbrp,12ML.DH20.Mixed all together inside a 2.5lb fire extinguisher then sealed.watched temp./pressure . Made sure it stayed above 127 degrees for 1hour after intitial heaat/rxn was done. the poured a little out and red fell to bottom .so swim then add wizard charcoal/naptha / toulene/colemens mix.lyed tilll 13 then let cool for 10min and poured fluid in 2lt.np rinsed h20 layer 3times the ph to 6.4.

geezmeister

  • Guest
on the salt...
« Reply #4 on: October 29, 2004, 07:26:00 AM »
I am not going to comment on your method; I haven't tried it. The time seems too short for full reduction IMHO but I have no actual experience with pressurized reactions of that nature.

You did not wash the reaction fluid before basing, and you pulled with a mixture of solvents which should be able to pull any non-polar soluble trash in the reaction fluid along with the freebased meth. You based the reaction fluid very heavily. You washed the nonpolar mixture with water alone. The solvent was loaded with sodium ions.  When you titrated these grabbed the chlorine and salt formed. 

You should have some pseudo or some unreduced intermediates somewhere. Its odd to lose the amines altogether. They may be in the salt. You could extract the salt with alcohol to see whether the amines may be there.

The other possibility is that you did not clean the pseudo sufficiently and it contained trash that carried over and became a salt when you titrated. There are some foilants that aid an abet that result, but you usually will have perfectly good meth on the first pull, then salt after it.
You did not mention the source of your feedstock or how you cleaned it, and that could be a major part of the problem.

I have the hunch the reaction did not complete and you did not clean the reaction fluid before basing or wash the extraction solvent well enough before titrating. Pill gakk may have just compounded your problems.


reeB_relliM

  • Guest
Very curious.......
« Reply #5 on: October 29, 2004, 07:54:00 AM »
I certainly don't mean to high-jack anyones thread, I do appologize. Just one quick question though.

Geezmeister - Very curious, does toluene need to be water washed to get rid of any crap in it???  Y'know, just like Colemans fuel needs to be washed to get rid of the oilly rust inhibitors that it contains?

Please advise.
reeB


lovintweety

  • Guest
pill stock
« Reply #6 on: October 29, 2004, 08:36:00 AM »
red 30's quick water rinse and methonal rinse (dereds them) then i put in a filter and suspend them in "heet" about 6inches from the bottom of my getto sep. i leave them undesturbed and you can watch the pse fall in to the bottom layer. once bottom is full i pull screen/filer up slowly to see if more falls if not i drain bottom of thru filter and dry in m-wave pse scrape of pan with now effort.so i assume that it's gak free. i start w/1200  30mg and end up w/2.25 per 100 returned pse.(not like the old days when i would get bak about 30 per 100pills. Up till 3 years ago i would get back about 90-95% returned finished product in  fire extinguisher method.(had 2 flask blow up on me so i like the sealed pressure safe way now.plus its easy to hide since i don't have privacy like i wish possible and am very portable.i tried the alcohol salt thing but most of it dissolved and still was salt when dried.but you said to ?wash the reaction fluid prior to baseing ? and wash the n/p solvent ? I am self taught so i am skeptical on trying new things but am willing to try anything to fix my problem since i don't have a lot of time to do failed reactions.And everything i see from the streets is to trashy to do or it's that "bunk glass" or as i call it "keefed speed"like some do to weed because the kick is gone .do you need to wash wizard lighter fluid (double charcoal filtered) i just started using colem and the rust inhibitor did bother me but it's hard to find 100% mineral spirts now a days

wareami

  • Guest
Tolly rinsing...
« Reply #7 on: October 29, 2004, 08:40:00 AM »
reeB_relliM:
Toluene str8 from the can is not riddled with water soluble contaminates so there is no need to pre-wash prior to use.


lovintweety:
In addition to what geez says...I'm inclined to believe that the reactant ratio's are whacked and not sufficient to reduce....even in a pressurized system.

Under pressure, I would assume that the HI would need to be at or above 50% aqueous prior to adding the feedstock and that requires a specific molarity and precise measurement of all reactants and precursors.

I'm also going out on a limb here.
What is the purpose of using multiple NP solvent mixes?
It seems likely that with all the different solvents mixed that together they might interfere with amine solubility.
Dual solvent NP extractions are good for sidestepping certain gaaks...but selectively.
Therefore random NP mixing without purpose or reason seems like it's adding excess varibles to the troubleshooting process and tends to leave bees looking like when pulling salt and god knows what else. ;)

Try pulling the amine with a single NP and see what happens!


wareami

  • Guest
Naptha...
« Reply #8 on: October 29, 2004, 08:45:00 AM »
Go to any paintstore and aquire VM&P Naptha...
Odorless 100% mineral spirits will work for pulling amines but not as well as warm naptha.


lovintweety

  • Guest
i use to use 8oz I (bb's)/2oz pse/1oz lab...
« Reply #9 on: October 29, 2004, 09:04:00 AM »
i use to use 8oz I (bb's)/2oz pse/1oz lab grade red/50ml h2o (8/2/1/50ml  =i/pse/lgrp/dh20 )but a new friend talked me in to  2.5/2/1 ratios what do you think is best

geezmeister

  • Guest
washes / ratios
« Reply #10 on: October 29, 2004, 09:21:00 AM »
The tolly used to extract freebase meth from the reaction fluid should be washed before gassing or titrating. No need to wash it before using it to extract the freebase meth, but it should be washed after that.

Same with charcoal lighter fluid, and camp fuel. You can prewash Coleman's to get some of the antioxidant out, or you can buy a different brand of camp fuel that does not have the antioxidants.

A straight alcohol pull of today's deredded 30 mg pseudo tabs will not yield pure pseudo. The assumption that the pseudo you get with your method is gakk free is erroneous.

The fact that the salt in your evap dish dissolves in alcohol suggests that it is not NaCl. The salt you have was formed when you titrated a mixture with polymers from the pills in it. I have had this happen before. I recall having similar problems with one of the orange gakks when it was introduced. I had a small yield of excellent meth from a first pull, and nothing but salt after that. One of the polymers holding your amines is ambipolar, and will salt out of the nonpolar extraction solvent.  Or so I suppose. Your pill extraction method is substandard for the newer gakks, and if you solve that problem first you should not experience the same problem again.
 
Do the non-polar washes of the reaction fluid before basing it, and wash the extraction solvent before gassing or titrating. You should do this as a matter of course, and it will improve the cleanliness of your product.

I discussed these washes in

Post 428410

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

As to the ratios to use in the fire extinquisher, I will not hazard a comment. I haven't done a reaction that way and cannot say from personal experience how any set of ratios work under those circumstances. As to the ratios I use, see

Post 534545

(geezmeister: "on ratios and envelopes", Stimulants)



lovintweety

  • Guest
thank you for your input 1 more ?
« Reply #11 on: October 29, 2004, 12:01:00 PM »
thank you for your time and input but i have one more ?. and that is what method do you recommend for the pills(red 30's shiny coat).I would like some thing that is  space and time consumtion minimal.since i don't have a lot of either but sometimes you have to do what ever it takes.and i hate renting motel rooms for more than 1 day if i don't have to.(have kids so don't do anything at my place)

tina_craig

  • Guest
Uncle Fester's "Deconstructionist Thought
« Reply #12 on: October 29, 2004, 12:26:00 PM »
Uncle Fester's "Deconstructionist Thought" thread, only thing really time consuming is reading the entire thread which is a must.


wareami

  • Guest
De-redding
« Reply #13 on: October 29, 2004, 12:30:00 PM »
Read and follow these threads!

Post 499089 (missing)

(UncleFester: "deconstructionist thought", Stimulants)

Post 529156

(evilscripter69: "Best extraction method. well tested", Stimulants)

Post 535119

(evilscripter69: "Ghetto FB extraction w/ 80% + returns", Stimulants)


It's unlikely that a fast easy pill clean will be effective enough to obtain pristeen clean feed.
The best way to shave any time of any extraction method is to become as familiar with the procedure as possible.
This involves conceptualizing and then practice.
For that there is no substitute or shortcut!

Shiny reds contain a membrane coat in between the dye and the pill surface and are usually easy to de-red with just acetone and h2o rinses!
Don't let the h2o cut into the pill surface or you risk activating gaaks.

The dull red pills don't have this membrane and make de-redding a bit more difficult.
But as Jacked recently pointed out in another thread...the dyes today contain filter cloggers and are more syrupy than they use to be a year ago+.


Scottydog

  • Guest
Salt
« Reply #14 on: October 29, 2004, 06:58:00 PM »
The first time that SWIM ever dreamed, he ended UP with a pile of salt as well. He titrated in a metal skillet. He even used the water purification tablets (as mentioned in another current thread) as a substitute for I2. Live and learn!  ::)

Not that this is what happened with you but when titrating to get the meth hydrochloride, if some of the NaOH based fluid is syphoned with the freebase laden NP when the HCL acid is titrated in, the NaOH will combine with the HCl to create NaCl, table salt.

Meth is soluble in methanol and salt is not, shake up the crude salty product with methanol and filter out the salt and then evaporate to see what you have left.

If you get nothing back with the exception of the salt in the filter, then chances are that you didnt get the Ph high enough when basing and the meth never made it into the NP as freebase and is most likely still waiting for you in the mother A/B jar. That is of course, if the rxn completely reduced to begin with and if not, then pseudo/iodoE will bee waiting.  ::)

Nice avatar Ware!! I think one of the kidz is dressed UP as SpongeBob, "toilet-papering" houses?  ;D  ;D


ChemoSabe

  • Guest
More De-redding tips
« Reply #15 on: October 29, 2004, 08:49:00 PM »

Post 530144

(ChemoSabe: "Red Removal", Stimulants)