Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2    4  5
Author: Subject: Preparation of anhydrous AlCl3 in DCM - photos
aonomus
Hazard to Others
***




Posts: 361
Registered: 18-10-2009
Location: Toronto, Canada
Member Is Offline

Mood: Refluxing

[*] posted on 16-7-2010 at 17:52


I think one of the problems with the recent experiment was the rubber tubing contaminating the reaction.

If you're desperate for a dispersion tube of some sort, check out your pet store. I did find what appeared to be a HDPE plastic frit which *may* be solvent resistant. (in the form of a plastic air 'stone' for fish tanks)
View user's profile Visit user's homepage View All Posts By User
peach
Bon Vivant
*****




Posts: 1428
Registered: 14-11-2008
Member Is Offline

Mood: No Mood

[*] posted on 16-7-2010 at 20:05


Quote: Originally posted by watson.fawkes  
Sulfur crosslinking holds vulcanized neoprene together. Even though there's no sulfur in the chloroprene monomer, sulfur is added to the polymer for vulcanization in order to stiffen or harden it. If you're smelling sulfur compounds like H2S, it's coming from degradation of your tubing. Given that you had a piece of it sitting in close contact with a Lewis acid, it's hardly surprising there may have been some depolymerization or other attack. If you knew the smell of chloroprene, it would help diagnose what happened.


Thanks watson! I did think sulphur had to be involved somehow, given the smell. I don't think it was H2S it's self, it wasn't rotten eggy enough, but there was definitely 'that smell' about it. The predominating smell was burning rubber. As I say, I've used it around HCl(g) before and not had problems. But the combination of the solvent or the Lewis acid has not helped. There was an awful amount of curious fuming (more than I'd expect from AlCl3), lack of HCl(g) and that horrible smell upon exposure to moisture. The yellowing in the solid could also be due to something sulphur based. I was hoping I might find some of your chloroform in this, and wanted my DCM back anyway. But I'm sorry, I'm going to have to abort on redistilling this one.

Quote: Originally posted by entropy51  
Given the simplicity of the 120 year old methods for successfully making AlCl3 in the lab, this thread is well, inconclusive. Gassing Al with dry HCl works, every time.

[Edited on 17-7-2010 by entropy51]


I bet gassing hot Al alone works like a charm. Not too sure about the solvent methods. If anything, it seems to be fairly inefficient in terms of absorption. I may repeat this when my glassware is finally back and I can do it with an all glass setup, as things changed when that piece of neoprene came into contact with the DCM + possibly Lewis acid. It wasn't doing this earlier, when I was only using it to direct the dry HCl(g) and exhaust around.

Quote: Originally posted by Sedit  
Entropy there are a gazzlion writeups spaking of the solent method and many claim success. I myself have had limited success as well but I think his down fall here is the use of DCM bar non.

Th solvent method has a quaint charm about it that you dont get with the ho method and I would love to see this synthesis become fruitful.

Ill share a bt of stuff monday, nothing important really just a few notes that seem strange with DCM as the solvent.


You're taking the weekend off from Science Madness?! How dare yar! Yar Land lubber YAR! :P

But seriously, I'd really like to hear those observations. I thought DCM would be quite a nice choice, as it seems to pick the gas up well, doesn't react with the Lewis acid and the acid isn't particularly soluble in it either, making recovery easy.

Apart from avoiding the need to heat the glassware up, I would also like this method to work as it seemed to be producing fine white precipitate earlier on. Which would make recovery and subsequent measurement easy; not having to scrape sublimed and then resolidified lumps off the glass or grind them up would be good.

I do suspect, however, the failure is the result of that piece of tubing.

Quote: Originally posted by blogfast25  
See, at this point I'd quit while you're ahead, if I was you.

This whole experiment reminds me of another thread in which a serious and knowledgeable experimenter wasted hours trying to follow a patent that... wait for it... called for the reduction of KCl with Mg at RT in organic solvent media. It too sounded about as plausible as Cold Fusion, it too didn't work. I'm all for thinking outside the box but it doesn't always lead to satisfaction.

Diligent effort though... :cool:

[Edited on 16-7-2010 by blogfast25]


This is the point where I tend to agree. Watson's heard me going on about toxic versus harmful or irritant, but clouds of odd smelling fumes pouring off polymers are generally not great at all.

There is ZERO chance I'll be using neoprene in contact with the DCM + acid again.

There's a patent out there about Wack'ing eugenol through to a ketone. It actually lists tens or a hundred plus different substrates and is essentially someone listing off everything with a double bond that they've Wackered with Methyl Nitrite. I tried their eugenol method, down to the letter, and just kept getting brown sticky gunk. I even tried swapping the oxidizers around. No luck.

It's worth noting that a common 'trick' when patenting something is called 'ring fencing', which is to try and list off as many other possibilities as possible to block others from making slight changes and repatenting it. Having distilled my third or four batch of suspect tar, I began wondering if they'd actually run this experiment or just made up the numbers; or to be kind, omitted some important detail. I also discovered a Tetrahedron entry explaining why it wouldn't work for eugenol.

I don't remember where this solvent suggestion came from in particular. I simply saw it being mentioned in forums and thought I'd give it a go.

My brother happens to be an IP lawyer, so PM me if you need some free legal advice for patenting your new super product. ;)

Quote: Originally posted by aonomus  
I think one of the problems with the recent experiment was the rubber tubing contaminating the reaction.

If you're desperate for a dispersion tube of some sort, check out your pet store. I did find what appeared to be a HDPE plastic frit which *may* be solvent resistant. (in the form of a plastic air 'stone' for fish tanks)


OooooOooo no.

Even having experience using this tubing with this gas, sucessfully, I did find myself questioning how wise it was to use it within the reaction space it's self.

I needed to do so as my wash bottles are still in the post and the downtube wouldn't reach into the solvent.

I've heard from people using aquarium frits before, and having them fall apart on exposure. Even borosilly frits will fall apart around strong bases.

A lesson I didn't really need explaining again, it has to be glass all the way.

When the glass turns up, and my patience has leveled up to normal again, I may try it using fritted wash bottles, as it would be good if it worked. But I'm not improvising anything involving the DCM + acid combination with regards to glassware.

Thanks for the replies everyone. It takes a lot of effort to gas something for hours on end, then do the washing up, then the photos, then the post, so it's really good to hear feedback.

Now I'm off to get a massive mug of tea (at 4am), recover from all those beers and eat my syrup soaked banana fritters from the chippy, which have probably gone even soggier by now. And maybe shoot that magpie if it doesn't shut up.


It's going to wake the damn rock doves up, I'll never hear the end of it then.


"Coo Cooooo Coo" "You said that last time"


[Edited on 17-7-2010 by peach]
View user's profile View All Posts By User
kmno4
International Hazard
*****




Posts: 1497
Registered: 1-6-2005
Location: Silly, stupid country
Member Is Offline

Mood: No Mood

[*] posted on 17-7-2010 at 08:52


Quote: Originally posted by Sedit  
....there are a gazzlion writeups spaking of the solent method and many claim success....

"gazzlion writeups" - it can be interesting.
Can you give here some references, links, for let's say... eeee... 2 ones ?
Of course,please do not give any patents, nobody is interested in rubbish.
View user's profile View All Posts By User
IrC
International Hazard
*****




Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline

Mood: Discovering

[*] posted on 17-7-2010 at 12:01


I think the ones saying this approach is a waste of time are missing the point. I think she is doing the right thing, experimenting and learning. How many lights did Edison try? If he quit after 3 or 4 we would have Russian bulbs (since there was an inventor over there inventing the same thing during those years) and Edison might not be so well known? For all we know Peach will come with a new procedure or some new catalyst which makes her solvent method work? If you do not try you never succeed?

Note I said she referring to Peach as it is the only way this quote makes sense.

"If you like that, you'd love my underpanties. They won me an award, $20, for a photo of them, which I believe has now been publicly circulated."

Thinking about reactions possible I do know most of the possible products like to eat organic tubing. DCM alone is going to do this, especially if hot. Years ago I bought DCM in 5 gallon buckets to depot laser power supplies which to keep you out were a mixture of various silicone compounds and sand. It would eat anything I tried from latex to neoprene to taigon tubing (unsure of it's composition), in general everything you could buy in the form of rubber or plastic so she needs to work on that part of the experiment. I quit using DCM after monoxide nearly took me out. It would eat every glove I bought eventually (usually sooner than later) allowing the stuff to leak in and stay in skin contact as well as breathing the fumes even though I really tried to have positive ventilation. I am sure most know DCM in our body converts to carbon monoxide carried by the blood from either inhalation or skin contact. So you should really have someone to monitor things since by the time you realize it you could very possibly need a blood transfusion to survive.

I imagine some of the reaction products can eat her tubing faster than DCM alone yet reading the quote below from Wiki I wonder about temperature and if these reactions listed below can all occur. One would think she did not have enough heat, since 400–500 °C is stated?

From Wiki:

Dichloromethane is produced by treating either methyl chloride or methane with chlorine gas at 400–500 °C. At these temperatures, both methane and methyl chloride undergo a series of reactions producing progressively more chlorinated products.[1]

CH4 + Cl2 → CH3Cl + HCl
CH3Cl + Cl2 → CH2Cl2 + HCl
CH2Cl2 + Cl2 → CHCl3 + HCl
CHCl3 + Cl2 → CCl4 + HCl

The output of these processes is a mixture of methyl chloride, dichloromethane, chloroform, and carbon tetrachloride. These compounds are separated by distillation.


I like your methodical well documented work Peach keep it going as to me it is interesting reading and fits in line with the reason we love to experiment.




"Science is the belief in the ignorance of the experts" Richard Feynman
View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 17-7-2010 at 12:57


Quote: Originally posted by IrC  
I think the ones saying this approach is a waste of time are missing the point. I think she is doing the right thing, experimenting and learning. How many lights did Edison try?


Let me tell you this, son, and I'm pretty sure Peach will agree with me: the difference between Peach and Edison was that he had something to go on: an electrical resistance heats up when a current passes through it. From there to a working prototype was hard technological work.

In the case of RT production of AlCl3 we know that without a catalyst to strongly reduce the activation energy of the chlorination reaction no reaction could take place without violating the Laws of Physics. Don't take my word for it: read up on 'activation energy' and atomic theory in general.

If Peach wants to continue this line of investigation her first line of enquiry must be the development of a suitable catalyst. That requires fundamental understanding of the chlorination reaction mechanism at the atomic/molecular level.

If she can pull that off, hats off and in the air to her. But until that becomes the approach, AlCl3 at RT in solvent media is like flogging a dead horse: it WILL NOT come alive by sheer will power.

In essence all she's doing right now is leading dry, cold HCl over dry, cold Al: the DCM is nothing but a spectator. We know that that doesn't work, if anything does her works proves that very convincingly... :)


[Edited on 17-7-2010 by blogfast25]
View user's profile View All Posts By User
peach
Bon Vivant
*****




Posts: 1428
Registered: 14-11-2008
Member Is Offline

Mood: No Mood

[*] posted on 17-7-2010 at 13:25


As far as it not working, have a look at the first set of photos and the photo of the amber bottle. That was elemental Al, dry HCl(g), no catalyst and all glass at room temperature. The solvent is green and the aluminium is reacting. When the reaction is finished, the green is gone and the solvent is opaque. There is pure white precipitate in the solvent the next day, separating from the aluminium layer, and the solvent has cleared to transparent.

I'm open to suggestions as to what that is if it's not AlCl3. Your possible reagents are elemental Al, HCl(g), DCM and borosilicate glass.

The solvent does make a difference, by changing the availability of the gas. E.g. concentrated acids often don't attack things until you add a little water to disassociate them. What happens if your pour hydrochloric acid on Al?

The evidenced is given by that piece of tubing. Neoprene doesn't react with dry HCl(g). None of the tubing before that piece has responded in a manner anyway near similar. I've used it before with dry HCl(g) and it doesn't react like that. Look at the tubing before and after the flask, it's fine. In fact, the tubing in the flask is fine as well. Only the portion below the surface of the liquid seems to have reacted.

But it does in the presence of DCM or the lewis acid. Either way you look at that, you're point is wrong. If it was the DCM that indicates the importance of the solvent in changing the reactivity of the gas. If it was lewis acid, that means I formed some of the acid in the first instance.

So no, based on that factual evidence and some logical reasoning, I don't agree.

Quote: Originally posted by blogfast25  
the difference between Peach and Edison was that he had something to go on: an electrical resistance heats up when a current passes through it. From there to a working prototype was hard technological work.


An ironic statement to make given the above observations.

As to Edison, he 'borrowed' the observations of one of his students with regards to thermionic diodes.

[Edited on 18-7-2010 by peach]




View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 18-7-2010 at 07:54


Quote: Originally posted by peach  


I'm open to suggestions as to what that is if it's not AlCl3. Your possible reagents are elemental Al, HCl(g), DCM and borosilicate glass.


[Edited on 17-7-2010 by peach]


Did you isolate/analyse the white precipitate? No, so we don't know what it was. I've seen a lot of 'precipitates' that turned out to be a trick of the light or pure perception. Recently I saw a green precipitate I thought might have been PrCl3. Couldn't prove it though... Maybe next time.

What you need indeed is a proton transferring solvent, much like water in a sense. A Lewis acid indeed. Or a Lewis acid than can be added to the mix or is soluble in a particular solvent. That's what's needed. I don't think you're close, TBH...


[Edited on 18-7-2010 by blogfast25]
View user's profile View All Posts By User
peach
Bon Vivant
*****




Posts: 1428
Registered: 14-11-2008
Member Is Offline

Mood: No Mood

[*] posted on 18-7-2010 at 09:38


Quote: Originally posted by blogfast25  


Did you isolate/analyse the white precipitate? No, so we don't know what it was. I've seen a lot of 'precipitates' that turned out to be a trick of the light or pure perception. Recently I saw a green precipitate I thought might have been PrCl3. Couldn't prove it though... Maybe next time.

What you need indeed is a proton transferring solvent, much like water in a sense. A Lewis acid indeed. Or a Lewis acid than can be added to the mix or is soluble in a particular solvent. That's what's needed. I don't think you're close, TBH...


[Edited on 18-7-2010 by blogfast25]


I'm no where near some of the guys on this forum in terms of theory, but you're no where close to me in terms of being able to use your own senses; like your eyes to look at those photos and your mind to interpret what might be happening.

You have Al, HCl(g) and glass to work with and you're still telling me I have something that comes out of a green solvent, turns the solvent opaque (like a salt falling out of it), then clears to white and crystallizes to a white ppt and it's not AlCl3?

I get the feeling there are a lot of arm chair chemists here. Tell me, specifically, what else could have formed. That is both white, precipitated form aluminium and involved those reactants. You're a brave boy to be telling me what I observed.

If you can't reply with a specific answer, you loose. If you don't reply, you loose.

The fact is, those initial pictures are of AlCl3 forming.

I asked you specifically to tell me what it was if it wasn't AlCl3 forming, and you entirely ignored me. I have prodived the evidence. The reagents, that the solvent was green and reacting, went opaque and then cleared, released a white precipitate (AlCl3 is opaque white). Where's the alternative answer?

A trick of the light? Come on! Even those photos show the Al is separating from the precipitate. And they're poor compared to the reality.

Tell me what it is if it's not AlCl3. You can't, because it is. Because it's the only thing that could have formed from those reagents. Stop flogging the dead horse that is you ego. You're an armchair chemist, and quoting my own results like they're yours.

I pointed out the neoprene tubing. The solvent and lewis acid. Both ignored.

Have you tried dissolving a Lewis acid in a polar aprotic solvent like water? Plumes of HCl(g) are the answer. You think that might be why I've chosen a polar aprotic? You have zero idea what you're talking about.

Water with AlC3? WHAT!? You're talking about hydrated salts. And AlCl3 in a hydrate form doesn't function as a hard lewis acid.

I have one question alone for you to answer. What is it if it's not AlCl3. Again, you have Al, HCl(g) and borosilicate glass as your reagents. If you don't answer, you're trolling.

I'm a SHIT chemist, and this is what I'm competing with?

[Edited on 18-7-2010 by peach]




View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 18-7-2010 at 11:18


Quote: Originally posted by peach  

I get the feeling there are a lot of arm chair chemists here. Tell me, specifically, what else could have formed. That is both white, precipitated form aluminium and involved those reactants. You're a brave boy to be telling me what I observed.

If you can't reply with a specific answer, you loose. If you don't reply, you loose.

The fact is, those initial pictures are of AlCl3 forming.

I asked you specifically to tell me what it was if it wasn't AlCl3 forming, and you entirely ignored me. I have prodived the evidence. The reagents, that the solvent was green and reacting, went opaque and then cleared, released a white precipitate (AlCl3 is opaque white). Where's the alternative answer?



Oh dear, oh dear, oh dear. Feeling a little piqued, Peach? Arm chair chemists? As opposed to you producing stinky goo and a white precipitate you claim to be AlCl3?

Remind yourself not to become a scientist: you'd be in for far greater criticism than I have meted out. In science we don't 'lose' or 'win', not if we're honest about things.

You've not 'prodived' the evidence: the material wasn't isolated and characterised. Why not? Not sure how to? Too much of an 'armchair chemist'???

Please also tell me how Al + HCl + DCM + borosilicate glass result in 'something green'?
View user's profile View All Posts By User
IrC
International Hazard
*****




Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline

Mood: Discovering

[*] posted on 18-7-2010 at 12:43


blogfast25 please explain why you are attacking this nice lady for coming here, spending long hours experimenting, taking pictures, documenting, posting here, which I thought was the reason for this site? She did her best, asked others of greater knowledge for their opinions, yet the gist of what I get from your posts is you are calling her an idiot who should give up chemistry.

You think your head is so very big.

Almost forgot to mention but it looks to me that unlike yourself she is actually doing something in her quest for learning, something you are not doing. Why don't you do the experiments yourself if your head is so very big and show her proof of her error if it exists.

[Edited on 7-18-2010 by IrC]




"Science is the belief in the ignorance of the experts" Richard Feynman
View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 18-7-2010 at 12:51


Quote: Originally posted by IrC  
you are calling her an idiot who should give up chemistry.

[Edited on 7-18-2010 by IrC]


And where did I do that, dearest? Learn to read.
View user's profile View All Posts By User
Fleaker
International Hazard
*****




Posts: 1252
Registered: 19-6-2005
Member Is Offline

Mood: nucleophilic

[*] posted on 18-7-2010 at 12:53


People are really convinced this can't be done in solution?

People are really convinced that HCl gas (let alone chlorine) doesn't attack aluminum ?

Might try this in chloroform, with a small crystal of I2 (or droplet of Br2) added--that would be my choice for performing this reaction.

[Edited on 18-7-2010 by Fleaker]




Neither flask nor beaker.


"Kid, you don't even know just what you don't know. "
--The Dark Lord Sauron
View user's profile View All Posts By User
IrC
International Hazard
*****




Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline

Mood: Discovering

[*] posted on 18-7-2010 at 13:01


Quote: Originally posted by blogfast25  
Quote: Originally posted by IrC  
you are calling her an idiot who should give up chemistry.

[Edited on 7-18-2010 by IrC]


And where did I do that, dearest? Learn to read.


I have been reading for almost 60 years. Along the way I learned it is not just each individual word but rather how they are structured to convey a point. From "Remind yourself not to become a scientist" You've not 'prodived' the evidence: the material wasn't isolated and characterised. Why not? Not sure how to? Too much of an 'armchair chemist'???

This is insulting to her or to anyone this would be spoken to. How is armchair in the picture looking at the well documented work she posted here. Where is your work?

One can only assume after reading the lengthy and hard work she posted you are saying she should give up. Only an idiot would do so having walked as far as she already has along the path of greater enlightenment so one can only surmise you are calling her an idiot. You are trying to discourage her and this pisses me off.

The problem is not my ability to read it is your ability to speak. Or write.


[Edited on 7-18-2010 by IrC]




"Science is the belief in the ignorance of the experts" Richard Feynman
View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 18-7-2010 at 13:03


Quote: Originally posted by Fleaker  
People are really convinced this can't be done in solution?

People are really convinced that HCl gas (let alone chlorine) doesn't attack aluminum ?

Might try this in chloroform, with a small crystal of I2 (or droplet of Br2) added--that would be my choice for performing this reaction.

[Edited on 18-7-2010 by Fleaker]


The people aren't convinced by this series of experiments, Fleaker, that's not the same thing.

Where would the I2 come into it? Soluble in CHCl3 and thus an initiator? It's possible but I've never seen it...
View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 18-7-2010 at 13:05


Quote: Originally posted by IrC  

The problem is not my ability to read it is your ability to speak. Or write.


[Edited on 7-18-2010 by IrC]


And I think you've got very long toes. And that pisses me off...
View user's profile View All Posts By User
IrC
International Hazard
*****




Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline

Mood: Discovering

[*] posted on 18-7-2010 at 13:12


Your honor, the defense rests it case on the last testimony by the defendant.




"Science is the belief in the ignorance of the experts" Richard Feynman
View user's profile View All Posts By User
Fleaker
International Hazard
*****




Posts: 1252
Registered: 19-6-2005
Member Is Offline

Mood: nucleophilic

[*] posted on 18-7-2010 at 13:19
Thinking out loud


Quote: Originally posted by blogfast25  


The people aren't convinced by this series of experiments, Fleaker, that's not the same thing.

Where would the I2 come into it? Soluble in CHCl3 and thus an initiator? It's possible but I've never seen it...


No, there are many things wrong with this set of experiments.

I2 is very soluble in chloroform, and will certainly react with aluminum--it (and bromine) does so neat and vigourously to give the polymeric halides. Even tin metal reacts with iodine in refluxing toluene, and Sn is much less active than aluminum. I suspect this reaction would be better done using chlorine gas, particularly if one adds a catalytic amount of mercuric chloride to remove the oxide. Perhaps also a better coordinating inert solvent is needed--issue being, few solvents are inert to a potent Lewis acid. I think iodine crystal would promote the formation of the aluminum trichloride.

Still, kmno4 said something quite salient--that the solvent may react with the metal to form an organometallic, and polymerize or react with trace oxygen. This could be some of the darkening that was seen by peach and explain any ebullition in the solution rather than hydrogen gas.

I've never tried to make AlCl3--it's so cheap and commercially available. Shipping is more expensive than the damn compound.

EDIT: Let's all keep it civil, friends. We're here to discuss science, and our respective failings in our methods, not showcase immaturity. Let's not insult each other, nor peach's efforts to at least attempt this reaction. Peach has done more (home chemistry) than I've done this past year.


[Edited on 18-7-2010 by Fleaker]




Neither flask nor beaker.


"Kid, you don't even know just what you don't know. "
--The Dark Lord Sauron
View user's profile View All Posts By User
12AX7
Post Harlot
*****




Posts: 4803
Registered: 8-3-2005
Location: oscillating
Member Is Offline

Mood: informative

[*] posted on 18-7-2010 at 14:48


Blogfast25, I thought you were better than this.




Seven Transistor Labs LLC http://seventransistorlabs.com/
Electronic Design, from Concept to Layout.
Need engineering assistance? Drop me a message!
View user's profile Visit user's homepage View All Posts By User This user has MSN Messenger
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 18-7-2010 at 19:10


OK someone requested the work I said I would add but its late and tommorows monday so I got alot of shit to get ready in the morn.

But What I think I did conclude is DCM sucks. I used Napthas for my first test I spoke of earlier with catalytical amounts of HgCL2. Howver using DCM and an attempt a I2 as the initiator give me completely different results. AS the DCM evaporated I expected to see some fuming of somekind and perhaps I2 leave the test tube.

However I got a nasty thick purple goop instead that would char indicating polymerization. The iodine was locked in this polymerization as well if that helps anyone conclude what might be going on. No amount of heating this goop would free any iodine omly cause charing of the goopy mess.


Im going to give it a larger scale run just to put and end to it but I must setup first and could take me a week before I prepaired because I want a control, I2 initiator and one with HgCL2 as initiator.

For references I talked about look over at Erowid there are more then a few claiming success and they provide the references and patents at the end of the writeups as far as the solvent method is concerned.





Knowledge is useless to useless people...

"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story before."~Maynard James Keenan
View user's profile View All Posts By User
IrC
International Hazard
*****




Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline

Mood: Discovering

[*] posted on 18-7-2010 at 20:37


I know I am not the chemist most here are and I still have not figured out the green color Peach mentioned, but is it possible the white solid is aluminum hydride?

Possibly this site has info you can use on the subject of Catalysts.

National Centre for Catalysis Research http://203.199.213.48/

While I know the experiment is not the same, he is using DCM and AlCl3 and talking about a green colored result, possibly there is something in the following thread which may give you ideas about what is going on in yours? Whatever reaction is occurring, as someone else mentioned I think the tubing involved in the reaction should be considered.

http://www.sciencemadness.org/talk/viewthread.php?tid=11607


[Edited on 7-19-2010 by IrC]




"Science is the belief in the ignorance of the experts" Richard Feynman
View user's profile View All Posts By User
Eclectic
National Hazard
****




Posts: 899
Registered: 14-11-2004
Member Is Offline

Mood: Obsessive

[*] posted on 19-7-2010 at 02:30


What happens if you use Et2O? As I recall the adduct of AlCl3 and Et2O is stable and distillable.


http://www.freepatentsonline.com/3843774.html

[Edited on 7-19-2010 by Eclectic]
View user's profile View All Posts By User
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 19-7-2010 at 05:51


There is a thread somewhere that speaks of using hydrated AlCl3 in DMSO to form an adduct which anhydrous AlCl3 is the decomposition product of perhaps its worth looking into. I tryed small scales of it but never got my DMSO dry enough to get it to work correctly.




Knowledge is useless to useless people...

"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story before."~Maynard James Keenan
View user's profile View All Posts By User
blogfast25
International Hazard
*****




Posts: 10562
Registered: 3-2-2008
Location: Neverland
Member Is Offline

Mood: No Mood

[*] posted on 19-7-2010 at 06:03


Quote: Originally posted by 12AX7  
Blogfast25, I thought you were better than this.


Tim, I don't think you've really read what I wrote, at least not all of it. And some of us being called 'armchair chemists' wasn't exactly Peach's finest hour either...

As far as I'm concerned it's water under the bridge now, I'm not good with grudges :)
View user's profile View All Posts By User
peach
Bon Vivant
*****




Posts: 1428
Registered: 14-11-2008
Member Is Offline

Mood: No Mood

[*] posted on 19-7-2010 at 11:02


You still haven't offered a single option for what may have been forming if it wasn't AlCl3. In fact, you haven't a single piece of actual scientific thinking, at all.

Al + dry HCl(g) in borosilicate glass effervesces and -----> white precipitate in DCM

Green solvent is a sign of chlorine or a chloride being in solution. The solution is green, then turns opaque after effervescing, then clears when a precipitate falls out of solution. And AlCl3 is not particularly soluble in DCM, and it's a white crystalline solid.

Tell me what the white precipitate is if it's not AlCl3. A very simple question, which you seem known the answers to.

This is the third time I'm asking you the same question.

I'm sick to death of this random, baseless arguing polluting my thread. If someone gave me a specific answer and said "No, it hasn't worked because of .....", I'd care. But that hasn't happened.

I don't hold grudges either. I'm too busy to be bothered remembering peoples' user names on internet forums. I'll argue with you alone, then agree with you alone in another thread. But I haven't seen any attempt to explain this, other than complaining.

I don't want any more arguing, I want Blog alone to reply with specific alternatives. And to explain why it was likely those and not AlCl3; as you seem sure it wasn't, so I assume you have evidence for that.

Knock out the arguing and look at those photos. AGAIN, FOR THE THIRD TIME, Al + dry HCl(g) in borosilicate ----> green solvent, effervescence, white precipitate.

Lets keep in mind you're the person who suggested doing this in "like water" solvent, shall we.

Give some scientifically reasonably answers as to what it is if it's not AlCl3.

I would urge everyone else to stop replying now. Give Blog alone a few days to reply.

FOURTH TIME, SPECIFIC ANSWERS.

If you don't reply with something scientifically reasonable and post some more complaining, I'll speak a moderator about you. Reply with something scientifically worthwhile or don't reply.

[Edited on 19-7-2010 by peach]




View user's profile View All Posts By User
IrC
International Hazard
*****




Posts: 2710
Registered: 7-3-2005
Location: Eureka
Member Is Offline

Mood: Discovering

[*] posted on 19-7-2010 at 11:13


Does this white precip have a jelly consistancy as in aluminum hydroxide?



"Science is the belief in the ignorance of the experts" Richard Feynman
View user's profile View All Posts By User
 Pages:  1  2    4  5

  Go To Top