Baal came across a man on the roadside the other day, selling all different kinds of containers. After careful consideration, Baal left with a food-grade,55gal drum, w/a locking lid device, & lined with a chem-resistant coating for a mere $7.00. First a hole was drilled in the lid and a 3/8"brass fitting was installed and hooked up to an air compressor and filled with air to 200psi to test pressure capability. Brass fitting was then topped off with a 175psi poppet valve. Into the drum went 20L>MeOH,400g>Al foil chunks & 200g>thin Al flashing cut into 1/4" strips, 600mg>HgCl2, this was stirred with a cordless electric drill fitted with a home-made stirrod & paddle for about 5 mins. Then another solution consisting of 500g>Ketone, 400g>Nitromethane, & 500ml>MeOH was prepared and ~150mls of this was added to the drum and stirred for ~2 mins. Now the MeOH was becoming more gray & amalgamation was present, this was periodically stirred for a period of just a few short mins. The bubbling pace was picking up, and now at about the 15 min. point, the rest of the Ketone solution was quickly dumped in. The lid was then quickly affixed to the drum, it was then sealed with the locking device and a nylon safety strap was wrapped around the drum lid for extra safety(in hindsight it wasnt necessary). A garden hose provided cold water flow across the top & the drum was then periodically "rocked" over the next hour to help with the mixing. During this time, the 'poppet valve' only went off twice for a second or so. The drum was then set atop 2
hotplates set on medium and it was periodically 'rocked' over another period of 2.5 hours, at which time the hotplates were removed and the drum was allowed to cool for a bit before the lid was removed. A 15L>35%NaOH solution was quickly prepared using bags of ice in order to keep the heat down, and 15L>Toluene was added to the drum and then stirred overhead on high. The NaOH was then added slowly and this whole shebang was stirred for 1 hr. at which time it was allowed to settle into its 2-layers. The top Toluene layer was siphoned off into a small plastic garbage can containg 7L of brine, this was stirred for 10 mins then allowed to separate. The top Toluene layer was siphoned off into another garbage can containing 7L>H2O, stirred for 10 mins, Toluene layer was siphoned off into garbage can once again. Then ~1/2kg>Dried MgSo4 was added to the Toluene and stirred for 5 mins, this was then allowed 20 mins to settle. Baal then went to prepare his 'Battle gasser', which is a modified 2-gal. plant sprayer. Then to the dismay of Baal, he discovers that he needs more Hcl than whats on hand. H-store opens in 4 hours, time for a quick nap.
More to come soon......
GODISNOWHERE