jackhole (Stranger)
11-01-03 21:12
No 468162
      Successful [Large] RXN     

A 12-liter flat-bottom flask was charged with 700g (3.47 mole) pseudoephedrine, 840g (3.31 mole) iodine, 250g (2.02 mole) red phosphorus and 700ml water, and was lightly refluxed in a heating mantle for about 40 hours.

At the 40-hour mark, the flask was removed from the heat source and quenched with an approximately equal volume of water (2L), and 138g red phosphorus was filtered out.  The filtrate was returned to the flask, whereupon the flask was further diluted with more water to recover the last of the red phosphorus clinging to the flask.

The reaction fluid was taken up three times in 2L toluene, each time the toluene and reaction fluid vigorously shaken and the toluene phase discarded.  A 25% NaOH solution was used to basify the reaction mixture to pH 12.8, and the freebase was pulled three times in 1.5L toluene.

Anhydrous hydrogen chloride gas was generated in a separate 2-neck flask by filling the flask 1/3 full with NaCl and adding just enough 37% hydrochloric acid to form a paste texture.  Concentrated sulfuric acid was added dropwise with a sep funnel extending into one neck, and the generated anhydrous hydrogen chloride gas was bubbled through glass tubing extending from the other neck into the freebase/toluene mixture to precipitate a total of 550g (3.69 mole, 78.6% yield) product, which upon filtering displayed a completely white powder.  The solvent was subjected to bubbling a total of three times, the fourth time failing to precipitate any further product.

A bioassy revealed that no recrystallization was necessary, but a recrystallization was performed for cosmetic appeal.  The recrystallization was done from 99% IPA over a period of about 1 day to afford mostly clear shards over an inch long, quarter inch wide, and several ml thick.  It should be mentioned that not all of the shards were of this size, but rather half, the other half being gradually smaller down to the last <1%, which failed to grow larger crystals.

Note: The red phosphorus and iodine used both were of lab grade quality, and the pseudoephedrine was extrated from an array of pills per VideoEditor's "Straight to E" extraction technique.  No solvent boils before extractions or recrystallizations after were performed to the pseudoephedrine.

Jizzy Jizzy Bang Bang
 
 
 
 
    Rhodium
(Chief Bee)
11-02-03 00:53
No 468196
      Great lab procedure, but the numbers are very off     

Something is fishy with this writeup, as you say you had a 95% recovery of phosphorus, while in reality half of it should be consumed for you to be able to achieve that yield.

Also, as red phosphorous has a negligible solubility in aqueous solutions, it doesn't make any sense that more of it would precipitate upon dilution of the post-reaction solution with water.

Other than that, the lab procedure is excellent, other than the use of a flat-bottomed flask in a heating mantle.

When using solvent amounts like this, it is important to recycle it by washing it with brine (a concentrated table salt solution) and then distill it for reuse, collecting the fraction boiling within 2°C of 110°C, discarding the cloudy forerun and the impurity-laden residue.
 
 
 
 
    callen
(Hive Bee)
11-02-03 01:54
No 468203
      ...and then bake at 400*.     

Would you please state the temperature that you cooked at. I'm a little confused by the wide ranges of temps that I've read in various posts.Some say 150*c. for P-P Rxns, 180-190*F. for long, wet refluxes...or up to 110-120-to 125*c.Which is the way to go?

callen + A.L.F.
 
 
 
 
    jackhole
(Stranger)
11-02-03 02:04
No 468207
      Typo corrected - that 238g RP was 138g     

And more water was added to the flask to recover some remaining red phosphorus which just happened to be stuck to the bottom of the flask.

Speaking of the flask: it was round, but with a flat bottom - not a volumetric/Erlenmeyer flask, if that's what you were thinking, but not a round-bottom fask.

The temperature of this reaction was actually never measured.  Heat was employed to create and maintain slight bubbling of the flask contents.  In reactions performed where the temperature was measured, 100-110 C was the required temperature for slight bubbling.  As this reaction had identical behavioral properties to all others (except for the size of it), it was assumed that the temperature of this reaction was 100-110 C.

The original write-up was corrected.

Jizzy Jizzy Bang Bang
 
 
 
 
    geezmeister
(Of Counsel)
11-02-03 03:27
No 468221
      great meth     

Sounds to me like you have a nice pile of very good methamphetamine. Good ratios, temps, times, enough water. You should have primo meth there. smile

Now if we could just get some shorter-time cooks to try this a time or two, and see how significant a difference there can be with the additional water and time, at the lower temp and without the fuming and smoking.... but for some reason they just won't give it a try... like I didn't... for years. blush

Only took one long wet reflux for me to come around. laugh

ICMOI I
 
 
 
 
    SHORTY
(Hive Addict)
11-02-03 04:31
No 468232
      If timed right ....     

I agree with geez.  For the impatient bees such as myself just start the next rxn before you run out of your personal stash and then you won't have to rush it.  For those worried about getting caught, if done properly, this can rxn is rather easy to run unnoticed even in a small apartment.

It wasn't Me!
 
 
 
 
    wareami
(Hive Addict)
11-02-03 04:58
No 468237
      It's awe in the timing     

I agree with shorty. Ibee was trying to come up with an extraction stategy for bulk extraction that would utilize similar thinking.
If one were to stockpile and get a headstart with just an extraction team, the cook could bee able to pump out stash regularly on time. The trick is in giving the extraction team the headstart!

I think jackhole's name should bee "jackpot".laugh He sure hit it and I'm with Geez on his assumption!!!wink

http://www.chemhead.org
 
 
 
 
    jackhole
(Stranger)
11-02-03 07:05
No 468251
      No justification for a quickie of this size of RXN     

There is no justification for rushing a reaction and "forcing" it to complete hot, when you're dealing with hundreds of gramssmile  Or maybe there is justification, if you're attempting become the epitomy of 'pitiful'laugh

Jizzy Jizzy Bang Bang
 
 
 
 
    Osmium
(Stoni's sexual toy)
11-02-03 13:57
No 468290
      > A 12-liter flat-bottom flask was charged...     

> A 12-liter flat-bottom flask was charged with 700g (3.47
> mole) pseudoephedrine, 840g (3.31 mole) iodine, 250g (2.02
> mole) red phosphorus and 700ml water, and was lightly
> refluxed in a heating mantle for about 40 hours.


Why don't you give any more details about how the ingredients were added to the flask? In that order written above?

Did you encounter any problems during workup?

I'm not fat just horizontally disproportionate.
http://www.whatreallyhappened.com
 
 
 
 
    wareami
(Hive Addict)
11-02-03 16:15
No 468307
      Good Question!!!     

Osmium touched on a point that I was wondering as well!
How did the work-up GO?
Usually if there were any probs with gaak, they would manifest themselves in the final work-up if they weren't rid of on the front side!
Ibee could only fantasize about a rxn of that magnitude and he likes jackholes style concerning patience and mindset!
For ghettobees staying within the heat constraints, a 2liter winejug would suffice I would think. Just split the rxn in two and run them separately.
Ibee learned that Ideaology from jackedlaugh
He also wouldn't consider anything but mixing in the order E and I2, dh2o, then RP....but that's just him!
Peace of the reaction

Have FUN-Bee SAFE


http://www.chemhead.org
 
 
 
 
    jackhole
(Stranger)
11-02-03 17:47
No 468325
      Osmium & wareami...     

This is the order in which the precursors were added:

1. Pseudoephedrine
2. Iodine
3. Water
4. Red Phosphorus

No details (or order) was given about how these were added to the flask because it is this bee's experience that the same outcome would have resulted, regardless of the order in which they were added.  As long as the iodine and red phosphorus aren't added in together, the addition order should be irrelevant to the reaction, work-up, and final product.  This wasn't mentioned because most bees should be aware of this, having read such info elsewhere or from personal experience! smile

The only "problem" during this particular work-up was formation of a very small interface between the freebase and the reaction fluid during basing.  It must have been at most 1cm thick.  That was the only "problem" - like it was stated in my first post - a high yield was achieved, and the final product was indeed high-quality and bright white, without any further purification required.

Jizzy Jizzy Bang Bang
 
 
 
 
    Rhodium
(Chief Bee)
11-02-03 20:16
No 468353
      Recrystallization is always required     

Recrystallization is always required (unless you distill) when working up methamphetamine synthesized by any HI variation to remove any unreacted precursors, as well as the very toxic iodo-ephedrines and aziridines invariably formed as byproducts in the reaction. As they too are amines and form white hydrochloride salts, they will carry through an A/B, as well as being visually indistinguishable from pure methamphetamine.
 
 
 
 
    wareami
(Hive Addict)
11-02-03 22:05
No 468374
      Now cums the mass debate...     

I beg to differ here rhodium but since I'm no chemist or have the ability or experience to precisely do a professional analysis, maybe I should just shut-UP!
But this is Ware here, so y'all don't get off the hook that easily!smile
Based on experience, I say that most of those impurities are taken UP and cooked off with the long wet reflux.
It's the very last selling point I have in my bag`o`treats as a salesbee!cool
Ibee's done both the fasthot and dry plus numerous longwet refluxes and the difference in end product is like day and night ware impurities are concerned. The methods of analysis only consist of sight and bioassay.
While as you say these impurities cannot be detected with the naked eye for the reasons stated(all amines), their presence can be detected upon consuming said product.
In addition, the final work-up carries some visual clues as well concerning impurity types and amounts.
I do agree that good lab technique and protocol dictate that distilling or rextalling is required...
But I'll let you have the last word on whether my reasoning and experience carries any weight or validity regarding your admonitions to rextalize if not distilling.

Mind you, I'm not challenging your expertise in this area.
Just trying to understand better to improve the end result.

Generally with product that contains consistant amounts of impurities as a result of the reduction method, upon rextalling, the yield lost should be equivalent to those impurities. Correct?
What if after the longwet reflux and rextalling that this yield loss was very minimal.
Would the rextalling still bee a neccessary step?
Thanx Chief!


Peace of the reaction

Have FUN-Bee SAFE


http://www.chemhead.org
 
 
 
 
    jackhole
(Stranger)
11-02-03 22:16
No 468376
      Yield loss is less than total impurities present..     

I know this was directed towards Rhodium, but I'd just like to comment on a few things:

Impurities will remain even after several recrystallizations; if a recrystallization or several recrystallizations were guaranteed to remove all impurities, then virtually all recrystallized meth would posess the same psychoactive effect.

Recrystallization is required to compete visually with the current product flooding the streets nowadays, which happen to be huge, beautiful, crystal clear shards.  While the street product likely contains over 50% dimethylsulfonyl methane, it has been preferred time and time again over a purer product that is a powder.  Recrystallization affords a product that looks nearly identical to the huge shards, but with twice the potency, and only THEN is it preferred over the "glass" that is flooding the streets today.

Jizzy Jizzy Bang Bang
 
 
 
 
    WizardX
(Wizard Master)
11-03-03 03:59
No 468424
      This Order.     

I would do it in this order.

1. Water
2. Iodine
3. Red Phosphorus
Make your HI first, then...
4. Pseudoephedrine
 
 
 
 
    Rhodium
(Chief Bee)
11-03-03 12:03
No 468473
      Rxtal all Meth for the sake of your health
(Rated as: good read)
    

Based on experience, I say that most of those impurities are taken UP and cooked off with the long wet reflux.

Correct, in theory 100% of those byproducts will in time be reduced to meth, but without analyical equipment you do not know for sure if that has happened in each and every reaction you perform. There are also those minor freak byproducts (dimers for example) which cannot be reduced to meth still in the mixture.

While as you say these impurities cannot be detected with the naked eye for the reasons stated(all amines), their presence can be detected upon consuming said product.

I think that they can show toxicity at lower levels than is detectable by bioassaying. I bet you cannot feel any difference between pure meth and meth containing <1% aziridines/iodoephedrines, but even at those small concentrations they will be able to alkylate both DNA and other vital biomolecules in your body, leading to increased cancer risk and general deterioration of mucous membranes.

Generally with product that contains consistant amounts of impurities as a result of the reduction method, upon rextalling, the yield lost should be equivalent to those impurities. Correct?

Yes, if the recrystallization was performed with an optimal amount of solvent.

What if after the longwet reflux and rextalling that this yield loss was very minimal.
Would the rextalling still bee a neccessary step?


Not for the subjective experience of the product, but I believe that the time spent on recrystallization is well worth the lowered risk for cancer and other health-related problems.
 
 
 
 
    geezmeister
(Of Counsel)
11-03-03 17:59
No 468495
      note on reflux crystals
(Rated as: good read)
    

My experience recrystallizing meth produced in a long wet reflux is that the loss in weight is minimal compared to the push-pull product, and the crystals form much more quickly, all other things being the same. There appears to be less marked of an improvement in quality with the refluxed product, but there is a noticeable improvement.

Tweakers around here would rather have the raw powder, and complain the crystals do not give as "good" a rush or as "good" a buzz as the powder. While my opinion of "good" differs from theirs, the fact that they note the difference between the two suggests recrystallziation is still beneficial.

ICMOI I
 
 
 
 
    wareami
(Hive Addict)
11-03-03 22:31
No 468545
      You may see me tonite with an illegal smile     

It don't cost very much,
But it lasts a long while!

Thank You Rhodium and Geez:
My main concern was health related and both replys answered my questions and then some!
Ibee's end result is see through crystal clear.
Appearance WAS his guide prior to reading this!
He always wondered if further refinement would help minimize the health risks since he's never been able to associate a marked difference in quality through bioassay after rextalling compared to not rextalling.

Wizardx: Thank you as well because you reminded me of what Ballz and Orgy had been telling the Kidz all along!
Next romp in the mudpuddle they will incorporate that mixing sequence.
Peace of the reaction

Have FUN-Bee SAFE


http://www.chemhead.org
 
 
 
 
    Organikum
(Hive Addict)
11-04-03 17:10
No 468701
      thats a way to do it     

Hi made first - long refluxed 36 hours, already POPEYE told this being the biker receipt.

Another way to do this is to start with no water, RP, I, Pfed. PI3 is much stronger in halogenation action as HI, but this is a hot hot thingie - Jacked is best to tell. Of course if some GAA is used from start it is not so hot, H3PO4 works also. Later some water - depends on how dry was dry.... LOL
This pathway got fucked up at the HIVE as ppl added water from start. You cannot dance on both parties the same time baby.....

Nobody ever spoke of anhydrous.
You cannot say a reaction is bogus which is done a thousand times every day all over the world.


But actually the long wet reflux is the way to go. Add some GAA or H3PO4 and you will need much less RP/I.

And cut back on the iodine! thats actually whats killing yields and making byproducts! Oxidative cleavage of ephedrine by iodine is a usual way of determination of ephedrine content in plant extractions. All free iodine is bad. It is a catalyst - damned!
btw. it was was Osmipum who said that he thinks an oxidator like I2 in this reduction cannot be right.....

3 time molar iodine - the catalyst. The post is fraud anyways....
boasting, posting, boasting......


are you all glad to see me back?
yes?
smile
ORG

love and peace and some truth so unavoidable......
 
 
 
 
    Rhodium
(Chief Bee)
11-04-03 18:47
No 468715
      XS I2?     

this is a hot hot thingie

And gives a not not pure product, consisting of large amounts of unreduced iodoephedrine/azridines.

Oxidative cleavage of ephedrine by iodine is a usual way of determination of ephedrine content in plant extractions. All free iodine is bad.

Can you provide us with references? I have only seen HIO4 being used for such cleavage. It sounds very interesting, and is a great argument for adding any (pseudo)ephedrine last of all, after all the iodine has been reduced to HI by the RP/H3PO3/H3PO2.
 
 
 
 
    Organikum
(Hive Addict)
11-07-03 18:00
No 469462
      I used the time     

and did what perhaps nobody has done before - I read all the articles. And the more interesting ones not only once.

The ephedrine cleavage for determination of ephedrine content by the amount iodine used up in the procedure was done during the practical organic laboratory lessons at a german university. I will send you the text with reaction mechanism as soon I am able to upload stuff again. (in german of course)

If you were right on what you say on ayiridines and this Rhodium, than every halogenation of alcohols with phosphorus/iodine by I3 as described in VOGELs, the Gattermann and the ORGANIKUM (just to name a few) would have the same bad results. But they all speak of 90% to quantitative yields - probably a conspiracy I guess.

must go
ORG
 
 
 
 
    Rhodium
(Chief Bee)
11-07-03 19:06
No 469485
      You are discussing a different reaction step     

If you were right on what you say on ayiridines and this Rhodium, than every halogenation of alcohols with phosphorus/iodine by I3 as described in VOGELs, the Gattermann and the ORGANIKUM (just to name a few) would have the same bad results. But they all speak of 90% to quantitative yields - probably a conspiracy I guess.

The halogenation of the benzylic alcohol to the corresponding iodide probably goes to completion relatively quickly. 

I am mostly talking about the further reduction of iodoephedrine to methamphetamine, which does not go to completion unless given time to do so. The aziridine formation is a intramolecular cyclization of iodoephedrine (favored by high temperatures), and has thus nothing to do with the alcohol being iodinated in the first place.
 
 
 
 
    BOS
(Newbee)
11-14-03 03:09
No 470751
      Holy Shit!!!Comfirmation of suspicions by...     

Holy Shit!!!Comfirmation of suspicions by scienticians.

Someone finaly putting it in a scientific type voice.
I like it..laugh

Halogenate the ephedrine then hydrogenate it.I get it.Sounds like hydrogenation `sept replacing ya precious metals with a halogen catalyst.(I know,Iknow it aint the same but...)

Anhydrous? I believe this has been spoken of.
Yet No-one tends to listen when it aint written all nice-like.

Orgy,Great to have you around.Now I would like some clarification on the HI concentration to byproduct/racmerization issue I was once told,as you have just replaced it with a more plausible(in my head anyway)explination pointing to free I2.Please?This is very interesting("is this the right thread?"he thinks to himself).

Make the HI first.Why?-because you can.Why not?
At the very least you could use visual indication to realise you have made at least a decent% of HI containing sollution(like or unlike that red shit Argox made up).

Cook on low heat.Why?-Because that is how the scientists do it.If Warlock can do it with sunlight so can you.What else do you have to do?
I see no reason why you cant cook it hot as fuck to produce some HIacid fast, and then let it cool conciderably before the addition of your ephedrine,and proceeding from there at an almost ambiant temp(well not quite-but still nowhere near 100c.)Why should the rate of reduction/halogenation have to compete with the decomposition rate of aqueous HI anyway?Like snatch and grab.
Are there not alternative methods of iodinating without the need for either HI or RP/PI3?Certain IODIDes perhaps?
Which points me to the HCl/H3PO4-KI/NaI system of producing something Hydriodic related.

Org,when you speak of dehydrating your HIacid, I assume you are theoretically producing HIgas and some muriatic.orrect?
Why didnt I think of that crazy.
Oh No,I have those crazy thoughts again.

As you may or may not be able to tell,Ive been into the cabinet again.Forgive me Im new.blush



Of interest to anyone who likes to fuck with electricity
and believes that Iodine and Ephedrine can not be reduced in one pot.Again,carbon is the choice.More info available if desired.
The modern electro?Patent US4702804
 
 
 
 
    jackhole
(Stranger)
11-14-03 06:29
No 470786
      My comments     

Make the HI first.Why?-because you can.Why not?

Because it is easier for me not to.  It saves me time and I get a great product at a very respectable yield.

I see no reason why you cant cook it hot as fuck to produce some HIacid fast, and then let it cool conciderably before the addition of your ephedrine,and proceeding from there at an almost ambiant temp(well not quite-but still nowhere near 100c.)

What is so inconvenient of heating the contents of the flask to a relatively low 100 C and allowing it to reduce?  You don't even have to monitor its progression.

Org,when you speak of dehydrating your HIacid, I assume you are theoretically producing HIgas and some muriatic.orrect?

I was not aware that one could produce MURIATIC acid! laugh 28 degrees Baume, is it?laugh

Jizzy Jizzy Bang Bang
 
 
 
 
    BOS
(Newbee)
11-14-03 07:30
No 470799
      Hi jackhole, Congrats on your large rxn.     

Hi jackhole,

Congrats on your large rxn.

I wonder at your need to respond to my jive???
Please do not feel that I was knocking,nor was I advising.
Simply commenting for the sake of it.

What harm is there in dropping your temp a notch, in the name of purity?I am sure your product realy kicks some ass
as Im sure many a bee`s does likewise,but why try to be scientific in writeup,yet leave it at that?Again my comment was not directed at you,as you already seem to have your shit together nicely.
 laugh

JH-Because it is easier for me not to.  It saves me time and I get a great product at a very respectable yield.
-What is so inconvenient of heating the contents of the flask to a relatively low 100 C and allowing it to reduce?  You don't even have to monitor its progression.

Come now...You have time to reflux for 40hrs and perform a semi-thorough work-up,yet you cant spare an hour or two and
change the order in which you introduce reactants to a flask? What harm is there in giving it a go?
Or shall I just crown you as meth-god now,seeing as your system is so simple,flawless,and high-yielding?

-I was not aware that one could produce MURIATIC acid!  28 degrees Baume, is it?

How is it I seem to miss all the funny parts?
What are you telling me here?
Seriously,I am no chemist,so please tell me what happens when you take the water from HIacid and react it with dry HCl gas?I know it sounds stupid but I kinda had the idea that those hydroniums might be more comfortable around chlorid rather than iodide ions.
Have I totally misunderstood the definition of de-hydration?
Tell me,tell me I want to know how this works.

No offence meant,nor taken.

Peace.
B.O.S.
 
 
 
 
    jackhole
(Stranger)
11-14-03 08:38
No 470812
      Seriously,I am no chemist,so please tell me...     

Seriously,I am no chemist,so please tell me what happens when you take the water from HIacid and react it with dry HCl gas?

Why, if you took water and were to "react" (I prefer to use the term "introduce") it with HCl gas, you would create anywhere from a dilute HCl solution in water up to a concentrated 37%, I believe.

Jizzy Jizzy Bang Bang
 
 
 
 
    SHORTY
(Hive Addict)
11-14-03 14:36
No 470847
      Isn't that muratic then?     

I have always thought that what you described is muratic acid or hydrochloric acid or HCl.  Aren't they all the same thing?

It wasn't Me!
 
 
 
 
    jackhole
(Newbee)
11-14-03 21:26
No 470901
      Muriatic is a trade name     

Muriatic is a trade name, that's all.  I was being sarcastic more than anything.

Jizzy Jizzy Bang Bang
 
 
 
 
    ragnaroekk
(Hive Bee)
11-23-03 00:37
No 472581
      dehydration     

If you vent HCl gas into HI in H2O a partial dehydration of the HI takes place - say the HCl and the HI compete for the water. So HI is freed from the hydrate and can iodinate the ephedrine more easily acting as "fuming HI" would. Lower temperature - less byproduct.

Rhodium to say the reduction step is the problematic one is plain wrong.
Read Gattermann Wieland on halogenations for this for example and realize the consequences from the fact, that NEVER iodoephedrine is found as a byproduct. Damn! Thats obvious!

Honi soit qui mal y pense
 
 
 
 
    Urban_XTC
09-10-04 07:59
      iodoephedrines
(Rated as: misinforming)
    
 
 
 
    BullwinkleMoose
(Hive Bee)
09-10-04 08:04
No 530601
      NO     

Iodoephedrine is not a byproduct !

Iodoephedrine is 'Iodine Holgenated Ephedrine '
Is an intermediate that gets reduced to meth

I quote Eminem;  Yet I listen to Deep Purple

fuckin moosed
 
 
 
 
    Urban_XTC
09-10-04 08:30
      iodoephedrine
(Rated as: misinforming)
    
 
 
 
    psilly1
(Stranger)
09-10-04 15:40
No 530634
      If the rxn is R-OH+H-X=R-X+H2O, R-H+ I2, Iknow     

If the rxn is R-OH+H-X=R-X+H2O, R-H+ I2, Iknow I skipped the phos, but my point is, if I2 is a catalyst in the reaction to meth, why the hell does it matter if R-X is being produced, since it is goig to anyway.Does it not have to lose the damn OH group, replaced with I- then reduced to the goods. Why so much controversy about not forming Iodonated ephedrine.
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-11-04 02:17
No 530725
      12.8?     

Why did you stop basifying at 12.8? That kind of yield whit that low of a base pH is strange to say the least.. Did you use a meter to check it?
Also that high of a yield with an interface problem is a strange thing thing as well..
muratic means marine acid, it is not a trade name

Tighten Up!  (UH)
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-11-04 02:41
No 530730
      one last thing     

Just for the record there is no such thing as a dry reaction. H2O is always introduced to the reaction. A 700 gram reaction would start with 200ml H20 in a PUSH PULL and would generate more as the reaction took place.. Again for the record , Jacked recommends a LWR over a push pull any time. The yields are to close between both reactions to give that as a reason but there is a considerable quality difference and after recrystallizing a couple times there is no difference in that area of discussion..
 As far as the birch goes compared there is a difference between product and Swim knows the difference is in the people doing it.. People subject to getting there shit from a source using RP/I2 and change to a source supplying the birch method notice a big difference and complain about it... What is actually going on is the people have gotten use to a certain impurity in there shit and when it is omitted (like from the birch compared) it is not only noticed but missed...

Jackhole, If your going to do a write up on your rxn then do it in detail, You should be wanting people to be able to follow your work them selfs with the same results. This is what a write up is for.. Not just to be bragging about the size cooks you preform.. Also you need to answer Rhodium's inquires of 95% returns on the RP.. That size reaction would have consumed 50 maybe 60 grams of RP easy.

Tighten Up!  (UH)
 
 
 
 
    chronic_cook
(Hive Bee)
09-17-04 03:48
No 531708
      That post was very basic which I guess isnt a...     

That post was very basic which I guess isnt a bad thing! But straight 2 E? with a plethera of mixed pills seems nuts! Especially with 250G LG RP & 840 G LG I2, What the hell, am I the only one who had problems with that teqnique? Not to mention OG 2 out the ass on my post work-up! But anyways Rhodium is right those iodoephedrines pull right through an AB and they will fuck your world up bigtime. But a complete wet rxn should clear those up, not the only problem is restraining from comsuming the waste left over from a recrystallization when you run out! But I would also like to hear more details about that omega rxn. with the amount of water you used is like a 1:1e ratio why so much?? damn, you'd think that would just take longer to get a complete rxn. Also, why didnt you just gass with HCL..that shit always worked for me...alot easier then what you did, are there any benefits in that method or did it just sound good on the forum?
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-17-04 09:04
No 531743
      question     

BullwinkleMoose, what you say about Iodoephedrine not being a byproduct makes sense but after the reaction when everything should have been converted to meth then would'nt it be considered a byproduct or maybe just an impurity?

Tighten Up!  (UH)
 
 
 
 
    wareami
(Hive Addict)
09-17-04 17:59
No 531797
      Out on a limb....     

Jacked: I'm going out on a limb here
Not speaking for the moose...or attempting to intercept his answer with my own.
But it's been my experience that iodoeph is the necessary intermediate to meth.
The literature backs that UP from what I've read!
Iodometh(if such a thing exists[crazy) is completely different I think and just describes under-reduced meth w/impurities that weren't given time to fully reduce.



but after the reaction when everything should have been converted to meth then would'nt it be considered a byproduct or maybe just an impurity?




I think the correct answer is neither in this case. Side-rxns take place with that substance that in turn create the impurities. When the reaction is stopped prematurely and worked UP, the resulting product will contain impurities. Any Iodo's will be left behind during the work-up.
Free Iodine from post-rxn solution can be oxidized & removed with sodium thiosulfate.
I would suspect Iodoeph to be result of an under-reduced rxn.
Yield reports confirm a lower yield of meth when these intermediates are present. Instead of meth xtals obtained....nothing is obtained because the Iodo's stay in the basified solution.
Heavy emulsion during work-up also substantiates this occurance.
Yes...less than clean feedstock will also create this but the longer cooks usually provide relief to a small degree.
That tells me that full reduction of dirty feedstock can only occur given the time necessary to counter the buffering effect that gaaks play in rxn.
Ibee's done rxns at all stages(Superclean feed) and stopped them purposely during the early LWR rxn experiments to record the yields and meth/pfed percentages.
Most bees at the time thought Ibee flipped his wig cause who in their right mind would create failure scenarios in order to achieve meth???
Well the cats outta the bag on that note and Ibee will never stop that line of investigation in order to reveal what works best under any condition.
The strength mystery sparked these early experiments.
When Iodo's are present they account for expected meth weight and yields can be used to back this up.
This is part of what compelled Ibeeware to push the time/temp & hydration envelope to absurd extremes to unheard of levels.
To this day it's difficult to expect bees to adopt that tradeoff when they can have product in a fraction of the time it takes for a full reduction.
I think you'll agree that impurities are created by side- rxns in the less controlled faster cooks.
The old journals contain references and instruction that pointed to lengthier, milder rxns producing higher yields and in higher purity.
I guess the arguement will always exist between that which can be done in half the time, producing some of what bees are after in a potent enough form to pass for the real thing.
But evidence and experimentation leads me to believe that less impurity exists in a fully reduced product because the time was taken for the rxn to proceed to completion, cooking off or fully converting those intermediates instead of stopping the rxn before that takes place.
The ancient alchemist deluxe undoubtably has been performing this rxn for longer than most and has incorporated steps and procedures that minimize the iodo's presense in the end-result.
But for anyone that performs a curbshot or a superassman style rxn....those impurities run rampant.
I guess the answer is this....
What most think is fully reduced at the first sign of meth, does not exclude that product from higher levels of impurities that when ingested/consumed have similar stimulating effects on the CNS!

Allowing the rxn to proceed past those suggested cook times has always produced a superior product with less health related cramping and impurity associated jawclenching hellrides!
Again....not answering for the moose...these are just my observations based on Ibee's personal experimentation!


You Laugh at me because I'm different
I laugh at you because you look the same
 
 
 
 
    java
(Hive Addict)
09-17-04 18:29
No 531804
      Need to Monitor the Reaction......     

One thing I learned early in the hobby was TLC. With TLC  the reaction has always been able to be followed by simply spotting the starting material and the intermediate and finish product as reference. Case in point doing meth via chloro-ephedrine (a necessary intermediate ) by monitering the choorination one would know when all the starting material was chlorinated. Followed in this case by hydrogenation which also was monitored until the TLC showed no intermediate product. So with the reference one could spot the finish product and by the rf spots one could tell if the finish product had starting material or the intermediate , also some unknowns have been known to show up, present.

By monitering the steps there is no carry over of unreacted material (minimal), and the final product is almost 100% finished priduct.

I do agree that the iodoephedrine is an intermediate product and if it shows at the end , it only says that the reaction was not 100% complete.

TLC=thin layer chromatography

It is better to die on your feet than to live on your knees...Emiliano Zapata
 
 
 
 
    jackhole
(Hive Bee)
09-18-04 05:50
No 531927
      Iodoephedrine = Iodomethamphetamine     

Iodoephedrine = Iodomethamphetamine - they're one in the same, people just choose the way in which they refer to the molecule. It's the same molecule though.

Jizzy Jizzy Bang Bang
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-20-04 17:29
No 532335
      reply     

Well bottom line, If it ain't meth it don't belong in the bag. Anything that ain't meth is an impurity, hence if you was to measure purity of a substance, anything else in that substance would be impure correct.
 And by the way Ideo is the missed link in what people long for after recrystallizing.. Shit a simple acetone wash will rid you of Ideometh. Wear, You claim a 48 hour LWR wont have Ideo present? Well a fast push pull after a simple acetone wash wont either..

Tighten Up!  (UH)
 
 
 
 
    wareami
(Hive Addict)
09-20-04 18:25
No 532339
      I hear that!     

Jacked:
Well I can't argue with that...not that argument is my style anyway.
We're here to learn and expose the facts, as well as, enlighten ourselves and others toward obtaining the purest product possible.
The simple fact that this still creeps into the discussions from time to time is ample evidence that there's always room for improvement and tightening UP that undefined slackspace in organic chemistry.
I will say this and stake my rep on it.
Along your same line of reasoning, Iodometh is not the only product we're concerned with eliminating that are the result of side-rxns and impurity production in shorter timed cooks.
And you're absolutely correct with the observation that impurities removed, equal reduced overall yield of pure meth.
Those experiencing 30-70% yields are typically the result of pulling a rxn before it's done FULLY reducing.
If 30% impurities are presest in the end-result...following a tone wash and the recommended recrystallization, your final yield will be lower, equalling the amount of impurities removed.
So we agree that impurity = yieldloss!

And as you say jacked....most people are accustomed to those impurites and want them in there dope and think they got ripped off when they get pure shyte.
The impure by-products created in side-rxns enrooute to pure meth account for some CNS stimulation to boot.
Red Phosphorus is a stimulant by itself(not saying peeps are slamming RP)
But RP's presense and interaction with the other reactants account for some of those side-rxn impurities.
They are necessary intermediates just like Iodo, like we hear of like the h3po3__>h3po4, phoshine, etc....created enroute to full reduction.
Pull a rxn before it's time and yields suffer from the impurites left in the basified solution whether or not they are soluble in acetone!
This is why recrystallization is so necessary as a recommeneded practice to insure their removal.
I can't emphasize this point enough that low yields are the result of impurities present, in most cases.
How they get there is simple and how they are removed is simple. What's not so simple is explaining that longer ccoks times equal less impurity-more pure meth.
The numbers speak for themselves and have since I made that correlation long ago.
I set out to verify my suspicions and they proved to me to be correct.
So Again I stand by full cooking times to cook-off or to fully align those molecules that equal purity in product and higher yields of meth.
I can only speak for Ibee's experience with yields in the HI/RP as they differ from hot/fast and the LWR, but they are higher than most bees reports and he attributes this to side-rxn cookingoff/completion in the LWR, compared to removing them at the end of shorter cooks.
Again...No disrespect...and not argueing, just my attempt at reaching a meeting of the minds for better understanding.
You're teachings about patience and The HI/RP, taught this student!

And 48hrs LWR is not a constant fixed in the HI/RP rxn...
It's a gaurantee for newbees to succeed by.
Something that wasn't so prevelant around here in Ibee's early learning as a newbee.
You Jacked should recall Ibee's screams after the 14th failure in a row using the modified p/p(balloon)blushwink

You Laugh at me because I'm different
I laugh at you because you look the same
 
 
 
 
    Organikum
(Wonderful Personality)
09-21-04 00:31
No 532387
      For what reason ever, iodoephedrine is no...     

For what reason ever, iodoephedrine is no impurity in HI or RP/I reactions. Whereby chloroephedrine is a wellknown impurity in catalytic hydrogenations.

I am not going to guess why this is this way, I done this before, but the forensic literature shows after my best of knowledge no iodoephedrine as impurity.
You may bet your ass if this had been found some forsensic DEA funded "scientist" would have baked his elaborated article on this, with testing on rats, mice, brainscans and cruel impact on every living being.

Actually it would be quite interesting how iodoephedrine turns one on - or off laugh

so near, so far......
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-21-04 04:55
No 532422
      reply     

Hell I cant argue that... And am not trying to.
 I wonder wear it would separate in a TLC. And it would separate as the other byproducts do.
This is not a debate on the results of two different rxns. Its a simple question. If iodeo would be considered an impurity or a byproduct. DEA says its not an impurity. They must like the old style dope. I know they hate Ice with a pashion...

Tighten Up!  (UH)
 
 
 
 
    Organikum
(Wonderful Personality)
09-21-04 12:47
No 532478
      And you will find no unreacted ephedrine in...     

And you will find no unreacted ephedrine in the final product of a (successful) RP/I style reaction, except one fucked up the formation of HI at start.
Unreacted ephedrine after a successful RP/I or HI reaction is quantitativly destroyed in the standard workup. The NaI formed by addition of lye to the postreaction and the strongly basic conditions (ph14 hey!) do the trick.

(I sent Rhodium the reference for this times ago...)

Except for lousy workup and new gakk the RP/I is an astonishing clean reaction yielding very pure product. Steamdistillation and a second A/B + recrystallisation give finest product - to fine for many as it seems as d-meth smoked and even snorted is prone to debrain many users fast and effective.
I cant see anything bad in cutting with non-toxic compounds as long as the price is adjusted accordingly. But thats my personal opinion of course, nothing more.

so near, so far......
 
 
 
 
    geezmeister
(Of Counsel)
09-21-04 17:40
No 532511
      sleeper dope?     

Iodoephedrine is an unfinished intermediate, rather than an impurity in the reaction. It might be considered as something other than an impurity, or it may have a signature close enough to meth that the government forensic "expert witnesses" lump it with methamphetamine in their reports and that is why it doesn't show up as an "impurity" in their reports.

I see forensic lab reports that list the substance tested as methamphetamine/pseudoephedrine and methamphetamine/ephedrine/pseudoephedrine without further comment.  The usual lab test is for the presence of controlled substances, not the concentration of controlled substances or the contents of the substance tested. Forensic lab reports do not list the impurities or contaminants or cuts in the substance tested, but only the controlled substances or regulated substances, such as pseudo.

A standard forensics test report would not list iodoephedrine as its presence is not material to the prosecution of the case. Such a report will not list the presence of MSM or any other cut. I recall federal lab reports that reported the purity of the drug sampled by percentage... i.e., methamphetamine of 50% purity. The report did not list the other ingredients, however.

The federal sentencing guidelines contain provisions for sentencing under "mixture or substance containing" provisions when the substance seized is not relatively pure. Federal lab experts can evaluate a sample for the purity of the drug. In some circumstances they have to-- for instance if the prosecution wants to punish possession of "Ice" the lab has to report the substance tested was at least 80% methamphetamine. If the substance is below that level of purity, it is charged as meth, and if its really dirty its charged as a "mixture or substance containing" methamphetamine.

mostly harmless
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-21-04 19:59
No 532531
      I agree with Organikum.     

I agree with Organikum. I also agree with Geez. And Wareami. 
 I also stand behind what I'm saying and that is "anything being in a product other than the product itself is a fucking impurity! unless of course your target is an intermediate. Then the damn meth would be the impurity..
:intermediate: A substance formed as a necessary stage in the manufacture of a desired end product.
That substance is not the desired product now is it? There fore it is an impurity.. I rest my case. I wont reply to anymore of this nonsense so carry on and explain it to someone else less hardheaded..

Tighten Up!  (UH)
 
 
 
 
    memeep
(Newbee)
09-21-04 20:22
No 532532
      Iodoephedrine     

That substance is not the desired product now is it? There fore it is an impurity.. I rest my case

...and it will cease to be an impurity as soon as you have strongly basified at the end of the reaction because any that may have been present will cyclise.

...it's turtles all the way down!
 
 
 
 
    geezmeister
(Of Counsel)
09-21-04 22:10
No 532555
      E v. Pseudo?     

Orgy-- your comment may be correct with Ephedrine. I have a lot of experience with pseudo, and just a little with ephedrine. Your comment isn't accurate with pseudephedrine, however. I had enough failures learning how to make meth that had pseudo in the evap dish rather than meth, or a mixture of pseudo and meth in the evap dish, to agree that hard basing will do pseudo in. If hard basing did, the pseudo would not have been there -- taste, smell, crystal pattern. But it was pseudo... no doubt about it.

It always reacted well the second time around, as I recall.

On a similar note, I have had reactions, and watched others do reactions, that produced a white crystalline powder that looked, tasted, melted, smoked --- just like methamphetamine. However, the net effect of the use of the drug was to put the user to sleep. I have seen "meth" like this that had long legs when it rocked right back up... stuff that burned clean on foil or glass, but just did not do anything other than make you sleep.

I realized even then that the common problem those reactions had was an insufficient amount of actual phosphorous compound. All of them were less than complete reactions. Some may have been caused by the phosphorous being coated by a wax or gakk, and some may have been caused by using red phosphorous that was more glass and trash than red phosphorous. I can't recall seeing this phenomena with hypo or phos acid cooks.

I always assumed the product in the evap dish that put you to sleep was an intermediate that did not completely reduce. It certainly wasn't methamphetamine, and it wasn't pseudoephedrine. What besides an intermediate could it be?

The a/b did not break it down, and acetone did not wash it out. So what, I wonder, was it. I always figured it was iodoephedrine, but that was just my speculation. Sleeping Geez is something to avoid making, for certain.

mostly harmless
 
 
 
 
    Organikum
(Wonderful Personality)
09-21-04 22:41
No 532561
      There are several forensic articles available...     

There are several forensic articles available in which impurities specific to for a RP/I reaction are analyzed by sophisticated means including GC/MS and soothsaying.
The forensists even ran the reaction short in a try to maximize impurities - simulating reality somehow or whatever so I remember this right.

We know from these articles about aziridines, which were first discovered in analysis of product and then the reaction mechanism adjusted in theory as so often, about P2P and some minor byproducts.
We know also from these articles that after a standard workup neither (pseudo)ephedrine nor iodoephedrine is to be found in the product. This is backuped by analylis of street samples AFAIK. Not the samples analyzed for determination of the content of meth - but those for writing nice articles in forensic literature about dangerous compounds found in street-meth, cashing in some goverment money and getting some cheapo points on the publication scale.

I myself was convinced that unreacted ephedrine might be a impurity of lousy reactions. It isnt. And neither is iodoephedrine. The nonexistance of pfed is easily to explain, why no iodoephedrine thats a point of discussion. But the discussion is about "WHY NO" and not about "IS THERE ANY". 

After my best of knowledge, this may be not much but I try my best, bad quality of meth from RP/I is caused by shitty workup or lately by non-removable gakk or gakk-reaction-products coming through all A/B´s and recrystallizations.

I have no doubt that meth made by Jacked was and is first class.
Also meth by Geez is probably consumable, but for propagating this evil "titration" Geez gets a malus from me. Overall quality suffered badly since ppl started to dump some dirty  hardwarestore muratic acid into their nonpolar and then evaporated the liquid. And that no A/B anymore. Thats dirt, containing all shit from the nonpolar and from the muriatic. Gassing was MUCH cleaner.
Thats no titration, thats an obscenity.

No offense Geezemeister, but whats true must be told. Ya have enough merits otherwise
laugh


This iodoephedrine is a made up nonsense discussion - learn a better workup, do a second, a real A/B and a real recrystallization and your problems will be gone.
But most just cant await to get some product into their pipe and then brains gone anyways.
Not Jacked.


I hate it to sound like Osmium.
Fuck.
Out here.
ORG

PS: I have seen no pseudoephedrine specific articles, thats a point, but I doubt this makes a difference. But I have no prove.
Nevertheless I am anxiously awaiting the next generation of forensic articles on impurities, dangerous and nasty impurities which is highly probable to come. The impurities caused by different plastics, dubious OH-group carrying compounds and shit called gakk.

so near, so far......
 
 
 
 
    abominator
(Hive Bee)
09-21-04 22:42
No 532562
      Re:Sleep Aid Dope     

EDITED


Swim has done what he and some others refer to as "sleep aid dope", this is exactly what Geez describes, a mixture of unreacted pseudoephedrine(apparently azirdines) and some other impurities that will give a rush when consumed but will bring on sleep to a user with a tolerance.  Swim has used this dope and went to sleep while typical street users thought it was the shit, go figure.  Those were hard times and after one particular bag of sleep aid, swim decided that never again would he purchase street dope, no matter how long it took him to gather the precursors.

Swim apologizes for talking out his ass.  He never claim to have TLC equiment.  He was only trying to relate his personal experience, as it may help to further our knowledge of how impurties affect us.

G69
 
 
 
 
    Organikum
(Wonderful Personality)
09-21-04 22:51
No 532564
      You have not done an analysis onto your ...     

You have not done an analysis onto your product so your talking about what the impurities are is talking out of your ass.
TLC is easy.
Do it or shut up.

so near, so far......
 
 
 
 
    geezmeister
(Of Counsel)
09-21-04 23:20
No 532569
      probably right     

Orgy you are probably right about titration. That is why I took to gassing, and later distilling. My comments about sleeper meth are historical and from several years ago. Your observation about azirdines is most likely the answer to sleeper meth. That also ties in to the observed inadequacy of the phosphorous compound in those reactions.

I take no offense to your doubts about the quality of my product. We are all entitled to reasonable opinions, right or wrong... laugh

mostly harmless
 
 
 
 
    wareami
(Hive Addict)
09-22-04 01:31
No 532588
      And Now...     

You didn't think y`all would escape my two cents without me knowing about it did ya?shockedcool
I either posted something today that met with it's demise, or I didn't post it.
It's all good though cause it contained truths that make me shudder...having lived them.
We'll not go there right now, in more ways than one.
Rhodium recommends a steam distillation followed by re-xtal after an HI/RP rxn.
Without the access to a GC/MS, I too get frustrated like Jacked whenever this discussion arises without a definitive resolve.
I hate to think, as Orgy says, our only resolve will come by way of a Twisted Bias Forensic Analysis of meth seized via evidence and forfeiture from a "God only knows" type method of production.
The type rxn plays as large a role as source of the starting material.
Orgy...I have to disagree with the way you handled abominators remarks...it's not your style and not beecumming of you! Especially after the last remarks you made in the previous post toward the king of one liners at shutting one up.
I shant spank you however cause I know you meant well!laugh
TLC will not help me identify the substance! It will tell it's present or not. Who do you recommend I should call to tell me my first rf mark is pure d-meth??? mmmmmkay!!!
And will they bee so kind as to tell me the exact names of substances in the middle marks that I tested from "pulled on purpose" rxns for this test??? MmmmmKay!
Case rested on TLC versus GC/MS that I don't have!
While it may be true that NaI causes decomposition or destruction of unreduced pfed/eph...This possibly might not be the case in the removal of free I using Na2S2O3 from the post-rxn solution prior to basing.
Org, I did take note however of that little figure in () pH14wink
Neither here nor there!
Okay...Now!
Case Reopened!wink
I aim to drop everything right now to discover where I need to go to get this solvent used in TLC or a suitable substitute as well as the type paper needed.
Jacked, I recall us both participating in that TLC thread.
Seen it suggested several times since so there must be something there for us chemhacks. I'm game! I'll bite! I bite at chemistry anywayblush And a little nonmenclature never hertz I always say.
I aim to put an end to this once and for all.
I also refuse to dance around a subject without having a grasp of proper terminology as I feel I've brought a knucklesandwich to a gun fight lacking the formal education.
If those bees are concerned enough about these impurities presence in their consumable product, they'll choose the routes of cooking that help ensure those aziridines are cyclized fully into a fully reduced product.
The only rxn I've seen on this board that substaniates this insurance of full reduction is the long slow controlled route!
Let your Yields guide you since we know
Impurity=Azidirine=By-product=intermediate=under-reduced intermediate=iodoephed/iodometh=FUCKIN TRASH
Subtotal=YIELDLOSS
Meth subtracted by YIELDLOSS=20-90% meth
Class over!
(Hey I didn't know I had class today?blush)
I didn't!
But with any luck and a miracle, I'll have some class tomorrowtongue

If it ain't broke....you ain't been tryin hard enough!
(Here...let me at it!)wink
 
 
 
 
    Organikum
(Wonderful Personality)
09-22-04 11:22
No 532669
      Geez, I have no more doubts about your product     

Geez, I have no more doubts about your product now as you told me you gass again...laugh

Also I want to add two things:
- I have seen pseudo coming through the reaction inc. workup myself - protected by gakk.
- I know the "sleepy meth" too. But it is only known to long-time and/or heavy users and I suspect this being related more to effects coming from using much a long time than from impurities. I have also seen somebody falling asleep after taking 1/2g ultrapure meth (clear shards, double recrystallized, from labgrade E) - you fall asleep when you take to much too I say and after a long time of using the drug it is possible that your body says "time to sleep" although you just have slept 24 hours.
The usual regualary user has such an amount of sleepdeprivation accumulated that sleep is not a symptom which is to assign to anything anymore. Paradox reactions are common then, like taking a stimulant and feeling sleepy. One may not think this vanishes after a week or two without meth. Half a year up to a year thats it.


Meth is what I love. But tweaking is not what I love. Meth is a very potent drug and I need it clean for two purposes: For the better turn of pure meth. For its only possible to dose correctly with pure meth. Undefined product sends me tweaking sooner or later, always, just because a correct dosage is not possibly to find. This says overdosed sooner thasn later.
I have seen only undefined product coming from heavily gakked pills.


ORG

so near, so far......
 
 
 
 
    geezmeister
(Of Counsel)
09-22-04 20:58
No 532729
      no argument here     

Orgy... you have no argument here. You comments match my historical experience. I recall watching my mentor fire a very large dose of what appeared to me to be very good meth...and fall asleep within minutes. He was suffering from severe sleep deprivation at the time.

Sleep deprivation will also impair your judgment of the quality of the meth taken... and help lead to overdosing.

Your last comment is an anthem for a number of bees, myself included. I could not agree more with your comments.

mostly harmless
 
 
 
 
    Jacked
(Ancient Alchemist Delux)
09-23-04 08:36
No 532801
      I get it     

I get it... Thanks memeep, Now I understand were these post are coming from... Well put!
 I was in asumphion and generalized the ideo as an impurity as any thing else found in a finished product, how it got there was not in my problem area. My bad..
 Wareami, TLC is easer than you think to put together. PM me an I will share what I have learned about it.
 This is a good read and explanes well   http://www.chem.ubc.ca/courseware/121/tutorials/exp3A/columnchrom/

Tighten Up!  (UH)