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| Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists. |
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# 1

2003-07-18, 02:44
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SWIL has been getting bored of just reading and helping, and since he hasn't done any in quite a while, he decided to scrape up some goods, and get a small Nano going.
The 2 grams of MBRP was mostly pre-used, except for about .5 g that was collected recently from 100 matchbooks. It was subjected to 4-5 ISO soak/rinsings, a paint stripper soak(contents: Methanol, Tolly, Acetone, Xylene), 2 ISO rinsings, 4 dH2O washes, and 2 acetone soak/decantings. The RP was then dried completely and powdered easily by rolling the clumps in SWIL's fingers. It was a light maroon color, and had the particular smell he enjoys.
The I2 was collected from 3 30ml vials of 2%, 47%IPA, also contained sodium iodide and purified water. The 90 ml of Iodine tinc. was mixed with 15-20 ml HCL(31%), 100 ml of dH20, and approximately 70 ml of H2O2. After 20 minutes, the solution had become the color of dark tea. The crystals which had precipitated at the bottom, where small, but needles nonetheless. It resembled silvery/gray/purple cotton candy, quite fluffy. The liquor was decanted, and more water was added. Shaking and dancing commenced. Now, when the I2 crystals settled, the water was the color of light/just right tea. This water was also decanted, not disturbing the I2 crystals. More water was added, and then it was all swirled and poured through a single coffee filter. The crystals underwent further dh2O rinsings, until they bunched together in the center of the filter, and also left minimal yellow tint to the water. The filter was squeezed. Paper towels were bunched around it, and pressing commenced by way of SWIL's foot. The bundle was unwrapped, to find a silvery/gray sparkling mass of crystals, SWIL guessed about 4 grams. Good technique, if the yield was indeed 4. But no scales were used. SWIL has run these type of Nanos before, and he knows what he is looking at.
The Feedstock was cleaned by way of E-gull, and acetone soaks. It was alky extracted, and the crystalized product underwent further Tone soaks. The original feed was known to contain the Orange Gak. The resultant yield was 3 grams. The yield percentage is unknown, as it was unknown how much phed was left in the feedstock.
The RP and E was thrown in the salt shaker. 1 ml of dH2O was added, and then the powdered I2. It did nothing. The ingredients sat upon one another, in layers. Kind of like a sand sculpture you get from a fair, you know the ones that come in a twisted bottle or something.
SWIL grabbed the shaker and added another .5 ml dH2O, expecting this to ignite the fun. Again nothing. He violently shook the shaker until all of the ingredients had properly mixed. He looked at it, and set it down for further inspection.
SSsslsslslslsssss....
Was the sound of it firing off once it was mixed. Large plumes of yellow smoke began to bellow from the flask. SWIL quickly attached his make-shift, ziplock balloon, and secured it with wide tape.
A strong exothermic reaction could be felt through the glass. It was hot, almost as if a lighter was on the other side.
The reduction RXN had begun. The shaker was set on his light bulb. The heat is unknown, but SWIL intends to check it this run.
So far, so good.
SWIL is planning his attack on the A/B carefully. His last batch with this feedstock was Orange Gakked, but still EXTREMELY potent. He intends to sidestep that bastard this time by possibly using a less harsh base than NaOH. He is thinking sodium sulphite, but is having trouble finding that.
Anyways, the reaction is running fine. SWIL plans to run it as long as it takes. Approx, 36 hours at 170-185 F.
Till SWIL can report back,
Lukky D
[This message has been edited by lukkydleprachan (edited 07-23-2003).]
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# 2

2003-07-18, 03:07
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Good post. SwiM says he agrees, although he's only on his 2nd rxn.
The RP was tedious & time-consuming to obtain, although, it was also cheap & easy.
The pfed presented the biggest hassle & SwiM intends to devote more time into getting that shit clean.
The I2 was surprisingly easy, but a bit messy & burnt SwiMs eyes a bit. He ended up with 2.8g from 100ml of 2.5% which he's happy with for now.
The rxn itself seemed to be the easiest part, although SwiM thinks that by the time he'd got to that stage he had a feel for what he was doing.
He says he didn't weigh his first yeild, since he was more interested in whether or not the shit he was about to swallow was gonna kill him- it didn't, the scrapings kept him awake for three days though~
He'll weigh the next one.
EDIT: SwiM thought it was fucking amazing how the I2 cloth managed to magically clean itself.. he thought it was great, haha.
[This message has been edited by Masahed (edited 07-18-2003).]
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# 3

2003-07-18, 03:23
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Monograph Number: 8757
Title: Sodium Sulfite
CAS Registry Number: 7757-83-7
Molecular Formula: Na2O3S
Molecular Weight: 126.04.
Percent Composition: Na 36.48%, O 38.08%, S 25.44%
Line Formula: Na2SO3
Properties: Small crystals or powder. It is fairly stable and does not oxidize as readily as the hydrated sulfite. Sol in 3.2 parts water; sol in glycerol; almost insol in alcohol. pH about 9. Keep well closed. LD50 i.v. in mice: 175 mg/kg, Hoppe, Goble, J. Pharmacol. Exp. Ther. 101, 101 (1951).
Toxicity data: LD50 i.v. in mice: 175 mg/kg, Hoppe, Goble, J. Pharmacol. Exp. Ther. 101, 101 (1951)
Derivative Type: Heptahydrate
Properties: Efflorescent crystals. Unstable, oxidizing in the air to sulfate. Sol in 1.6 parts water, about 30 parts glycerol; sparingly sol in alc. The aq soln is alkaline and dissolves sulfur. pH ~9. Keep well closed in a cool place. Note: The commercial heptahydrate (about 90% pure, the remainder consisting chiefly of the sulfate) has been largely replaced by the commercial anhydr salt (about 96-99% pure) which is more stable.
Use: Chiefly in photographic developers and instead of "hypo" for fixing prints; bleaching wool, straw, silk; generating SO2; as reducer in manuf dyes; silvering glass; removing traces of Cl in bleached textiles and paper; preserving meat, egg yolks, etc.
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# 4

2003-07-18, 03:45
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It was suggested for use by geez, what do you think about Sodium Sulphite as a base, Pikk? It only goes to pH 9? That wouldn't be high enough would it?
Lukky D
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# 5

2003-07-19, 00:26
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nope not high enough . at least i dont see how it would be.
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# 6

2003-07-19, 09:34
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If SWIL is lukky enough to find Sodium Sulphite(Na2So3), then he is planning to try a mixed base. Composed mostly of Sodium Sulphite, but he plans to use the NaOH to make up the extra. He is going to use narrow range pH strips, his keen eye, and patience(of course!) to side-step this orange bottome feeder.
Currently, the reaction is just chillin'. Sizzlin' at 180 F, SWIL guesses. It's a little runny, but the baggy smells just right!
He's run reactions like this before, he knows what to feel, look, and smell for.
Lukky D
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# 7

2003-07-23, 00:15
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From SWIL's observations of the beginning of this reaction, he felt that the quality of the MBRP must have been still quite good. The force that it started with convinces SWIL that his cleaning was quite sufficient.
SWIL admits that the I2 from 2% tincture that was used, was quite damp, and not so clean. Realizing that with such a long, wet reaction that he is doing(and the hole in the bag/balloon that has allowed minimal amounts of water escape) that some I2 may be boiling out, before having the chance to create HI. If SWIL's guestimations of the amount of I2 was off(say it was 3 grams instead of 4), then this reaction could may prove incomplete at 36 hours.
SWIL collected another 2-3 grams from 2 more 30 ml bottles of 2% tinc. He cleaned this much better, and dried it fairly well. He was not worried about the extra moisture this new I2 contained, as he the water level in the reaction was down from it's original mark. He chucked about 2/3's of the I2 that he now had into the reaction.
The rxn took off again. This time SWIL did not remove it from the 180 degree Farenheit heat. Yellow smoke began to fill the balloon again. Within 10 minutes, the reaction had doubled in size.
The reaction was now at about 6 hours cook time total, at 180 F. SWIL planned to continue the cook in sections, as time would allow.
Lukky D
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# 8

2003-07-23, 05:01
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swinc has dreamed of finally getting a rxn that went ok (good, but not the greatest). did not have the doubling in size. is this something that should have happened?
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# 9

2003-07-23, 08:43
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SWIL has never seen this before, but then again, he has never added fresh I2 at 180 degrees F.
He has heard it should double, but this is not always the case. SWIL is not sure of the logic, or if it is good or bad. In this case, SWIL was just reporting what he was watching.
Lukky D
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# 10

2003-07-24, 01:30
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SWIL forgot to mention, that realizing this would be the last time adding precursors, that he could replace his ghettofied ziplock/balloon with a punching balloon. He sealed it with electric tape that claimed to be flame retardant and high heat resistant.
The reaction is now standing at about 12 hours of cook time. The color has changed from dark brown, to a golden/amber/red that sits a top a lower layer of maroon RP. When swirled, the top layer becomes more red and mixes with the RP. This begins to settle into two layers immediately, however; it does not fully seperate for at least 10 minutes. It looks pretty wet, but the contents are still giving off yellow smoke, so SWIL knows this reaction is doing it's job.
The balloon is starting to give off a certain odor that SWIL enjoys, and the oily droplets near the bottom of the flask tell SWIL that he is well on his way. Nearing the top of the flask, the droplets become more watery, and vary in color from clear, yellow, or red. The drip back down the flask walls, and as these droplets hit RP chunks clinging to the flask walls, another reaction can be seen happening. The clear droplets become quickly clouded yellow/white, SWIL wonders if this is more HI being produced???
Everything looks in order, the reaction will go on.
Lukky D
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#11
 2003-07-24, 05:01
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pikk 
Regular
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Re: The Nano- It's not as hard as it sounds!
i hate to say this LD but when doing a hot fast cook when it doubles in size it is usally done. when you added the extra i2 you kicked the rxn in to overdrive causing it to finish. also you need to find a better ballon for your rxn . also bro check your old hotmail acount if you dont have it anymore let me know i need to send you a email .if you got my email let me know..
pikk
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#12
 2003-07-24, 05:24
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morgan 
Regular
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Re: The Nano- It's not as hard as it sounds!
what feedstock did you use to get the eph out of--and what other feedstock do you know of that contains eph thank you
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#13
 2003-07-24, 06:09
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lukkydleprachan 
Regular
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Re: The Nano- It's not as hard as it sounds!
Pikk,
With SWIL's visual observations, he would guess that you are correct. The HI level was adequately high to reduce the amount of pseudo in the reaction, at that heat. SWIL wishes that he had let the reaction cool before adding the excess I2, and it could have possible saved his long, wet.
The reaction looks near complete, but still shows some signs of incompletion. SWIL is guessing it's the excess I2.
SWIL is going to pull it now, and check it out.
Lukky D
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#14
 2003-07-24, 20:29
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Regular
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California somewhere....
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Re: The Nano- It's not as hard as it sounds!
Lukky..."2 ISO rinsings, 4 dH2O washes, and 2 acetone soak/decantings."
Pardon Switrd's ignorance, but could you explain the process of "decanting"?? Thank you in advance 
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#15
 2003-07-25, 04:16
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Wicked_Rain 
Regular
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Re: The Nano- It's not as hard as it sounds!
quote:Originally posted by AlwaysTired:
Lukky..."2 ISO rinsings, 4 dH2O washes, and 2 acetone soak/decantings."
Pardon Switrd's ignorance, but could you explain the process of "decanting"?? Thank you in advance
decant means to pour off or siphon off said liquid
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#16
 2003-07-25, 06:54
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lukkydleprachan 
Regular
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Re: The Nano- It's not as hard as it sounds!
Basically, once the solids have settled out of the solvent, then the liquid is poured/syphoned off without disturbing the settled solids.
This allows the solvent to "extract" the gakk/dirt/polys/etc., hence cleaning the solid. NOTE: The solid must be insoluble in the solvent being used in order to decant. Otherwise, it will be extracting it, and product will be thrown away when the liquid containing the extract is decanted.
Lukky D
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#17
 2003-07-31, 02:57
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stuckdaydreaming 
Regular
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Re: The Nano- It's not as hard as it sounds!
BUMP What's up Lukky?
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