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    Aquarium
(Stranger)
09-23-01 14:42
No 216379
      Obscure Meth Synth...    
   
Fictional situation:

I am about to try this obscure meth synth.  I’ve done a search and must have browsed thru hundreds of pages that came up in these searches and noticed that there is not many detailed write-ups on this specific procedure.  One I found was on Rhodium’s page and by Wizard X which is what I would like to try.  I would like to present it here in detail before it is actually performed since there may be something I overlooked in the hundreds of pages on this seemingly old topic.  I did find a few things here and there though and have a I few questions about the process.  I have a lot of lab experience but have never synthed meth and have no microscale equipment so I’ll start off here:

I have pure ephedrine.HCl, red phosphorus and 55% HI.

In a 12L RB flask I place the following:

8 mol ephedrine HCl (1614g)
400g red phosphorus
3400 ml 55% HI (24.88 mol HI)
3” egg shaped stir bar

Question 1.  Do I add these in any particular order or rate?

The 12L is then placed in a 12L soft heating mantle which will be on top of a heavy duty magnetic stirrer.  On top of the flask is placed vertically, a 1000mm long ‘triple-surfaced’ condenser with cold water flowing thru.

Question 2.  I have read that some use a tube attached to a vacuum adapter on the very top of the condenser where the tube then goes to an inverted funnel submerged in a bucket of water and this is supposed to get rid of the noxious fumes and smell.  I have also read just to exaust it outdoors with or without and activated carbon filter placed inline.  At this scale, I am not sure which would be most practical.  Either way, ventilation will be very good.  Which method should I use?

This step I will perform in low light conditions or use an aluminum foil light shield on the flask.  I have read in the Merck that the HI can decompose under light and someone even posted a ref where the yields were better if preformed in the dark.  With stirring and no thermometer, the contents are brought to a gentle constant reflux for 25h, then the heat and stirring is turned off and left to cool for an additional 12h.

Question 3.  Do I have to baby-sit the reaction for the entire 25h time or once it reaches the slow reflux, can it be left alone for the remaining duration?

Question 4.  Am I to expect dirty colors, gasses, fumes, bubbles, violence or inconsistency in the reaction?

The reaction mix is dumped into a 20L or bigger HDPE bucket containing 14L of distilled water.

Question 5.  I’ve never used distilled water before.  In this case, does the water have to be distilled water or can I use plain tap water for all steps that require water?

This is then manually stirred with a big stick for a few moments, then the red phosphorus is vacuum filtered.

Question 6.  I would like to re-use the red phosphorus if possible.  I have read that people just rinse this with water (distilled?) and sometimes with acetone the grinded with a mortar and pestle.  How do I thoroughly clean this and how many times can I re-use this?

Enough 40% NaOH is added to bring up the pH to 14.

Question 7.  At this scale, there will already be a significant volume of liquid for one person to manipulate all at once.  To reduce this volume can I use concentrated or pure NaOH instead?

I assume this will heat it up and after the addition of NaOH so I will wait until it cools.

Now I do not know what the entire volume will be but might have to divide this into 2 steps.  If this will all fit, it is now placed into a 22L sep funnel and extracted thrice with 1.5L of toluene.  If it doesn’t fit, I may place it all into a 50L carboy with a spigot on the bottom and use overhead stirring instead of shaking.

Question 8.  I have read that some use Et2O and some use toluene but never read anything about DCM or pet ether.  I would prefer something that I would not have to evaporate so I can proceed directly to crystallization.  What other solvents can I use for this?

The solvent/freebase extracts are now washed with 1L of water then dried.

Question 9.  Wizard X says to use sodium carbonate and I’ve read that others use magnesium sulfate and I also read to be careful of freebase absorption and to rinse the drying agent afterwards which is standard procedure.  What are the best drying agents to use for this step?

To the dried solvent/freebase I add concentrated (pre-bubbled) IPA/HCl then vac filter.  The toluene is miscible with IPA.  I am assuming that the crystals are not soluble in the toluene and the amount of IPA will be minimal.  The crystals are then collected and dried in front of a warm blowing fan overnight.  I assume from what I read that these crystals will be clear and not white.  If they are not completely clean, I will rinse with acetone.

Question 10.  Can I expect a minimum molar yield of 80% (~1186g)?

Some discussion and concerns (probably more to come after trial synth):

In the Merck, it says that 1.5% H3PO2 (hypophosporus acid) can be added to prevent discoloration and regenerate the HI.  I am guessing that this is useless for me and would add the burden of acquiring it.  The 12L flask is single necked and I have no way of monitoring the temperature of the reflux but am familiar with slow addition of heat to bring it all up to a gentle reflux which I suspect will be approximately 125 deg C.  Wizard X says to add crystals of sodium thiosulfate to remove the free iodine.  The Merck says this is soluable in water so I assume this is just an ‘indicator’ that will form NaI or something like that, but might be wrongfully dismissing the usefulness of this step.  I am also skipping the distillation of the freebase because I am assuming that it will be very clean and the method of crystallization I am using is not just adding aqueous HCl and evaporating the whole mess.  I also read that it will be hard to separate the iodo-ephedrine and feel no need to try to do this or try to convert this further.

I am a little bit confused on the very detailed, informative, but complicated posts by xtaldoc about the 6.6x molar ratio of I to ephedrine.  I plan on doing just a simple melting point determination to try to determine the approximate purity of the product.  Another question:  Should I wash the mix with toluene or something similar BEFORE the addition of the NaOH?  I also read that Bizarium was going to do a modified write-up on this procedure with extraction tips, but do not know if he ever posted it and I could not find it.  If someone saw this, could you please point me in the right direction?

Thank you for reading and I do plan on posting a detailed outcome if anyone is interested.
 
   
 
   
    terbium
(Old P2P Cook)
09-24-01 00:33
No 216470
      Re: Obscure Meth Synth...    
   
I hope that you are joking about trying this for the first time using such large quantities of material. This could turn into a (personal) disaster.
 
   
 
   
    foxy2
(Distinctive Doe)
09-24-01 02:37
No 216492
      Re: Obscure Meth Synth...    
   
Blast Shields Up Scotty!!!

Do Your Part To Win The War
 
   
 
   
    seelight
(Stranger)
09-24-01 03:18
No 216502
      Re: Obscure Meth Synth...    
   
Really, for your own sake, don't do this.  You don't have any idea what your working with.
Start small, for the first time to get an understanding of how these chems behave together, and then work up slowly.
Microscale equipment isn't too hard to come by. Try out curbshots nano which doesn't require any hard to get equipment.  Then go from there.

or you will be obscure..




I come in peace
 
   
 
   
    Aquarium
(Stranger)
09-24-01 05:22
No 216516
      Re: Obscure Meth Synth...    
   
No, I am not joking, but thank you.  I do have a some idea what I am dealing with and am no complete stranger to this scale.  This is exactly why I posted it first, to get some feedback and opinion and this was exactly what I was afraid of.  That is why I have so many questions.

I am not a complete stranger to chemical reactions, it's just this one and from what I read, this 'slow reflux' is not as unpredictable and violent as the p/p and that is why I wanted to do this one instead.  I am just looking for help to answer my questions and then I will make the decision on whether or not to try it.  I will be very careful.  Maybe I will start at a smaller scale.  After all, the largest scale I ever worked at in university was like 500ml flasks.  But I did use this large scale equip in various different mdma/mda synths over the years, hypothetcially, that issmile

Actually, I do have one piece of smaller equipment so maybe I can scale it down a little.  I have a rotary evaporator that can hold up to a 5L flask and it also has an oil bath that can reach high temperatures and the condenser can be setup for reflux.  This way I can cut the scale down quite a bit.  Now the more I think about it, I think I have a small hot plate and can use a small oil bath and flask, and somehow rig up the big-assed condenser, but the questions remain the same!

Anyways, THANKS!  And as I said, same questions though, ignore scale and I hope I get more opinions and advice.laugh
 
   
 
   
    Jacked
(Ancient Alchemist Delux)
09-24-01 07:25
No 216545
      Re: Obscure Meth Synth...    
   
Shit that is small scale, I think you will have better results with the larger reactions myself, but what do I know, Swim on the other hand says by all means go for the gusto.
Referring to:

Question 1.  Do I add these in any particular order or rate?


Yes Swim would get the reaction underway and add the ephedrine in last and slowly, Thats with this big of run. 

Referring to:

Question 2.  I have read that some use a tube attached to a vacuum adapter on the very top of the condenser where the tube then goes to an inverted funnel submerged in a bucket of water and this is supposed to get rid of the noxious fumes and smell.  I have also read just to exaust it outdoors with or without and activated carbon filter placed inline.  At this scale, I am not sure which would be most practical.  Either way, ventilation will be very good.  Which method should I use?


Well that would depend on your location and if it can handle an oder unnoticed. The best thing is the less thing, If you have good venting, use it. The condenser should not be blowing shit out of her as if it was a push pull set up so just keep cold H20 going through her with a gentle reflux and an exaust system running.

Referring to:

Question 3.  Do I have to baby-sit the reaction for the entire 25h time or once it reaches the slow reflux, can it be left alone for the remaining duration?


You should know the answer to that if you are familure with chemical reactions. Can you keep your heat regulated over long periods of time to maintain the reflux safely?? I could not answer that one for you. Swim don't watch nothing that fucking long.

Referring to:

Question 4.  Am I to expect dirty colors, gasses, fumes, bubbles, violence or inconsistency in the reaction?


Only if the start is hot, This is not a violent reaction the reflux, 57% HI and P in the amounts of H20 will not get out of hand. The molarity of the HI will drop though as the rxn moves on, I would try and start with a higher % than 57 it will cut your time down but the start will be critical and could get out of hand... That's Swims foreplay. He's got to have it on the edge before he can fuck anymore.. poor bastard..

Referring to:

Question 5.  I’ve never used distilled water before.  In this case, does the water have to be distilled water or can I use plain tap water for all steps that require water?


Ok now I seem to be wasting my time. With that kind of start your talking about why the hell wouln't you spend 3 fucking dollars on distiled water. Of course you can use tap water. You can use ditch water, torlet water, you name it. But why? The cheapest thing on your list would be distiled water. I have ran out of time, I will evaluate this again tomarow and will complete my answers to your questions based on the responce I recieve on what I have already layed out for you. No disrespect intended I'm just tired and need some rest.. Later




The end result is directly connected to the effort applied
 
   
 
   
    Aquarium
(Stranger)
09-24-01 08:12
No 216556
      Re: Obscure Meth Synth...    
   
Thanks Jacked.  You've given me motive to stick to the scale as written (kinda...but still scared now).

About the distilled water, I knew that was a stupid question frown.  I've always used tap water and it wasn't about the cost of the distilled water.  I've just never noticed a difference in yield when substituting tap water when preforming other reactions.  I wanted to know whether this specific reaction would be extra sensitive to tap water, like it is to light.  I realize tap water can contain Cl and a bunch of other crap so if I am not sure, I would have always gone with the distilled water in a new reaction and will do so now. 

I do not understand how I can start with a higher conc. of HI than 55-57%.  From what I read, the max. conc. is about 57%.  I would guess to acqure and add I2 crystals.

When I am more familiar with the reaction, then I can judge on how long I can leave it alone for so that I don't have to watch it for the full 25h.  I think I should be able to maintain the heat safely.  I have a heat controller for the heating mantle, so I'll take the heat up to a very gentle reflux and monitor it very frequently for hours and hours and if it seems like I do not have to change the heat setting anymore and it is at a gentle reflux where the condensation ring is about 1/3 the way up the condenser, I will check it less frequently for the remainder of the 25h.

To get the reaction underway before the slow addition of the ephedrine, would you recommend bringing it all up slowly to the slow reflux first, then slow addition of the ephedrine thru the top of the condenser?

I look forward to further help!  Thanks!  smile 
 
   
 
   
    Grouch
(Hive Bee)
09-24-01 11:53
No 216613
      Re: Obscure Meth Synth...    
   
You might want to look at this:

http://www.rhodium.ws/chemistry/meth-pd-h2.txt

and this, choose the SS one and teflon coat it:

 
   
 
   
    epistemologicide
(Hive Bee)
09-24-01 12:41
No 216624
      Re: Obscure Meth Synth...    
   
are you fucking nuts!!!

seriously, wait untill some how your rxn fucks up, it can happen to cocky people and those that think they know every thing about a synth they are attempting for the FIRST TIME

do an ounce and get the procedure down pat,

fuck, thats just insane.shocked

hatred of ontological wastes, and the marathon!!!!
 
   
 
   
    foxy2
(Distinctive Doe)
09-24-01 12:54
No 216632
      Re: Obscure Meth Synth...    
   
Ahh
Thought you were talking RP/I at first.  I would hate to watch someone try to do an RP/I at this scale when they don't know what order to add the reagents.  That could be very ugly. blush

In this theoretical scenario I don't think you need to worry excessively about HI decomposition.  As long as the flask was not in the direct sun it should be fine.  And it would only decompose to H2 and I2, the I2 would get recycled by the RP so its insignificant.

I think this reaction starts out vigorously and then gradually declines with time.  So a good mantel set at a low reflux should not require babysitting.  Probabbly best to be fairly close for at least an hour. 
And I would have a big bucket of bakeing soda(neutralize HI if it breaks), a bucket of water (fire and HI) , a fire extinguisher (fire).  A proper lab set-up will minimize these events.  No duct tape in this one hehehehe.

For the RP cleaning I think a dilute HCl wash, followed by water rinse and an acetone rinse should be fine.

Referring to:

In the Merck, it says that 1.5% H3PO2 (hypophosporus acid) can be added to prevent discoloration and regenerate the HI.  I am guessing that this is useless for me and would add the burden of acquiring it.



The RP serves the exact same function as the hypo.  Have you no interest in what happens in that flask???  After all what funn is theoretical chemistry when you don't know what reaction id happening.

tongue






Do Your Part To Win The War
 
   
 
   
    Jacked
(Ancient Alchemist Delux)
09-24-01 13:16
No 216639
      Re: Obscure Meth Synth...    
   
You can get away with tap water no problem but the idea not the fact that you can use it, It's the fact that short cutting leads to other areas that cannot handle shortcutting and you get yourself into trouble. Use the best you can in any instance, this guaranties troubleshooting will be greatly reduced and success will be one more step closer before you even start... Now ware were we, Oh a solution of HI can only saturate to 57% the rest gasses off, It's like opening that bottle of reagent grad HCl that plumes a gas cloud ever time,,,
Anyhow higher concentrations is how the push pull reaction goes down in an hour and a half instead of the 25 to 35 hours you have in mind.....
Referring to:

Question 6.  I would like to re-use the red phosphorus if possible.  I have read that people just rinse this with water (distilled?) and sometimes with acetone the grinded with a mortar and pestle.  How do I thoroughly clean this and how many times can I re-use this?


Yes you will be able to recover the majority of the red P, you can look to the search eng. under MBRP and read how the dirty fucked up shit is cleaned, The lab grade should be cleaned similar but not as extensive. You can reuse as many times as it prefires hot... This also you can look up for reference to preparing the P for further rxn's.

Referring to:

Question 7.  At this scale, there will already be a significant volume of liquid for one person to manipulate all at once.  To reduce this volume can I use concentrated or pure NaOH instead?


You can use it strait up, Swim recommends a 50% maximum because of the ionic changes taken place in the solution first rather than the rxn flask. And this is how Swim learned.

Referring to:

Question 8.  I have read that some use Et2O and some use toluene but never read anything about DCM or pet ether.  I would prefer something that I would not have to evaporate so I can proceed directly to crystallization.  What other solvents can I use for this?


Look use toluene unless you are going to kerplunk this mess, I just posted a thread about naptha under the question about hypo thread above this one go there and read it. As far as other's Yes they will suffice. Why not go with the normal here, Toluene or xline is the two recommended at the hive for this kind of rxn....

Referring to:

Question 8.  I have read that some use Et2O and some use toluene but never read anything about DCM or pet ether.  I would prefer something that I would not have to evaporate so I can proceed directly to crystallization.  What other solvents can I use for this?


You will not be able to evap the non-polar solvent and get a xtal. The meth freebase is not a solid and will remain an oil until the HCl is produced.. Either by gassing or by addition of HCl to the non-polar with a substanchel amount of polar below it for the salt to fall too..

Referring to:

Question 9.  Wizard X says to use sodium carbonate and I've read that others use magnesium sulfate and I also read to be careful of freebase absorption and to rinse the drying agent afterwards which is standard procedure.  What are the best drying agents to use for this step?



Exactly what wizard X says, he will not steer you in the wrong direction.

Referring to:

Question 10.  Can I expect a minimum molar yield of 80% (~1186g)?



If everything goes right yes.


Referring to:

Some discussion and concerns (probably more to come after trial synth):
In the Merck, it says that 1.5% H3PO2 (hypophosporus acid) can be added to prevent discoloration and regenerate the HI.  I am guessing that this is useless for me and would add the burden of acquiring it.  The 12L flask is single necked and I have no way of monitoring the temperature of the reflux but am familiar with slow addition of heat to bring it all up to a gentle reflux which I suspect will be approximately 125 deg C.


This is only for storage not important in this case...
and a gentle reflux is the target temp. if it does not reflux at 125 arnt you going to go a little higher, or vice versa? Gentle reflux until separation

Referring to:

Wizard X says to add crystals of sodium thiosulphate to remove the free iodine.


I'm here to tell you a rxn that big if you add thiosulphate in the acidic conditions of the rxn before basifying you will create a poison gas that could be dangers to your health, It can be added in the basifying procedure if you will but do it at a higher pH than from jump street...

Referring to:

the Merck says this is soluble in water so I assume this is just an ‘indicator' that will form NaI or something like that, but might be wrongfully dismissing the usefulness of this step.  I am also skipping the distillation of the freebase because I am assuming that it will be very clean and the method of crystallization I am using is not just adding aqueous HCl and evaporating the whole mess.


Well I beg to differ, the bees steaming over the goods do it because it affords a very clean product. They are doing the same rxn as you and are very good at it I might add. Don't you think this is for a reason, If you are going to produce a cleaner product not ever doing this before my hat's off to you. Your a better man than I...Now back to reality, The thiosulphate will help get that white crystal right of the bat but you will need to further purify the product by cold acetone washes and recrystalision by duel solvent.

Referring to:

I also read that it will be hard to separate the iodo-ephedrine and feel no need to try to do this or try to convert this further.


And why the hell not... The thio will help you here, Acetone washes will also clean this up a bit.. Stick with purity, It's worth twice the duckies and is worth it in the long run, even if you plan on having the largest personal stash in the history of the large cook.
Oh yes hell yeah wash the pre base rxn with toluene first, this is no bullshit. It helps twice as much as the trouble it is. no sense not doing it..

Damn this is a rarity I answer or attempt to answer that many questions in a row, That is a heel of a thing you ask of a fellow bee, Next time isolate them to a few per post, They will get many more responses than just one board bee that happened along and was in a half ass mood anyway... Tighten the fuck up,
Jacked









The end result is directly connected to the effort applied
 
   
 
   
    Aquarium
(Stranger)
09-24-01 14:57
No 216663
      Re: Obscure Meth Synth...    
   
Grouch:  That looks very interesting, but yes, I will look into that too.  I'm just trying to work with the equipment I have on hand.

And NO, I am not cocky, nor am I a stranger to handling large amounts of nasty shit.  That is why I am asking for help here and I found a 6L flask with the same ball joint size as my 12 so I'm cutting everything in half and I can still fit the 6L RB in the 12L soft mantle because it is soft and will wrap around.

foxy2:  Yes, I am very interested in the theory and am looking into it.  I was just lazy at the time after all this school BSwink  This was just stage one and THANKS for the help.  It is much appreciated!  I kinda know the answers to a lot of the questions too, but just double checkin and looking for more details from the people here who are obvoiusly much more familiar than I.

I guess the order, I'll add the aq. HI first, start the stirring cold, add the RP slow and slowly take it up to reflux over time, then add the ephedrine slow.  My 'room' is well equipped with safety things.  Too many to discuss.

Jacked:  Yes, I'll start with the slow reflux first and maybe in the future I'll try and look for ways to cut down the number of hours.  Toluene is fine.  They sell it OTC where I am.  I just was looking for the best and I guess that is it.  I know the freebase is not a solid.  The way I would crystallize it is by adding pre-gassed conc. HCl in IPA to the dried toluene/freebase, a calculated overshoot to acidic pH, then either filter or evaporate some or chill.

Yes, I will bring it up to the right reflux without even noting the temperature.

I don't think I am interested in the thiosulphate because of the gas and scale and I don't have it anyways.  I was not critical about the distillation of the freebase; I just think my method of crystallization would be better and cleaner than adding conc. aq. HCl then evaporating the mess.  It's more work, but I do know of course that distillation of the freebase would be a cleaner product and if I did this, I would still stick to the pre-gassed IPA.

I thought that the 'pre-base' mess should be washed first before extraction.  I just don't understand why it Wiz X didn't include it in the details.  That was wierd.  I considered that crucial. 

But anyways, I am going to look into this further, and take ALL your advice and even look into the theory.  I've decided to cut the scale in exactly half and begin after I look into the theory so hopefully within a month or so.  I thank you all and appreciate the information and help very very much and will definitely keep everyone posted if they are interested.  I did notice that there is MUCH detail on the P/P, but not a huge amount on the slow reflux.  I'm in no rush.  I understand that was a lot to ask, but I did put effort into it as best I could first to minimize the 'dumb' questions and much of it is just my need for support and confirmation.  I can't believe the amount of help I got in less than 24h.  You guys are fuckin awesome!!

MUCH THANKS!  smilesmilesmilesmilesmile

I'll keep an eye on this thread..  Thanks again!






 
   
 
   
    StickIt2TheMan
(Newbee)
09-24-01 15:16
No 216666
      Re: Obscure Meth Synth...    
   
Here goes.... Rhodium will you comment if in error please...?

Question 1. Yes... Mix the Eph and the Rp together first in the flask and place into an ice bath. Cooling this mix helps the reaction begin at a slow and controlled rate once the HI is added.


Question 2. Use the condenser with the tubing which forks into 2 hoses vented to a succession of 6 organic vapor cartridges which are constructed 3 each into a pvc "cross")(OVC - like on army surplus gas masks)

Question 3. Never leave it unattended!!!

Question 4. Expect dirty colors, gasses, fumes, bubbles, violence and inconsistency in the reaction and know what to do for each event.

Question 5. Use only DH2O.... other waters contain minerals, metals, and organics which are no good for good product!

Question 6. Clean and re-use indefinitely the Rp just as you stated.

Question 7. Yes... but add the NAOH slowly in small amounts and allow to react completely between additions.

Question 8. This solvent will not be used for an evaporation step... rather it is used as a stable transport for the M freebase until the hydrochloric salt is formed... which is then dropped into DH2O or gassed for immediate crystallisation.

Question 9. Magnesium Sulphate Heptahydrate (Epsom's Salt) is easily acquired and should be "fired" at 500 degrees for 3 hours- this is done prior to use.

Question 10. No... you will be way lucky to get anywhere near that yield... especially for your initial attempts.

Yes... Do add the thiosulphite and filter... this removes the extra iodine left overs.

Yes... Do a n/p wash of the reaction mix prior to NAOH addition. Toulene is great. Other non-polar solvents are acceptable.

Yes... Do a molecule repair and cleaning with the addition of Naptha and Ph'ing to 10 with NAOH and heating until loud "kerplunks" can be heard.

Yes... Do a DH2O wash of the n/p-meth mix after separating from reaction mix.

Whew.... how'd I do, Rhod-I-Ummmmm?


cool

Paint a pretty picture.... hang it on the wall.
 
   
 
   
    Prdy2GO
(Newbee)
09-24-01 17:53
No 216685
      Re: Obscure Meth Synth...    
   
dont use tap water unless you want to leave nasty stains on the foil.
And xothermic mother fucker. Add naoh slowly
SLOWLY!!! you dont want to get a runnaway or worse lie lock would be a real bitch, but then you wont have to use the septorary... he he hee
...
..
.


Hum did you get that?
 
   
 
   
    Grouch
(Hive Bee)
09-25-01 02:21
No 216837
      Re: Obscure Meth Synth...    
   
No offense to anyone, but read carefully before answering this guy's questions.  They have already been answered.  He's talking about the slow reflux. 

As for the reflux, at that temperature and that gentle of a reflux, you might not need such a fancy condenser.  Maybe an air cooled home made one would do.
 
   
 
   
    BenWiFFen
(Line Monitor)
09-25-01 03:47
No 216879
      Re: Obscure Meth Synth...    
   
Along time back we would take a vinegar bottel or one that would fit in the flask and tape the two together and reflux for 12 hrs. We were young and dumb but it worked. We didn't want a 100% seal just tape worked fine.It Never dryed up on us.
 
   

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