popi (Stranger)
03-22-04 15:39
No 496622
      e/rp/I2 Reaction     

Rp was added to hot I2 and E,h2o.Way too fast! and smoke came and went a few minutes later.The reaction was e:10,mbrp:6,I2:13  ,dH2o:3.5ml.With additional rp,I2,H2o as needed.The smoke was bad,how bad?.Swim wonders how much chem's were burned?Rp after this smoke is still reuseable?Re-Worlock.Won't do that again!
 
 
 
 
    geezmeister
(Of Counsel)
03-22-04 17:24
No 496640
      more water, less heat     

Add more water at the start. This was too dry anyway,in my book. Never heat these chems up to mix them. They will react and generate their own heat, anyway, and you only speed that reaction up by having some of them hot to start with.

Read more. Waste less.

mostly harmless
 
 
 
 
    barkingburro
(Hive Bee)
03-22-04 17:41
No 496645
      heating when mixing     

on the subject of chems heating when mixed, can any-one explain the mechanism for what causes a mixture of h3po3, i2 and d/h2o to be so endothermic? seems odd since rp, i2, and d/h2o is so exothermic
 
 
 
 
    popi
(Stranger)
03-22-04 18:06
No 496656
      Has the E burned off?     

Thanks!As is written 5ml or 8ml dh2o for a lwr.Swim knew it would smoke, but not that bad. Swim saw a old Worlock thread for a hotter quicker reaction and was sidetracked.Big mistake!The bad part is there alot of lost E?

the walls have ears
 
 
 
 
    Newton
(Hive Bee)
03-22-04 20:23
No 496678
      The bad part is there alot of lost E?     

The bad part is there alot of lost E?

What did the smoke look/smell like? What does the remaining reagent mix look like? Is it still wet/sludgy?

I guess most of the e is still intact, as reactions dryer than this still yield some useable product. As Geezmeister suggested, add some more water and run a lwr with the recommended reagents ratios / reaction temperatures / duration.
 
 
 
 
    Ganzas2003
(Hive Bee)
03-22-04 22:38
No 496690
      was it voloptous smoke?     

was the smoke like red and suddenly all reaction vessel is kinda orange???

that happens when u do quick reactions and start heating right at the beginning...what should take like 20 minutes minimum took like 5 seconds???

in my experience some lost will be noted but keep it going.

cheers and global peace
 
 
 
 
    popi
(Stranger)
03-23-04 02:23
No 496742
      orange smoke     

The smoke smelled like rp,I2 did'nt think too much at the time as I was lifting the condenser out of the flask to stop the pressure.It was strong and intense 6 gms at once at 150c,it was a sight...was orange,yellowish hue with drabs of red.Went dry so I had to add h2o and is a liquid now after the dry spell and sludge.It is dark close to black now,Hi is present,after I thought I had to add more I2 a gm or so.Oil bath is down to 100c.
 
 
 
 
    popi
(Stranger)
03-23-04 02:37
No 496745
      How did you know?     

Ganzas ,Swim just read your post and lol,you saw it too,eh?Your words!,yes it was very voluptuous! Very colourful orange.What was the smoke rp:? e:? or both?,can a big burn like that ruin the rp?

the walls have ears
 
 
 
 
    Ganzas2003
(Hive Bee)
03-23-04 09:29
No 496814
      yes..     

i saw it. It ruined my first 4g PFed try in the terms of getting 1g at the end. After that i allways have an ice bath close. But I think u didnt want to do a quick so u probably have made wrong your calculations....From what ive read here. Long WET Reflux is supposed to be a WET thing.
Those fires will not happen. Reaction is "safe".

THAT IS ONLY A CONCERN WHEN U DO QUICK REACTIONS.

and for that have that ice bath close and dont heat from the beginning coz once the reaction starts getting faster u simple cannot "stop it" by the Ice since u will crash the glass. Start slow and apply heat holding the flask in hand like 3 seconds....dont let it start very fast...when that happens place in ice...but then again dont let it stand in ice indefenately forever...thats the problem in the quick reactions...they are good for observation.

LWR IS BORING. Boring=better yield & quality and safer.
 
 
 
 
    place
(Newbee)
03-23-04 18:23
No 496858
      Using water in every rP/I reaction     

Do you have to use water in ALL E/rP/I/ reactions? Also the fast hot dry onces?

In every synth. they talk about the chems beeing liquid after some time, but the nano SWIM made, was pretty dry!

Flipside
 
 
 
 
    geezmeister
(Of Counsel)
03-23-04 18:50
No 496860
      Yes     

Even the dry reactions take some water. Aside from impure precursors, which will doom any reaction to failure, the principal reason for newbee failures in rP reactions is too little water.

Why fight the odds? Take the time to do a long wet reflux and save your sanity, your precursors, and your pocket book. Increase your chance of success. Improve the dope you make. The dryer reactions CAN be pulled off successfully IF you know what you are doing. Even then, the quality of the product will seldom match that of the LWR, and the yield never will. I say that from experience with both types of reactions. The LWR is like falling off a log compared to the dry cooks. Why do things the hard way?

mostly harmless
 
 
 
 
    Relux
(Stranger)
03-24-04 05:06
No 496980
      I fucked up in a similar way, gassed my house     

When attempting a pretty dry reaction with a pushpull, I didn't realize until too late that there was an iodine crystal in the flask joint. The mixture was slightly heated and went off with a whoosh, essentially filling my house with a choking white gas (presumably HI) which stained many things brown. A bit more iodine was added after stopping the reaction finally in a ice bath, and the reaction was continued in a way I figured might work (so many freaking ideas, directions, procedures, ratios times, how the hell should I decide which to do? mad ). In the end I obtained slightly yellow large rhombic/rectangular pillar like crystals as the acid form, which turned to a fishy smelling oil in base. This substance did not smell quite right. This did burn without residue. This did produce a high. The high was almost uncomfortable, quite anxiogenic, crampy and did not prevent sleep. What the hell is this shit? Anybody know the properties of iodoephedrine?
ps. The yellow of the crystals was removed during a recrystallization to produce a product with similar crystal structure (smaller crystals, same shape) that did not seem to produce the same degree of buzz.
 
 
 
 
    ADDkid
03-24-04 06:03
      The red smoke that came off was PI3, ...
(Rated as: misinforming)
    
 
 
 
    popi
03-24-04 17:09
      #1 problem for all newbees
(Rated as: incomprehensible)
    
 
 
 
    place
(Newbee)
03-25-04 01:07
No 497110
      Well     


  geezmeister : Why fight the odds? Take the time to do a long wet reflux and save your sanity, your precursors, and your pocket book. Increase your chance of success. Improve the dope you make. The dryer reactions CAN be pulled off successfully IF you know what you are doing. Even then, the quality of the product will seldom match that of the LWR, and the yield never will. I say that from experience with both types of reactions. The LWR is like falling off a log compared to the dry cooks. Why do things the hard way?




Well, SWIM would still like to try a hot dry rxns before attempting LWR. Can you give any precisely ration between ephedrine/water (assuming LG precursors)? Like 5mL/10g eph.

rgs, place


Flipside
 
 
 
 
    SHORTY
(Hive Addict)
03-25-04 02:05
No 497123
      Well no,     

Thats the fun of a hot, dry rxn you gotta figure it out for yourself which is where the symptoms geez stated start to occur.  So you see your probably already frustrated and you haven't even started yet.  Hopefully you got a big pocketbook, alot of freetime, patience and luck cause your heading down a long winding road even though you could take the expressway.  It will take you alot longer than 48 hours to get reasonable results from a hot dry cook.  So actually the lwr is most likely the fastest way for a newbee to get some good results.

It wasn't Me!
 
 
 
 
    ADDkid
(Hive Bee)
03-25-04 03:06
No 497143
      Could someone educate me on the last comment     

Could someone educate me on the last comment that I made, it received bad karma, and I would like to know where my mistake is. Is it false to believe that red P, and Iodine make PI3, or is it false to believe that moisture and PI3 make H3PO4 and HI,  Any else that I stated was just my theory, and I believe that I made that clear.
 
 
 
 
    CharlieBigpotato
(goat)
03-25-04 05:09
No 497172
      seeking education:     

what is it about humans that must see all matters in 2 extremes?

i've only got 2 ears; one for the evil voice; one for the good.

you must either do the 36-48 hour nonsense; or you must do the 2 hour nonsense...that was the nonsense that was "all-the-rage" a few years ago; when people would brag about the product and post digi-pics of its lurid desirability; along with rave reviews concerning the absurd, yet sexy, push-pull unit.

ya'll bee out there with this crap, but i love you anyways
 
 
 
 
    Anonymium
(Stranger)
03-25-04 06:35
No 497187
      Re: Can you give any precise ratio between...     


Can you give any precise ratio between ephedrine/water (assuming LG precursors)?




1ml water/40g ephed.  If rp is used or I2 is homemade they're probably somewhat wet and you can lower the amount of water added to 1/2ml. 1ml is equal to one full 100unit insulin syringe. If you need to add more you can always do it as the reaction progresses.

 
 
 
 
    popi
(Stranger)
03-25-04 08:58
No 497210
      "jones,en "for a hot , dry reflux     

Place: Read post 497110,then read it again 2 or 3 times!Search Geezmiester and read all post's. If then you don't get it click on Popeye,Worlock,Methead,Placebo profile's,click read good post's or all and you will find your answer. I am not able to do that because I am not a chemist these guys are ...the best!There is no ratio,for a hot dry formula,you have to controll it and it is dangerous and hard.It depends on your heat, percusors,glassware altitude etc.If you are a real smart ass,best you pm Warami,Geezmiester or any other bees that know what they are doing to save you your money,time and your clothing.Do you have a "Toast"Fire Proof Rain Coat"?? YOu might need one!                                                                                                                         Shorty:The long and winding road to a short dry reflux, has cost me 29gms of no gak sudo,and 10 days time. On 5 reactions!Place listen to shorty,it could dry up!be too wet!start a flask fire!blow a flask or a cheap salt shaker,test tube,soya bottle..whatever.Balloons blowing up and knocking the flask over into the oil bath has happened more than my once.Shorty you know .Thanks for the input.Love your posts and could ya send me your write up on your gas patent?My computor is fucked.

The walls have ears
 
 
 
 
    Osmium
(Stoni's sexual toy)
03-25-04 09:18
No 497214
      I am still desperately waiting for an ...     

I am still desperately waiting for an explanation of how this reaction is supposed to proceed with just a few percents of water.
I guess it all boils down to 'faith based science'. Good luck, and lots of faith... you will need it.

BUSH/CHENEY 2004! After all, it ain't my country!
 
 
 
 
    popi
(Stranger)
03-25-04 09:47
No 497218
      Osmium that post is not my baby!     

How can you give a precise ratio? when your I2 is probably wet?dry:?,or mbrp wet? or dry:?What is it man? Wet or dry:?I used 3.5mls and it flashed like a meteorite hitting the Palm Springs desert!Orange gak plumb of smoke!P13 Osmium? I was told.

The walls have ears
 
 
 
 
    popi
(Stranger)
03-25-04 10:01
No 497220
      Sexy "push" n" pull"     

Never had one of them Charlie.Have pics from the Lwr though and pics of the bomb [orange] in the kitchen:!Don't know how I'll clean it up...
 
 
 
 
    popi
(Stranger)
03-25-04 10:08
No 497222
      Kid you know the answer     

you'all get bad Karma sometimes,it depends what ya say?like chemistry you have to be perfect!

the walls have ears
 
 
 
 
    Rhodium
(Chief Bee)
03-25-04 15:38
No 497267
      ADDKid     

The red smoke that came off was PI3 [...] The iodine and Phos. react naturally to form PI3, which is a gas.

Phosphorus(III)Iodide has a melting point of 61°C and a boiling point of 227°C.

http://www.webelements.com/webelements/compounds/text/P/I3P1-13455011.html

I belive that [...] some species of PH3 are formed when the reaction has reached equilibrium

If you read the recent discussions about phosphine and phosphonium iodide you will see that these species can and will form well before equilibrium is established (equilibrium is defined as the point in time where no net reaction longer occurs, i.e. after anything reducible has been reduced).

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    popi
(Stranger)
03-25-04 15:53
No 497269
      Finished Reaction     

Taking the elder bees advice boiled the post rxn fluid 5min.Fluid looked cloudy yellow,rp fell fast.Based to 14 and distilled,putting a spoon of sand in!thanksVD.A shit load of lovely smelly oil came down,cleaned twice with Xylene and PH'd to 6.Evapped and got my sudo back!Yup again.It was the I2[no big crystals,black not grey] or the E[no pinwheels,chalky crystals+light fluffy cotton candy texture]...

wanted:live in female maid for cleaning stains in kitchen
 
 
 
 
    wareami
(Hive Addict)
03-26-04 03:14
No 497401
      Will it ever sink in?     

Most bees will sink rather than swim if they can't learn to read between the lines anywaves?
This is not directed at anybee specifically so unruffle yer feathers and ~Just Wing It~.
For quite some time bees have been being pushed toward longer cooking times! Do ya'll think that it is any one or two bees doing this pushing?
C`mon now?
The feedstock is a major change in this scenario since most are still working with OTC pill sources.
A bee doesn't dictate how long the rxn runs before it's completely reduced.
The bee with experience will gently guide others toward what is working for them based on the changes they experience!
This longer cooking time is the best gaurantee a caring bee can give to another when guiding or suggesting how the rxn should go down.
The hows and whys would fill a book and for brevities sake, some of the most simplist common sense judgement calls are left to the reader.

H2O is your friend regardless of the feedstock source in the HI/RP rxn. Many bees have concusions from trying to drive this point home!
If ya'll don't mind working UP pfed after 12hours of reacting followed by another 12 hrs typing and looking for answers to where ya went wrong, then so bee it.
The solutions are all here for the taking and the LWR is geared for the most likely success a bee will have today when working with OTC pills, regardless of the extraction method!
Many bees have poured their hearts and souls into steering bees toward obtaining the cleanest feedstock available.
Those same bees slaved for months on end trying to develope a failsafe method for achieving success.
Unfortunately The Curbshot will not work 9 times out of ten today! In it's day it worked 3 out of 5 times.
What does that say about the starting materials?
The LWR contains built-in safeguards aside from the encyclopedia of information that's been provided UP until now.
Until it's employed verbatim, the rewards will likely remain as mysterious and eluding as meth itself, for those bees without the WarewithAWE to pull it off to begin with!wink
In the first sentence, Ibee can spot a bee a mile away that's done his homework and the necessary trial experimentation.
Anybee that isn't drying their precursors prior to weighing them out must not be serious about the importance that ratio plays in the rxns ability to reduce pfed to meth. They doom themselves to repeated "Back To The Drawing Board" syndrome.
Is is laziness? Or is it complacency that fuels these undersites, prerequisites to failure?
Ibee says It's this simple.
•Obtain yer feedstock and precursors!
•DRY them completely and THEN portion them out:
•10g E
•12-13g I2
•8g MBRP
•5-8ml dh2o

Mix however ya want but making HI first is less stringent(harsh) on the pfed.
Cap off with balloon or condensor after thoroughly mixing AWE the ingredients.
Place flask in an oilbath and run at 95-100°C for 36-48hrs
36 hours for the 5ml dh2o ratio and 48 for the 8ml dh2o ratio.
During the first 2 hours the reactants will be liquid and will have risen some, depositing precursor on flask sides above the pool....SWIRL to bring all the red back into play that might have gathered above on the glass and then put back on the heat.
Stir the rxn every 8 to 12 hours to insure decent recycling of HI.
If the rxn can't GO all the way in one shot, Pull it off,  note the time, and resume later for alotted time.
It really is that simple and if the benefits and merits of this LWR don't make beelievers of bees, Ibee will eat his hat!

Ummmmmm....errrr....uhh...Ibee is not an advocate of running less than pristine clean feedstock but he's made that area his lifes work and passion. That doesn't mean he's above looking at things through other bees eyes by purposely falling short of his HIGHer than normal standards in attempts to prove what'll work and what won't. Many inactives will live and thrive being bombarded for 6-24hrs....
Not many stand a chance for very long past that but they will create some nasty side rxns that require an additional time under that pummeling to be rendered null and void or at the very least incabable of doing what they were invented and employed to do!
So....when you finally do fall off that log into the sWhirlpool of success, Keep Swimmin cause thar's no turnin back once ya walked the plank....
Docked-Oars Ordersshocked
~JUST WING IT~


a little less conversation, a little more reaction
 
 
 
 
    elfspice
(Hive Bee)
03-26-04 06:04
No 497440
      dry cooking *does* work... but....     

Os, small amounts of water will form 57% HI with rP and I2 floating around. However, this also risks lots of other problems, flask fires, for one (lwr can't have a flask fire except in extreme circumstances), decomposition of the ephedrine via oxidation from high temperatures... and never mind the fact that the HI cannot form without water, and thus you end up with a lot of subliming I2 staining up your tubes turning them black and stinky.

The thing is, all these newbies don't understand the principles behind the reaction, otherwise they wouldn't be so stupid. the rp makes the I2 into HI, and HI reacts with pseudo/ephedrine when in a 57% (ie concentrated, fuming) solution of HI. So making the HI is the most important thing in the reaction. (yes sorry i know wise bees know this i'm aiming this at newbees) (oh just cos it says newbee in my doesn't mean i'm really new around here ;) oh and of equal importance is that the HI remains concentrated in the solution

The amount of water to add should be no more than is required to turn all the present I2 into HI at 57% concentration. I presume that 57% figure bandied around refers to weight/volume ratio, meaning that you want the level of water to be about 43% of the iodine/water together, or in other words, about 75% of the weight of iodine (weigh the water), probably a little less to ensure that the HI concentration doesn't drop below the level it requires for reactivity. This assumes you have enough phosphorous to react into the 57% solution, plus enough extra to match the amount of ephedrine to be reduced (that's 1 mole of elemental iodine per moles of ephedrine)

This isn't as easy to get right for ghetto kidz with wet reagents, but you can get it closer to being right...
 
 
 
 
    popi
(Stranger)
03-27-04 10:31
No 497664
      White crystals! Newbees read this.     

Ware did these crystals come from?Do not smoke these kid!!What are they?There not gogo! Another day,another suprise.Saw a small pool of white,foaming little bubbles.This is not right,so bee checked the condenser and sure enough it was harvesting a small pile of white crystals,to the point of blocking the gas flow.Back to the drawing board brought bee good results!Read Warami's Dea-Egull pull and arose to find the pristine pinwheels!Not great yeilds,focusing on Quality now.Can't seem to get the New straight to E solution to reach 105c.Video Editor has a greeeat formula!How long can it take to 105c?Many thanks to V.E.,Warami and Geezmiester for there thread's.'Too Much Acid',my I2 is grey:little cigar crystals now.And the E has the pinwheels plus new powder mbrp ,not sand- like mbrp.In the post...'it's not the weight of rp, it is the surface contact'.Thanks G for that is the formula for success.Bee's Not re-using the last rp that burned in the P13 smoke fire we had.It is brown so I will leave it.Bee wants to check the 8mls h2o:that is not per gram is it? and for VE's [calcium chloride gasser],Bee has a bag of calcium chloride,which has water as an ingredient,sodium chloride and potassium chloride.Is this the right chemical.?Used as ice removal.Rodium,thanks: found a rubbing compound 70%ethanol,with camphor ...got it but it does not sound right.Camphor?And big search found Naptha v&p called Coleman's.It's in Camping section of sounds like "Ball 'her'Mark". SquidDippy found a small, one hand shear that cut's more than 25 strikkers at once! Squid you'll love em.They are orange and black called "Fiskars" found at sounds like " Sheome Riko",Place them in a vision ware pot on low heat with Isoprop alcohol70%,stir,twice,3 to 4 min.decant.No shaking,no bottle.Brilliant Squid!Thank ya'll.Peace

Wanted:Female Live'n'Cook that can pile match covers
 
 
 
 
    popi
(Newbee)
04-01-04 04:31
No 498396
      Lot's of Hi white crystals     

Thanks,bees Short,Gee,Wear and mods!Read the post and did'nt realize it was the Same as Shorty's. It was Hi crystals not Lye.I thought I fuckd up. I have that pale yellow post sol to base that I saved.There was alot of Hi!!! so after 36 hrs Bee is pulling.If not finished,can I react the post sol again?It was set for 48 hrs,and I pulled it at 36.Having no smell to it matter?

Stove is clean but Counter?needs a pro cleaner=Chica
 
 
 
 
    wareami
(Hive Addict)
04-01-04 06:11
No 498406
      Pessimism will get you no ware....     

smile
Walk that plank with confidence!
Thares no room for negativity if yer invoking the proper incantations and wareing the right beanie!tongue

a little less conversation, a little more reaction