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plante1999
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[*] posted on 9-7-2012 at 18:15
I need a challenge


This is a long term project, up to one year in half.
I have read so much book about inorganic chemistry that I think I could make most if not all inorganic compound if I had time and a reasonable budget and I want to know if I overestimate me. This is why I made this post. I'm looking for a challenge to make an inorganic compound that is very exotic and very complex to make and there is no experimental easily available. The compound need to be completely inorganic, a polymer of ((CH3)2Sn)n composition would be considered inorganic since there is no carbon-carbon bond. The compound can use rare or costly element but I would need help to get them cheaply/free if possible. This is a long term project, so the compound could be made using very difficult to find starting reagent.


Thanks!

[Edited on 10-7-2012 by plante1999]




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[*] posted on 9-7-2012 at 19:16


here are some ideas and their uses:

LiAlH4 - a useful reducing reagent

BBr3 - to break some ether bonds

SOCl2 - to make acid chlorides

NOClO4 - to have some fun!

honestly, if you want to make an exotic compound or follow a 20+ step procedure, you should go for organic chemistry, such is making 5-amino tetrazole from urea and NH4NO3, then forming that into copper nitrotetrazolate ( c'mon, who doesn't want a vial labeled CuNT;)), or form 5-aminotetrazole into isocyanogen bromide and such.

another long winded prep is starting from benzene and going to modafinil or brady's reagent.

just my 2 cents-




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[*] posted on 9-7-2012 at 20:56


Perhaps aluminum trihydride, that is a simple compound that is challenging to make.

Aluminium hydride is a reactive reducing agent, but is noted for its selectivity in not reducing nitro groups [in general]. Aluminum hydride decomposes in air and violently reacts with water, and even sealed containers of AlH3 are known to degrade within a few days. But it does not spontaneously ignite.

AlH3 also has around a 10 percent higher specific impulse than aluminum powder in solid rocket propellents with ammonium perchlorate.

Quote:

LiAlH4 + AlCl3 → 4 AlH3 + 3 LiCl

"ether solution aluminium hydride is prepared after precipitation of lithium chloride"

but one would think that it would be the AlH3, not the LiCl that would precipitate from ether, maybe they got it switched around? So if you do this, you might check first to see whether the precipitate if flammable before dumping it. Wikipedia then goes on to say that the solution requires immediate use, otherwise the AlH3 will precipitate. Does this means that the LiCl will precipitate first, and then the AlH3 will slowly also start to precipitate?
Or more likely, wikipedia made a mistake, and it is only the AlH3 that will do any precipitation, the LiCl will stay perfectly dissolved in the ether? When AlH3 is dissolved in ether, H3Al•O(C2H5)2 is the complex that has formed. I read that there has to be more than 10% by weight of AlH3 dissolved in ether for it to be able to precipitate from the solvent.

ZnCl2 will work instead of AlCl3, and has the advantage of being more easily dried, but the yield (relative to the expensive) is lower, and ZnH2 would also form with the AlH3.

Concentrated sulfuric acid works, apparently. It probably has low yields, I would think some of the LiAlH4 reduces some of the acid before the main reaction can go to completion. This is likely a very violent dangerous reaction, so AlCl3 is probably best.
2 LiAlH4 + H2SO4 → 2 AlH3 + Li2SO4 + 2 H2

"Reaction of sulfuric acid with NaAlH4 at 92–100°C in pure toluene leaves undissolved pure crystals of aluminum hydride"

Electrolytic Method
Molten sodium aluminum hydride as the electrolyte, an aluminum anode, and an iron wire submerged in mercury (which acted as the cathode since mercury does not dissolve iron) The sodium Hg amalgam cathode prevents side reactions and the hydrogen produced can be captured and reacted back with the sodium mercury amalgam to produce sodium hydride.

Industrially, it may now be possible to prepare AlH3 directly from the elements: aluminum was hydrogenated to trihydride at 8.9 GPa and 600 °C. (Too much pressure to be done in the laboratory)

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[*] posted on 9-7-2012 at 22:41


Plante1999, let's be somewhat more realistic. Try to make and isolate CuCl, such that you have a nice vial with a white powder in it, which is pure CuCl. I think that this synthesis already is a true challenge for you. I have tried myself and it is amazingly difficult to isolate this compound without partial oxidation.



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plante1999
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[*] posted on 9-7-2012 at 22:47


Quote: Originally posted by woelen  
Plante1999, let's be somewhat more realistic. Try to make and isolate CuCl, such that you have a nice vial with a white powder in it, which is pure CuCl. I think that this synthesis already is a true challenge for you. I have tried myself and it is amazingly difficult to isolate this compound without partial oxidation.


I could try this as well the Aluminium hydride. I posted this thread exactly in the objective to know if I am overestimating me or a very good inorganic chemist. And by the way only my simple synthesis are repertoried on the net;), all my complex titanium compound synthesis are only repertoried in my notepad. But I did make other complex inorganic compound as well. I think I could make most, but I need a challenge to prove it or to prove me that i'm not as good as I think I am. With my logical mind I add doubt on the possibility that I could make most inorganic compound but still I want to know if I am wrong I need few ideas of inorganic compound then I will probably make a poll to chose the challenge.

Maybe It is some sort of teenager mood...

Thanks!

[Edited on 10-7-2012 by plante1999]

[Edited on 10-7-2012 by plante1999]

[Edited on 10-7-2012 by plante1999]

[Edited on 10-7-2012 by plante1999]




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[*] posted on 10-7-2012 at 01:35


What about the creation, then isolation of thiosulfuric acid? Not as simple as just mixing Na thiosulfate with an acid. It decomposes in water. Wikipedia (http://en.wikipedia.org/wiki/Thiosulfuric_acid) briefly describes one of its synthesises as reacting anhydrous Na thiosulfate with HCl gas in diethyl ether at -78oC. But it says on the page that it decomposes to H2S and SO3 below 0oC. Probably fairly difficult to synthesize, and would be a real challenge.
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[*] posted on 10-7-2012 at 01:59


This would be rely difficult to me since Dry ice is banned where I live but I can get temperature to -80 if I want but not for a long time, it is not the best compound ever for my challenge since the challenge is not to make it, it is to keep the temperature to -80 for all the procedure + the time it need to take picture of the product but still good idea, Thanks!


EDIT: Fallowing the same type compound you mentioned there is HSCN, (SCN)2 and (SCN)3 that can be considered suitable compound for the challenge. The (SCN)3 is made with the (SCN)2 reaction with thiocyanate salt in some unknown condition to me, both The (SCN)2 and (SCN)3 are very prone to self decomposition but are stable for some time a RT.


[Edited on 10-7-2012 by plante1999]

[Edited on 10-7-2012 by plante1999]




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[*] posted on 10-7-2012 at 03:01


Chromium II acetate is moderately difficult and a good test of air sensitive technique.

http://www.tulane.edu/~inorg/Lab%20Manual/Experiment%203.pdf

[Edited on 10-7-2012 by ScienceSquirrel]
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plante1999
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[*] posted on 10-7-2012 at 03:09


Quote: Originally posted by ScienceSquirrel  
Chromium II acetate is moderately difficult and a good test of air sensitive technique.

http://www.tulane.edu/~inorg/Lab%20Manual/Experiment%203.pdf

[Edited on 10-7-2012 by ScienceSquirrel]


Already made, it was very fun to make actually. Reduction of dichromate with HCl zinc and then dumping in sodium acetate to make the brick red compound. If I find the vial I will post a picture, I'm not sure if it oxidized in a one year period tough.




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[*] posted on 10-7-2012 at 03:12


I love the way you make your chemicals from "scratch" in the prepublication section. What I'd love to do but can't is to make calcium carbide and use that to make benzene by passing acetylene through a hot copper tube. I'm not to sure if it's a project with enough difficulty for you but making calcium carbide would be fun plus it's nice to get an aromatic compound from an inorganic one. I know the project I propose doesn't fully meet your requirements (of being totally inorganic) but I'd love to see you do it. :) I'm of the understanding that making benzene from acetylene is difficult to get right and the information of how to do it doesn't fall off the Internet easily (at least not for me).

Maybe another interesting project would be to make activated carbon. Easier said than done I think.

Type 3A molecular sieves is also of interest to myself but I've never researched how to make them so I don't know if that project fits your requirements.
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plante1999
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[*] posted on 10-7-2012 at 03:18


Quote: Originally posted by madcedar  
I love the way you make your chemicals from "scratch" in the prepublication section. What I'd love to do but can't is to make calcium carbide and use that to make benzene by passing acetylene through a hot copper tube. I'm not to sure if it's a project with enough difficulty for you but making calcium carbide would be fun plus it's nice to get an aromatic compound from an inorganic one. I know the project I propose doesn't fully meet your requirements (of being totally inorganic) but I'd love to see you do it. :) I'm of the understanding that making benzene from acetylene is difficult to get right and the information of how to do it doesn't fall off the Internet easily (at least not for me).

Maybe another interesting project would be to make activated carbon. Easier said than done I think.

Type 3A molecular sieves is also of interest to myself but I've never researched how to make them so I don't know if that project fits your requirements.


Even if it does not meat completly the requirement (Too easy and partially organic) it will be added in the poll since making benzene from the carbide is additional, making the carbide wort to be putted in the poll (The requirement is it need to be done without calcium metal) but I would only try to make benzene from the acetylene if someone is kind enough to send my some mercury metal/cinnabar to make mercury II sulphate with it, much more efficient catalyst than copper.

But for ''fan'' of my work I could do it no as my challenge tough, if that make sense.

[Edited on 10-7-2012 by plante1999]

[Edited on 10-7-2012 by plante1999]

[Edited on 10-7-2012 by plante1999]




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[*] posted on 10-7-2012 at 08:58


Quote: Originally posted by plante1999  
I have read so much book about inorganic chemistry that I think I could make most if not all inorganic compound if I had time and a reasonable budget and I want to know if I overestimate me.


You have overestimated yourself by far. No professor would even claim such things! Chemistry is not about being able to repeat preparations, but to rationalize them. Nature works in ways that are hardly intuitive, if you are too cocky She will revenge :). The division to inorganic and organic chemistry is really a rather arbitrary one. If you want to do chemistry basic knowledge of inorganic, organic and physical chemistry are essential. The Thing in chemistry is understand how all these areas are all intertwined (and also what physics has to do with this).

If you are up for a REALLY tough challenge try this: Devise and prepare a previously unknown compound containing a stabile radical.

[Edited on 10-7-2012 by kavu]
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plante1999
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[*] posted on 10-7-2012 at 09:09


Quote: Originally posted by kavu  

Devise and prepare a previously unknown compound containing a stabile radical.

[Edited on 10-7-2012 by kavu]


I will add this one, oxygen have stable radical. It should be ''possible'' to discover one ore ''easy'' to make one that is know but It was not what I was actually saying, I think could make most of the know inorganic compound.




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[*] posted on 10-7-2012 at 09:14


If you are feeling confident with your laboratory routines, start doing the real chemistry. Change reaction conditions, check what happens, try to rationalize what would happen and so forth. Using your literature try to apply it to a new scenarios... This will prove to be much more valuable than just repeating procedures. Have you done air and moisture sensitive synthesis, do you have access to such facilities?

Another big challenge would be to devise a C-H activating complex using the first row transition metals :)

It's also noteworthy that a great deal of modern inorganic synthesis requires organic manipulations as well.

For a more realistic test: Try to synthesize silver tetratungstate in a mmol scale. It will require a steady hand and attention to detail, but is doable. For refecence: page 76-79 Inorganic Synthesis, Vol. 22, 1983 Inorganic synthesis Inc.

[Edited on 10-7-2012 by kavu]
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[*] posted on 10-7-2012 at 12:53


Try to make NaBH4 in a batch size of at least a few grams. If you can show us how to do this without undue expense many will be grateful I'm sure.



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[*] posted on 10-7-2012 at 12:57


That would be a huge help, as Magpie says. I have needed some for a while for experiments with carbonyl compounds and to develop my ideas for multistep syntheses.

Perhaps you could try starting from Borax; this would be very useful as it cheap and readily available.




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[*] posted on 10-7-2012 at 13:10


@Magpie - its entirely possible. It was a project I was planning to undertake until I was lucky enough to fall on plenty for my needs, although I may still get round to it just to show the preparation in action. No need to waste expensive/difficult to aquire/make sodium hydride either.
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[*] posted on 12-7-2012 at 05:19


Quote: Originally posted by plante1999  
I have read so much book about inorganic chemistry that I think I could make most if not all inorganic compound if I had time and a reasonable budget and I want to know if I overestimate me.

You give the answer about your self-overestimation already in the question above. If you are still in the process of reading secondary literature, then you can not even consider yourself as a beginner. By a rule of thumb, someone who only read books is a total noob and someone who already started reading articles is a beginner. Only when you get trough the experience of peer reviewed publishing, can you consider yourself an expert (accepted by peers). This is the criteria in a professional environment and I see no reason why an amateur environment would have any different criteria (maybe just a different publishing criteria).

You should give your learning the due timing. In chemistry, just like in any science, you only start feeling confident in your knowledge and skills when you realize that you know nothing. I know this sounds counter-intuitive, but that's one of the bases of science, nicely explained already by Socrates, before the scientific method was even developed:

"I know nothing except the fact of my ignorance."




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[*] posted on 12-7-2012 at 11:52


Quote: Originally posted by plante1999  
I have read so much book about inorganic chemistry that I think I could make most if not all inorganic compound if I had time and a reasonable budget and I want to know if I overestimate me.

Ha ha. Make crystalline carbonic acid H2CO3. No C-C bonds, easily available chemicals and known to exist. We're waiting for the neutron diffraction patterns.

https://en.wikipedia.org/wiki/Dunning%E2%80%93Kruger_effect

Quote:
all my complex titanium compound synthesis are only repertoried in my notepad.
Does your notepad also contain hard analytical data or is your only analytical method "wishful thinking"?

Quote:
Devise and prepare a previously unknown compound containing a stabile radical

Inorganic chemistry is full of stable "radicals" and unknown compounds. No challenge there.

Bizarre thread.
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[*] posted on 12-7-2012 at 15:07


Go for beauty, borazine.

Except for the reduction of the resultant trichloroborazine most of it can be done, with difficulty, from OTC materials.

Another option would be to give potassium perbromate a try. Easy to say, hard to make. The challenge of course being making yourself some fluorine. Again, difficult, dangerous, but not impossible at home. I posted in the fluorine thread instructions to make a fluorine cell at home that was published when fluorine chemistry was flourishing in the 70's (well, not make it at home, but at your school). Bragging rights for certain. You can't even buy it last time I checked.

If you don't worry about things going boom (which amusingly enough I consider the aftermentioned two synthesis safe) there is a laundry list of unstable compounds you could try out, chlorine tetroxidefluoride, chlorine azide, chlorine nitrate, dichlorine heptoxide, nitryl perchlorate.

My advice, find a metal you like, download or buy the relevant copy of Comprehensive Treatise on Inorganic and Theoretical Chemistry and try to make the compounds that no longer exist. It amazing how many compounds are listed for some metals, high oxidation states, mixed oxidation states, etc. that neither hide nor hair can be found of in modern references. Do they exist? Did someone see something that wasn't there or misinterpreted it? Or will you be the first person to make one of those compounds in a century?




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plante1999
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[*] posted on 12-7-2012 at 15:17


Thanks for the comment, BromicAcid. Fluorine does not scare me, explosives does however. Borazine will by added as the idea of en old refference ''inexistant'' compound, and Perbromate.



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[*] posted on 12-7-2012 at 22:52


Plante1999, as you may have guessed from the answers in this thread, you cannot consider yourself an expert. There is so much to be discovered and I think that indeed home chemists still can discover amazing things, or simply rediscover amazing things which are totally forgotten since tens of years.

A nice example of the latter is the strange iodide/sulphur dioxide complex. You can easily make it from acidic sulfite solutions and a solution of an iodide. It has formula [I.nSO2](-), I don't remember the value of n, it is somewhere on my website. A nice challenge would be to isolate such a compound as e.g. the potassium salt.

Some compounds also are very dangerous. An example: I made ClN3 (chlorine azide). It is a colorless gas, and it is as powerful as detonating gas. I bubbled the gas through water with some soap in it and then ignited the bubbles of ClN3 which are formed at the surface of the soap-water. Impressive, but you really must know what you or doing, otherwise more than just the bubbles may explode!

So, I would suggest, first stick to more mundane, but still very challenging chemistry. In my previous post I mentioned making and isolating CuCl. If you can make some CuCl, isolate this such that it remains pure white and put this in a nice vial and can make a write-up of how you did it, such that others can repeat your procedure with typical materials available for a home chemist at decent cost, then you are impressing me. It is not the direct usefulness of CuCl which is that important (there are many other much more interesting chemicals), but the procedure to make and isolate it is valuable on its own.

[Edited on 13-7-12 by woelen]




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[*] posted on 13-7-2012 at 10:41


Quote: Originally posted by weiming1998  
thiosulfuric acid - it says on the page that it decomposes to H2S and SO3 below 0 C.

I doubt this. Even SO2 oxidizes SH2 at room temperature (if the two gases are bubled into water a milky white precipitate of sulfur will form). SO3 is an even stronger oxidizer than SO2. (although dilute sulfuric acid will not oxidize SH2)
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[*] posted on 17-7-2012 at 05:24


Plante1999, try this:
http://www.chem.utoronto.ca/IChO.Ontario/en/general.html

It'll be really fun!!!
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[*] posted on 17-7-2012 at 06:04


Quote: Originally posted by AndersHoveland  
Quote: Originally posted by weiming1998  
thiosulfuric acid - it says on the page that it decomposes to H2S and SO3 below 0 C.

I doubt this. Even SO2 oxidizes SH2 at room temperature (if the two gases are bubled into water a milky white precipitate of sulfur will form). SO3 is an even stronger oxidizer than SO2. (although dilute sulfuric acid will not oxidize SH2)

Anders Hoveland is right. SO3 and H2S are totally incompatible. H2S2O3 decomposes mainly to SO2, S and H2O. This reaction is not instantaneous, it proceeds slowly.

There, are, however, many side reactions and a really complicated mess is formed with all kinds of polythionic acids. You can actually smell this mess, it has a smell, very different from plain SO2. If you acidify a cold solution of Na2S2O3 with e.g. dilute H2SO4 and put that aside and you do the same with a similarly concentrated solution of Na2SO3, then you very well smell the difference. The Na2SO3 gives a 'clean' smell of SO2, while the other has a strong (stinky) component of smell besides the smell of SO2. Try it, it is an interesting little experiment on its own.




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