We need a new nano synth!

[kris_1108]

Hi
I think The Hive needs a good LWR nano synth for newbees. I have seen candles at a local supermarket that will burn for 40hrs (well it sais they do, anyway.) I was thinking you could have the glass piece from your thermometer (just mark it with a nikko pen where the 100'c is..), inside a test tube, with a baloon on the test tube. You would have to be able to easily adjust the height between your candle & test tube for temp control. And maybe use a 'mini oil bath' for the test tube, to keep temps more consistent, or a sand bath, or no bath at all!

This may work, assuming that the size of your candle flame wouldnt vary too much over the 24hr period. As for the post rxn, maybe use a simplified steam distillation, with a long glass tube as a distillation condenser (wrap it with a layer of damp cloth and keep the fan on it to cool?), and some sort of 'elbow' or flexible tube to adapt the test tube to the condenser.

This could possibly be an easy way to reduce ~2gms of pseudo, with maybe 50% yield?

Is the 24hr candle idea rediculous? Would an A/B be easier than the steam distillation?
What does everyone else think? Has anyone got some of their own thoughts on a nano synth?

[geezmeister]

Take a shot at it. Try your ideas out, work out the bugs, report what happens, good or bad. Do that post that becomes the new nano method.

I dare you.  

[SHORTY]

Is it absolutely necessary to have candles and custom testtubes etc.?

I mean an electric hotplate, real flask, real condenser or ghetto one will do fine (as will a balloon for a small cook)can be obtained quite easily and inexpensively.

How can you have 2 synths for the same reaction using the same precursors anyway?

Why complicate the process of adding 3 chemicals and some water to a flask and placing on a hotplate set at 100C for at least 36hours.

Actually, i think that all these newbees want a writeup that can bee done in a few hours.  Unfortunately that is not possible with rp/i rxns.  No matter how you do it and no matter what kind of equipment you have, the time is gonna remain the same for high quality, good as it gets meth.

Unless, of course, you can get hold of some hypo.  Then you can make the same high quality in as little as 1 hour! 

So instead of trying to think of a new curbshot writeup, why not research and develop a process for making hypo?
For example, your own urine is a source as well as animal bones.  Although i personally wouldn't take part in the urine experimenting.  There are many other possible sources for making hypo. You just gotta find um!

[navarone]

well a nice long pyrex testube will work perfectly.
extracting rp from SWIDK (source which i dont know) its easy with some nice solvent and some coffe filters.
for many...iodine is a tricky thing to find. but google is ur friend in that....trust me.
a 24 hour candle is not needed...since the proportions of the e i2 rp are way smaller...the reaction should be much quicker..about 6 hours.
a tricky thing is the condenser.
the temp for a nice reaction is about 100c.
it wont take long until the whole testube will reach 100c so the baloon might melt.
but i came out with another way of making a ghetto nano condenser.
for this kind of synth u need the following things
1 long big pyrex testube
2 thin medium testube
2 clamps or something that would do the same.
dry ice
6 hour candle.
(the big and the small testube should have a close size diameter)

a thermometer is not necessarely needed
just test the apparatus with only water and see at what distance from the candle the water starts boiling.
the stand can be anything of course...i use one of those floor long lamp bars
a heat resistant clamp is easy to construct
now the big testube is placed and the E 12 rp was putted in.
the little testube was filled with big chunks of dry ice(big chunks takes longer to melt)
20 or more ml of water were poured inside the big testube.
the little thin testube with ice was placed inside the big testube exactly in the middle..like shown in the pic
the candle was lit and  slowly the reaction starts.
keep another little testube with ice in the freezer.
lit the candle and the bubbling will start
the dry ice will last for about 2 hours. when u see that the ice inside is all back to liquid again, quickly change it with the one in the freezer.
the removed testube was emptied and filled with dry ice and left in the freezer again.

remember to keep eye on the reaction...dont just go out or start watching tv or the ice will melt and the hi will escape.
just change the testube everytime u sees the ice has melted.
if u wanna keep the reaction going for more than 6 hours....buy some more candles.

there u go....u got a ghetto mini condenser.

i never tried this before since im having problems extracting iodine but im pretty sure it will work..if u do it carefully of course.
ill let u bees try it out and tell me if it works propely..ok??

hope this came in handy
sorry for my bad english

c ya guys

navarone

[ChemoSabe]

Like my recent post concerning curb's nano implied, as long as you are not a resident of the US or Autralia Curbs nano might still be a valid intro to the process.

Intro. Intro. Intro. Should I say it again?

But don't waste your time on it if you are from the US or OZ and your precursor source is that of OTC decongestant and bronchodilator products.

should I say that once or twice more?


Shorty's 10g LWR is the one to look at. It's definitely a nano recipe. Since it's even a challenge for veteran bees to now push it beyond yeilding more than 5gs of end product plus the fact that newbies will realistically initially net about half of that figure,.... would any of you argue against the fact that ending up with 2.5gs would qualify as a nano amount?

That final amount just barely gets you enough to make recrystallization a practical endeavor.

And now with the arrival of the newest acrylic supergakks you'll be damned lucky to even end up with that.

I'm not trying to be a partypooping bubble buster here, just being realistic.

You aren't being fed bullshit about this.

For those of you who haven't yet finely polished your search engine skills I'll spoonfeed you a clue to the location of Shortys recipe. It's just a few posts away from this one.

Post 482573

(ChemoSabe: "Hit Single Version", Stimulants)

A further clue for those who somehow still couldn't find it with that first one.....  "this should work...".

Anyone who's still lost after that clue should just quit right now. You'll never succeed with all the real world hurdles you'll need to clear concerning all this.

PS - Someone please shoot me if I now start turning into Osmium as upon proofreading this I think I'm definitely showing symptoms.

[wareami]

The only typo I can find is in the diagram itself where it states to use 20ml dh2o for 2g of E. That's excessive.
Even though the rxn may complete in 6 hours, Ibee finds that longer cooking periods in the range of 36-48 are more benefitial in many ways...

But Nice Write-UP!
In return....here is a sure fire I2 Extraction method that Ibee uses and it works like a charm everytime.
He calls it

Ibee will use the 1 ounce 2% I2 tincture bottles for example. Scale UP as necessary.
If using 7% I2 tincture, increase amounts of ingredients used...
For example:
Every 1oz 2%tinc requires ¼ oz bleach
Every 1oz 7% tinc requires ¾ oz bleach

Materials Needed for 5 ounces of 2% tinc
•Quart size plastic jug with tight sealing cap(squeezable)
•Half Gallon size jug
•Panty Hose {with or without ho's}(Take the Ho's out first )
•Rubberband
•Funnel
•Coffee filters and/or paper towels

Ingredients needed
•5-1oz bottles 2% tinc
•1¼ oz household bleach
•1ml Concentrated sulfuric acid(h2so4)
•dh2o

1.Empty all 5 tincs into quart jug
2.Add bleach, cap and shake.
3.Uncap and add h2so4, cap and shake
4.Uncap and fill with dh2o, cap and shake.
5.Let set for 2 minutes then uncap.
6.Fold PantyHose so that six layers will cover the jug opening then fold down and afix securely with rubberband over the top.
7.Position funnel inside half gallon jug.
8.Turn Quartsize jug upside down and Decant liquid into funnel by gently squeezing the sides until all liquid is gone.
9.Undo Rubberband and Open top and flood with more water to about half quart line to wash I2 xtals.
10.Repeat step 6,7,8
11.With jug still upside down undo rubberband and pull away P-hose. The xtal ball should be either on the P-hose or stuck in the neck of the jug.
12.Transfer the xtalball onto 6 stacked coffee filters or papertowels and fold sides over onto top of xtalball and squeeze out excess moisture.
Open paper then transfer I2 xtalball onto new paper and wrap ball UP and stand on the wrapped ball to squeeze all excess moisture out!
There ya have it!

[wareami]

Allow me Chemo...
>would any of you argue against the fact that ending up with 2.5gs would qualify as a nano amount?
By loose definition, anything under 10g is nano

I tend to agree with Chemo about his concerns and the reasoning behind his philosophy on this.
The size of the LWR rxn is only limited/governed by ratio and flasksize.
Everything else should run identical.
Those looking for a nano write-up need only follow the guidelines as they were presented here time and again.
To reproduce a Curbshot style write-up will result in thesame problems those faced with applying those instructions right out of the box.
Many have tried the curbshot only to come UP empty handedon the first try and needed to incorporate other variables ripped from other write-UPs before they could make the rxn work.
On the Other Hand....those that followed Jacked's, Worlock's, or placebo's write-ups succeeded fine but those were just a tad more sophisticated to newbees.
All bees want a straightforward way that is fail proof.
That is asking alot.
Ibee was going to translate a new LWR write-up for me to post but it seems that the time would be better spent n unraveling the mystery's of the newest gaaks!
Without runnable feedstock, bees don't stand a chance even if they had a bee do a housecall and show them firsthand how to do it! So the answer isn't in a write-UP at this stage but one will come from Ibee's corner when other areas are addressed first!

"Burnt Leftovers...." Shhheeeeeeeeeesh!!!
Ibee's Humbled Chemo...

[SHORTY]

Post 482658

(SHORTY: "This should work...", Stimulants)

[moo]

Dry ice in the test tube acting as a condenser? Why? The area of contact between the dry ice and the test tube will be minimal, and the cold carbon dioxide escaping the "condenser"  won't do you much good either.

You are way better off with plain old ice water because the water cooled by the ice has maximal contact with the test tube and furthermore the ice has larger heat capacity (read: cooling capacity) than dry ice. It is simple as that.

[kris_1108]

SHORTY
No, the candles etc are not necessary. I agree, If you've got the equipment, why would you try to do it with a test tube etc?

Yes, an electric hotplate, flask & condenser can bee obtained easily and inexpensively, but doesn't that take out all the fun of doing a nano?! Ive done a few nanos, yielded a tiny 20% but I loved them! I made my own speed!

I just thought it might be 'cool' to be able to make a little bit of speed with a small, ghetto setup, minus the flasks and condensers and the hotplate.

>>Why complicate the process of adding 3 chemicals and some water to a flask and placing on a hotplate set at 100C for at least 36hours.

Doing it in a test tube with a baloon and a candle is complicating it? I disagree. You are right, it is off the beaten trail, however I do not think that is much more if any more complicated.

I do see what you and Chemo are saying. It just seems that plenty of bees are trying curbs nano, and having trouble. If it could be 'updated' then they will have more success.

I dont know what it is, but there's something thats a bit exciting about doing a nano. Maybee I'm just wierd, though   . Any way Ill have a think, and Im keen to have have a go.

[ChemoSabe]

The mian reason I personally would recommend lab glassware is that it's designed to safely handle the heat stresses necessary in chemically oriented labwork. Meaning quick fluctuations in temperature that would easily and sometimes explosively shatter or badly crack other articles of glass.

The open flamed candle issue, while it surely can be safely done in the duration of an hour (24 or 48 gets rather "iffy"), is something most would be better avoiding. It can never escape being some sort of realistically potential fire hazard plus the sheer overall usefulness of a decent hotplate should outweigh all considerations of using a candle as a heatsource.

But for those of you truly living like cavemen it might be your only option. how's that candle powered computer working out for you cavebees out there anyways?  

There are some who are still going to cause dangerous events to occur even if they've got lab grade everything so acquiring good lab glass and other lab apparati by no means completely assures your safety in the lab. But they certainly beat out nearly any ghetto setup in terms of general overall safety. 

I'd also never claim that acquiring good lab glass would always be the safest thing to be doing either. It can be and  often is a quite suspicious thing to do. But it's certainly not an impossible or necessarliy expensive or absolutely in all circumstances a suspicious thing to do.

And if you can manage to get it it's definitely to your advantage for both safety and success in chemistry oriented endeavors.

And having and using it does not take anything away from that "I did it myself" feeling that going ghetto also gives you. It does increase the odds of you having that feeling more frequently and to a higher degree than before.

If you ever find yourself in the emergency room prior to admission to an ICU with 3rd degree burns while a fire cheif & crew, a hazmat team and a narcotics investigator are simultaneously at the scene of the scorched and smoldering remains of your little ghetto lab you might have wished you'd had a safer setup.

There are still many arguments that staunch ghetto enthusiasts would have on this topic to make their points in favor of "going ghetto" too but obviously I'm not one of them.

[SHORTY]

Although i do consider finding a safe way to hold a testtube over a candle for 24 hours more difficult to achieve than putting a flask on a hotplate.  You couldn't leave it unattended because the candle or testube would have to bee adjusted as the candle burned down.  Ventilation would have to be configured so that it wouldn't disturb the flame etc... 

However, my motivation for making meth is not because its fun.  But if that is your goal and it makes you happy then by all means have at it.

[kris_1108]

Hi
Swik has been working on a LWR nano synth, atleast for himself.
The test tube would be held with one of those big steel paper clamp/clip devices, which is screwed to a simple stand. A glass thermometer rod would be in the vessel, which has a fluoro-tube condenser atop. This assembly was tested with water; the point of condensation was about 150mm up the 5/8 x 12" tube. The plan is to steam distill the goods out. Swik can use the existing vessel & condenser, the next problem is...


...how to attach the top of the vessel to the condenser?
Swik was thinking about using some flexible transparent tubing with a 3mm (~1/8) inner diameter.

Has anyone had much experience with steam & flexible tubing? Is there any reasong why it would not carry the steam over into the condenser?

and SHORTY - Could you please guide me with getting the white coat off the inside of a fluoro tube? thanks.

EDIT: woops i just found a post that sais you use sponge/coathanger wire/dishsoap. cool, thanks.

As for the time, well, we all know that it is best to go for 24/36/48hrs. However if one was to reduce 10mg of pseudo, surely it would not take 24hrs..(?). Does that mean with such small amount (2gms) Swik could reflux for less time? Or would 24hrs still be far better than (say) 12hrs on a 2gm reduction?

[SHORTY]

I use plastic tubing for connecting my external steam source as well as the boiling flask to the condenser.  It works fine fomr me .

As far as the rxn being faster for smaller amounts i would say it will bee the same time whether its 10g or 100g as long as the ratios are scaled up and the correct flask size is used.  Look at it this way, if it takes 10 minutes to boil an egg then does it take 20 to boil 2?. (i beleive it was Rhodium who said this a while back .

[kris_1108]

cool so plastic tubing will work,
thanks Shorty.

I understand the egg thing but I spose I thought I could get away with less time on such a small amt.. I wonder if it is truly the same time to reduce .1gms and 1kg???
It depends on the nature of the reduction; is it mostly mechanical or a percentage?

Lets say, In a 10gm wet rxn, after 2hrs of reflux, only 2gms of the pfed has been fully reduced.
Has it taken 2hrs to reduce 2gms OR has it taken 2hrs to reduce 20%?
If the former is the case, then a 2gm rxn could bee completed in 2hrs..
If the latter is the case, then, only .4gms of the 2gm rxn would be reduced after 2hrs.
Is the reaction ALL percentage? or ALL mechanical? or a mixture of both? (could it bee 70% pecentage and 30% mechanical..)
Shit I hope that made sense  
What do you bees think?

[CharlieBigpotato]

do the math.

factor in the radius.
do the double blind if need bee.

or better yet, beelieve in magic.
at the risk of offending some bees, i'm still inclined to say that i feel sorry for anyone that has to hang in there with a  a 3gm rxn for 48 hours; especially newcomers that will bee stressed out the entire time; and by the end of it, when they really need their smarts,

well, they're so wasted that they do something stupid.

i can't motivate for convincing anyone of anything concerning this subject.

but i feel sorry for any newbee that feels compelled to nurse a 3 gm rxn for 2 days.

everything we know is wrong. almost everything.
i hope we can agree on that.

nothing i have ever done has made any sense, according to the loudest noise du' jour.

bee safe, young fools.
we need you for other tasks than incarceration.

let in light

[Relux]

Kris, I think I understand your questions about the mechanical/percentage of the reaction mechanism, in which case my answer is that it is entirely percentage. If the system is homogenous (heat is the same throughout, consistency is identical throughout, distribution of reagents is consistent) then the reaction will procede the same regardless of how big it is, or small. Think of it in terms of a unit. One unit of reacting substrates will produce some percentage of that unit worth of product. One unit could be 1000kg or .5g, but all will react the same. Reactions rely on contact between reagents, and also upon the kinetics of that contact. If there is a certain amount of some chemical and a certain amount of the other in a solution, one striking the other occurs in the same frequency whether you have 1ml or 1L.
  Also think about the fact that the rate of product formation decreases more or less exponentially. 1gm of substrate producing .2g of product in two hours would leave .8g of product which in another two hours would produce .16g of product and leave behind .64g. This is of course a slight bit oversimplefied due to neglected equilibria and recycled reactants, but more or less still holds true. (by the way, I have no idea if 20% reacts in 2 hours, but I think you meant that as an example anyway)

[kris_1108]

hi relux
thanks for your reply, and the explanation of how the reaction works. I understand what you are saying. Is it true for even the smallest amount? (e.g one molecule of pfed?). What about two molecules? I know that this sounds a bit extreme (only fleas do one molecule cooks   ) but I am just checking that the reaction is infact, entirely a percentage reduction.

I cant get my head around the fact that (e.g) 2 of 10 gms would take 2hrs but 2 of 2gms would take 24+ hrs. Its like you can reduce 2gms of pfed in 2hrs if you add an additional 8gms! (all these figs. purely example!)

Maybe some things just arent meant to bee fully understood (e.g women). hehe
AH no offence anyone  

[kris_1108]

Hi
Swik has been pissing around with steam distilling out of a test tube. He has just been practicing with h20 in the tube.

The plan was to connect the top of the test tube to the fluoro tube condenser via small plastic tubing. The problem is that NO steam enters the condenser via the plastic tube (small, ~3mm Inner.Diameter tube). The tube HAS to bee fairly small cos big tubes dont like making sharp bends. I am guessing that the tube is staying too cold and the steam is condensing before it gets to exit.

Any suggestions as to what to try next?

Thanks

[Rhodium]

I cant get my head around the fact that (e.g) 2 of 10 gms would take 2hrs but 2 of 2gms would take 24+ hrs. Its like you can reduce 2gms of pfed in 2hrs if you add an additional 8gms!

It hasn't got to do with the amout of pfed you add, it's about the other reactants.

If you use 2g pfed and add five times the usual amount of HI/RP (what you would normally use for 10g pfed), then you might be able to perform the reaction five times faster (in theory, in practice other factors sets in, as this is a multistep reaction), but usually people don't want to spend more reactants than necessary.

Anyhow, this effect is called the Law of Mass Action, and is explained all over the net:

Simple cartoon:

http://www.yorktech.com/science/analogies/massact.htm

With equations:

http://www.science.uwaterloo.ca/~cchieh/cact/c123/massacti.html

[kris_1108]

Rhodium, thanks for that.
Things are clearer now.
So you can almost entirely reduce pfed in a short time, however this is not practical because massive amounts of RP/I2 would have to be used. I also imagine there are other 'side effects' of using huge excesses if RP/I2.

Maybe my nano rxn could use a slight excess of HI and a reduced rxn time of 12 - 16hrs.

BTW I am still having trouble designing a way to carry the steam over in to the fluoro-tube condenser. Another option would be to use one of those U-shaped fluoro tubes, but cut one end short to make a 'candy cane' type section. The shorter section would be attached to the flask and the steam would flow up, and in to the u-bend, and down the 'vertical' condenser...

Does anyone know how to 'cut' a fluoro tube shorter without shattering it?

[Relux]

I'm assuming by fluoro-tube you are referring to a fluorescent light tube. Cutting thin glass can be extremely difficult to do well, but if it's like the light I'm looking at then the glass is an ok thickness and a few methods might serve you well.
  One old tyme method is to make a scratch on the tube along where you want it to be cut and then take a red hot glass rod and touch it against the scratch. When you do this the scratch will cause a crack which propagates along the direction of the scratch you make, and usually end up extremely accurate if done right (or at least when using borosilicate glass tubes. Your tube I presume is composed of a soda glass, which would probably work the same if not better). If that doesn't sound fun you could always try to tap the glass tube at the crack with some type of small hard object. To scratch the glass you could use a diamond ring, a sharp piece of lava rock, a glass scratcher   ,and probably many other things. Make sure to practice further up on the part you will end up trashing to get your method down.

[elfspice]

fluoro tubes are horrible things (gah) for the same price you can get a 1/2 inch outer diameter 24 inch long borosilicate glass tube or 1 inch diameter soda glass...

about us$15 will get you a glass cutter regardless, the main thing it has to do is score the glass with a continuous scratch along at leas1 1/4 of the diameter (i would say to be safe with such thin glass you want to score the glass all the way around) and then grip one side with one hand and put pressure on the point where the crack has been made. Glass usually just comes clean apart when a continuous scratch has been made through it. This is partly why old flasks become more prone to breaking too btw, little scratches create points at which the glass can easily crack.

A simpler method of making the glass shorter, and cheaper, which an older lady explained to me was put a piece of thread around the diameter of the glass at the point you want it to break, put kerosene on the thread and light it up. The heat gets high really fast and thermally stresses the glass all the way around the glass at the same time and should make an almost perfect break, it might be a little more wonky than if you used a glass tube cutter instead, but serviceable

oh and before you go breaking it trying to put a cork in the end, be VERY VERY careful, those beaded edges they put on things is not just to stop it cutting you, it increases the strength of the neck of the opening. I would think you would be well adviced to get a propane torch or gas stove element and heat the edges of the glass at both ends to fire polish it (fluoro bulb glass should be soda glass as they don't get much about about 50 degrees) if it's borosilicate it will still fire polish but not so easily. Firepolished edges will be a little stronger and less prone to breaking when you put a cork in, but the full thick bead and taper is the only way to make the neck of a piece of glass strong enough to be treated casually when putting a cork in it. so be careful if you intend to put corks into glass tubes.

You could feed steam into it by getting a much wider mouthed container (there's a brand of coffee making flasks and funnels and things and they come with a special cork designed to put a large funnel into it (a percolator funnel), and it is possible to put a roughly 1 inch diameter tube through it, although i found it was better to use a funny piece of hollow rubber i found that has a circular indent that the other rubber mates with, and it all goes into a 20mm outer diameter tube or 12.5 even (the rubber sleeve ring stopper thing is made of silicone and was made from the combo stopper/pump for a kitchen baster thing designed to be a liquid dispenser). In the side of the funnel cork it is easy to drill a small hole through which a steam hose could easily be fed into the flask. A small flask with a one hole cork is a good way to generate steam imho, simpler than messing with a jug or buying a pressure cooker (unless you have some other use for it)

vinyl hosing is great for most things except it softens quite rapidy in contact with boiling aromatic solvents.

hehe, in fact, if you are only doing the old ephedrine reduction thing, forget about using the condenser, just use a long length of vinyl hosing, if it's about 800mm long it should be tall enough to act as an adequate air condenser. The vinyl might stain a yellow colour but hey, who cares, it's like $5 a metre. Seeing the head of steam climbing up inside a vinyl tubing was very exiting for me, watchign the little arrays of droplets forming at the point of condensation...  

If you have a good look, maybe on ebay, or perhaps some other places, you should be able to find a much cheaper non-ground glass jointed condenser (i've seen 200mm liebigs in glass without ST ground glass joints for like us$22)

[kris_1108]

Hi
Relux and Elfspice, thanks for the info guys!
My fluoro tube has one jagged end and one 'tapered in' end so I can modify it now to be much more serviceable.

I 'spose I could use a vinyl tube for my experiment, however I thought I would just use the same tube that will be the condenser aswell.

Also Elfspice thanks for the stuff about steaming. I had a dream that I talked to my old man, and he suggested a small right-angle plastic piece from the hardware store, with an ID of approx 10mm and a ~1.5mm wall thickness. It would bee heated up and bent a bit more to an angle less than 45°.

The synth that I am trying to design is supposed to bee very ghetto, so the methods that you guys have described to me are a great help!

Swik is currently trying all ideas out with just using h20 in the test tube.

The basic plan is to-
Do a ~12-18hr reflux with a slight excess of RP/I2.

Steam distill out the gold.

Remove the bottom water layer with a syringe

Add hcl untill ph7

evap

Shmoke.

----

About the excess ratios - Geezs' ratios are around-about (1 E) (0.75 RP) (1.2 I2) (0.8mL dH2O). Maybe I could use a 20% increase on all reagents EXCEPT the pseudo.
However geez sais here

Post 449625 (missing)

(geezmeister: "reaction parameters", Stimulants) "The amount of water has a direct relationship to yield and to overall purity. I find it much easier to obtain good yields and superb quality if the water is in the range of 0.8- 1.2 per gram of E, given a 1: 1.2 ratio of E to iodine. The amount of water in the reaction seems to have a relationship to the time needed to reflux. At the low range of 0.8:1 water:pseudo completion in 20-24 hours has been the norm..."

So Im a bit confused exactly WHAT to increase to make the rxn happen a little faster...
increase rp AND i2 AND dh20?
OR increase rp AND i2?
OR use LESS dh20?
OR use MORE rp/i2 and LESS dh20?
aaaaaargh!
Geez, pleez help!

[geezmeister]

For a faster reaction you want more HI and/or more heat.
All you really should add with the ratios that you intend to use is a little more I2; go with a ratio more like 1:1.5 rather than 1:1.2. Increase the temp to 110-115C. Expect yield to fall off some with this ratio.

I would leave the water as is if you wanted more HI in the flask. Wareami does his LWR's with a 0.5:1 ratio of pseudo to water but refluxes as long as I do. I would be more inclined to leave the ratio for water at 0.8 ml/gm and increase the iodine a little, which with the excess rP you have will produce more HI, which should be contained in the water you have.

[kris_1108]

Geez thanks for the further info on the rxn parameters.
Cool so all I need is a tad more iodine to speed the rxn up a bit, I am thinking 12-16hrs?
I would like to up the temp a bit, but those cheap thermometers only read to about 100°c and a bit more (in my experience). So I am limited by the range of the thermometers, what about everyone else? Do the cheap glass thermo's in your area go up to about 100-110°c? Or more?
Swik has a candy thermometer but it is bigger than the test tube.

[chemlush]

Ok, been at it for about 1year now. Still no honey, but the journey is teaching me new things every time. Though I am still surprised that I2 has been a dificulty for some. I2 was the easiest so far for me to extract from 7% iodine tincture.

1pt 7% iodine tincture
3pt hydrogen peroxide
1/2 cup HCL

using a gallon milk jug mix iodine with hydrogen peroxide:SHAKE, let sit 30 minutes. the mix in HCL:SHAKE, let sit 30 minutes. the put in dh2o to the top of milk jug:SHAKE. then decant orange dh20 leaving grey shinys in jug. REPEAT dh20 2 times. on last dh20 shake real well and pour into a nylon stocking and rinse well by pouring dh20 onto stocking and twisting stocking well. WEAR GLOVES face covering and goggles!! or feel the burn and wear the stain.

[kris_1108]

Hi
Swik had a quick go of steaming over some water over from a test tube, through a plastic elbow (slightly less than 45° angle), and into a glass tube fluoro condenser.

The steam would NOT come over into the condenser. I think the plastic elbow was staying too cold, and the steam was condensing in there. I dont think the assembly would have got much hotter if I let it run for longer..

I think I could
a) heat the elbow with a hair drier during the distillation process
or
b)use a fish tank pump to assist the steam in coming over

do you bees think a) or b) would bee ok?
Or something different?

[SHORTY]

Although i still don't understand why you are doing this...

I would think if you increased the heat it will eventually come over.

[geezmeister]

Chemlush: You are using way too much acid and way too much peroxide. Your yields will improve significantly if you reduce each. Rather than half a cup of acid, use a fluid ounce (about 25 ml). Rather than three pints of 3% H2O2 use one. You don't really need that much. Stir well, let sit overnight.

You will find you have higher yields of cleaner iodine using these ratios and a little patience. No gummy black iodine leaching into filters or paper, no HCl smell.

[kris_1108]

Shorty,
thanks for your help; I do understand that you dont understand what is the preactical reason for designing a nano LWR synth.
I also agree that the quickest way to meth for a newbee is by following a procedure like the one detailed in "this should work." (If I can get the pfed together I would definitly do a 10gm rxn myself. )
The situation that Im in at the moment doesnt really allow me to put much time in to extractions and reactions etc (Cant wait 'till I move out!).
Designing a practical, easy to follow, ghetto nano meth synthesis is a bit of a challenge for me, and gives me something else to do apart from work and spending time with the gf etc.
I will give up if I come to a dead end or if I get sick of it.
Oh and geez motivated me   ....

-------------

>>Take a shot at it. Try your ideas out, work out the bugs, report what happens, good or bad. Do that post that becomes the new nano method.

I dare you.

----------

Shorty you'll probably bang your head against the wall but...
..I cant increase the heat because the flame is close as possible to the bottom of the test tube!  
aaargh dont ya want to slap me!  
hehe
So I will try the hair drier or the air pump idea.

anyway thanks again for your assistance and patience (aswell as geez and others..)

will keep yous posted

seeya

[biotechdude]

Kris, are u using the candle to distill out from your testtube?  I'll slap u...

It is great thinking using the test tube for the nano and then a small plastic elbow to goto your condenser.  But u really need a bigger heat souce for distillation. 

This is because during the reaction the testtube is heated with a candle is left for 2 days with the only heat loss being slow and from the testtube to the atmosphere. 

However when distilling, the heat u add (from the candle) is carried away from the testtube and into the condenser; where the heat is rapidly lost to the atmosphere.  The candle or and small heat source cant keep up.

Buy a little portble gas camp stove for 30 bucks, or a bigger candle, or a lantern, or some hot oil ontop of the stove.  It'll work a treat...

[SHORTY]

And it wouldn't leave the black residue on the glass like a candle or lighter will.  Forget the blowdryer it won't get hot enough and will probably cause more problems than its worth.

How do you suppose a pump will help?  Are you going to try to use it as a vacuum or to bubble air into the solution?

Also, if you are testing the setup with only water in a new testube you might have problems with superheating cause there are no neucleation points to start the boil.  Try adding some boiling stones or a couple small pieces of glass.  Scratch an old lightbulb or other glass object with some coarse sandpaper and then smash the glass into little pieces and you'll have enough for a lifetime.

[chameyotch]

..at least in this bee's experience.  Never could figure out how to mix the precursors in one.  A hot sauce bottle worked better.

[kris_1108]

maybe I could add the post rxn solution to mums oil burner, and tell her to 'add some of that drain cleaner' and light 'er up. Actually I dont like the idea of waking up to the noise of a vacuum cleaner at 2:00am...

Thanks Bio & Shorty.
I understand now that the candle will not generate enough heat to make the steam come over into the condenser. Well it's more like 1 drop every 5 minutes in my recent experience.

The fish tank air pump idea is to force air into the vessel and thus force the steam outta there. (see

Post 310129 (missing)

(VideoEditor: "Easiest Post Rxn Steam & Clean for RP/I", Stimulants))

The idea of a gas torch is great! Its small and portable and very f*cking hot. That'll be something else to try. Hey before you mentioned the boiling chips, I went and smashed up a wine bottle and got all the match-head sized bits for boiling stones. Musta been reading your mind. They seem to make the boiling way more even and less bumpy/erratic.

Maybe I should just add xylene and gas it! That may bee easier... as long as there is no water or water droplets hanging around after the washes.

And yer all thinking, "hasn't he got something better to do?"...

thanks

bye

[chemlush]

will decrease the ratios to the specified amounts. and let sit overnite. the patience is there. thanks

[kris_1108]

SHORTY you may be able to help me here..

I cleaned out a fluorescent tube with some 'steel wool' attached to a coat hanger. Most of the white stuff came out, but some was left behind. I added the closest solvent within my reach (mineral turpentine) to the steel wool to assist the removal of the remaining white stuff. I then rinsed the tube out with acetone and then ethanol to wash out the oily mineral turps.
The tube looks 'cloudy' now, like the inside of it is dirty.

Did the mineral turps wreck the glass?
How can I fix it up now?
Is it an issue?

The tube was only AU$4.00 so Its no drama.

thanks

EDIT: Oh and BTW the 'Ghetto Small Scale LWR Synth' has taken a violent turn. Someone Who Isn't Kris is looking into using a salt shaker, on an ACTUAL HOTPLATE. His head would not think outside candles and test tubes. The candles flame changes size dramatically over the period of its burn. Poor bees would be left with iodometh or spacedope.

Still having fun..

[SHORTY]

You probably scratched it with the steel wool.  All you need to use is a soft sponge and a little dishwashing liquid.  After it dries then a acetone rinse would bee ok.

[biotechdude]

Swix's advice concerning a nano setup...

A hotplate with a small glass pyrex bowl or saucepan filled with peanut oil.  Your reaction vessel is a condiment (eg Soy sauce) bottle or small robust flower vase of suitable shape and quality.  Balloon atop of the reaction vessell for vapour containment. 

Then submerse the the flask in the right ammount of oil so that it just reaches above the line of the reaction solution.  Predetermine what oil temp 'nucleated' water boils at (say 120`C) and keep your thermometer in the same position etc... and guess what; maintain the oil at that temp for the duration of a LWR and it'll be at the optimum LWR reaction temp (100`C)!  Then after the reaction is done, perform your washes inside the cooled reaction vessel; and carefully suck off layers using a syringe (with extender tubing if required).

Then place the clean based reaction vessel back in the oil and crank it up for a steam distillation (or do a NP extraction).  Then use a proper condenser and distill and condense the freebase.  Then proceed to clean (using nano syringe separations) and then hcl it.      

Notes -

* Swix likes the idea of those little soy sauce bottles as they are thick and the neck acts as a condenser (better with the assistance of a fan); so u just attach a decent balloon on top and presto.

* Oil baths are better than flame heating as temperature flucuations are less pronounced.

* Cheap glass' (eg soy sauce bottle) main disadvantage is its low resistance to thermal shock.  That is, when it is rapidly heated or cooled it'll break.  That's why oil baths work better for nanos (then flame or direct hotplate contact) as the heating and cooling happens more gradually; and stress breakages are less likely (but not foolproof).

Hope that helps a little..

[kris_1108]

Thanks for that Bio,
Good to hear from you.
Great, now I won't bee able to take any credit for a nano write up, cos your ideas are great!  


The idea of a pyrex dish w/oil is cool. And the soy sauce bottle. Those hot plates get DAMN hot, swik done a test tube nano in an oil bath on his hotplate and the balloon got hot and melted (cough, cough..). I would like to use a fluoro tube condenser with the balloon attached on the end, to keep it away from the hot plate.

If a condenser is used, then maybe the thermometer could be inside the vessel (only worth it if its easier to have it in there..). BTW, what is 'nucleated' water?


Regarding post rxn, would it be better to -
*do not filter out the RP (avoid mechanical losses(?))
*do not wash with np (avoid risk of leaving some np behind)
*steam distill
*ph & evap for meth
*boil the meth 2x in xylene + 2-3x acetone rinse
(this is an attempt at minimising mechanical losses and the chance that there will be some np left in the vessel after the washes. The rp was not fltered out and the np washes left till the end)

OR would it be better to do it the normal way?

Would there really be much mechanical loss in the filtering of the RP?
If there is a little bit of np left behind after the washes (like 3 drops stuck to the wall of the vessel), does that even matter at all, before the steam distillation?

[livid]

to clean. no scrubing necessary. just rinse with pool acid.

[biotechdude]

Yeah haha, Bio is gettin his groove back after a little altercation between his face and the footpath  

Great, now I won't bee able to take any credit for a nano write up, cos your ideas are great!

Nah dude!, u ask the questions and set the threads direction, Swix is the dimwitted fool that answers...

From SHORTY
<<Also, if you are testing the setup with only water in a new testube you might have problems with superheating cause there are no neucleation points to start the boil.  Try adding some boiling stones or a couple small pieces of glass.  Scratch an old lightbulb or other glass object with some coarse sandpaper and then smash the glass into little pieces and you'll have enough for a lifetime.

Swix just meant as SHORTY suggested and dont try and heat up plain water...add a little glass or the like so it actually boils and you can caliberate properly...

Re condenser, if u can get the famed SHORTY flouro tube condenser to work well then that is obviously the better option.  Swix's only worry is the ability to seal (and re-seal) when water needs to be topped up; esp in a nano setup.  But if it all works well then go for it.  If the balloon gets hot in a soy bottle or the like, use a fan to cool the top, or use some fibreglass insulation tape where the balloon is connected, or get a bottle or vase with a longer neck.

Re thermometer; Swix has always prefered to put his outside after he has calculated the temp difference between oil and flask.  Not because his equipment cant handle it - as the correct stuff is used - but because it creates another potential 'fuck-up zone' (man, he's scientific..).  But if its looking robust then go for it as well...

Re nano post reaction workup; Swix wouldn't dick around with RP filtering etc, it doesn't hurt nor come over in the distillation.., maybe 1x NP wash before distilling if a good idea.  The main point is that a well executed steam distill (on a high-quality reaction) will do 95% of the 'cleaning' for you..the last 5% 'dick-around' steps are mainly for ensuring cosmetic value. The main step after distilling is the removal of the Na-water layer undernieth the fb as it'll create salty dope.

So Swix would just dilute, NP wash, add NaOH solution to ensure enough water in there to convert to steam and carry all the freebase, yet leave enoungh in there to leave the unwanteds in the reaction vessel in solution.

THEN, once u have the crude meth hcl, rinse with acetone and recrystalise if quantity and quality justifies its effectiveness.  Most often not in nanos..it'd take longer dicking round with it than it would to just get high and have a bad comedown...

[SHORTY]

Works great with a ghetto flouro tube type condenser.  Just rap it around the tube until it fits snuggly in the flask and you'll get an air tight seal everytime.  The tape can bee left on the condenser for the next rxn although you may need to add a little bit to keep it snug.

[kris_1108]

Livid suggested to use HCl to clean out the inside of a fluoroescent tube condesner.
Swik filled a small syringe with HCl and squirted it down an uncleaned fluoro tube, while rolling/tilting it.
The white powdery shit DISSOLVES with the HCl and leaves a nice, clear finish!
Takes minimal time too!
Thanks mate!