Author Topic: We need a new nano synth!  (Read 9873 times)

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kris_1108

  • Guest
I see
« Reply #20 on: March 25, 2004, 11:46:00 PM »
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

  • Guest
cutting glass tubes
« Reply #21 on: March 26, 2004, 03:07:00 AM »
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

  • Guest
glass tube cutter?
« Reply #22 on: March 26, 2004, 03:47:00 AM »
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...  8)

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

  • Guest
thanks
« Reply #23 on: March 26, 2004, 05:35:00 AM »
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

  • Guest
less time, more HI
« Reply #24 on: March 26, 2004, 08:50:00 PM »
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

  • Guest
Rayshi Owes
« Reply #25 on: March 29, 2004, 01:13:00 PM »
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

  • Guest
Simply I2
« Reply #26 on: March 31, 2004, 04:02:00 AM »
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

  • Guest
HELP ME PLEASE with STEAM
« Reply #27 on: March 31, 2004, 04:35:00 AM »
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

  • Guest
Increase the heat
« Reply #28 on: March 31, 2004, 03:45:00 PM »
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

  • Guest
too much!
« Reply #29 on: March 31, 2004, 04:53:00 PM »
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

  • Guest
ghetto
« Reply #30 on: April 01, 2004, 12:05:00 AM »
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!  ;D

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

  • Guest
like a candle in the wind...
« Reply #31 on: April 01, 2004, 03:44:00 AM »
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

  • Guest
A butane torch would work great
« Reply #32 on: April 01, 2004, 09:07:00 AM »
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

  • Guest
testtubes suck..
« Reply #33 on: April 01, 2004, 09:56:00 AM »
..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

  • Guest
candles are (only) good for your oil burner
« Reply #34 on: April 01, 2004, 11:15:00 AM »
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

  • Guest
thank you geezmeister
« Reply #35 on: April 01, 2004, 10:41:00 PM »
will decrease the ratios to the specified amounts. and let sit overnite. the patience is there. thanks

kris_1108

  • Guest
Cloudy Fluoro
« Reply #36 on: April 02, 2004, 11:46:00 PM »
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

  • Guest
Probably Scratch it
« Reply #37 on: April 03, 2004, 12:01:00 PM »
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

  • Guest
nano setup
« Reply #38 on: April 04, 2004, 10:38:00 AM »
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

  • Guest
Thanks Bio!
« Reply #39 on: April 04, 2004, 01:02:00 PM »
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?