April 16, 2005

After reading a certain PDF, Bulletin 105, I found that the action of NaOCl on DMSO should give Cl3CSOCCl3 and I figured this compound should be insoluble in fall out of solution.  As such I put 2 milliliters of DMSO into a test tube and added fifteen milliliters of 10% NaOCl to it.  It heated rapidly much hotter then I could handle to hold and stayed very hot for several minutes.  Seeing as how I only had a little precipitate (Picture above) I transferred to a larger flask and added more NaOCl, much more, 200 ml total.  The mixture heated again and became cloudy.  A few hours later I was rewarded with a powdery white precipitate in the bottom of the flask.  I filtered and a small amount <.2 grams was recovered.  It smelled strongly similar to hexachloroethane.  It appears to be successful however I have no specific use for this chlorinated product.

I had some black drain cleaner that has been sitting around for awhile being somewhat useless so I decided to take some action.  The black color is often attributed to colloidal carbon in the solution from attack of the sulfuric acid on the PTFE containers it's stored in.  Additionally there are no stringent purity standards for over the counter drain cleaner as it is not meant for human consumption.  There are also other things, corrosion inhibitors, surfactants, etc.  Concentrated sulfuric acid combined with strong peroxide is known as Piranha solution and it is noted as a very strong oxidant.  It will oxidize carbon to CO2 and I figured it would also destroy most of the other organic material.  

As such 15 milliliters of so of 12% H2O2 was added to a 250 ml beaker and 50 milliliters of drain cleaner was added.  The mixture fizzed and heated a little and I added a magnetic stir-bar and sat on a hotplate to heat on low heat.  It continued to fizz and the color went away leaving a light yellow solution ( in the above picture in the background you can see the untreated acid, black, and the clarified acid on the hotplate, yellow).  I added some more acid because it was still fizzing so I figured it had some clarifying power left and it did.  All in all over 125 ml of acid was treated and looks nice, though diluted from its original strength.

I had not looked up any data on this oxidation or other procedures.  I was just eager to test out the ability of DMSO to decarboylate the acid thus formed.  So I added a milliliter of xylene to 25 ml basified H2O2 but before the xylene was added the peroxide was already breaking down from the basic solution.  Never the less, the two reagents were mixed and occasional stirring was done until slight emulsions formed which broke down quickly.  I let this continue for one hour and then removed the none too diminished xylene layer.  I acidified the aqueous layer hoping for the acid formed to precipitate.  No luck.

April 29, 2005

Today's goal was to prepare boric oxide by dehydrating boric acid.  Simple enough in principle.  I've done it one time before but it was about two years ago.  I placed 200 g boric acid into a electric skillet and put it on high heat for two hours.  The whole mass liquefied in thirty minutes and after two hours it was still liquid but considerably thicker then it was when it first became liquid.  I figured it was good enough but then for the hard part, crushing it.  I would dip in a metal scraper and take up a thin layer while it was still semi-liquid and allow it to cool in a thin sheet then take a mortar and pedestal to it.  This was arduous work and a pain in the butt and especially hand.  Got a blister and gave up after a while, dehydrated boric acid is a glass like material after all.  What would come in handy here is a ball mill.  Also I've been considering running this in a solvent of sorts.  Maybe heat boric acid with constant stirring at 200 C for two hours then decant off the mineral oil and wash with acetone to remove it.  That way things would stay a powder, well, if they don't clump.

Current Comments

3 comments so far (post your own)

That sure is quite neat way to make HCOOH, I could try it out :). The formic acid has been on my "to-do" list for quite long too. The distillation of ants has crossed my mind few times .. but it would not be fair for those little ants would it :(.

Posted by kaviaari on Sunday, 07.9.06 @ 12:25pm | #32

I have distilled formic acid several times using a borosilicate retort. Acutally, im doing it again right now. I'm using a cheapo electric metal coil hot plate. The retort bottom is mabey 6" from the coil. I have to turn it on and off as its lowest setting is too high if kept on for much longer than 20 minutes, the retort arm gets too hot too effectivly condense the vapors. I need to rig it up to a dimmer swith. For the most part i followed frogfot's page. I have mabey 50mls so far from this batch. Good luck next time you try it.

Posted by asilentbob on Thursday, 09.7.06 @ 21:48pm | #35

Final yield from my runs is 136ml of ~56% formic acid. My solution started changing colors near the end like yours though. I'll probably do it again with the same glycerin that is left in the retort.

Posted by asilentbob on Friday, 09.8.06 @ 16:57pm | #37

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