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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
 2003-12-04, 19:24
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DarkSky 
Regular
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Dreaming of H
SWID told me hes planning on having a dream Sunday morning about H3PO3 and was hoping that it would not turn into a nightmare like the last time. SWID did say that the nightmare was all his fault though.
Now this is a 3-hour dream and heres how SWID hopes it will go:
10gE/15gI/10gH3PO3, 2ml Dh2o. Mix all together and heat at 150° for 1 hour then, over the next hour raise heat to 190°. For the last 30 minutes of the dream run heat up to 210° and maintain. SWID only has 3 hours to dream and then he MUST clean up so he was hoping that this would make for a good dream
SWID would appreciate any feedback or suggestions that his friends can offer. SWID has only attempted to dream about H3PO# one other time and was hoping that this would be a dream to remember
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#2
 2003-12-04, 22:49
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kman 
Regular
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Re: Dreaming of H
If you only have three hours, then how are you going to recrystallise? That takes a little time, too.
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#3
 2003-12-04, 23:08
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DarkSky 
Regular
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Re: Dreaming of H
The whole process will take 3 days. SWID will do the actual rxn on the first day and collect the honey. On the second day the A/B process will be finished and the re-crystalization will be started with the end product collected on the third day.
But SWIDs problem is he cant find any reliable information listed using H3PO3 and was hoping someone out there could offer some suggestions as to whether his E/I2/H3 portions are correct and is the cook temperatures he is using for the amount of time he has avaliable for the actual "cook" portion of the rxn will surfice.
SWID was hoping that there was someone out there that had some actual expertise in this area and could offer him some help
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#4
 2003-12-05, 02:02
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sawdust 
Regular
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Re: Dreaming of H
I`d like to know this myself, I have had problems in this area with the rxn. It seems to be a problem with the H3. the three atoms of hydrogen affixed to the phos. atom is blocking the iodine from connecting to the phos. atom , leaving a purple mess to be cleaned up. After many unfruitful attempts to produce honey, I put aside my H3 until a proven method becomes available.please let me know if your dream comes true.
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#5
 2003-12-05, 02:18
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pikk 
Regular
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Re: Dreaming of H
this might help you guys i found it looking around dont sound to hard....
P-fed Reduction to Methamphetamine with Hypophosphorus Acid and Iodine
By Pebble
Assuming that you have extracted P-fed from your pills, you are now ready to convert the p-fed to methamphetamine. The structure of P-fed is so closly related to methamphetamine, that people have learned to alter it's structure in order to convert it to methamphetamine.
What one is actually doing is reducing a benzylic alcohol. In our case, it appears as OH in P-fed. So, we strip this off completly and throw on an additional H (Hydrogen) to the p-fed. So, by removing the OH and adding a H we have thus altered the structure and have created methamphetamine.
This is for small-scale reduction of P-fed to methamphetamine. If one wanted to make meth in the range of ounces, etc. I would not reccomend one cook in an open container. Fire or explosion are at a much higher risk when cooking anything above 10 grams using this procedure. This is why the Push/Pull apparatus is so popular. No, fumes, smell, and IT CAN reduce the risk of injury if something does go wrong. Notice I said IT CAN. There is no fool-proof method of safety when working with chemicals of this nature, unless proper lab equipment, etc are used; and this still does not elimanate the dangers, just reduces the probability that an accident will happen.
If one wanted to have 5 grams as their finished peoduct, than 6-8 grams of P-fed. Some can get 90% yield where others may only get 35% yield. This takes time to perfect, but results will vary WITH YOU.
Take your 8 grams of p-fed and put this into a 250ml. flask or pyrex meassuring cup. Slowing add Iodine crystals unto the p-fed is mixed well with the iodine. You don't want it very purple, just enough iodine to where all the white is no longer visible. Remember, you mix the iodine and the P-fed up as you go along, you just don't throw it in and go from there. O.K., a good way to meassure your Hypophosphorus acid is to use a ratio of 1ml. for every gram of P-fed that you are using. 50% or 30% Hypophosphorus will work, but you might want to add more Hypophosphorus acid if it was 30%. I have seen "LAB GRADE 30%" act no different than 50%. So, you make the call, just do the math to equal out the 30-50 ratio if using 30% Hypo.
O.K. put in you Hypo. Doesn't take much. Take your cooking vessal and move around slowly to mix the acid with your I2 and P-fed. You'll notice that the contents will start to liquify. It will look red, so agitate the cooking vessel until it turns yellow. After it has turned yellow, place on heat. You can use gas or electric on this small cook. If using a electric eye, place an iron skillet or something over the eye. Usually Med heat to High will be O.K., you might have to experiment to see what works best. You don't want it to get to hot, so remove give it a couple of swirrls. Place back on and leave on heat, repeating this a couple of time if neccessary. When it befins to boil, let it, for about 10 sec. and remove and let it sit, DO NOT SHAKE. You will notice that it just keeps boiling. It may do this for 30 sec. or more and then quit. This is your first major reaction. Take a little wiff of the smoke, you'll notice that it'll take your breath away. Don't worry about dying from this, it's O.K., just smells bad.
Agitate it a few times and crank up the heat a little. Remember, don't let it get to hot, but don't let it cool down either. When it begins to boil a second time, remove it after about 10 sec. and let it sit. After you remove it from the heat, it will continue to get faster and faster and really smoke. This is your second major reaction and this is what does the conversion of your P-fed to methamphetamine. If you removed it a second time and it hardly did anything. Than try again to ensure that it converts. If you take another wiff you should notice that the smell is bearable now, and actually quite pleasant in some cases. There are about three distinct smell that let you know it converted. If you pay attention in the beginning to the smell, you notice the difference and it's very noticable. Keep agaitating and letting it sit, maybe place on heat source for a few secs. and remove and agitate. It's done, but it should go to a golden or yellow looking oil. Or it may go very clear looking with only a touch of yellow. Or if it turns green or is dark this is O.K. Sometimes this happens with the use of H2O2. As long as no particles or floating around.
Let it cool down at this point. The whole reaction should have lasted no longer than about 10-20 min. After the cooking vessal is WARM to the touch add colemans and lye and the lye wash. If it got to hot and is like caemel syrup on the bottom, a piece of wood can be used to mix the dope up to get to going. If you don't stir up the contents in a situation like this, your lye will never push your dope up into the coleman lyer. Also, if your lye begins to go into your coleman layer, a little alcohol around the edges and a few drops in the middle will keep it down. After the wash, draw up your coleman fuel layer, for some it turns purple. The lye should have been added until the p.h. read +13.
Next, put the coleman/dope layer into a 20 0z. coke bottle and add an equal amount of distilled water. Use HCL to gas the coleman/dope layer so that the HCl will push the dope into the water. It all in there when the P.H. of the water reaches around 7. Stopping around +8 is safer than trying to go to 7. Turn the bottle over and lossen the cap until the water begins to fall into the evaporating dish. Make sure no coleman gets through. Now, just evoparate the dish with the water/dope and there you go!
If done correctly, you could have a 90% yield, but for many and new beginners the yield is usually around 35-40%. There are many tricks and little secrets that are involved that one can possess and learn as they do this. As for as quality, I dreamed of one line and it was so good I broke out into a sweat instantly. It has no bad comedown effects like I have expericed with the "Nazi Method" and doesn't cause sore muscles, etc. It's a fast and easy method for anyone wanting to aquaire a few grams of meth. for bigger quantities, cooking will be necessary, but everything else will remain the same.
--------------------------------------------------------------------------------
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#6
 2003-12-05, 02:29
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OZs2KEYs 
Regular
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Re: Dreaming of H
Swim thought H3PO3 was phosphorus acid flakes, not hypophosphorus.. swim doesnt know though.. is this correct?
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#7
 2003-12-05, 02:36
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pikk 
Regular
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Re: Dreaming of H
swip would add his chems like this
1. Water
2. Iodine
3. Red Phosphorus
Make your HI first, then...
4. Pseudoephedrine
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#8
 2003-12-05, 02:41
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DarkSky 
Regular
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Re: Dreaming of H
OZs2KEYs is right, H3PO3 IS phosphorus acid flakes, not hypophosphorus, they are different compositions.
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#9
 2003-12-05, 02:45
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pikk 
Regular
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Re: Dreaming of H
and another this is from geez ....
Conclusion is that the synth does in fact work, works well, and may replace I2/redP as the standard HI synth.
Do not be afraid to do this synth. It works.
Note: yield was in the 7.2 grnm range, after heavy sampling for bioassay. Swig thinks the yield can be easily improved.
----------
SWIG decided to do this synth again. Eager to do this again, he collected 13 grams of freebase pseudo from an assortment of pills still available on the local merchant's shelves when he got there, by his full-cure-straight-to-bee-method (for the truly anal retentive.) Yield was very good, given the 15.1 grams of freebase pseudo available in the pills.
He added the water, H3PO3, and I2 to the flask and fitted the condenser and balloon before adding any heat. He did this based on results with the long wet red P/I2 reflux and adding the pseudo after the other ingredients calmed down after making the HI, and postulating those benefits to this synth.
As the oil warmed, the reaction producing HI took place very quickly and cleanly. It fumed and smoked less than the previous effort, which was done with the pseudo in the flask. He did not observe the heavier inital yellowish fumes, which he wanted to avoid if possilbe. The production of HI seemed to proceed faster and with less smoke, and it seemed to take place at a lower temperature than 80°C. Note the use of the word "seemed." These were the observed, noticed events...but are largely subjective observations. He did not get to measure the temp as he tried to do, suspending the thermometer through the condenser. He instead dropped his thermometer down the condenser, being the clumsy fellow that he is, and this broke the bulb end off the thermometer. He realizes now just how nice that adapter would be. And he learned one of the two reasons he now has for using such an adapter to do this.
After the HI was produced, he turned the heat off, and let the oil bath cool for about twenty minutes before adding his pseudo freebase. This he elected to do through the condenser, which was as stupid an idea as he has had this week, with two exceptions. One was trying to use a string to lower the thermometer down the condenser to measure flask temperatures. The other was using the broken thermometer to tap the pseudo down the condenser tube into the flask. Not that it did not work, it did. SWIG, being the clumsy fellow that he is, dropped the thermometer another time or two and had to retrieve it from the flask. This was not partiuclarly difficult. He did have a string attached, after all. Since he did not have an adapter. Which would have been very useful.
Having added all his pseudo, he began heating the oil bath. Shortly afterward, a considerable amount of smoke came from the oil bath, which he attributed to pseudo spilled while adding it to the flask. The unmistakable "plink" of glass divorcing itself from the rest of the apparatus was followed by a billowing plume of smoke from the oil bath as the contents of the flask merged with the oil through the no-longer-connected-to-the-top bottom of the flask. And he learned the second reason for using one of those adapters he does not have to fit a thermometer to a single neck flask and still attach a condenser. Overlooked that one before, yes he did.
Hew was glad he had that big fan ready to clear the room's air (even if it meant making the place as cold as it was outside) and thankful he was far enough from the rest of humanity to avoid having a "helpful" neighbor call the fire department.
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#10
 2003-12-05, 03:03
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pikk 
Regular
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Re: Dreaming of H
h3po3 is Phosphorous Acid no matter what form it comes in....
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#11
 2003-12-05, 03:07
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Re: Dreaming of H
H3PO2=Hypophosphorus.
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#12
 2003-12-05, 03:44
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OZs2KEYs 
Regular
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Re: Dreaming of H
Swims lost. If H3p03 is hypo then what is phosphorus acid flakes? Which brings about a better rxn for the money, and which is "least" watched?
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#13
 2003-12-05, 04:02
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pikk 
Regular
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Re: Dreaming of H
flakes are still around . as for the acid it is watched really hard now. this is why most are using the flakes now
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#14
 2003-12-05, 04:10
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OZs2KEYs 
Regular
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Re: Dreaming of H
Ok, so where could one find a good write up or two on useing flakes?
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#15
 2003-12-05, 16:31
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DarkSky 
Regular
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Re: Dreaming of H
OZs2KEYs, you are right again! Last night I spent several hours scanning well over 1000 posts at the Hive in search of such information. About 1:00 AM I found what I was looking for. Seems like the Great Geezmister has done some pioneering research in this area and posted a paper on his findings. I found the information VERY informative!
It looks like SWID is going to have to make a few changes to his Dream if he wants it to be pleasant. Most of the information I found talked of 18 to 24 hour rxn's and most were done on 10gE runs, Well, SWID does not have that much time so hes going to drop down to a 3g Nano and do a little experimenting. From the info I researched I believe that something of this size is possible in the time restraints that confront me.
I hope Geezmister does not mind but I am copying hes post form the Hive and posting them here. Please note that the following is not 1 long quote but a collection of several over a period of several days.
I hope everyone can benefit from this information as much as I have!
THE FOLLOWING IS GEEZMISTER'S POSTING'S ON H3PO3 rxn:
"Phosphorous Acid Trial
(Rated as: excellent) Bookmark Reply
A short time ago SWIG poured ten ml of dH20 into a flask and added 10.5 grams of phosphorous acid flakes. These were swirled until the acid mostly dissolved, leaving a few flakes still to be dissolved. This was not particularly exothermic. To this mixture was added 11.5 grams of very dry I2 obtained from tincture which had been fairly well powdered before adding; this was stirred until it appeared to have dissolved and the mass resembled a mixture of dark crude oil. Ten grams of pseudoephedrine freebase crystals were added to the solution and stirred until they appeared to have dissolved or dispersed uniformly throughout the mixture.
The flask was placed in an oil bath and a 400 mm Liebig condenser fitted. Water with a temperature a little above freezing was circulated and the oil was slowly heated. A thermometer suspended into the flask through the condenser was used to monitor the temperature of the flask contents.
When the contents of the flask reached 80° a reaction began which produced a thick yellowish smoke for a few seconds; this quickly gave way to white smoke, not as dense, which cleared to a thin white smoke, became a mere wisp, then disappeared entirely. A balloon was quickly fitted to the condenser when gas production began; it filled to softball size and remained there until it was necessary to remove it to lower the thermometer. No noticeable gas loss occurred during the reaction. This reaction took place very quickly and violently, and did not last very long. It was similar to the reaction which occurs when I2 is added to hypophosphorous acid. It was as vigorous, as quick, and as short-lived as that observed with hypo.
The contents of the flask went from dark black to thick, creamy pale yellow. The contents of the flask began to bubble steadily, although not with the vigor or number of bubbles observed with a hypo cook.
As the temperature inside the flask reached 90° the color of the solution darkened. Bubbling remained the same. At 100°C the mixture was even-textured and resembled vanilla pudding. At 107° the contents of the flask became noticeably more active and the mixture was clearing and becoming transparent. SWIG's best estimate of the time elapsed to this point is about twenty-five minutes.
When the mixture reached 110° its color appeared to change to gold, but this may be affected by the color of the oil bath. It also became completely transparent. Clear. You could see the bottom of the container holding the oil clearly. No solids were in the flask. Again, this reminded SWIG of a hypophosphorous/I2 reaction after the bubbling in the latter becomes hard to sustain without continuous heat, and the reaction nears completion.
My intention was to bring the internal temperature of the flask to 118° and reflux for the night. The oil bath reached a maximum temperature of 170° (measured by a candy thermometer) I was unable to get an accurate reading of the thermometer in the flask because of the heavy condensation on the walls of the condenser and the failure of SWIG's knot in the string suspending the thermometer. (Okay, SWIG was not a good boy scout.)
At approximately 1:00 am SWIG concluded that the oil bath temperature at its maximum setting would not heat the bath beyond 170°C, the flask's internal temperature would not get hotter than 112-114°C, and the reflux would remain stable about half way up the condenser unless the water in the reservoir got too warm over time. SWIG decided he might as well leave the reaction as it was. The reservoir of water was replaced with fresh cold water. No difficultly had been encountered with the heat produced by the reaction at that time.
The mixture will be allowed to reflux for approximately eighteen hours, at which time SWIG will be free from the chains of employers and other obligations and be free to pursue his avocation as an alchemist.
The reaction is being monitored by his ill humored assistant and sidekick, who was given bread and beer before being chained to the water pipes in the lab and told not to fall asleep until SWIG returned.
SWIG observed that the reaction proceeds much the same way that a hypo reaction does, at least after it reaches the initial 80° temperature--which seemed to be the temperature at which the phosphorus acid and I2 reacted and made HI. From that point the reaction proceeded as fast as a hypo reaction does to a clear state. The color of the mixture could not be determined while the flask was in the oil bath; the color of the oil and transparency of the mixture made judging the color difficult. The time between first heating and becoming transparent was a sufficient period for a hypo reaction to have completed.
SWIG has discussed the reaction with a couple of street cooks in his area. They told him they had been taught to dissolve the phosphorous acid in water, add the ephedrine, then add the I2, and put it on heat with a sturdy balloon until it really goes wild. They are instructed that when the contents of the flask become clear, as long as it has been fifteen minutes, the cook should be considered as complete. SWIG believes they are quitting too soon. He thinks their mixture is being pulled to quickly and has not completed at this point. His bioassays of the product of other cooks' phos acid meth leave him with the impression of half-reacted, unfinished meth, not unlike what is obtained after a short, hot, dry cook with very clean pseudo and fresh red phos. Good for street dope, not complete by SWIG's standards.
SWIG is concerned about not being able to achieve the intended 118° temp inside the flask with the oil bath. He otherwise has the feeling that the synth is similar to the hypo synth and that if the initial concentration of HI is high enough it should complete fairly quickly and completely. All the same, he wanted to reflux the mixture to give it every opportunity to finish.
Results later, after bioassay, most likely.
Phosphorous Acid Works
(Rated as: excellent) Bookmark Reply
SWIG got to the lab about seven last night. He sniffed the top of the condenser and smelled that smell he loves to smell. He turned off the oil bath, removed the condenser, and took the flask out of the bath so he could get a good look at it. Pure gold. Reminded him of the look of the flask after a hypo/I2 cook completes. The honey was, however, a good deal more viscous than the honey from a hypo cook.
He added boiling dH20, three times the volume of the honey, to the flask and swirled until the honey was thinned out. There is nothing to filter out of the honey. The honey is thick and oily, and if filtered a lot of it would be trapped by the filter. The honey is washed with Xylene, then hot naphtha. Neither solvent appears to be contaminated with reaction byproducts. The honey is based with a 20% NaOH solution. It bases very quickly with less NaOH than is usually necessary after a rp/I2 cook.
Hot naphtha is added to the flask and the contents swirled several times. The naphtha is allowed to sit on the honey for ten minutes, then is decanted. This process is repeated and the two volumes of naphtha combined and washed with brine, then warm water, then cool water. The rinse water is added to the based honey in a coffee pot and a third volume of naphtha added. A little additional base is added to the honey, which is then heated slowly until it just begins to boil. The coffee pot with honey is removed from the heat, covered, and put away for processing in a day or two.
The meth was extracted with dilute aqueous HCl. The evaporation dish skinned completely over. The meth was almost transparent even in this state. The contents of the dish were flashed with acetone which mostly boiled off, leaving a good quantity of very white crystals. A sample was set aside for testing, the meth panned to one corner, and acetone collected and placed in the freezer. The meth was rinsed once with fresh acetone, which was also collected for later use. Boiling IPA was added to the evaporation dish to dissolve the methamphetamine. The alcohol solution was filtered through a Charmin Plug, concentrated to near saturation, and acetone added. The beaker containing the solution was left on the counter in a room with an ambient temperature of about 50 degrees F.
While practically all the material panned to the corner of the evaporation dish dissolved readily in hot IPA, the Charmin plug collected a noticeable small layer of slightly pinkish fine clay-like particles. These particles had a smell similar to the odor one sometimes found in meth produced with an excess of hypo.
The test sample from the evaporation dish was placed on foil and melted. It gave off an odor found where an excess of hypo was used in the reaction. The vapor had a bitter, nasty taste. Very light brown to tan deposits remained on the foil after the sample was vaporized.
After two hours the crystals which had precipitated in the alcohol solution were filtered off. The mother liquor was filtered through a Charmin plug, this one more packed more tightly than the previous one. This filtering also left a small layer of very fine dark pinkish tinted clay-like powder on the plug. The mother liquor was concentrated and the beaker placed in the refrigerator. In about an hour the crystals which had formed were harvested and the mother liquor combined with the alcohol used to rinse the evaporation dish, the funnels, and glassware that might contain meth. The filters used to harvest the crystals were soaked in alcohol, wrung out, and that alcohol added to the beaker. This was again filtered and concentrated, covered, and placed on a shelf in the cool room for crystal formation and later collection.
The collected crystals weighed 4.7 grams. This does not represent the yield from the first two pulls as there is still a significant amount of meth in the alcohol solution which should form crystals. The third pull should add to the overall yield.
The crystallized product, when vaporized, did not have the smell noted earlier nor did it have any unpleasant or noticeable taste. This must be contained in the fine silt that Charmin plug removed. The vapor is very smooth to inhale. SWIG inhaled about five or six good pulls from a pipe before realizing he should have quit after four. this does not seem to have the same strength as the product of a long wet rP/I2 reflux, but it is very close. With refinement of the synth and some experimentation with the temperature and perhaps a little less phosphorous acid or a little bit more I2 the results should be equivalent to the product of a hypophosphorous/I2 reaction.
Initial impression was that this synth definitely does work as advertised. Dual Friedrich condensers are sheer overkill. Cold water will be sufficient if one uses a 400 mm or longer condenser. Heat was not a problem after all. Gas containment was not a problem.
The violent reaction described in the write-up is the same HI producing reaction one encounters adding I2 to hypophosphorous acid. The reaction takes place immediately with hypo. With phosphorous acid, it did not take place until the solution reached approximately 80°C. At that time it proceeded with a vigor similar to that of the hypo/I2 reaction forming HI, and just as fast. No significant bubbling occurred until the temperature of the solution was at or above 100°C. The bubbles were never that small, and this is attributed to the viscosity of the solution. SWIG did not have a stirrer, and believes that a stirrer would be a a good addition. The solution is not as fluid as a hypo solution or a redP/I2 solution and is too thick to allow bubbling of the type SWIG tries to achieve in the other reactions. The viscosity may make complete reduction a little harder to obtain without stirring.
SWIG is of the opinion that a reflux at 118° is not necessary. He did manage to measure the internal flask temperature and it reached 114°. The deep fat fryer he used will not reach its stated maximum temperature, but it does come close. SWIG thinks the higher temp is not necessary. He plans to run the next such reaction in the 100-105° range. The reaction may complete quite satisfactorily at or above 80°. SWIG thinks the author of the write-up selected the boiling point of the solution as the reaction temperature and that the selection was not made for reasons relating to the reduction of ephedrine.
After arriving at home SWIG did note a slight twinge of paranoia associated with the meth, although nothing along the lines of shadow people or faces in the woods. He thinks the higher temp may be responsible for this. On the other hand, he does not notice any jaw tightness or teeth grinding, and he usually detects the start of that problem if the cooking temperature exceeds 107-110.
The synth itself is quite easy. It has several good aspects worth noting, aside from the availability of the phosphorous acid. Not needing to filter the contents of the flask allows washing and basing of the honey in the flask. Given the right flask, no separator funnel would be needed to extract the meth. The volumetric flask SWIG used allowed him to neatly decant the solvent without difficulty. Yield should be in the excellent range. The product is almost as potent as the product of his recent long refluxes, and he beieves a little adjustment in technique, temperature and equipment will achieve the same potency as the hypo cook does. Yield may be in the same range as the hypo cook, and if it is this synth may be the synth of choice for the clandestine cook.
Over all the synth reminds him a great deal of the hypophosphorous synth, only this synth is safer and does not have shelf life concerns and concentration concerns that the hypo synth entails.
His current impression is to buy stock in companies that manufacture phosphorous acid, although he may just buy the acid itself until it is listed, which is inevitable and may happen fairly soon, as this synth is becoming more widespread and may catch on like wildfire.
Imagine. No more matchbook strikers to scrape.
The reaction used pseudoephedrine freebase derived from 120 time-release caplets. The pseudo was very clean, extracted by the Straight to Bee method subsequent to Xylene, naphtha, and acetone boils. SWIG has no idea how pseudo that is not this clean would react.
Conclusion is that the synth does in fact work, works well, and may replace I2/redP as the standard HI synth.
Do not be afraid to do this synth. It works.
Observations from a second synth Bookmark Reply
SWIG decided to do this synth again under the light of the moon in the Ozarkian woods but changed his mind when he realized it was too cold outside, and returned to the confines of his makeshift lab.
Eager to do this again, he collected 13 grams of freebase pseudo from an assortment of pills still available on the local merchant's shelves when he got there, by his full-cure-straight-to-bee-method for the truly anal-retentive. Yield was very good, given the 15.1 grams of freebase pseudo available in the pills.
He added the water, H2PO3, and I2 to the flask and fitted the condenser and balloon before adding any heat. He did this based on results with the long wet red P/I2 reflux and adding the pseudo after the other ingredients calmed down after making the HI, and postulating those benefits to this synth.
As the oil warmed, the reaction producing HI took place very quickly and cleanly. It fumed and smoked less than the previous effort, which was done with the pseudo in the flask. He did not observe the heavier initial yellowish fumes, which he wanted to avoid if possible. The production of HI seemed to proceed faster and with less smoke, and it seemed to take place at a lower temperature than 80°C. Note the use of the word "seemed." These were the observed, noticed events...but are largely subjective observations. He did not get to measure the temp as he tried to do, suspending the thermometer through the condenser. He instead dropped his thermometer down the condenser, being the clumsy fellow that he is, and this broke the bulb end off the thermometer. He realizes now just how nice that adapter would be. And he learned one of the two reasons he now has for using such an adapter to do this.
After the HI was produced, he turned the heat off, and let the oil bath cool for about twenty minutes before adding his pseudo freebase. This he elected to do through the condenser, which was as stupid an idea as he has had this week, with two exceptions. One was trying to use a string to lower the thermometer down the condenser to measure flask temperatures. The other was using the broken thermometer to tap the pseudo down the condenser tube into the flask. Not that it did not work, it did. SWIG, being the clumsy fellow that he is, dropped the thermometer another time or two and had to retrieve it from the flask. This was not particularly difficult. He did have a string attached, after all. Since he did not have an adapter. Which would have been very useful.
Having added all his pseudo, he began heating the oil bath. Shortly afterward, a considerable amount of smoke came from the oil bath, which he attributed to pseudo spilled while adding it to the flask. He was correct that the smoke was caused by pseudo, but incorrect about its route to the oil bath. The unmistakable "plink" of glass divorcing itself from the rest of the apparatus was followed by a billowing plume of smoke from the oil bath as the contents of the flask merged with the oil through the no-longer-connected-to-the-top bottom of the flask. And he learned the second reason for using one of those adapters he does not have to fit a thermometer to a single neck flask and still attach a condenser. Overlooked that one before, yes he did. Kind of like welding up a hole on a gas tank that is almost empty and forgetting that knowledge about oxygen, gasoline, and sparks. Not a wise thing for one to do.
Glad I had that big fan ready to clear the room's air (even if it meant making the place as cold as it was outside) and thankful I was far enough from the rest of humanity to avoid having a "helpful" neighbor call the fire department. (See, there is something to be thankful for in most situations...)
Have you ever noticed that this sort of thing only happens when your sack is nearly empty?
Is that a reality check I sense looming on the horizon? OH NO! It IS!
Well, I leave the progress of clandestine science (and the H3PO3 synth) to others for the moment. Until further notice you may refer to me by my new nickname, Sleepy. I prefer that nickname to Dopey although I do admit it is as appropriate. I know the meth gods had to have something to do with this. When Sleeping Beauty comes to give me a kiss and wake me up (am I in the wrong fairy tale here?)I must write Zibarium and see which incantation I did incorrectly of forget to do. (He has the other half of the book of incantations, the part with the index. I just have the table of contents.) Anyway, I hope he has it, because it looks like I need it.
Geez the Sleepy, being out of precursors for the time being and free falling into yet another reality check, bids one all a short adieu. The bed beckons. I was afraid this might happen.
Read my first post in the thread again Bookmark Reply
For those of you asking about condensers and flasks and temps, go back and read my posts in this thread again. I tried to be thorough in describing what I did, what I observed, and I put everything I could into those posts. The rest of what I can add is guessing and speculation.
I know most of you never got to do a hypo (H3PO2) reaction, which is sad because they are way too cool and fast to believe. The only really wild part about one is when it makes HI all at once as the I2 is added. I had to either chill the ingredients or add the I2 in portions to keep from blowing the apparatus apart with gas pressure for twenty to thirty seconds. After that there were no problems, at least if I didn't overheat, make phosphene gas and set the whole gas trap on fire spontaneously. Which I did more than once.
The vigor of the reaction with H3PO3 that I saw was the same vigor I saw with H3PO2-- when the I2 reacted to make HI. It was the same type of experience, perhaps not as sudden and violent, and probably keyed by temperature...at about 80 degrees C. That means you can drop the I2 in and seal the apparatus up, sit back and wait for the smoke to billow up. Its like doing a hypo reaction with a control on making the HI...actually more user friendly than Hypo ever thought of being.
I did a small reaction with a 400 mm Liebig. It was more than enough for that size. I have done the one reaction successfully. I have no idea what happens at 75 grams. I'd just be guessing. Why not start out at 28 grams and work up? What's the hurry? Do the reaction once and get a feel for it, then work up. I don't have all the answers, and damned little experience with the reaction. I just happen to have done it successfully. I hoped to give some insight into what to expect, and perhaps I have. You need to run with this ball-- no one has the answers to the questions you ask right now-- go find them and tell us what they are.
Take what I posted for what its worth and forge ahead...all I can say is the synth works and the meth it makes will make you smile...
I think the lead post's suggestions were in fact overkill as far as condensers, and suspect the temps that are recommended are not needed. I could be wrong. I have been wrong many times and admit it when I am. The solution is very viscous, unlike the H3PO2 solution. Stirring, with a magnetic stirrer, or a mechanical one if you don't have a magnetic one, would probably improve the results. My guess. I didn't have a stirrer.
I would suggest scaling up on this one in steps and seeing how it goes as the size increases. I would hesitate to do a 75-gram reaction without previous experience on this one. The reaction which makes HI is vigorous, for sure. And do use a condenser. You want the HI to stay in the flask, and not be absorbed by water in a push-pull tank. HI in the tank does you no good in the reaction. Use a condenser, use a balloon, use an inner tube if you want. Keep the HI in the flask, that's the point. Its the HI that drives the reduction. All the HI in the world won't help you if its in a push-pull tank and your precursor is in the flask.
Once you get the HI made, you aren't going to have pushing and pulling like you do with a dry reaction. After I had the HI made, I didn't need the balloon for gas containment. The condenser was sufficient.
I really can't add more to what I have already posted. Just scale up slowly and try this.
And remember-- I never reached 118°C and do not know what happens there-- but I do know the synth makes meth without reaching 118°C. My instinct tells me if you don't have to go that hot, you don't want to go that hot.
That's instinct, and feel. Not science. Maybe if you get to 118 the recycling takes over and the reaction finishes more quickly. May be. Why hurry something that works? Why use more heat if it is not needed and may produce unwanted side reactions and contaminants?
Good enough? Your turn.
reflux temp Bookmark Reply
I suggest you cap the condenser with a thick balloon etc. and not use the push pull tank. That would give the HI gas a place to go (the water in the tank) and you probably want to hang onto all of the HI you can. This reduction is not going to push or pull like a rP/I2 reaction would. It will fume violently as it makes HI when the solution reaches the 80°C mark. After that, the reaction seemed fairly tame, particularly after it went completely clear. Most of the time involved comes after the solution clears...and the length of time it takes to obtain complete reduction is a guess at the moment.
If you are limited by the size of the condenser, you could most likely reduce the temp of the solution as low as 100°C and maybe a little lower.
Scale it up Bookmark Reply
Ten grams was a really small reaction. Scale it up. With a one-liter flask and that size condenser you have a huge safety range. I'd want a smaller flask for that small a reaction, personally.
As to crashing it out, I don't do many alcohol extractions anymore; when I did I would evaporate to near dryness and flood with chilled dry acetone. Your method will in fact work; I have done it that way, but prefer the flashing by flooding method. If you have PEG-laced pseudo, you should consider dripping the warm alky extract, saturated with pfed, into chilled Xylene. Filter the Xylene, grab the clean pfed.
Rather than drip the water in, why not mix the phos acid and water and combine with the I2, heat with the condenser in place to make the HI, let it cool, remove the condenser, add the pseudo, reattach the condenser, and bring the temp up slowly. I suspect that may be a common sense route to even better meth with this synth. Get the HI made, add the pseudo, then add what heat you think is needed."
There you have it everyone, straight form the pen of the Great Geezmister
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#16
 2004-04-22, 00:20
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sitbcknchill 
Regular
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Re: Dreaming of H
i stumbled onto this post while diggin deep for some answers, wanted to keep it around for a few days
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#17
 2004-04-22, 01:26
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DarkSky 
Regular
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Re: Dreaming of H
Impressive sitbcknchill, you were definately digging deep for this one! H3 cooking has come a long way since then and there is some good info avaliable now.
I wish all the newbees would take a lesson from your example and learn how to research as well as you.
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#18
 2004-04-22, 10:26
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gottagogo 
Regular
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Re: Dreaming of H
Well, I slyfully (if that's a word) acquired a little computer time and decided to drop in on ya'll for a click. Looks like that old saying is indeed true, "The more things change, the more they stay the same."
I know a couple of guys who would love to try their hand at something different, but it seems as though the ever elusive flakes may simply be unobtainable for some garage bartenders. They do exist, finding the words in a chemical supply catalog is a piece of cake. Actually holding the can in your fat little hands is another story.
Yes, many a frustrating hour has been spent tracking this prize, and more than a few times it has looked like it was down to a simple matter of logistics.......but, no, it just never happened.
I feel so sorry for those poor bastards every time I see them. So, if any of ya'll care to take pity on their poor tired souls, just send a key or so to ole gogo. I'll make sure they get it.....safe and sound.
By the way, try to refrain from abbreviating H3PO3 as H3. Some old fart may see it and immediately think (well, actually consider since thinkin' would not be part of the equation) that someone has come up with a new novel reduction technique, and get all excited over nuthin'.
You wouldn't want that to happen, would ya?
kirb, pikk, jam, AM, shooter,tryp, wicked, all the really smart dudes, up and comers, and assholes that I love to hate,
PEACE
[This message has been edited by gottagogo (edited 04-22-2004).]
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#19
 2004-04-22, 23:16
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sitbcknchill 
Regular
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Re: Dreaming of H
quote:Originally posted by DarkSky:
Impressive sitbcknchill, you were definately digging deep for this one! H3 cooking has come a long way since then and there is some good info avaliable now.
yeah there is some pretty well written out there now, swird likes to compare the old with the new, one persons from another, in every which way, facts, numbers, ratios, possible problems, hazards its a must man, it keeps ones ass from gettin killed, and teaches one how to make kick ass dope  thats why swird bumps posts
no real need to ask questions
[This message has been edited by sitbcknchill (edited 04-22-2004).]
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