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Author: Subject: What reagent would you like to see an illustrated guide for?
kclo4
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[*] posted on 31-7-2008 at 14:53


Personally I think with len1's talent, making some of the simple molecules or ones that are easy to get would be waist of such talent, and the pictures wouldn't even be that important, but that is just what I think.. :P
No offense, but KNO2, N2H4, and HCl are not really that hard to get or make. Making them in a complicated way isn't to helpful for the board, and since len1 is asking, I think he wants to be as useful as possible to the board, right?

Just In case you didn't know, Potassium Nitrite can be produced by grinding Potassium Nitrate and Carbon into a very fine powder in 2:1 molecular ratio and then heat until it ignites. I've done this reaction, and it seemed to work well, and if it needs to be pure, fractional crystallization probably wouldn't be all that hard at all.
2 KNO3 + C = 2 KNO2 + CO2

Do they make Al powder from molten Al and steam? That sounds very interesting but also kind of improbable... Seems to me that it would simply react with the Al and make Al2O3 and H2, and wouldn't you want it to be water not steam? I imagine you would inject water into molten Al and the heat would cause the water to flash boil and blow Al particles everywhere. - have a link about it?

Len1, have you decided on anything or do you still want more suggestions? Perhaps you could, when you get down to the top 10 or so chemicals, make a poll and have people vote for what ones to make first? - just an idea

I think more members should make illustrated guides, that would be great! especially for the Home Chemistry society
http://www.homechemistry.org/index.php?title=Main_Page

I'll make it a personal goal to make some sort of illustrated guide.. eventually when I get my new sink installed and get the scale, as well as a few chemicals that are coming. :D
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[*] posted on 31-7-2008 at 16:39


Quote:
Originally posted by kclo4
Personally I think with len1's talent, making some of the simple molecules or ones that are easy to get would be waist of such talent, and the pictures wouldn't even be that important, but that is just what I think.. :P
No offense, but KNO2, N2H4, and HCl are not really that hard to get or make. Making them in a complicated way isn't to helpful for the board, and since len1 is asking, I think he wants to be as useful as possible to the board, right?


No, they're not hard to get. But availability misses the point and fun of the chemistry. To add to that, availability comes and goes.

Quote:
Just In case you didn't know, Potassium Nitrite can be produced by grinding Potassium Nitrate and Carbon into a very fine powder in 2:1 molecular ratio and then heat until it ignites. I've done this reaction, and it seemed to work well, and if it needs to be pure, fractional crystallization probably wouldn't be all that hard at all.
2 KNO3 + C = 2 KNO2 + CO2


How were you able confirm nitrite formation?

Quote:
Do they make Al powder from molten Al and steam? That sounds very interesting but also kind of improbable... Seems to me that it would simply react with the Al and make Al2O3 and H2, and wouldn't you want it to be water not steam? I imagine you would inject water into molten Al and the heat would cause the water to flash boil and blow Al particles everywhere. - have a link about it?


Water vapor or air is blown into molten aluminium and aluminium dust forms. The product is usually dark grey and looks almost like zinc dust (Gmelin Al [A] 165). The original reference is Aluminium Bronze Powder and Aluminium Paint, New York 1927, J.D. Edwards.
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kilowatt
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[*] posted on 31-7-2008 at 17:36


Why not just melt aluminum and force it through a small orifice to atomize it? It could be atomized and collected under an inert atmosphere. An electrostatic charge between the collection vessel walls and the orifice could help it atomize.

[Edited on 31-7-2008 by kilowatt]




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len1
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[*] posted on 1-8-2008 at 01:09


Thanks once again for the very interesting suggestions. I particularly like something that has an industrial chemistry bent to it. Plus with a bit of uncertainty in the result to make it an adventure. Although sometimes what seems like a tried and tested procedure can turn out to be a fizzer - Vogels hydrolysis to benzaldehyde to wit.

Of the things I hadnt thought off I liked the idea of hydrogenations and transition metal catalysts - but ill have to figure out what to make with that.

I also liked LiAlH4, but on checking the local Sigma-Aldrich stockist theyve plenty in stock and I couldnt find anywhere the word restricted. A concern though is the price $500/500gms for a piddly 95% grade, and it doesnt get cheaper with quantity. I wonder if it that might make it worth synthesising - even proper labs might have trouble running a research program with that price. What do people think?

I have just stumbled on one that Im even better prepared to synthesise - K, theres none in the country according so Sigma, it has to be brought in from the States at a cost of $117/50gms for 98%. Theres also this - Castner makes no claim to K for his cell, why? Is that because he didnt see why anyone would be interested in 1891, or does K dissolve much better than Na in the caustic bath so theres not even the narrow temperature window - I guess thats the element of adventure.

[Edited on 1-8-2008 by len1]
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[*] posted on 1-8-2008 at 02:53


Personally I would most like to see 1,2 Butylene Oxide. Another big one is DCM. While you're at it THF would be good :P

Ferrocene or carboranes would be formidable challenges and very interesting.

Practical fluorine would be a very impressive feat IMO.

Phosphorus would be awesome too. I might give it a try some time soon if circumstances permit.

Butyl Diglyme would be extremely useful for metal refiners.

Affordable Nafion style fluoropolymers would be interesting and very handy for many things electrochemical.

Nitronium tetrafluoroborate would be very nice.

BTW I think what you are doing is really great, keep up the good work!
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[*] posted on 1-8-2008 at 02:56


yep im with K nice one. make it real pure please.



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[*] posted on 1-8-2008 at 07:09


Len, potassium has been made with a Castner cell, as has NaK alloy. It is more soluble in KOH, less energy efficient and more bothersome because of that, but likely to be practical on a small scale. The greater reactivity of potassium can be troublesome.
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[*] posted on 1-8-2008 at 09:53


Quote:
even proper labs might have trouble running a research program with that price. What do people think?


Never underestimate how wastefull a research lab can be :) Once you see all that can be thrown away, all the purest/most expensive reagents used while ordinary grade would be more than enough... A friend of mine told me he was asked to get all the solvents and reagents in max. purity from the most expensive distributors, even though there where not needed, because it would be descrediting in the experimental otherwise :o So the costs where easily doubled just to say "All solvents used where of purest grade bought from ****", even for column chromatography.......

I'll stop rating there :)




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[*] posted on 1-8-2008 at 10:22


Quote:
Originally posted by 497
Ferrocene would be formidable challenges and very interesting.



Even more interesting would be cobaltocene. It's red & pyrophoric!

I am personally interested in polyphosphoric acid from orthophosphoric acid. I think it can be done with a lot of heat in a heavy-duty metal retort. Basically you would be cooking it to drive off water.

[Edited on 1-8-2008 by Ritter]




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[*] posted on 1-8-2008 at 10:29


Quote:
Originally posted by Ephoton
yep im with K nice one. make it real pure please.


Ill do my best. How about kosher? Call it Kosher-K. No seriously while searching their catalogue for pyridine (someone mentioned) I found they stock it in Kosher grade!??

Not_important, you dont by chance remember where youve seen that? It would be useful.

Klute, and I thought I worked in such a govt physics lab. Its better than your friends story - people dont just buy expensive stuff when cheaper would do, theybuy it when they dont need it at all. What the hack its taxpayers money. Ah but recently the cows started to come home - having wasted millions they might not be able to afford wipes any more - I suggested we might even have to bring our own toilet paper ..
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[*] posted on 1-8-2008 at 10:48


Currently I have no reagent to propose, at least no inorganic one. As far as organic reagents go, I think an illustrated preparation of some sulfonyl chloride like TsCl, MsCl, EtSO2Cl, etc. would be great, especially considering how useful these are. Admittedly these reagents, as far as I know, can also be bought from chemical suppliers without troubles, but I thought they would fit Len's tradition of sulfur and chlorination chemistry. Also, more or less all the needed literature is already supplied on the forum.

[Edited on 1/8/2008 by Nicodem]




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[*] posted on 1-8-2008 at 10:59


I am not proposing a product, but a methodology.

Start from, dirt, rocks, minerals, plant extracts and other naturally occuring materials and see how many transformations you can do using only naturally occuring things to end up with something really unexpected given the starting materials!:)

Start at the real ground floor of chemistry!

I plan to do this sometime, but I need more space first.




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[*] posted on 1-8-2008 at 11:00


Aww come on! Just plain old potassium??? :P

Really that would be quite interesting. What do you people need it for?

Quote:

polyphosphoric acid from orthophosphoric acid


AFAIK the only way do go is heat the crap out of it in a copper crucible. I suppose it could be dehydrated by something like B2O3, but I don't see the point in that.
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[*] posted on 1-8-2008 at 11:16


A second thing comes to my mind. It would be nice if acyl chlorides would become available for more persons, but inorganic stuff like thionyl chloride, sulphuryl chloride and phosphoryl chloride would be very nice as well. In many countries these are VERY hard to obtain and having a method available for synthesizing such chemicals at home would be great.



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[*] posted on 1-8-2008 at 11:48


Quote:
Originally posted by 497
Quote:

polyphosphoric acid from orthophosphoric acid


AFAIK the only way do go is heat the crap out of it in a copper crucible. I suppose it could be dehydrated by something like B2O3, but I don't see the point in that.


I want to be able to recycle it rather than disposing of it & buying new PPA. That way sounds expensive & wasteful.



[Edited on 1-8-2008 by Ritter]




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[*] posted on 1-8-2008 at 13:10


Quote:
Originally posted by Schockwave

How were you able confirm nitrite formation?



I added Conc. Hydrochloric acid to my Potassium nitrite and a large amount of NOx was produced, and that would never happen with Potassium Nitrate. I don't know how pure my Potassium nitrite is since i have never attempted to figure it out, but it seems to be pretty pure.
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[*] posted on 1-8-2008 at 14:19
Zirconia


Kirk's work talks how zirconium silicate can be processed with either sodium carbonate or hydroxide to leave free zirconia (aka Zirconium dioxide). As most pottery sources generally only sell zircopax or zirconium silicate, and lye fusion followed by hydrolysis in water would be quite interesting. Especially since the hobbyst only needs to perform a chlorate boosted thermite to get zirconium metal to add to his element collection.



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[*] posted on 1-8-2008 at 14:57


What about some CVD? Pyrolytic boron nitride, metals and alloys, metal oxides like alumina and zirconia, even pyrolytic graphite. These require gaseous reagents in the proper ratios at low pressure and moderate to extreme temperatures.



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[*] posted on 1-8-2008 at 16:02


Here's a proposition:
- Find a good method of making thionyl chloride
- Use the thionyl chloride to make anhydrous AlCl3
- Find a good method of making NaH
- React NaH with Lithium salt => LiH
- Find a way to purify LiH
- Use LiH and AlCl3 to make LiAlH4
- Purify the crude LiAlH4

Also, other interesting thoughs are:
- P2O5 from phosphates/other common phosphorus bearning stuff? And then use to dry reagents/produce SO3/N2O5 :P
- Acetic anhydride via Sulphur chloride (I cant remember which chloride, it's been mentioned on SMDB before though)
- Diborane and it's use as a reducing agent; advantages/disadvantages/limitations
- Phosphorus... Once we have a method of producing the white allotrope, maybe you can extend your studies and find the best method of converting this into the red kind :P much nicer stuff to work with :D
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[*] posted on 1-8-2008 at 16:45


I'm getting fairly intereste din diborane too, but there isn't much to it experimentally speaking, it can be generated from NaBH4 with lots of reagents: BF3, AlCl3, I2, TFA, H2SO4, etc

I guess Len is looking for a litttle more challenge :)




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[*] posted on 1-8-2008 at 16:55


P2O5 is definately useful in the lab :P and fairly hard to get hold of :( but getting a decent amount from a viable method other than burning elemental phosphorus ought to be a decent enough challenge :P
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[*] posted on 2-8-2008 at 15:08


Quote:
Originally posted by kclo4 I added Conc. Hydrochloric acid to my Potassium nitrite and a large amount of NOx was produced, and that would never happen with Potassium Nitrate. I don't know how pure my Potassium nitrite is since i have never attempted to figure it out, but it seems to be pretty pure.


Great then it's another possible way to get nitrite. But the reaction does not always go as theoreticized, and it's possible to end up with side products like K2CO3, K2O, etc. I also know too much carbon will get KCN (Polverone has done some experiments with this).
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[*] posted on 2-8-2008 at 15:30


Triethylborane

The fabled green flame, inflames on contact with oxygen and poisoning by trace amounts results in auditory hallucinations.

Only kidding :-D
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[*] posted on 2-8-2008 at 16:58


Triethylborane is just made via a grignard reaction, quite interesting though, I'd like to try it someday when I have a suitable setup and the time and guts to do it. Speaking of borane fuels, I have a complete synthesis for pentaborane that I got from a pdf of some medical journal. It can be found here on page 15. http://www.idecefyn.com.ar/mmcv08/O1.pdf Oh yes, and Triethylborane is quite innocuous when compared to pentaborane.:o

[Edited on 2-8-2008 by kilowatt]




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[*] posted on 2-8-2008 at 18:26


I am kidding about triethylborane, I cannot see it as a home chemistry target.

If you want to die in a hurry, try messing about with stibnite, readily available down your local rock shop and you can make all sorts of antimony compounds from it with ease.
Boiling with zinc powder and hydrochloric acid is particularly recommended.
Acute stibine poisoning is slow, agonisingly painful but inevitably deadly at quite low doses.

[Edited on 3-8-2008 by ScienceSquirrel]
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