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	All 71 posts	Subject: Recycling of HI + new RP substitute		Page: First Last



Rhodium (Chief Bee) 08-10-02 05:22 No 344011	Recycling of HI + new RP substitute (Rated as: excellent)	Bookmark Reply
	Here is a document which goes into detail on how to sustain a HI reduction of alcohols with continous recycling of formed I₂ back to HI, using aqueous phosphorous acid (H₃PO₃) as recycling agent instead of the watched Red Phosphorus/Hypophosphorus Acid. I have never heard of anyone using phosphorous acid for this purpose before, have I missed something or is this a completely novel idea? H₃PO₃ costs only around $40/kg, but it does not readily regenerate HI from I₂ at room temperature (but easily at the boiling point of an aqueous solution), and I believe that is the reason they have forgotten to schedule it, its functionality is not directly obvious to non-chemist meth cooks, and therefore its popularity has been as low as not alerting the DEA, and they most likely didn't think of it either. Partial reactions Ephedrine + 2 HI -> I₂ + H₂O + Meth H₃PO₃ + H₂O + I₂ -> 2 HI + H₃PO₄ Overall reaction Ephedrine + H₃PO₃ --I₂--> H₃PO₄ + Meth The overall reaction is simply phosphorous acid being oxidized to phosphoric acid and Ephedrine reduced to Meth, while any added HI or I₂ is just recycled in the reaction. Their preferred molar ratio between ephedrine/HI/H₃PO₃ is 6:9:5, and with their molar weights being 165.24:127.9:82.0 (ephedrine considered freebase and HI a 57% solution), the mass ratios are the following: 9.9g Ephedrine freebase 20.2g 57% HI(aq) 4.1g H₃PO₃ If you want to use I₂ instead of 57% HI, use the amounts below: 9.9g Ephedrine freebase 10ml Water 11.4g Lab Grade I₂ 11.5g H₃PO₃ Experimental suggestion: In a 250ml Round-bottomed flask with a 24/40 ground glass neck, carefully add the phosphoric acid with good stirring to the water (exothermic!), then the finely powdered lab grade I₂ is added, followed by the ephedrine freebase. The flask is fitted with two sequential Friedrich condensers with ice water running through them to compensate for the vigour of the following reaction. With good stirring, the reaction mixture is placed in an oil bath (or heating mantle) and slowly heated to reflux temperature with vigorous magnetic stirring. At about 100°C a powerful exothermic reaction sets in and frothing commences, and after a while you will attain the reflux temperature of ~118°C. The reaction mixture was refluxed overnight, cooled and worked up as usual. Reference: Org. Proc. Res. Dev., Vol 3, No 5, 352-356 (1999) (http://www.rhodium.ws/pdf/hydriodic.recovery.pdf)



foxy2 (Distinctive Doe) 08-10-02 05:34 No 344014	They didn't schedule it cause nobody knew.	Bookmark Reply
	I have never heard of anyone using phosphorous acid for this purpose before, have I missed something or is this a completely novel idea? Yes its novel. I don't know of anyone who has used it. But I do know someone who has seen various references analogous to the one you posted. They were going to try it sometime. Rhodium You just opened the floodgates!!! Those who give up essential liberties for temporary safety deserve neither liberty nor safety



lugh (Moderator) 08-10-02 05:43 No 344017	Differences	Bookmark Reply
	Note that the researchers used two Freidrichs condensers to control the very exothermic reaction, and that a nitrogen atmosphere was used



foxy2 (Distinctive Doe) 08-10-02 06:01 No 344019	hehehe	Bookmark Reply
	Now that I ask him, my friend had that ref. and this patent. They are pretty much the same. Patent US5516960 Those who give up essential liberties for temporary safety deserve neither liberty nor safety



wareami (Hive Addict) 08-10-02 06:14 No 344023	LughLughLugh!	Bookmark Reply
	Lugh:Always bursting my balloon with exothermic atmospheric considerations! Rhodium:Thanx for checking into this route. Ibee had run into some facts while researching a post by aquagirl in AquisitionForum regarding List Schedules of HypoPhos! It was unclear as to whether aqueous phosphorous acid had the properties necessary for a reduction. He's tried researching the chemistry books available at the time and only came up with info related to the differences between Phosphorus and Phosphrous. I also believe Scottydog had inquired through PM about phosphorous acid a while back, but in Ibee's mind...Geez, Mnkyboy, and WizardX were the experts concerning the phosphoric routes! Foxy2:Yes! I believe SWIF2 might be right about the Floodgates! Peaceof the ^reaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami



morpheus (Hive Bee) 08-10-02 13:51 No 344119	recycling	Bookmark Reply
	Five stars Rhodium! Guess it shows why your chief bee My nomination for my newly created 2002 Avagadro award goes to you.



Psalty (Stranger) 08-10-02 15:09 No 344153	This would be significantly more OTC than rp or ...	Bookmark Reply
	This would be significantly more OTC than rp or hypo. A quick search of phosphorous acid sources reveils that its potassium salts are used in fertilizers as an alternative to phosphates in NPK formulations. Having one less oxygen molecule than phosphate, phosphite has a much higher degree of solubility and mobility in the membranes of plant foliage and roots, making it more readily absorbed by plants. Hmm... Looks like yet another fertilizer may be stigmatized by its clandenstine uses. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



Rhodium (Chief Bee) 08-10-02 16:40 No 344180	The meth bunny	Bookmark Reply
	That sounds really good. As no iodine is ever consumed in this reaction (only converted into iodide), it can be recycled indefinitely by the aid of hydrogen peroxide oxidation of the aqueous mother liquors gotten after extracting your product. If Phosphorous acid salts are as abundant as you say, this invention can really become a perpetuum mobile of meth synths. More Phosphorous acid info: http://www.biagro.com/chemdiff/



BenWiFFen (Line Monitor) 08-10-02 17:00 No 344185	Close but no...	Bookmark Reply
	BenWiFFen: ""EVERYMAN's" HI" (Newbee Forum) Close but no doobee. Sign here____________________



Scottydog (Hive Bee) 08-10-02 18:59 No 344221	Swis may be wrong as usual but in other words, ...	Bookmark Reply
	Swis may be wrong as usual but in other words, the lower voltage electrolysis application that hypo was discussing at the end of Lugh's thread lugh: "Hypophosphoric Acid Synthesis" (Acquisition Forum) might have functionality as a starting point to obtain the necessary phosphorous acid? In this thread Swis asked if HCL could be used as an electrolyte and Hypo said it would result in phosphoric acid. Will phosphoric work as well as the phosphorous acid? Are they one and the same and if not can someone please explain the difference? It would be so beautiful to start from scratch. (Electrolysis) For fun and education sake. Considering this acid is not regulated, Swis understands that this caveman electrolysis is not totally necessary. Using the low voltage electrolysis and a dilute solution of H2SO4 as the electrolyte, Hypo says that the end result would also contain hypophosphorous acid. Would the small amount of hypo acid interfere with using H3PO3 as the recyclant in this newly revealed process or would it further help in the reduction? Swis likes to turn a molehill into a mountain. So much info to ingest that Swis' brain is about to explode. It is obviously easier to just buy the H3PO3. On another note Swis notices this method calls for the addition of water. H3PO3 comes available in solution in concentrations listed at 85%/15% water. Can this theoretically be used "as is" without actually adding h2O to the mix? Is Swis on track or is he still confused by the ic/ous endings? God its getting deep around here. Forever learning! Thanks Rhodium... ___________ Refuse/Resist



PrimoPyro (Hive Prodigy) 08-10-02 19:09 No 344224	Buy It	Bookmark Reply
	Just buy the acid while its available. It isnt expensive. You might get confused on the ic/ous endings because lots of people fuck them up and state them wrong. There are no such things as hypo_______ic acids or per______ous acids. From lowest oxidation state to highest, the possibilities are: Hypo______ous acid ______ous acid ______ic acid Per______ic acid So for chlorine oxyacids, you have hypochlorous acid, HOCl, chlorous acid, HOClO (or HClO2), chloric acid, HOClO2 (or HClO3) and perchloric acid, HOClO3 (or HClO4) Just about always (I cant think of a single exception, but Im covering my ass anyway) the number of hydrogens stays the same for all oxyacids of the same central species, only the number of oxygens vary. Ah, one exception would be hyponitrous acid, there. PrimoPyro



blondie (Hive Bee) 08-10-02 19:49 No 344236	phosphorous acid	Bookmark Reply
	if the salt was available how would you go to the acid?



foxy2 (Distinctive Doe) 08-10-02 20:20 No 344255	Coming Soon	Bookmark Reply
	Hold tight blondie. It will either bee here soon or really early in the morning tomorrow. The salt is WIDELY available right now. Pick up a 55gallon barrel while you can. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



wareami (Hive Addict) 08-10-02 20:36 No 344263	ESEE description!	Bookmark Reply
	Scotty: The easiest description in the difference between the spelling suffixes...-us and the -ous is: The element ends in -us and the +3 compounds end in -ous. Chemical Principals and Properties Second Edition Peaceof the ^reaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami



Psalty (Stranger) 08-10-02 20:36 No 344264	Titrate your salt with a strong acid, such as ...	Bookmark Reply
	Titrate your salt with a strong acid, such as HCl, to convert back to the acid. KH2PO3 + HCl ---> KCl + H3PO3 pKa = -7 pKa = 1.5 Separating the KCl from the H3PO3 wouldn't bee too difficult. H3PO3 is very soluble in EtOH but KCl is considered insoluble in EtOH. So, one could boil of the water after the titration, add EtOH to the solid mass, stir vigorously, and then decant the supernatant leaving the KCl behind. Alternatively, one could perhaps exploit the great differences in the melting points of KCl and H3PO3. KCl melts at >700C while H3PO3 melts at around 74.7C. You could heat the solid until the H3PO3 melts and then remove the liquid H3PO3 somehow. Someone please correct me if I'm wrong, or if these procedures have some inherent dangers that I've omitted. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



foxy2 (Distinctive Doe) 08-10-02 22:27 No 344275	Salty	Bookmark Reply
	Your a bright cookie. And a smart chemist to. The only possible problem might bee the inerts which are bound to bee in fertilizer grade KH2PO3. I wonder what those inerts would typically bee? o-Phosphorous Acid - MSDS DATA (100%) B.P. Text: 392F,200C M.P/F.P Text: 165F,74C Spec Gravity: 1.7 Solubility in Water: 30% Appearance and Odor: WHITE OR YELLOWISH HYGROSCOPIC CRYSTALLINE MASS. Stability Condition To Avoid: FLAMMABLE, POISONOUS GASES MAY ACCUMULATE IN TANKS AND HOPPER CARS. Materials To Avoid: VIOLENT RXN W/BASES &/OR OXIDIZERS. REACTS EXOTHERMICALLY W/WATER. CONT W/ACETIC ACID RELS FLAMM PHOSPHINE. (ING 2) Hazardous Decomposition Products: THERMAL DECOMP PROD INCLUDE HIGHLY TOXIC OXIDES OF PHOSHOROUS, FLAMM HYDROGEN AND PHOSPHINE GASES. Handling and Storage Precautions: MAY BURN BUT DOES NOT IGNITE READILY. FLAMMABLE, POISONOUS GASES MAY ACCUMULATE IN TANKS AND HOPPER CARS. Other Precautions: MAY IGNITE COMBUSTIBLES (WOOD, PAPER, OIL, ETC). http://www.setonresourcecenter.com/HMIS_Msds/096/BNBGF.HTM Someone want to get this Journal Article, I don't have access to this one. Its a review of the preparation and reactions of H3PO3 and H3PO2. Tervalent phosphorus acids. Dahl, O. Organophosphorus Chem. (1991), 22 87-113. ISSN:0306-0713. Abstract A review contg. 97 refs. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



PrimoPyro (Hive Prodigy) 08-10-02 22:40 No 344277	Man.....	Bookmark Reply
	I find myself recommending chemical suppliers more and more and more lately to people struggling with scraping chemicals from OTC sources and wondering wtf is in them. This chemical is not illegal, not watched, and is relatively inexpensive. On top of that, you know some good reasons it's used for in case someone were nosy enough to ask. What is holding you back from just calling up a chemi company and ordering a 1kg "sample" followed by a 10kg order for your crops? If they want you to set up some sort of account, do it, its almost always free. Fuck, its so easy I cant stress how easy it is with words. And once you have an account set up, the only question you'll ever get when you make an order is, "Do you have an account with us, Sir?" And you just say yes, it is under ____ ____. Whatever accounts you set up will be for NONSUSPICIOUS chemicals, though. You buy your suspicious chems with a Fake ID and an Anonymous Credit Card, a la MaDMAx. (UTSE) Trust me, its easy as pie, and you'll get so much better results. PrimoPyro



alphacentauri (Stranger) 08-11-02 02:04 No 344299	About H3PO3 purchase	Bookmark Reply
	H3PO3 comes available in solution in concentrations listed at 85%/15% water, you say. Now what is the industrial/analytical use of this stuff? I mean, when you ask for it, you'd better have in mind a ready innocent explanation, even if it's not yet watched. What about the preservation of these solutions? Can they be stored up for long without decomposition or losing their Normality? Thanks a lot.



foxy2 (Distinctive Doe) 08-11-02 02:28 No 344306	H3PO3, phosphorous acid (Rated as: excellent)	Bookmark Reply
	Ok Pyro You are now my purchaseing agent. Thanks for volunteering! Preparation of high-purity phosphorous acid. Patent JP03028115 Abstract High-purity H3PO3 is prepd. by adding H2SO4 to CaHPO3 contg. sludge obtained as byproduct in NaH2PO2 manufg. process, removing formed CaSO4 to give crude H3PO3 soln., selective extg. H3PO3 with org. solvent, such as n-butanol and isobutanol, and countercurrent contacting with H2O in a multistage extn. app. The extn. app. is composed of extn., 1st and 2nd purifn., and recovery sections. HCl is added in the extn. section and org. solvent is recycled in the extn. process. A portion of the aq. H3PO3 from the recovery section is used for extn. of alkali metal impurities from the org. phase in the 2nd purifn. section and added with aq. alkali metals for the extn. of SO42- impurities from the org. phase in the 1st purifn. section. Phosphorous acid. Patent US4278647 Abstract Na3PO3 solns., contg. P 1-12 and Na2O 1-50% and obtained as a waste from the manuf. of PH3 by treating white P with NaOH, are used. The Na3PO3 solns. are satd. with HCl to ppt. NaCl and sep. a Na-free soln. of H3PO3 in HCl. Thus, 500 g of a waste soln. of Na3PO3 contg. P 9.3 and Na2O 17.3% was satd. under cooling with 40L HCl/h, and the NaCl ppt. in an amt. of 176 g was removed to obtain a filtrate with 22.4% H3PO3 and only 0.038% Na2O. Phosphorous acid from industrial waste material containing phosphites. Patent US4330515 Abstract H3PO3 is prepd. from phosphites in industrial wastes. A strong inorg. acid that will remove the cation of the phosphite is added to dissolve the waste. Also, a soln. of the phosphite in H3PO3 is passed through a cation-exchange resin to form a H3PO3 soln. Thus, a mud contg. Ca phosphite was dispersed in a H3PO3 soln. H2SO4 was added to ppt. all the Ca2+ as gypsum. The conversion of Ca phosphite was 99.2%. A typical waste is that formed in the manuf. of Na hypophosphite. Pure phosphorous acid. Patent DD206363 Abstract Pure H3PO3 for the synthesis of organophosphorus compds. is prepd. from P4O6 and H2O at a mol ratio £1:6.5 in an inert gas atm. The conversion is carried out at 50-70° and 100-300 rpm in the presence of activated C preheated at >500° in air. The amt. of activated C is 0.05-1% to that of P4O6. Thus, 220 parts of P4O6 was dripped in a suspension of 117 parts H2O and 0.22 parts activated C preheated at 1000° for 1 h. The P4O6 was added under stirring at 250 rpm until the temp. reached 112° followed by cooling the reaction mixt. to .apprx.70° and addn. of the remaining P4O6. After completion of the conversion (.apprx.15 min), the soln. was filtered and the supersatd. filtrate was crystd. to obtain >99%-pure H3PO3 crystals contg. 37.7% P(III). Corrosion resistance of materials in phosphorous acid production media. (Some russian report) Economically alloyed stainless steels, such as 08Kh22N6T [12661-77-7] and 08Kh21N6M2T [12661-69-7], etc., were tested for corrosion resistance in H3PO3 manufg. media. Oxidn. of hypophosphite ion to phosphite ion in highly alk. media was employed in prepn. of H3PO3. Different steels acceptable for manuf. of app. used in the subsequent stages of H3PO3 manuf. were selected. The above stainless steels were the most resistant at 90° in alk. media of Na hypophosphite oxidn. The high-alloy steel 06KhN28MDT [12661-60-8] was suitable during H3PO3 concn. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



RepVip (Newbee) 08-11-02 03:03 No 344312	TSP - Trisodium Phosphate	Bookmark Reply
	Trisodium Phosphate is readily available at hardware stores as a degreaser, at least in my area. Also: Usage: used as softener, washings, detergent of boiler, rust handling agent, scavenger of molasses, dryer of dye intermediate, developer of photograph, fabric mercerization agent, coagulation agent, rubber latex and medical preparation. However, TSP is Na3PO4 • 12H2O. Originally, I was thinking it could be used as Psalty suggested with KH2PO3, converting it into H3PO3. And then I realized it was Na3PO4 and not Na3PO3. I suppose you could make a salty solution of phosphoric acid.. but this helps none because it is not phosphorous acid Is it not possible to convert from phosphorous to phosphoric? Well, as Scottydog said, "It is obviously easier to just buy the H3PO3." Using the 85%/15% phosphorous acid solution is most interesting to me!



Psalty (Stranger) 08-11-02 04:03 No 344321	You could always say that your using it because ...	Bookmark Reply
	You could always say that you're using it because you make you're own NPK formulations for hydroponics purposes, and then also purchase some urea while your at it. But then again, that may raise some suspicions too. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



Rhodium (Chief Bee) 08-11-02 05:56 No 344334	Phosphorus/Phosphoric Acid FAQ	Bookmark Reply
	Please read this carefully, it seems like half of you haven't understood the basics: Phosphoric acid is H₃PO₄ and that is what is sold as an 85% aqueous solution. The salts are called phosphates, and include TSP, which is Na₃PO₄. This is NOT the acid we are looking for, phosphoric acid cannot reduce anything. Phosphorous acid is H₃PO₃, and is a crystalline solid. Its salts are called phosphites, and are used as fertilizers. This is the acid we want. There is no practical way of turning other chemicals into phosphorous acid, so the only realistic option is to either aquire pure phosphorous acid, or an alkali phosphite (sodium, potassium or calcium phosphite for example) and treat the salt with acids, as in foxy2: "H3PO3, phosphorous acid" (Stimulants). If you were to aquire a mixture of phosphorous acid (H₃PO₃) and hypophosphorous acid (H₃PO₂), then that mixture could definitely be used directly in this synthesis, but you would have to re-calculate the amount needed to perform the reaction, depending on the ciomposition of your acid mixture. H₃PO₃ is able to recycle one I₂ molecule to 2 HI, while H₃PO₂ can recycle two I₂ molecules to 4 HI. Please note that there should always be a certain amount of water present in the (pseudo)ephedrine reduction reaction, and that the mixture should be refluxed overnight to give satisfactory results. This procedure is not suitable for "dry reaction" stunts, you will have to reflux the aqueous solution. The reaction can much likely be optimized further for a specified substrate like pseudoephedrine (the original reference was aimed at generic aliphatic polyalcohols), BUT, before trying to substitute anything or change the reaction conditions, run the reaction exactly as I outlined above, record the yield and purity, and then change reaction parameters, one at a time, such as increasing/reducing the reaction time, or the relative amount of water/phosphorous acid/iodine/HI. Do not run any large-scale experiments before the method has been perfected, stay at a batch size of 10g or below, preferably about 2.5-5g for economical reasons. Do not sell or give away any product of this reaction before we have uneqivocally established that the product is pure d-methamphetamine without any impurities like iodoephedrine or unreacted starting material.



VideoEditor (Hive Bee) 08-11-02 07:09 No 344365	Clarifying	Bookmark Reply
	Checked my supplier and they had it listed two ways: Phosphorous Acid Crystal PAC Phosphorous Acid, 70% Solution We definitely want the crystal right? No benefit in the solution? Real Men Don't Preview Their Edits



wareami (Hive Addict) 08-11-02 07:23 No 344370	Water Water Everyware!	Bookmark Reply
	VE: The only benefit in the 70% would be: No need to add h2o to the rxn! Peaceof the ^reaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami



Psalty (Stranger) 08-11-02 07:27 No 344373	The crystal is preferable; that's the reagent ...	Bookmark Reply
	The crystal is preferable; that's the reagent Rhodium and the paper mentioned. It costs less too. With the 70%, you have to pay for their water + the extra weight that the water adds to the shipping (I'm assuming you are referring to an aqueous solution). The uncertainty in the solution's concentration may bee a concern as well. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



VideoEditor (Hive Bee) 08-11-02 09:32 No 344396	some mo' info	Bookmark Reply
	Real Men Don't Preview Their Edits



OCD (Stranger) 08-11-02 12:03 No 344416	related ref (for H3PO2)	Bookmark Reply
	Tetrahedron Letters 42 (2001) 831-833 Hypophosphorous acid-iodine: a novel reducing system. Part 2: Reduction of benzhydrols to diarylmethylene derivatives Part 1 discussed reduction of diaryl ketones accept responsibility



Rhodium (Chief Bee) 08-11-02 13:43 No 344446	Hypophosphorous acid¯iodine: a novel reducing ... (Rated as: excellent)	Bookmark Reply
	Hypophosphorous acid¯iodine: a novel reducing system. Part 2: Reduction of benzhydrols to diarylmethylene derivatives Tetrahedron Letters Volume 42, Issue 5, 29 January 2001, Pages 831-833 Apart from its use as for reductive deazoniation of diazonium ions,[1] there are few reports of the use of hypophosphorous acid (H3PO2) as a reagent in organic chemistry.[2] By the same token, there are not many reports of hydrogen iodide as a reducing agent for organic compounds. [3, 4, 5, 6, 7 and 8] We recently reported that a mixture of hypophosphorous acid and iodine (the latter in catalytic amounts) in refluxing acetic acid is an efficient reducing agent for diaryl ketones. [9] Fluorenone, dibenzosuberone, and a variety of substituted benzophenones were reduced to the corresponding methylene derivatives in 97¯100% yield. We now report that a wide variety of benzhydrols bearing both electron-withdrawing and electron-supplying groups are reduced to the corresponding diarylmethylene derivatives very cleanly and in high yield ( Table 1) (Eq. (1)) by this reagent system. The diarylmethylenes are isolated in pure form (NMR and GC¯MS analysis) after a simple workup. This procedure is competitive in terms of ease, cost, and yield with previous methods for deoxygenation of benzhydrols, including lithium¯ammonia,[10] Fe(CO)5,[11] diiododimethylsilane, [12] zinc iodide¯sodium cyanoborohydride, [13] triphenylsilane in trifluoroacetic acid¯methylene chloride, [14] sodium borohydride¯trifluoroacetic acid, [15] iodine¯acetic acid¯red phosphorus, [16] and lithium aluminum hydride¯aluminum chloride. [17] Acetic acid is the preferred solvent for these conversions: reduction was slow or negligible in chloroform or benzene, and conversion of the benzhydrol to the corresponding methyl ether was observed in methanol. The ether was however slowly converted to diphenylmethane upon continued reaction. Reduction occurred in quantitative yield in almost every case. 4-Methoxybenzhydrol underwent cleavage of the O-methyl group and partial esterification of the phenolic group under the reaction conditions (run 3); similar behavior was observed previously with 4-methoxybenzophenone.[9] Hydrogenolysis of halogen atoms was observed during reduction of 4,4-diiodobenzhydrol (run 12), but not with 4-bromo- or 4-chlorobenzhydrol or 4,4'-dichlorobenzhydrol. Benzyhdrols containing nitro or ester groups were not investigated; it is known that nitro compounds are reduced by hydrogen iodide [18] and we have found that esters are hydrolyzed (not reduced) under our experimental conditions. We are exploring methods to avoid this. The actual intermediate in these reductions is probably the carbocation formed by protonation of the alcohol. Consistent with this hypothesis, benzhydrols bearing strongly electron-withdrawing groups are reduced noticeably more slowly than benzhydrols bearing electron-supplying substituents (runs 6, 7, 12, and 13). However, sampling of a 1:1 mixture of 4-methyl- and 4-bromobenzhydrol over a period of time showed that the two substances were reduced at about the same rate. The tertiary alcohols triphenylcarbinol and 1,1-diphenylethanol were reduced more readily than benzhydrol, which is also consistent with the rate of carbocation formation being the key factor in ease of reduction. A competing reaction during the attempted reduction of 4,4'-bis[dimethylamino]benzhydrol was cleavage to a mixture of 4-dimethylaminobenzaldehyde and dimethylaniline (run 8), presumably by hydrogen iodide; an old report showed that the same cleavage can be effected by hydrogen bromide.[19] The reaction is curious in that it is most readily understood as proceeding through initial ring protonation of 1, presumably facilitated by the para-dimethylamino group (Scheme 1). Selectivity: We previously reported that reduction of substituted benzophenones to the corresponding diarylmethanes can be effected in high yield by this same mixture of hypophosphorous acid and iodine in refluxing acetic acid.[9] We hypothesized that those reductions take place via the benzhydrol as an intermediate. However, benzhydrols were never observed when the reactions were sampled throughout their progress. The reason for this is now clear: benzhydrols are reduced much faster than benzophenones and can in fact be reduced at much lower temperature. When an equimolar mixture of benzophenone and 3,4-dimethylbenzhydrol was allowed to react for as long as 72 h at 60°C, the alcohol was completely converted to 3,4-dimethyldiphenylmethane without any detectable reduction of benzophenone to diphenylmethane! Similar results were obtained using mixtures of benzophenone with 4,4'-di-X-benzhydrol, where X is chloro, methoxy, or dimethylamino. Reduction of substituted benzhydrols can be carried out at temperatures as low as 40°C, although at the expense of longer reaction times. Reduction of 4-methylbenzhydrol (representative reaction): Iodine (1.00 g; 4.0 mmol), 4-methylbenzhydrol (0.79 g; 4.03 mmol), and acetic acid (25 mL) were stirred under nitrogen in a flask equipped with condenser. Hypophosphorous acid (50% aq.; 2 mL; 19.3 mmol) was added and the mixture was heated to 60°C. The mixture was stirred for 24 h, diluted with water, and extracted with hexane. The hexane was dried over MgSO4 and removed under reduced pressure. Analysis by GC¯MS showed only a single constituent, 4-methyldiphenylmethane,[20] produced in 100% yield.



foxy2 (Distinctive Doe) 08-11-02 15:21 No 344462	That sounds good(tet article)	Bookmark Reply
	If I were to try an H3PO3 reduction of a benzylic hydroxyl, using say the 70% commertially available H3PO3. I would try it exactly as above except use 2.9ml of 70% H3PO3 in place of 2ml 50% H3PO2. For the commonly reduced benzylic hydroxyl containing compound of interest the molar amount would convert to 0.67 grams. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



Psalty (Stranger) 08-11-02 18:13 No 344496	Reading that paper by Robinson, they seem to ...	Bookmark Reply
	Reading that paper by Robinson, they seem to indicate that the amount of water used in the reaction plays an important role in how much Iodoalkane was formed. They tried to keep their weight percent of water at around 40%, and indeed, if you look at their experimental section they did just that. The ideal amount of water may be different depending on the substance being reduced. Rhodium's proposed reaction puts the weight percent at around 25%. Only experimentation will tell what the right amount of water should bee. Hopefully, some bee can optimize the reaction to the point where no iodoalkane is formed. It seems that Robinson et al couldn't accomplish that with sorbitol though. How hard is it to seperate iodoephedrine from honey; does any bee know? There's not much information out there about its physical properties and solubilities, although some think it would be soluble in chloroform. I hope this reaction turns out to be as successful as it looks... The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



anOrangeDrip (Newbee) 08-11-02 19:04 No 344510	Re: Note that the researchers used two Freidrichs ...	Bookmark Reply
	Note that the researchers used two Freidrichs condensers to control the very exothermic reaction, and that a nitrogen atmosphere was used Is a nitrogen atmosphere required or did they just want to try it that way? So in addition to everything mentioned above, someone would have to produce enough nitrogen to completely fill an area. How long should it take to entirely fill a small room with nitrogen? For us newbies, how does a Friedrich condenser tie in with the nitrogen atmosphere? Friedrich Condenser When you meet a swordsman, draw your sword: Do not recite poetry to one who is not a poet.



Psalty (Stranger) 08-11-02 19:18 No 344513	Correct me if I'm wrong, but I think sticking a ...	Bookmark Reply
	Correct me if I'm wrong, but I think sticking a bleed tube into the reaction vessel, and plumbing N2 into it would be all that's required. You wouldn't have to conduct the reaction in a room that was filled with Nitrogen only. Trying to accmplish this may result in the death of a bee by asphyxiation. I think the point of using an N2 atmosphere, and thus excluding O2, is to prevent the H3PO3 from being prematurely oxidzed to H3PO4 (The I2 will eventually take care of that). I may be wrong on this too though... The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



foxy2 (Distinctive Doe) 08-11-02 20:14 No 344521	yes	Bookmark Reply
	I think the point of using an N2 atmosphere, and thus excluding O2, is to prevent the H3PO3 from being prematurely oxidzed to H3PO4 Yes oxygen will oxidise H3PO3 to H3PO4 As to the conditions in the Robinson paper. They are reduceing a much different molecule. I think pseudo is much easier to reduce and can probably bee done under more facile conditions. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



blondie (Hive Bee) 08-12-02 01:48 No 344583	thanks for the input	Bookmark Reply
	my gut feeling is that using a balloon such as with Curshot's nano would sufficiently exclude oxygen from the reaction. but still on the purification step - given an aqueous solution of NaCl or KCl and H3PO3 what would be the best way to drive off the water without risking oxidation to phosphoric acid? - before using an alcohol to extract the H3PO3. leaving it out at rt in a pan or boiling it off - anyone have any ideas - how reactive is phosphorous acid towards air?



BenWiFFen (Line Monitor) 08-12-02 05:45 No 344609	Sold in a silver plastic gallon	Bookmark Reply
	OH boy I can see coke and pepsi on somekind of watched list. The big chain hardware store sells a gallon of conctet and rust remover for 11$ it stinks a bit and rubber cloves should bee used. Makes one wonder about diatomaceous earth. Or putting paraffin to use. Sign here____________________



VideoEditor (Hive Bee) 08-12-02 06:26 No 344612	rust remover	Bookmark Reply
	Hey Ben I think the concrete rust remover is phosphoric acid, we want phosphorous acid. Go to the fertilizer store. Real Men Don't Preview Their Edits



Scottydog (Hive Bee) 08-12-02 07:22 No 344628	Thanks for the clarification...	Bookmark Reply
	Thanks bees for explaining the difference between the phosphorous acid salt and the "Ph down" H3PO4. Thanks also for the difference between phosphates and phosphites. My apologies for adding to the confusion. Phosphoric acid 85% solution > Hydriodic acid... (NOT) this process! Swis is a ghetto bee familiar only with homemade substituted eqpt. I imagine some kind of 24/40 adapter is necessary to run the two friedrich condensers in sequence? Swis is concerned with "shelf-life" of the salt. How long can it be safely stored before it starts to decompose? Thanks Rhodium, PP, V.E and everyone else for giving Swis a better and more accurate understanding... ___________ Refuse/Resist



Psalty (Stranger) 08-12-02 07:24 No 344629	Excellent question Blondie.	Bookmark Reply
	Excellent question Blondie. Some experimentation would definitly be in order. I would actually recommend boiling off the water for two reasons that are both purely speculative. First, while boiling vigorously, the water vapors leaving the surface at 760 torr would exclude more oxygen than water leaving the surfacce at room temperature with a partial pressure of 20-40 torr. Second, boiling off the water would of course take less time than letting the water evaporate at room temperature, thereby by shortening the amount of time available for H3PO3 to be oxidized. My only concern would be that the heat could possibly accelerate the oxidation of H3PO3. A melting point can be taken of the final product though. H3PO3 melts at 74.7C and H3PO4 is listed as melting at 21C. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



blondie (Hive Bee) 08-12-02 08:13 No 344638	evaporating	Bookmark Reply
	Psalty, yes that sounds good. i was thinking one additional step would be a small pipette-like glass attachment placed at the top of the flask so that the accelerated flow of water vapour would limit any air flow back into the vessel. <edit>



Elementary (Hive Addict) 08-12-02 09:54 No 344662	Phosphite fertilizers ??	Bookmark Reply
	I have never come across phosphite fertilizers in the uk, only phosphate. What benefits would they hold over phosphates fertilizers ? EDIT : Woops ! sorry guys I have seen phosphorus acid listed on a UK mail order chem site, but having the guts to order it is another thing ! I've got nothing to do today but smile !



Rhodium (Chief Bee) 08-12-02 10:19 No 344669	Why Phospite?	Bookmark Reply
	That has already been answered in this very thread: Psalty: "This would be significantly more OTC than rp or ..." (Stimulants)



Psalty (Stranger) 08-12-02 11:32 No 344679	Yes!! Blondie that sounds like a fantastic idea.	Bookmark Reply
	Yes!! Blondie that sounds like a fantastic idea. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



WizardX (Wizard Master) 08-12-02 19:23 No 344921	The Electrochemistry of H3PO2 & H3PO3	Bookmark Reply
	I posted this a while back in 2000 on my old Geocites site. Well, here it is again... The Electrochemistry of H3PO2 & H3PO3 http://angelfire.lycos.com/scifi/WizardX/downloads/H3PO2.zip Open the write.exe to read the .wri files. I wrote this in the Windows 3.1 Write many years ago.



xboXer (Hive Bee) 08-13-02 03:22 No 345027	of condensers vacuum and dry ice	Bookmark Reply
	would there bee problems, A) using dry-ice/acetone in the condensers for cooling the heat evolved? B) evap. of the H2O under a vacuum? The theoretical perpetuosity of a reaction coupled with an easily obtained precursor once again heralds the grand trumpeting of "The Law of Unintended Circumstances" Which should be viewed as evidence that "The more one attempts to control the individual's access to a substance or device, the more that particular thing shall increase with respect to it's popularity. Therefore the problems that the 'controller' faces as result will be a more resourceful and intelligent group of individuals." I find that a slice of irony pie. Give me the big slice and don't skimp on the whipped cream! (aka big brother) The journey of a thousand miles begins with a single step. Shut the door start the car!



Psalty (Newbee) 08-13-02 04:49 No 345043	using dry-ice/acetone in the condensers for ...	Bookmark Reply
	using dry-ice/acetone in the condensers for cooling the heat evolved? That might bee a little bit overkill, but maybee necessary if you only have one condensor. remember, the reaction has to run at around 115C. Also, the liquid pump will have to be able to handle the acetone and the subfreezing temperatures, i.e., a submersible pond pump from Home Depot probably won't cut it. evap. of the H2O under a vacuum? Yeah!! That's a great idea. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



Scottydog (Hive Bee) 08-14-02 16:38 No 345474	Orthophosphorous Acid	Bookmark Reply
	Helpful hints for newbees. When doing a search for chemical suppliers, Swis had better luck finding a source while searching under the keyword "Orthophosphorous Acid." Hope this helps... ___________ Refuse/Resist



Psalty (Newbee) 08-14-02 17:27 No 345482	I actually got mo' hits searching with ...	Bookmark Reply
	I actually got mo' hits searching with phosphorous acid. But doing both will give you more variety... The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



SPISSHAK (Hive Bee) 08-14-02 22:14 No 345584	Hate to bust the bubble on this but...	Bookmark Reply
	HI is generated by reduction of the Iodine by phosphorus acid and water at near or at the boiling point of water. There is problem with this, the iodo-ephedrine formed will cyclize (Elimination of H-X) at this temperature pretty easily, causing the intended reaction to fail. There may be a way around this though, like first producing the HI this way, then adding sufficient Red P to recycle the iodine formed in the subsequent step (at the temperatures in the system), then adding the compound to be reduced and doing the reduction at a reasonable temperature for an amino alcohol reduction. Problem solved?



Elementary (Hive Addict) 08-15-02 14:24 No 345755	Temp	Bookmark Reply
	the iodo-ephedrine formed will cyclize (Elimination of H-X) at this temperature If this is true, wouldn't this happen with the wizx HI reduction, as this is done at reflux temp. ? I've got nothing to do today but smile !



SPISSHAK (Hive Bee) 08-15-02 15:02 No 345772	Reflux is a	Bookmark Reply
	Vauge description of the temperature of a system. It does'nt always imply a boiling mixture. The best acid concentrations for this reaction are about %70, this is achieved by using a ratio of 1 part iodine, 1/2 part water (by weight) in an HI/RP reduction to make HI.] That puts the concentration around 73%. It's also best to add the amino alcohol to the mixture when it is hot. Don't know why but it works best that way. The preffered temperature here is around 160 degrees farenheight. That's when %60 yeilds are obtained. The acid concentration of %70 enables a faster reduction. By cyclization I mean to the methylaziridine, then other reactions ensue from that point. A theory is that HI cyclizes this amino alcohol by two different paths, the elimination that was mentioned above and by dehydration of the amino alcohol (this happens if the acid concentration is too high), which is why water is needed for this reaction but not too much. another consideration is the stereo configuration of the amino alcohol. Amino alcohols with R,R, or S,S configurations are more prone to this problem (like psuedoephedrine) but with R,S of S,R configurations the amino alcohol is more resistant to this cyclization, (like Ephedrine).



dwarfer (Hive Addict) 08-15-02 18:37 No 345855	Regarding the nitrogen purge	Bookmark Reply
	Could CO2 be used? dry ice at the beginning, to displace atmosphere: maybe even a side feed in ala foxy's note above? <<just a simple bircher boy dwarfer



foxy2 (Distinctive Doe) 08-15-02 22:47 No 345912	maybe	Bookmark Reply
	CO2 might work, but it might possibly bee reduced to CO. If you want some inert protection then use a balloon and nitrogen. Search google for "disposable nitrogen" You will bee rewarded with a very available souce of small amounts of N2 gas. Or just get a tank, its not any more suspicous than CO2. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



PrimoPyro (Hive Prodigy) 08-15-02 22:54 No 345914	party balloons	Bookmark Reply
	If nitrogen happens to be too much of a problem to attain, check out the local party stores and large Wally-world-type places that sell everything under the sun, and look for party balloon sets, they usually contain (or are located near) small, cheap tanks of helium gas. As you know, helium is quite inert. In fact, I'll give you a shiny nickel if you can somehow make a stable polyatomic helium compound. PrimoPyro



Psalty (Newbee) 08-16-02 17:28 No 346093	PP: Those damn noble gases, they don't like to ...	Bookmark Reply
	PP: Those damn noble gases, they don't like to associate with anything. Seriously, N2 isn't that difficult to obtain, nor is it suspicious. Grab yourself a small tank. It's handy to have around. And grab a regulator too. They come in handy for other things, like gassing your dank buds with CO2. The true danger is when liberty is nibbled away, for expedients. (Edmund Burke)



ChemoSabe (Hive Bee) 08-16-02 23:58 No 346165	Butane?	Bookmark Reply
	I'm really out of my element here (no pun intended) but what about butane? I don't even know if it's a straght element or a compound but it is a gas, I think. I just once recall it being a viable sub in a rxn that initially had suggested an argon environment. she showed me her immense menagerie of damaged sex toys, all of which she'd burned out from overuse



foxy2 (Distinctive Doe) 08-17-02 00:40 No 346177	I wouldn't	Bookmark Reply
	Using Butane is not worth the added fire hazard. IMHO. Those who give up essential liberties for temporary safety deserve neither liberty nor safety



fierceness (Hive Bee) 08-17-02 14:40 No 346288	some clarity	Bookmark Reply
	this thread could prove very promising.. there are so many tangents though its difficult to read/understand.. Basically, from what ive gathered (and correct me if i'm wrong) : 1) We should find some phosphite fertilizer and attempt the methods listed to convert it to the acid, as this more OTC method is more preferable to some bees, even though the acid is not watched. Foxy2 listed quite a few methods of doing this in foxy2: "H3PO3, phosphorous acid" (Stimulants). Hopefully these methods will produce workable phosphorous acid. Are there ways to test this for bees without a lot of special equipment? Maybe something along the lines of how RP can be tested by prefiring w/ i2? 2) Blondie and foxy2 seem to agree that the inert atmosphere requirement can be met quite easily, a la balloon or if one has to, helium is pretty easy to obtain as PP pointed out. 3) Blondie asks about an aqueous soln of Na/K Cl and H3PO3. I'm assuming this would be the product that is obtained when doing the simple Titration in Psalty: "Titrate your salt with a strong acid, such as ..." (Stimulants). However, I thought that foxy2's refs would be the ones that would have to be used because of inert ingredients in OTC fertilizer. Blondie's method would only work with the pure salt, correct? So, in foxy's refs the separation of NaCl or KCl is not needed, right? 4) SPISSHAK's post is, I admit, over my head and is what is causing me the most confusion. Are you saying the whole phosphorous acid process will not work with pseudo? Or are you saying that the water content must be perfect? 5) Iodoephedrine in the final product is also a problem. Now with the recent posts i've seen on chloroform production woes, is there another way we can separate any iodoephedrine from the honey? And why is this not a problem with one does just a normal reflux with RP/I/E ? 6) As for the acetone/dry-ice issues, foxy2 says that the reaction conditions would not be as harsh as the ones in the ref. So wouldn't just one condenser work with just cold water running through? I apologize if my post is redundant; I just thought that summing everything up and clarifying each issue might encourage experimentation and maybe this method will prove worthwhile.



SPISSHAK (Hive Bee) 08-17-02 17:02 No 346310	) SPISSHAK's post is, I admit, over my head and ...	Bookmark Reply
	) SPISSHAK's post is, I admit, over my head and is what is causing me the most confusion. Are you saying the whole phosphorous acid process will not work with pseudo? Or are you saying that the water content must be perfect? No What I'm saying is the temperature is too high (at which H3PO3 recycles Iodine) to have ephedrine in the system, it will cyclizise. So this would be a great way to make pre-rxn HI, but some red phosporous would have to be added after that to recycle the HI under conditions more appropriate for it's reduction. As far as water content goes, as long as the concentration of HI is between 57%-75% you're fine, it seems to go faster at the higher concnetration. 5) Iodoephedrine in the final product is also a problem. Now with the recent posts i've seen on chloroform production woes, is there another way we can separate any iodoephedrine from the honey? And why is this not a problem with one does just a normal reflux with RP/I/E ? Iodoephedrine is very unstable and it can be treated with strong base to detroy it. This converts it to methylaziridine, if you're real picky you can oxidize the methylaziridine with acidic Na2S2O3 (SWIM has done it) The PH has to be perfect though. [blue]



wareami (Hive Addict) 08-17-02 20:13 No 346337	pH?	Bookmark Reply
	The PH has to be perfect though. SPISSHAK: Perfect meaning pH 6.8-7.....? Peaceof the ^reaction Have FUN-Bee SAFE Everything Ibee says should be taken with a Large Grain of Sympathomimetic Amine Salt ô¿ôWareami



SPISSHAK (Hive Bee) 08-17-02 20:49 No 346339	been a while	Bookmark Reply
	since it was done I think the PH was lower than that, like 4-5. What was noticed was a black precipitate. I don't think aziridines follow the product into the NP layer anyway so it's really not important. But it was interesting (sodium thiosulphate oxidation of aziridines).



foxy2 (Distinctive Doe) 08-17-02 21:22 No 346344	Read Here! (Rated as: excellent)	Bookmark Reply
	Spisshak What I'm saying is the temperature is too high (at which H3PO3 recycles Iodine) to have ephedrine in the system, it will cyclizise. I would very much like to see some actual documentation of this. Something like cyclization rates versus temperature and pH. Even if the temperature was a problem, H3PO3 recycles iodine at all temperatures, I don't understand why you think 117C is necessary. This reaction should run just fine at 100C, I would expect it to take approximately 4 times as long as the reaction at 117C. So that means 8 hours instead of 2, not a big deal in my book. ****************************** SPISSHAK is incorrect Ok now that that I do some reading, I see that NONE of your "issues" is an issue at all!!! Aziridane formation is a GOOD thing, NOT a bad thing. Aziridanes are quantitatively reduced by HI to methamphetamine. If you have any aziridanes in your post reaction mix then your reduction is incomplete. If you need proof then read this document(specifically pg.17 or actual journal pg.113) http://www.rhodium.ws/pdf/meth.impurities.hip.pdf** Bee's there are no temperature issues, reflux away!!! Those who give up essential liberties for temporary safety deserve neither liberty nor safety



blondie (Hive Bee) 08-18-02 00:24 No 346386	Kewl.	Bookmark Reply
	Foxy, blondie luvs ya. <edit -not thinking>. where my friend lives he reports that the K salt is available as a pure solution otc - not part of any NPK formulation - the qty of inactives is therefore likely to be low. with all due respect to PP, buying phosphorous acid from a chem supplier means your relying on the salesperson being able to distinguish phosphorous from hypophosphorous - given the confusion already shown in this thread and for phosphoric acid, i think this still presents an element of (unnecessary) risk. [imho]



SPISSHAK (Hive Bee) 08-18-02 10:35 No 346459	thanks	Bookmark Reply
	for pointing that out foxy, I see what you are saying on page 17 of that article. That may also explain why racemic products are produced this way, as the ratio of the isomers is 3-1 cis/trans aziridines from the synthetic method they used to make aziridine as an analytical standard, so reduction of this logically gives an isomeric mixture.



WizardX (Wizard Master) 08-18-02 18:42 No 346551	Look at it this way...	Bookmark Reply
	2P + 3I2 ==>> 2PI3 2PI3 + 6H2O ==>> 2H3PO3 + 6HI Excess P will recycle the I2 and... H3PO3 + I2 + H2O ==>> H3PO4 + 2HI



aussie (Stranger) 08-22-02 05:53 No 347664	PHOSPHOROUS ACID PRODUCT IDENTIFICATION	Bookmark Reply
	I'm Trying ( sorry if it already been posted) http://www.chemicalland21.com/arokorhi/industrialchem/inorganic/PHOSPHOROUS%20ACID.htm PHOSPHOROUS ACID PRODUCT IDENTIFICATION CAS NO. 13598-36-2 ELINCS/EINECS NO. 237-066-7 FORMULA (HO)2HPO MOL WT. 82.00 HS CODE 2811.19 TOXICITY Oral, rat LD50: 1895 mg/kg SYNONYMS Orthophosphorous acid; Dihydroxyphosphine oxide; Phosphorus; Trihydroxide; Trihydroxyphosphine; DERIVATION CLASSIFICATION GENERAL DESCRIPTION It is a clear to yellowish crystalline solid with a garlic like odur melting at 73 C, decomposes at 200 C. It is very soluble in water and in alcohol. This compound contains one direct P-H bond (which is not very acidic) and only two hydrogens are bonded to oxygen and are acidic. The structure of this material is more correctly written (HO)2HPO. For this reson, this dibasic acid forms two series of salts, one containing the dihydrogen phosphite ion, H2PO3 - , and the other containing the hydrogen phosphite ion, HPO32-. This is an unstable compound that readily converts to phosphoric acid (H3PO4) in the presence of oxygen or on heating above 180 C. It is prepared by hydrolysis of phosphorus trichloride or tetraphosphorus hexoxide. Phosphorous acid forms salts called phosphites and also used as reducing agents because of its easy oxidation property to phosphoric acid. PHYSICAL AND CHEMICAL PROPERTIES PHYSICAL STATE Clear to yellowish Crystal MELTING POINT 73 C BOLING POINT 200 C SPECIFIC GRAVITY 1.651 SOLUBILITY easily soluble pH VAPOR DENSITY (AIR=1) AUTOIGNITION NFPA RATINGS REFRACTIVE INDEX FLASH POINT STABILITY APPLICATIONS Raw material to prepare phosphites; stabilizers for plastics; Water treatment Bleaching and Cleaning industry; Chemical manufacturing SALES SPECIFICATION APPEARANCE Clear to yellowish Crystal PHOSPHOROUS ACID 98.5% min PHOSPHATE 0.2% max CHLORIDE 0.015% max SULFATE 0.008% max HEAVY METALS 15ppm max IRON 15ppm max TRANSPORTATION PACKING 50kgs in bag HAZARD CLASS 8 (Packing group) UN NO. 2834 DESCRIPTION OF PHOSPHORUS Phosphorus is a nonmetallic chemical element in group 15 (nitrogen family, formerly Va) of periodic table; atomic number 15 atomic mass 30.9738; melting point ca 44.1 C (white); boiling point ca 280 C (white); specific gravity 1.82 (white), 2.34 (red), 2.70 (black); valence -3, +3, or +5 ; electronic config. 2-8-5 or 1s 22s 22p 63s 23p 3. The phosphorus molecule is composed of four phosphorus atoms, P4. Phosphorus exists in a number of allotropic forms [white (alpha and beta), red, black and/or violet] in the same physical state. White phosphorus is a white to yellow waxy substance which ignites spontaneously in air to form white fumes of phosphorus pentoxide and glows without emitting heat. Phosphorus is stored underwater as it is extremely poisonous, insoluble in water (but soluble in carbon disulfide). Commercial production of elemental phosphorus is prepared from phosphorite or phosphate rock (apatite, an impure calcium phosphate mineral) reacting with coke and sand or silica pebblesor at high temperatures in an electric furnace. Calcium silicate is produced as a by-product. White phosphorus is used as a deoxidizing agent in the preparation of steel and phosphor bronze. It is also used in rat poisons and to make smoke screens (by burning) for warfare. When white phosphorus is heated to about 250 C with air absence, it changes into the red phosphorus. Red phosphorus, a dark redish powder or crystal, does not ignite spontaneously unless heated to 200 C, does not phosphoresce and it is a little less dangerous than white phosphorus. It is used to make matches. Red phosphorus is prepared commercially by heating calcium phosphate with sand and coke in an electric furnace. Black allotrope is obtained industrially by heating at 300 C under pressure with a mercury catalyst. It has a layer structure and is stable. The major use of phosphorus compounds is in fertilizers, mainly as a mixture called superphosphate (calcium hydrogen phosphate), obtained from phosphate minerals by sulfuric acid treatment; and in nitrophosphates. Phosphorus is burned to make phosphorus pentoxide [phosphorus(V) oxide], a white solid used as a chlorinating agent in organic chemistry, as a drying agent and mainly converted to phosphoric acid used to make phosphates for fertilizers, electro chemical polishing and shaping, electroplating, metal cleaning and pickling in metal treatment by reaction with water. Phosphorus is highly reactive. A wide range of compounds is formed for uses in detergents, water softeners, pharmaceuticals, dentifrices, and in many other important applications. It forms metal phosphides and covalently bonded phosphorus(III) and phosphorus(V) compounds. Phosphoric acid can combine with certain alkaline elements to form salts called phosphates



acid_egg (Hive Bee) 08-27-02 16:00 No 349833	some chemistry	Bookmark Reply
	You might get confused on the ic/ous endings because lots of people fuck them up and state them wrong. There are no such things as hypo_______ic acids or per______ous acids. er...not quite correct Primo,...H4P2O6 is known as hypophosphoric acid...which incidently is 4 hydrogens for that particular oxy-acid not the expected 3.(when in doubt cover your ass! ) However this has very little to do with the thread and is just a chemical technicality,so I'll shut up now and stop confusing the issue. A chicken is just an eggs way of making another egg.



PrimoPyro (Hive Prodigy) 08-27-02 16:26 No 349843	You're Evil	Bookmark Reply
	I didn't think about polymeric acids. That's not fair. Will perform sexual favors for females in exchange for 1,2-dimethylaziridine. PM for details.



dwarfer (Hive Addict) 09-12-02 11:16 No 355666	Even Huge-er	Bookmark Reply
	Is this thread. << A little slow on the uptake, but this is revolutionary. The reflux could be subject to enhancement with the microwave, perhaps: the condenser is not a problem, as long as the vapor does not eat PVC. (????anybody know??_) Nifty: plants in yard showing phosphorus deficiency. Must acquire palliative immediatly.. dwarfer



bee186 09-13-02 03:30	Phosphorous Trichloride (PCl3) +H2O=>H3PO3 (Rated as: misinforming)	Bookmark Reply



bee186 09-13-02 07:23	huh? what did I miss inform about? Ill repair it? (Rated as: insignificant)	Bookmark Reply



ballzofsteel 09-14-02 00:59	Sorry if this is dumb. (Rated as: insignificant)	Bookmark Reply

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