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Author	Topic: Electrolytic Stuff
beeach Hive Bee	posted 03-23-2000 12:57 PM Hi YA - I have a recipe for electrolytic reduction and wanted to get some help from you guys. Here goes: First forming the the ester. 10 grams of ephedrine (from the Ma-Haung) into 100ml acetic acid. Then add 2ml of Concentrated HCl 32% , or 1ml of Concentrated HS2O4. Heat at 80 degC for 45 min. Now using a clay wine cooler (from K-Mart) that has been sanded and soaked in cold water for a day or two. Its set in the middle of of 3 gal bucket, and the ephedrine+acetic acid in placed in the clay cooler. YOU ARE SAYING THAT ONLY 100 MLS OF THE EPHEDRINE ESTER + ACETIC ACID MIXTURE GOES IN THERE. ADD 100MLS OF 10% H2SO4 SOLUTION TO THE EPHEDRINE ESTER MIXTURE. In the bucket a mix of a quart of distilled water to 200ml HS2O4 is poured around the the cooler. A piece of 3/4 inch lead wire 8 inches long is hung in the middle of the cooler, and another is hung on the side of the bucket. CLEAN THE SURFACE OF BOTH THE LEAD(Pb) WIRES WITH STEEL WOOL, AND WASHING WITH ETHANOL TO EXPOSE FRESH CLEAN LEAD (Pb) METAL. The postive + is hooked to the bucket lead piece , and the negtive is hooked the cooler piece. over head stirring is rigged to stir the ephedrine+acetic+ dilute sulphuric acid mix without fucking with the lead wire. OK ! REMEMBER THAT SOME POWER SUPPLIES THE CURRENT FLOWS FROM POSITIVE (CURRENT FLOWS OUT INTO THE CATHOLYTE), THROUGH THE CATHOLYTE, THROUGH THE CLAY CELL DIVIDER, THROUGH THE ANOLYTE, TO THE NEGATIVE (CURRENT FLOWS IN). GET THIS RIGHT! D.C. power is applied at 15vdc at 50 amps although the meter olny read 2amp being use in the cell. THIS INDICATES THAT THE CELL IS NOT CONDUCTING EFFECTIVELY. YOU WANT 12-13 VOLTS AND 5 AMPS OF CURRENT TO FLOW THROUGHOUT THE CELL. This is let run 6 hours. I THINK THIS IS EXCESSIVE IF YOU PASS A 5 AMP CURRENT, WHICH THIS TYPE OF CELL CAN DO. 1. WIll this work? 2. Does a piece of 1cm glass need to be put into the cell? 3. Where can I get this type of power supply already made? Thanks and love, beeach
beeach Hive Bee	posted 03-23-2000 04:42 PM Hi - One other thing that I just remembered. There was info about using a silver plated cathode or anode (does anyone have the link or the info for this?). I have heard of people using a silver spoon and a toy train power supply to do this. beeach
malaci Hive Bee	posted 03-23-2000 06:32 PM No it will not work for one you will not form the ester.Try 5-7 ml of GLACIAL acetic acid per gram and a few drops of H2SO4 or perchloric no 32% Hydrochloric.The electrolyte is only 3-5 ml per 100 ml of DH2O.If you go stronger on the electrolyte you will not be able to anodize correctly because the electrolyte will be to strong causing your black oxide to dissolve off.As for as your current goes you want to stay in the range of 30-40 ma per square cm of ingot.For your run time your way the fuck off where did you get this bullshit recipe.A toy train transformer will not work it causes AC ripple.If you pull a stunt like all that voltage your going to reduce your H2SO4 and fry your ester.You do not want the electrolyte getting hot at all.Have you seen any of the electro posts?
malaci Hive Bee	posted 03-23-2000 06:56 PM DISCLAIMER: THE FOLLOWING INFORMATION IS FOR INFORMATIONAL PURPOSES OR ACADEMIC STUDY ONLY. CHECK YOUR LOCAL, STATE AND FEDERAL LAWS, AND PROCURE THE NECESSARY PERMITS BEFORE UNDERTAKING ANY OF THE REACTIONS DESCRIBED BELOW. NEITHER BOZAKIUM NOR UNCLE FESTER SHALL BE HELD LIABLE FOR USE, MISUSE, INJURY, DEATH, IMPRISIONMENT OR FELLATION DUE TO THE APPLICATION OF THIS INFORMATION. "Festerlytic Hydrogenation" Preface: As those of you who have been following the chem scene this year know, the new book from Uncle Fester has been promised and promised by Loompanics since March or so of this year, with the release date continually being pushed back, despite the word that it was "at the printer's" in June. I have been privy to the manuscript of a very,dare I say, revoloutionary chapter of this book since much earlier this year, and out of respect for the author's need to make a living, not divulged any "trade secrets" though I have told of said formula's most vital element, and teased of the simplicity this new Fester Method. Now several months later, and nearly a year since the book was written it is still not available and we are now told by 'Panics to expect it in September sometime. Yeah, right (sarcasm here folks). Anyway, while discussing this with Fester, I mentioned how I had teased the swarm with hints of the new method , but hadn't divulged any "trade secrets". The embittered Fester, pissed at the gravelly hand-job Loompanics has been giving him(allegedly due to management changes or something) defiantly trumpeted "Divulge Trade Secrets!" I nearly busted at nut with both excitement and relief that I could now share this breakthrough with you, the scientific world. My shit-eating grin still aglow, Uncle excitedly gave me two new references which promise to significantly shorten reaction time. It is now my great honor to share this knowlege in the interest of the furtherment of science. Enjoy. --- Bozakium 1998 THE 1998 FESTER FORMULA: Electrocatalytic Hydrogenation of Ephedrine, Pseudoephedrine And Phenylpropanolamine Abstract: Reduction of the hydroxyl group of various 1-phenyl-2-aminopropanols and their substituted amino variants are easily and efficiently carried out by electrocatalytic hydrogenation of their respective acetic esters at a palladium or palladium-plated electrode in a divided electrolytic cell. Use of a lamb's skin prophylactic as an inexpensive yet effective cell divider is also demonstrated in this experiment. Materials: One (1) gram of purified ephedrine, pseudoephedrine or phenylpropanolamine. One troy ounce ingot of palladium Glacial acetic acid Concentrated sulfuric acid Sodium hydroxide Anhydrous HCl gas source pH-indicating paper Toluene Kling-Tite Naturalamb brand condoms Lead or graphite electrode 1/2-inch wide by five inches long Six one-inch alligator clips Several feet of 16 to 20 gauge insulated copper wire Variable DC power supply Ammeter capable of measuring up to 3 amps, with resoloution to 1/10 of an amp Voltmeter (optional) Procedure: One gram of ephedrine, pseudoephedrine or PPA hydrochloride is placed in a large test-tube along with 5-7 mL of glacial acetic acid. The test tube is heated in a water bath until all the ephedrine(in this case) hydrochloride is dissolved. A few drops of concentrated sulfuric acid are added. Mix it all together and LOOSELY stopper the end of the test tube to prevent steam from entering. Heat the water bath to just about boiling, and use it to heat the test tube and its contents for a few hours. This forms the acetic ester of the ephedrine, pseudoephedrine or PPA used in the reaction. The solution should appear clear and water-like, completely homogenous. After heating, the reaction mixture can be kept stoppered as is for a few days, but it's best to use it immediately after it's cooked. Next, mix up a solution of 5 mL of concentrated sulfuric acid in 100 mL of water. Take a 250 mL beaker, and place it on a magnetic stirrer. Clip a well-scrubbed Kling-Tite Naturalamb condom in one side of the beaker, and place a piece of lead 1/2 inch in diameter and a few iches long inside the condom. On the other side of the beaker, stand up a one-ounce ingot of palladium. Using alligator clips, make contact with the ingot, and wth the piece of lead. They are your two electrodes. Next, pour most of the dilute sulfuric acid solution into the beaker. Save enough that some can be poured into the condom so that the solution levels are about equal inside the condom and the beaker. The ingot of palladium should be almost completely immersed. The alligator clip should be up out of the solution, and there should be enough space left to add the ester reaction mixture from the test tube to te beaker without causing the solution level to reach the alligator clip. The surface of the palladium ingot should be lightly sanded prior to use. This increases its surface area a little and exposes fresh, clean metal. The piece of lead should be scrubbed free of grease and dirt. The wire lead to the palladium ingot can be clipped to the side of the beaker with a clothes pin or paper clip to prevent the ingot from falling over during the course of the reaction. A DC current meter (ammeter) should be put in series with the wiring. A good one can be had at Radio Shack for under $50.00. The wires are first hooked up so that the palladium ingot is connected to the positive pole of the DC power supply, and the piece of lead to the negative. The typical one- ounce ingot will have a face with an area of about six square centimeters immersed in the solution and one square centimeter up out of the solutuion. Only count the area on the side facing the lead piece. The back side doesn't count because significant current doesn't reach it. With this typical ingot apply about two amps for 30 seconds to one minute. Oxygen will bubble freely from the ingot, and hydrogen from the piece of lead. Blackening will be noted on the edges of the ingot, where the current is most intense, and a lighter discoloration on the flat face of the ingot. This pre-treatment is called anodizing. It has been found that anodizing increases the ability of the palladium ingot to adsorb hydrogen when the wiring is turned around, and the ingot is made the cathode. Next, redo the wiring so that the palladium ingot is attached to the negative pole of the DC power supply, and the piece of lead to the positive. Turn the juice back on and run between one and two amps of current for about 20 minutes. At first, the amount of hydrogen generated at the palladium ingot will appear small. This is because the Pd adsorbs hydrogen so well. After about five minutes of current passage, the whole surface of the ingot will freely bubble off hydrogen. After the 20 minute charging with hydrogen, begin magnetic stirring of the solution, and pour in about half of the ester reaction mixture from the large test tube. Adjust the current flow from the variable power supply so that a current of about 50 milliamps per square centimeter of palladium surface flows. If one has about six square centimeters of the ingot facing the piece of lead immersed in the solution, a current of about 300 milliamps is called for. This will result in some gassing off of hydrogen from the edges of the ingot, but over the rest of its surface the hydrogen will react before it bubbles off. The lead anode will form a brown layer of lead oxide, and will not dissolve at all in the sulfuric acid solution. Some surface particles will be kicked off the lead when it's first charging, but they don't make it through the condom. The lead anode can be replace with a piece of platinum if desired, but lead is a lot cheaper. Graphite is amother possibilty. Keep an eye on the current meter, as the current flow can change as the reaction progresses. Keep the current flow around 300 mA (0.3 amp) for the size ingot given in this example. When 1000 coulombs ( a coulomb is a unit of charge equalling one amp-second) have passed into the solution, add the other half of the ester reaction mixture from the test-tube., and continue at 300 milliamps until 3000 coulombs have passed through the solution. Let us use the 300 mA current to show an example of these calculations: At 300 milliamps, 1000 coulombs pass in 1000 / 0.3 Amps = 3333 seconds, or a little under one hour. 3000 coulombs pass in 10,000 seconds, or two hours, 45 minutes. 3000 coulombs per gram of feed material has been found to give good yields of a fine product, but by no means consider this number to be optimal. It may well be that a greater yield would be obtained by passing more current. It may also be that pseudoephedrine and PPA differ from ephedrine in their ease of electrocatalytid hydrogenation. I don't think that any harm can come from passing more current, within reasonable limits, so by all means experiment with the amount of current passed. During the course of thi reduction, the color slowly changes from its initially clear color to slightly tinted with yellow. It's not known whether this color change is due to some of the condom soaking out, or if it's a byproduct of the reaction. In any case, it's a remarkably clean reaction. When the desired amount of current has passed, the work-up and isolation of the product is very simple. The Kling-Tite condom is removed from the beaker. after pulling out (no pun intended) the lead electrode, the jimmy hat is, as is custom in some parts, flushed down the toilet. The anode can be used over and over. The palladium cathode is then rmoved and rinsed off. It too can be reused an INNUMERABLE (Bozakium's emphasis) number of times. The process of anodizing the palladium will have to be repeated prior to each run. Some fresh metal may have to be exposed on occasion by light sanding of the metal surface. An ingot of palladium should last for a lifetime. The reaction mixture should be poured into a sep funnel, and a 20 % NaOH solution should be added with shaking until the solution is strongly (13 + pH) alkaline to pH paper. Extract with two 50 to 100 mL portions of toluene. This should be plenty for one-gram of product. THe toluene extracts are then bubbled with dry HCl to get the crystalline hydrochloride product. After rinsing them off with some fresh toluene, they are spread out to dry. The most pleasantly surprising finding is that crank produced by this method doesn't give one the body and soul-wrenching hangovers so typical of the product made by the iodine-red phosphorous method.. This is a highly desirable way to keep one's own party rocking and rolling. If one should wish to produce more than a gram or so at a time, a larger palladium cathode should be used. Linking together more ingots of palladium would get pretty expensive, so a more economical alternative will be detailed. That alternative is electroplating some copper or brass screen with a thick coating of palladium. The simplest way to get this section of screen electroplated with palladium is to go to the yellow pages, look under electroplaters and find one who plates palladium. Ask for a plate build-up of several thousandths of an inch, so that enough Pd is deposited to last a while.. The Pd plated screen would then be used exactly like the ingot. First it must be anodized, then charged up with hydrogen in exactly the same way. The sole difference is that the greater surface area of the screen facing the condom-encased anode requires a correspondingly greater amount of current to be passed. Then, during the course of the reduction, again 50 milliamps per square centimeter of surface area facing the anode is used. The total of 3000 or so coulombs per gram of feed material doesn't change by increasing the size of the electrode. An alternative to this is plating the screen yourself, anodically dissolving a portion of the ingot to form a PdCl2 solution then..... sorry folks, this all of the manuscript I have, but I'm sure palladium plating is no national secret (yet). There is a company that sells an electroplating kit consisitin of a power supply, metal solution and a 'pen' electrode. As soon as I find their paperwork among my rubble I will post it. The lastest word from Fester is a couple of references from Indian journals on electroplating graphite electrodes with palladium, essentially giving a Pd black on C catalyst in the cell! 1) Krishnan, Electrochemica Acta, Vol 21, Pg 449-450 (1976) On the Electrochemical Reduction of Benzyl Cyanide to Phenethylamine with a Pd/C Electrode (note: The title may not be exact due to the illegibility of my chickenscratch transcription of my conversation with UF.) 2) Krishnan, Journal of Applied Chemistry, Vol 5, Pg 125-128 (1975) The greater activity of Pd on C (over straight Pd) results in a shorter reaction time. If anyone manages to find these references, please post them at the hive. I'd also be happy to answer anyone'e electrical questions, as long as you are not doing anything illegal of course. Enjoy. --- Bozakium
eQuine NewBee	posted 03-23-2000 07:35 PM Thanks Man! Awesome ! I couldnt find the book anywhere and have been to 3 large bookstores! Do you think we might rip the palladium coated pellets out of a catalytic converter? Ingots are kinda spendy. Iwas at a jewler the other night and he told me that all the palladium they ever mined would be the size of a small chair. This will be this bees next adventure!
malaci Hive Bee	posted 03-23-2000 07:52 PM Yea festers books are starting to get dropped by everyone nobody want to handle or carry them anymore.Make sure if you get that palladium it's not mixed with nickel alloy.Alot of people out their are now starting to fuck people around with palladium because of the price.
malaci Hive Bee	posted 03-23-2000 08:02 PM Scroll down to the first power supply the black 10amp that's what you want. http://www.jtz.com/mcart/index.cgi?ID=BQCACO&task=show&cat=Plating
Wizard X PimpBee	posted 03-23-2000 08:58 PM One guess who gave you the procedure beeach ?
malaci Hive Bee	posted 03-23-2000 09:15 PM I found a good way to test the ester to see if it is clean enough to work in the reduction.Take a few drops of the finished cooled ester and place them on a piece of glass if it turns to a oil forget it to much pill GAK.If it crystalizes your feed is pure enough then your good to go.
beeach Hive Bee	posted 03-23-2000 09:39 PM Hi Ya - Thanks for the info. I have a feeling that this procedure works as it was given to me by someone who KNOWS his shit. You know who you are and you are the fucking MAN! Anyway, I posted this as an alternative to using palladium. It is really expensive and the Fester formula only does 1 gram! There was also a way that used silver and what not, but I can't find it. Arrgh! One question for the Wizard - can the acetic acid that is used in the procedure that I listed (not Fester's) be from vinegar? Or does it have to be glacial? I love you Wizard! beeach
beeach Hive Bee	posted 03-23-2000 09:43 PM One more thing: Thanks for the link malaci. I used the search engine but there was not a lot of info on electrolytic reduction. Do you have info/posts using things OTHER than palladium (or platinum) or anything else that's really expensive? Love ya, beeach
malaci Hive Bee	posted 03-23-2000 10:08 PM That's where another problem comes in and that is buying palladium.I know it is very costly but it is worth it you'll always have it.The fester method has been tried with silver many times and it does not work unless you have a catalyts.I do think pt would work though but don't know for sure.Their is no limit on festers formula either it can be scaled up as big as you want to go if you have the stuff to do it with.This is not a cheap setup it's easy to spend $1,700 dollars on it like someone we all know has done.
malaci Hive Bee	posted 03-23-2000 10:14 PM I forgot to tell you that only Glacial acetic acid can be used.Why because water in the ester will reduce your yeild and you'll be lucky if you get anything back.
Nightbird Hive Bee	posted 03-23-2000 10:52 PM Wow MALACI! What a post (above)!Cool, thanks! Nb
badBoy Hive Bee	posted 03-23-2000 10:59 PM It is right off Rhodiums site. beechs was right off Wiz Xs' site. Has anyone had any luck getting into those pesky WiZxZips?
malaci Hive Bee	posted 03-23-2000 11:02 PM The write up does not belong to me it is not mine so no credit guy's.It was at the hive when i first started dreaming and somehow vanished so i thought i would put i back were it belongs for you guy's to see and learn.
malaci Hive Bee	posted 03-23-2000 11:16 PM It did not come off Rhodiums site it was posted at the hive before it made it's way to Rhodiums site.I think it's the same one though.I just have been going threw print outs of stuff on electro from last year and it seems alot of info is missing hear.
Wizard X PimpBee	posted 03-24-2000 12:14 AM badBoy: those pesky WiZxZips file are accesable ONLY by invitation. beeach: Only GAA as malaci indicated. malaci: the procedure beeach has proposed is NOT a catalytic reduction, you are NOT generation the H2 insitu, but an electrochemical reduction of the protonated benzylic hydroxy group.
AbSoLuTe Hive Bee	posted 03-24-2000 12:56 AM For your information Malaci Silver (Ag) does work, I do it often. There are a few tricks that U need to do to the PURE silver Shim BEFORE you anodize it. First, soak in 10% nitric for about 10 seconds to clean any shit off, rinse in DH2O place in a kiln and heat to around 850-900 Deg's Cent, or untill red hot, do not let it melt. Rapidly quench it in liquid Nitrogen, or if U dont have iot or cant steal some from the local Skin Cancer removal shop, then quench it in iced Brine. This will open up the Xtaline structure of the metal, almost to the level of Palladium. It will now absorb almost as much Hydrogen as the more expensive metal,Pd. Beeach, do a search for a post "Silver Dream Racing".
malaci Hive Bee	posted 03-24-2000 05:08 AM Yea AG does work and very hard but hear lately she has been having bad pains in her neck.She needs to quit worring about to many things at one time.I bet she lays in bed at night wondering what she should try next and this will cause stress.Take it easy Aqua-Girl it will all fall into place before you know it.I wish i had a pound of red phosphorus to give her because it would make her very happy.
badBoy Hive Bee	posted 03-24-2000 10:24 AM How do I get invited then, WiZ? I had plenty of chances to down those and now when I really need them I dont have them. waiting for an invitation to the big ball
Electro_Dreamer2 Hive Bee	posted 03-24-2000 04:37 PM You got to be fucking joking about the silver man.What or you going to use to reduce the ester silver black i don't think so.Have you read festers books if not you need to do so.I think that's fucking funny hey KrZ would you like some silver black for your master plan?You just don't seem to understand that the black oxide is what reduces the fucking ester do ya.Hydrogenation catalyts or pd pt and maybee nickel not silver.
beeach Hive Bee	posted 03-24-2000 09:57 PM Hi Ya - I was looking over the procedure as I await the supplies to arrive and was puzzled about a couple of things. As Wizard X pointed out this is not electrocatalytic hydrogenation so I am a tad confused. 1. After forming the ester via 10g of ephedrine + 100ml GAA + 1ml H2SO4 heated at 80C, this all goes into the clay cooler and additional dilute H2SO4 is added. The clay cooler or CHIA HEAD is in the center of the bucket. Isn't this the anolyte then? I thought that what was to be reduced would go into the catholyte (in the bucket) part. What's the deal? 2. Does a piece of glass need to be added to the cell for underneath the CHIA HEAD/clay wine cooler? In Wizard X's electrolytic nitro reduction file, there was a picture with a 1cm glass piece used. 3. How long would the rxn time be? The person who helped me correct everything said that 5 hours seems a bit long. So how long should I do it? 4. At the end of the reaction, the contents of the clay wine cooler are dumped out, concentrated or evaporated, and then simply dissolved in Toluene, dried, and gassed. Right? So how 'bout some help Wiz? Thanks and love, beeach
JackP NewBee	posted 03-25-2000 02:07 PM how about acetic anhydride w/ colbalt chloride catylist? is there any difference between ephedrine and ppa as far as electro is concerned?

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