May 1, 2005
(Apparatus used, one way valve is in the upper left hand corner, components are in lower right corner.)
Preparation of potassium from KOH and Mg
This was a repeat of my experiment preformed in December 2003. 10 grams of potassium hydroxide was layered into 5 grams of magnesium shavings in an iron crucible. This was fitted into a vessel with a one-way gas release valve. Heat was applied with a blow torch and within two minutes a reaction began evidenced by a popping sound from within the reaction vessel. The exit gasses were intentionally ignited with the aid of the blow torch and they resulted in an intense column of fire for a few moments. Heating was continued for ten minutes and occasionally the torch would be brought to the exit gas area in an attempt to ignite any hydrogen gas that may have been lingering there.
The vessel was allowed to cool for 30 - 60 minutes and upon opening it was found the interior was coated in a thin layer of white powder, likely condensed potassium vapor. When attempts were made to remove the cake of material that had formed at the bottom, a small globule of potassium was recovered but immediately combusted. The whole resulting mixtue combusted a few moments later. Upon examination of the slag at the bottom it was found that fracturing it showed small pieces of potassium held in the solid matrix that quickly oxidized from exposure to the atmosphere. Next time I will take the extra step of dousing the cooled product with mineral oil so that some potassium may be recovered without it spontaneously igniting in my hand.
4Mg + B2O3 ---> MgB2 + 3MgO
11 grams of boric oxide prepared by dehydrating boric acid was layered with 15 grams of magnesium shavings in a steel crucible. This corresponded to a slight excess of boric oxide as I figured the reaction would be hard to initiate and sustain. When I previously did an experiment to reduce boric oxide I did so with a stoichiometric amount of aluminum powder, however this was nearly impossible to ignite so a small amount of potassium perchlorate was incorporated, after which the mixture was combustible. However with the reducing agent here being magnesium I figured no additional step was necessary, but it was, especially since I had magnesium in excess to perform the above reaction. The reaction could not even be started with flash powder. The reaction was eventually accomplished, to what extent is unknown, by heating the mixture directly with a strong blow torch. A glow would spread through the mass, atmospheric oxygen moving it along. What I was left with had the 'feel' of charcoal when I crushed it and it was black. This was saved for future use.
May 5, 2005
Analysis of magnesium boride produced on May 1, 2005
The premise was simple, an apparatus, pictured left made completely from glass and air tight. Diborane is produced by dipping HCl in the separatory funnel on to the magnesium boride in the flask beneath it. The diborane then goes through the glass tubing and bubbles into the bubbler through the water. Diborane supposedly reacting with water to produce boric acid. The boric acid then being precipitated with HCl and weighed to give me an estimation of the magnesium boride content of the thermite product I obtained.
Immediately upon adding a few drops of HCl the whole flask filled with thick smoke. See picture on right. This may be diborane reacting with oxygen in the vessel to produce a fine smoke of B2O3 or it might just be thinking that because that would be a positive indication of what I wanted to happen. None the less the vessel stayed filled with smoke to the end. Lots of HCl was added but I could get no boric acid to precipitate from my wash bottle. However I did get an odd smell that I am compulsively describing as a cross between cured ham and gym socks. Nothing conclusive on this front, too bad. Might be good to take the 'magnesium boride' and reflux with NaOH and see if any NaBH4 is formed, should be simpler.
Feonton's Reagent Hungrily eats up local Hydrocarbons
A batch of Fenton's Reagent was made by mixing 150 ml H2O2, 30 ml HCl and dissolving steel wool in the mixture. This was used to treat some acetonitrile and other organics I had left. It destroyed approximately 40 ml of organics in 3 hours. Then after they were gone it heated out of control and frothed and spattered, no clue why.
Distilling Hydrazine from basified Hydrazine Sulfate
12 grams of NaOH were dissolved in 35 ml H2O and this was added with stirring to 20 grams hydrazine sulfate. After heating up on its own I was left with a solution that had copious amounts of solid at the bottom, likely sodium sulfate or bisulfate. This mixture was distilled with magnetic stirring in an oil bath and this setup is in the picture above. I used a separatory funnel as the receiving flask so I could take off different fractions of the distillate. But I added too much H2O so most of the distillation was spent collecting highly dilute hydrazine fractions and by the time the temperature rose to collect the hydrazine hydrate azeotrope there was barely anything there to collect. Next time use less water!
Using product from Magnesium Boride attempt to recover Boron Powder
The 'black liquid' obtained after adding HCl to my attempted magnesium boride was poured into a 450 ml beaker and hydrochloric acid was added. This mixture was brought to a boil and filtered hot yielding shiny crystals. These were put back into the empty beaker and distilled water was now added. This was again brought to a boil and filtered hot. The result was a dull black powder pictured above.
May 8, 2005
Preparation of hydrazine hydrate (again)
25 grams of potassium hydroxide were dissolved in 75 ml methanol. After an hour the dissolution was complete but once it was poured into a separatory funnel a small amount of the KOH precipitated, but not much. The separatory funnel was placed into a flask that contained a stir bar and 25 grams of hydrazine sulfate. The methanolic potassium hydroxide was added over the course of an hour and the solution heated slightly, there were still some 'chunks' in the end that appeared to have not reacted. The resulting solution was filtered and filtered again. This was placed into a 500 ml RB (24/40 ground glass) and setup for distillation in an oil bath. Over the course of three hours a fraction came over in the range of 70 - 80 ºC and a second fraction came over around 100 ºC. However I ran out of time shortly after the temperature finally started to climb out of the water boiling off range. The resulting mixture fumes slightly in air and is cloudy, probably from precipitated compounds.
One thing that I've been wondering, how is the action of hydrazine hydrate on glass justified, I've read that it attacks glass but I didn't observe it. Many preps to produce the hydrate rely on large amounts of KOH or NaOH and this is the reason some are run in silver retorts due to the ability of these compounds to attack glass.
Fenton's Reagent Runaway Again!
Today I took maybe 150 ml 12% H2O2 and 4 ml FeCl3 (aq) from a electronics supplier. 6 ml HBr (aq) was added to make slightly acidic and the mixture was mixed with some ethylene glycol to test out its properties. The mixture fizzed and bubbled for thirty minutes or so and suddenly started to heat quickly. The bubbles began to rise further into the jar and eventually overflowed the top. I used a hose to douse the reaction. I wonder what went wrong this time.....
May 21, 2005
Ethylene carbonate again
In December of last year I gave this reaction a try for the first time, see that entry for more information. This was my second attempt. I mixed together 92 grams of urea, 120 grams of ethylene glycol and 6 grams of zinc oxide catalyst. The reactants were allowed to react together for 2.5 hours with stirring in an oil bath under vacuum at between 130 and 150 °C (The difference in the setup this time being the fractioning column on the round bottom, this is because last time the solution caused appreciable condensate in the hose and therefore a loss of solution, the column eliminated most of this.). During which time ammonia was stripped out of the reaction vessel, went through the pump, ate away at the copper and made it travel into my gas wash bottle which was initially quite acid with H2SO4, but ended up basic and as can be seen from the blue color of the picture, contains appreciable amounts of beautiful tetramine copper.
When the reaction was complete the reactants were allowed to cool for 30 minutes then filtered using a hand vacuum pump. But the viscosity of the solution and the fine ZnO made filtration a hassle. So I had to replace the filter papers three times. Finally, seeing as how I had no sand I covered the bottom of my Buckner funnel with cotton balls and attached it to my compressor. This worked well and after a short while the solution was filtered. After filtration it was transferred back to the 500 ml round bottom from whence it came and was stoppered and placed into the freezer to force the solidification of the ethylene carbonate present. There are a number of steps that I have devised to purify the product that I didn't attempt last time so hopefully things will work out well this time.