Preparation of Cuprous Chloride -RatHead , Hive Novel Discourse


		dormouse (Member) 04-20-00 01:37 No 108306				Preparation of Cuprous Chloride -RatHead	Bookmark
						the Hive BB Novel Discourse Preparation of Cuprous Chloride profile \| register \| preferences \| faq \| search next newest topic \| next oldest topic Author Topic: Preparation of Cuprous Chloride RatHead unregistered posted 04-27-98 10:18 AM -------------------------------------------------------------------------------- Preparation of Cuprous Chloride. In a 100-mL. round-bottom flask, prepare a solution of 6 g. (0.002 mole) of powdered copper sulfate crystal (5-hydrate) and 1.8 g. of sodium chloride in 20 mL. of hot water. in a beaker prepare a solution of 1.4 g. of sodium bisulfite and 0.9 g. of solid sodium hydroxide in about 1.4 mL. of water, and add this solution to with swirling to the hot copper sulfate solution over a period of 5-10 min. Cool the mixture to room temperature, allow the cuprous chloride to settle, and decant off the liquid. Wash the precipitated cuprous chloride 2 or 3 times with water by decantation. The cuprous chloride is obtained as a white powder that darkens on exposure to air. Dissolve the cuprous chloride solution as (HCuCl2) by adding 7 mL. of concentrated hydrochloric acid and 2.5 mL. of water. Cork the flask to minimize oxidation and place in an ice bath. An alternative procedure is to dissolve 2.0 g. of commercial cuprous chloride in 7 mL. of concentrated HCl and 2.5 mL. of water. sunlight Member posted 04-28-98 02:45 AM -------------------------------------------------------------------------------- I prepared cuprous chloride by mixing copper wire, CuCO3 and a excess of comercial 20 % HCl and warming it near boiling point until all copper was dissolved. It was the deposition of a white powder (cuprous chloride). This product can't be dried because it oxydizes quickly, it was washed with water. Normal reaction is with copper wire or powder, CuCl2 and HCl, but I had then CuCO3. Also cupric chloride was prepared by reacting a solution of CuCO3 with an slightly excess of HCl, then evaporating water and finally, when product starts to turn brown, air dried to give a hydrate form. Cupric chloride has a beatiful green, like smerald, don't it ? Everyman Member posted 08-06-98 09:11 AM -------------------------------------------------------------------------------- Sorry to drag up an old post but I thought it was relevant. I have tried Ratheads synth above (using Metabisulphite and very badly estimated quantities) and it worked fine, precipitating a fine white insoluable powder which turned green when oxygenated in an SRV with MeOH. Heres a procedure for producing CuCl and CuCl2 from copper metal, nitric acid being the only non-OTC ingredient : http://chemistry.rutgers.edu/genchem/CuCl.htm Everyman Member posted 08-06-98 09:11 AM -------------------------------------------------------------------------------- Sorry to drag up an old post but I thought it was relevant. I have tried Ratheads synth above (using Metabisulphite and very badly estimated quantities) and it worked fine, precipitating a fine white insoluable powder which turned green when oxygenated in an SRV with MeOH. Heres a procedure for producing CuCl and CuCl2 from copper metal, nitric acid being the only non-OTC ingredient : http://chemistry.rutgers.edu/genchem/CuCl.htm Piglet Member posted 08-06-98 09:24 AM -------------------------------------------------------------------------------- I have got this stuff in the UK & Netherlands. Both times I went to a chemist (Apoteik) and ordered it without incident. Said it was for photography. Thought I would mention it because it's 1 less variable if some reaction doesn't run... Piglet Piglet Member posted 08-06-98 09:24 AM -------------------------------------------------------------------------------- I have got this stuff in the UK & Netherlands. Both times I went to a chemist (Apoteik) and ordered it without incident. Said it was for photography. Thought I would mention it because it's 1 less variable if some reaction doesn't run... Piglet ChemHack Member posted 12-21-98 03:31 AM -------------------------------------------------------------------------------- Copper Carbonate mixed with pink Zinc Chloride solution (welding reflux) yielded clear solution with green precipitate settling on the bottom. Zinc Chloride is water soluable. Copper Carbonate is water soluable. Copper(II)Chloride is water soluable. Copper(I)Chloride is NOT water soluable. So I'm guessing the precip is Copper(I)Chloride... Anyone ? Cherrie Baby Member posted 12-21-98 10:19 PM -------------------------------------------------------------------------------- I don't know a lot about chem. but I know that copper carbonate is not water soluble. dpHarma Member posted 12-21-98 10:38 PM -------------------------------------------------------------------------------- Simplest synth for CuCl2 came from Rhodium (I think) and is simply adding copper sulfate soln' to calcium chloride soln' while stirring, until no more cloudy ppt. forms, then evaporating the water and dehydrating the very deliquesent green salt until it's brownish white. dpHarma Osmium Member posted 12-22-98 04:24 AM -------------------------------------------------------------------------------- No, it was my idea ChemHack Member posted 12-22-98 04:09 PM -------------------------------------------------------------------------------- Yeah, that was Osmium's idea but I have something to add... If you simply add until no more precipiate then you will almost certainly have quite a bit of CaCl2 left dissolved in the water. Then you evaporate the liquid and everything looks fine. Store it in a plastic baggy and everything looks fine. Leave it out on a plate for a couple of days and it turns to bluegreen mush as the CaCl2 soaks up a buttload of atmospheric water! The best thing to do IMHO is to actually WEIGH the reactants before making the solution so that you can adjust the molar equivilants up front. Cherrie Baby: You are right about the Copper Carbonate not being water soluable. I don't know what I was thinking... Anyway the precipitate that I mentioned above is Blue, not green. I was getting my beakers mixed up. I am fairly sure that "something" happened because the pink is all gone and the greenish carbonate turned blue. dpHarma Member posted 12-27-98 11:07 AM -------------------------------------------------------------------------------- Only prob w/ weighing Calcium chloride is arriving at it's real state of hydration. fusing and heating til no more water vapour comes off then cooling and powdering in an anhydrous atmosphere is a lot of work dpHarma ChemHack Member posted 12-28-98 10:17 AM -------------------------------------------------------------------------------- Yeah but it is easy enough to make a "mostly anhydrous" amount. Heat the hell out of it and then pulverize it while it is still hot. Put it back under the heat for a bit and then go from there directly into a plastic baggie. The anhydrous powder is brown so it isnt very hard to tell when it has soaked up water.. dpHarma Member posted 01-06-99 09:18 AM -------------------------------------------------------------------------------- The anhydrous form of 'calcium chloride'??? is 'brown'? I don't think so. you must mean the cupric chloride. dpHarma ChemHack Member posted 01-06-99 01:53 PM -------------------------------------------------------------------------------- I was talking about Cuprous Chloride. You were talking about Calcium Chloride! Doh! I didn't read carefully. Shame on me! Regardless, I still think that it is very much worth your time to weigh the reactants. Pour the DampRid CaCl2 onto a cookie sheet and bake it in the oven. You can actually notice the reduction in size of some of the little pellets. Take them out and pulverize them while they are hot so they are nice and crunchy and then spread the powder back out on the cookie tray for another round of baking. I found that starting out with about 50% more DampRid than you need CaCl2 by weight is a good idea because it will lose a significant amount of water. -------------------------------------------------------------------------------- If you plan on doing a Wacker, it might be better to buy the shit from the chem supply house than to make it yourself even though it is so easy to make. The reason that I say this is that some people have reported with using Sodium Palladium Chloride instead of regular PdCl2. Someone posted that results were still poor even when adjusting for molarity. If this is true then perhaps the addition of NaCl hinders the reaction in some way. (Bright Star?) Making your own in this way will ultimately results in either extra CaCl2 or extra CuSO4 floating around. I don't KNOW that this would make a difference. Only speculating that it MIGHT. Also, the Copper Carbonate from the ceremics supply house is probably nowhere near "pure" and if it is used in conjunction with hardware store HCl there will undoubtedly be some amount of "other" stuff floating around in there... Hey Spiceboy, have you had any problems with the SRV using CuCl2 formed by this technique? ChemHack Member posted 01-06-99 01:59 PM -------------------------------------------------------------------------------- Oh by the way, the extraction of Copper Sulfate from that sparkly shit you throw in the fireplace for colored flames is a major pain in the ass to purify. The Home Depot sells Copper Sulfate crystals as "root killer" for septic systems. Our friends at "Instant Power" (the same people that make sulfuric drain opener) sell the root killer for ~$6/lb but there is another product in the same section (forgot company name) that is twice as much for only $1 more $7/2 lbs. The ingrediants label says 99% Copper Sulfate Pentahydrate. The crystals are blue and beutiful! Orpheus Member posted 01-19-99 08:12 PM -------------------------------------------------------------------------------- Here's my dream.. 1/2 tsp cacl2(damp rid) No Scale :-( 1.5 tsp Copper Sulate 5-hydrate (root kill) 350 ml HOT water Put in a 600 ml beaker with stirring( plastic straw) turned very cloudy light blue upon disolving everything.. let sit for maybe 10 min.. had a pure white silt on bottom and a sky blue clear overhead.. decanted off most of the liquid (tried filtering with doubled up coffee filters to an aggrivated failure) poured into Al foil sitting in a frying pan with about 2" of water in it. turned on the range top.. sizzling was heard.. and brown stuff emerged.. I thought Oh Shit.. it's eating the foil. paniced.. dumped the rest of the liquid in to the sink drain and looked at the foil.. it had a layer of brown shit covering it. upon moving it i noticed the foil was unscathed!!.. it was just dehydrating ( i think, because it was still wet to the touch) stuck the whole mess in the oven and baked at 225 for 20min or until dry brown.. is this CuCl2??? i havented tested to see the color change yet.. but the left over crud in the beaker was turning blue.. any ideas?? ------------------ Sweet Dreams -Orph- Orpheus Member posted 01-19-99 08:14 PM -------------------------------------------------------------------------------- Oh after about 20 min the shit in the oven started turning white again.. thought i'd let you know ChemHack Member posted 01-20-99 04:24 AM -------------------------------------------------------------------------------- I should point out that the CaCl2 + CuSO4 produces CuCl2, that is CUPRIC CHLORIDE not CUPROUS CHLORIDE as is stated in the title of this document... Orpheus Member posted 01-20-99 09:26 AM -------------------------------------------------------------------------------- Ok that's good.. but i did wonder about the success i had ( or lack there of) after i put about a 1/2 tsp in with about 100ml IPA and ran it in the wacker..( just the Alc. and Cucl2) .. pressurised to 40psi.. shook the hell out of it for 10min.. it turned pink. i think i still messed this up.. but i'll try it again.. i still have like 2lbs of CaCl2 and CuSO4.. looks like i need a second run.. ( with better equipment obviously) Thanks tho ------------------ Sweet Dreams -Orph-