Sciencemadness Discussion Board

Announcements of Articles in Progress

I am a fish - 12-12-2005 at 12:57

If you are currently writing an article for the Prepublication forum, you may want to make an announcement here. This is to prevent two people from independently submitting articles on the same topic.

Please note that:

Baphomet - 20-11-2006 at 03:00

Proposed: Preparation of Palladium Chloride catalyst from OTC materials. Includes GC/MS analysis and illustrations.

Baphomet - 20-11-2006 at 19:01

Design of a High Flux Solar Gasification plant, with diagrams and explanatory notes.

In summary, HFSG technology would use solar energy to depolymerise municipal waste and produce methanol and ethanol for use as fuel.

Note: I'm looking for other people who might be able to help with the design. CAD skills would be highly regarded.

chemoleo - 20-11-2006 at 19:05

Illustrated WHERE?

I am not sure what you are on about.
You have to at least SHOW the experimental approach taken this far, rather than just making a 'title line'.

So where's the hard data?

Baphomet - 20-11-2006 at 21:33

My interpretation of the first post was that this is a thread for the announcement of articles currently in progress. If more details are required then I will post what I have for the PdCl and HFSG articles when convenient. The Odour Control article is nearly finished and will be posted soon.

DeAdFX - 30-12-2007 at 01:00

Propose: Generation of Ammonia via hydroylsis of urea using V2O5/Na3VO4 as a catalyst.

Not the most interesting/orignal topic but you have to start somewhere...

12AX7 - 30-12-2007 at 01:04

That reminds me, I've been interested in seeing urea vapor and air passed over a copper catalyst to produce NO, and thus NOx, and thus HNO3.

I should build an apparatus for that some day and see what happens. If it works well and is easy to put together, it would be an excellent addition here, huh?

For that matter, I should "prepublish" some other things, too. It's about time I post something here...

Tim

Engager - 13-4-2008 at 14:00

Completed big compilation work on tetrazole derivatives, now it is avialable on russian language, may be found here in pdf version: http://rapidshare.com/files/106232090/Tetrazoles_rus_.pdf.ht...

Now it's being translated to english, i used auto translator + hand translation, but it still need corrections to sound good, by native language speaker, The_Davster corrected a part of it but he is very busy. Then this will be finished, i will place large pdf & forum versions of this compilation work here in prepublications section.

I'm working on a few projects

Fleaker - 29-7-2008 at 13:41

Articles currently in progress at the experimental stage (expect these in the coming weeks):

Palladium on carbon, Adam's catalyst, miscellaneous catalysts and special requests. Co-authored with NERV for his expertise on nickel catalysts.

Will cover preparation, practical usage, and (time permitting) characterization.


Synthesis of anhydrous aluminum trichloride and other halides from the elements.

Will cover preparation and subsequent purification via sublimation. I do have LiH so I may attempt LiAlH4.

Articles coming before the end of the year:

Black and White Phosphorus, An Illustrated Synthesis

Synthesis of cesium and rubidium metal from their chlorides.

Articles that are finished and pending prepublication:

The Synthesis of Dialkyl Sulfates*

Bromine, an Illustrated Synthesis


*I will likely not publish this synthesis. It makes use of hard to find precursors (oleum or chlorosulfonic acid) and it is a very dangerous synthesis that I have had problems with on the many occasions I performed it. I do not think this is something that should even be attempted out side of a well equipped professional laboratory. I will make available any information that members here request via U2U and answer any questions on it, but I strongly recommend against performing the synthesis. I had bad experiences with it.

DJF90 - 29-7-2008 at 14:24

Caesium metal :o??! I wonder what possible applications that would actually have in the lab?

JohnWW - 30-7-2008 at 08:04

Possible chemical reactions of Cs that K may not be capable of? I have heard of alkali-metal anions being obtained; - they would be VERY reactive, if so, and could only be obtained as Cs+ with Li- or possibly Na-. Also, it may just be possible to get He or Ne to accept an electron from Cs, to form anions He- and Ne-, isoelectronic with Li and Na, but again such a compound would be VERY reactive if it could be formed and probably stable only at low temperatures.

Of course, samples of Cs salts would be needed in an analytical laboratory as standards for calibration of analyses of waters and minerals for Cs by flame-photometry or atomic-absorption.

-jeffB - 30-7-2008 at 10:09

Quote:
Originally posted by DJF90
Caesium metal :o??! I wonder what possible applications that would actually have in the lab?


A powerful getter for high-vacuum applications. My day-job lab has a fair amount of rubidium for doing spin polarization on helium and xenon, and I think we're going to be using cesium as well, but polarizing helium-3 probably isn't a good home science project.

I've got a kg or so of pollucite that I bought on eBay years ago, and I've thought about trying to render out some impure cesium from that, but I doubt I'll ever muster the courage. I don't have great confidence in my technique.

[Edited on 7-30-08 by -jeffB]

plante1999 - 30-3-2011 at 11:38

my first and next prepublication , extraction of chromium.

Hexavalent - 14-4-2012 at 02:25

An amateur chemists' guide to PPE and lab safety.

Diablo - 24-6-2012 at 12:58

Electrosynthesis of trichloromethane and
Electrosynthesis of potassium permanganate

Random - 17-11-2012 at 14:52

Quote: Originally posted by Diablo  
Electrosynthesis of trichloromethane and
Electrosynthesis of potassium permanganate


did you actually make permanganate with electrolysis?

Digital Hepatitis - 18-11-2012 at 23:56

[1] Improved method of preparing 5-bromovanillin with bromodimethylsulfonium bromide (BDMS). Here's the representative article on the subject:

http://www.researchgate.net/publication/11680334_Electrophil...

Abstract:
AbstractIt has been shown that bromodimethylsulfonium bromide, generated in situ by treating dimethyl sulfoxide with aqueous hydrobromic acid, is a milder and more selective reagent for electrophilic aromatic bromination than elemental bromine.

Fair enough -- who isn't looking for a high-yielding OTC halogenation mechanism? All one needs to facilitate a BDMS-mediated bromination is DMSO, hydrobromic acid, acetic acid &/or hydrogen peroxide. While the yields reported by the authors are acceptable, they suffer from an appalling overuse of hydrobromic acid that leaves this method un-scalable (unless you have liters and liters of hydrobromic acid sitting around.) By generating BDMS in situ and refluxing the desired substrate (i.e., vanillin) in a suitable solvent (e.g., toluene) and removing the water from the reaction vessel by means of a Dean-Stark apparatus, yields can be attained comparable to the standard bromination procedure (i.e., slowly dripping elemental bromine in the substrate and acetic acid).

[2] Improved method for preparation of methoxy-3 methylenedioxy-4,5 benzaldehyde (myristicin aldehyde) from 5-hydroxyvanillin using a phase transfer catalyst.

Referencing European patent 0278875, myristicin aldehyde can be prepared in good yield by refluxing tetrabutylammonium bromide and 5-hydroxyvanillin in dichloromethane in the presence of a base.

[3] Have kicked around a vague idea for an aluminum isopropoxide FAQ detailing all of the methods for its preparation (iodine, HgCl2, etc.) but that is way off in the distance now.

m1tanker78 - 22-12-2012 at 11:26

Electrolytic separation of cupronickel - yields reasonably pure copper and nickel powders.

This will be a cleaned-up report of some experiments I did which are scattered around in a long thread.

Tank

Chloroform via Haloform Rxn. of Acetone and Sodium Hypochlorite

bfesser - 19-7-2013 at 11:42

I've been unable to find a good article in here for the synthesis of chloroform by the Haloform reaction between acetone and sodium hypochlorite. I've noticed that there's been plenty of discussion on this reaction on the board, but it seems that no one has taken it on themselves to prepare a SM publication. I'm willing to compile the information and data myself from everything that's been posted, but as i haven't actually performed this preparation, I couldn't give it that personal touch. Is there anyone out there who would like to work on this, or at least collaborate with me on this? If nothing else, I need someone who can contribute photos (or permission to re-use photos from existing posts).

Bot0nist - 19-7-2013 at 11:49

I can run it with extra strength bleach and acetone tonight on the stirplate, and seperate with a sep funnel, then upload the pics tom. My camera is pretty good.

bob800 - 23-7-2013 at 16:59

Extraction and Purification of Oleic Acid from Olive Oil

From this article: http://link.springer.com/article/10.1007%2FBF02631772#page-1

Brain&Force - 2-2-2014 at 13:38

Luminescence in terbium(III) salts:

Paddywhacker - 1-3-2014 at 23:34

Quote: Originally posted by bfesser  
I've been unable to find a good article in here for the synthesis of chloroform by the Haloform reaction between acetone and sodium hypochlorite. I've noticed that there's been plenty of discussion on this reaction on the board, but it seems that no one has taken it on themselves to prepare a SM publication. I'm willing to compile the information and data myself from everything that's been posted, but as i haven't actually performed this preparation, I couldn't give it that personal touch. Is there anyone out there who would like to work on this, or at least collaborate with me on this? If nothing else, I need someone who can contribute photos (or permission to re-use photos from existing posts).


Check YouTube. There is at least one step-by-step video.

New benzofuran compound

organichem - 14-7-2014 at 23:31

Currently I'm working on different things;
1) more convenient route to 2,3,6,7-tetrahydrobenzodifuran [especially improving cyclisation via Mg]
2) most actual project (to start some work on SAR):
I worked out a (theoretical) way to prepare a compound I haven't heard of yet
--> step 1: Al-mediated o-selective chloroacetylation

Waffles SS - 17-10-2014 at 00:58

Coming soon with:


The Volatile Chemist - 18-1-2015 at 12:11

Not exactly sure how this works, but I have an article I'm going to add to the pre-publication sub-forum for review, etc.

Use of Iron-Cyanide Anion Salts as Indicators Rev. 1

Volanschemia - 6-5-2016 at 23:18

I plan to write up a Prepub article on recrystallisation of Sulphur from Xylenes shortly.
I don't think that has been done yet?

[Edited on 7-5-2016 by Volanschemia]

Melgar - 16-10-2016 at 00:39

Writing an article about an Aluminum/Gallium/Indium/Tin alloy that can substitute for Al/Hg in nearly every case, but without the toxicity that's characteristic of mercury.

NitratedKittens - 6-1-2017 at 07:43

A Beginners guide to the large scale Fischer esterification
(With photos)



[Edited on 6-1-2017 by NitratedKittens]

Synthesis of ethylbenzoate

Pumukli - 8-3-2018 at 12:01

I finished my epic synthesis yesterday and now I'm compiling/translating the results into a Prepublication entry. Took some pictures as well, so you will get eyecandy too :-)

It was really "epic", lasted for 4+ days, utilized two different methods for esterification, made silly mistakes that slowed down even more the otherwise also slow progress of things.

I comitted more than five full A/4 pages of lab notes during this synthesis but in the end I reached my goal and now I have about 450 g sickeningly sweet / minty smelling water clear liquid in a closed flask.
Did I say I hate semi-micro when one can go macro? :-)

It still requires several hours of text and photo editing, translation, proofreading and such before I can upload the article. Within a few days I can finish it I hope. It will be my first prepublication attempt so please bear with me!

Synthesis of m-nitro-ethylbenzoate

Pumukli - 20-3-2018 at 11:16

The ethylbenzoate saga continues.

I'm over two batches, same procedure. The second one went more quickly and gave better yield. Ahh, the routine! :-)

Took pictures - as usual. :-)

Hopefuly can provide melting point data now on as well.

A few more days and I'll post the article.

VSEPR_VOID - 17-4-2018 at 10:05

I am currently composing a publication on the preparation of various ferrocyanide salts of copper. I intend for it to cover 3 or 4 and to be fully illustrated. I would be happy to hear recommendations on how to characterize said salts; All are inorganic, ionic and most insoluble in water.

I gave already purchase the reagents I require, gotten time scheduled at the lab for the project, and write several procedures and an abstract.

12thealchemist - 15-11-2018 at 11:38

Currently composing a publication on the preparation of potassium and sodium via the magnesium reduction alcohol catalysed process, and a short publication on the synthesis of tetraethoxysilane.

L-Proline decarboxylation trials

Pumukli - 24-11-2018 at 00:30

Started to translate/compile the results of my work with the decarboxylation of proline. It will be the essence of five months' "work", although the allocated time suffered a lot in the last 2 months due to interference from everyday life. :-)

Edit:
Finished the bulk of translation.
Now comes the picture editing, chemical structure drawing part.

[Edited on 5-12-2018 by Pumukli]

Pumukli - 24-11-2019 at 09:59

1,3,5-triacetyl-benzene synthesis
and its evaluation as a potential decarboxylation catalyst

The ultimate amino acid decarbox. catalyst arrived! Three (!) different keto-groups packed in a nice, symmetrical, compact molecule, each one is ready to bind with amino groups and catalyse the shaking-off of CO2! :)
What do you think? Will it perform as expected?

I'm putting together the article, deciphering hand written lab notes from seasons ago - just kidding, my hand writing is pretty and readable. :) What is not a joke though is I just finished the prolin decarboxylation experiment with this triketone a few minutes ago so the result is as fresh as one can get! :)

Stay tuned and try not to bite your nails too excessively - I plan to upload the article within days.

Pumukli - 2-1-2020 at 10:18

Unfortunately after my announcement life intervened and I'm in quite a turmoil in these days. I regret to say that I'm not so optimistic at the moment that I can upload the article anytime soon. Please bear with me!
I'll do the posting sooner or later I'm sure, but don't know the time yet.

[Edited on 2-1-2020 by Pumukli]

Cou - 24-1-2020 at 13:34

Making 2-chloroethanol from ethylene glycol and ZnCl2