Glass forming fritting

Prepared by melting a mixture of waste and glass-forming frit at 1150°C. 

The most important industrially utilized silicon compounds include chlorosilanes, methylchlorosilanes, silicones, silicon dioxide and silicic acids in different forms, silicates in the form of glass, water glass, enamel frits, silicate fillers, zeolites, silicon carbide and silicon nitride. 

The sample solution flows onto a piece of fritted glass through which argon gas flows. The flow of argon is broken down into narrow parallel streams of high linear velocity, which meet the thin film of liquid percolating into the pores of the frit. At the interfaces, an aerosol is formed and is blown from the top of the frit. 

A l-Iiter, three-necked, round-bottom flask is equipped with a mechanical stirrer, a thermometer immersed in the reaction mixture, a dropping funnel, and a gas vent. In the flask is placed a mixture of 96% sulfuric acid (25.5 ml, 470 g, 4.8 mole), carbon tetrachloride (100 ml), and adamantane (13.6 g, 0.10 mole), and the mixture is cooled to 15-20° with rapid stirring in an ice bath. One milliliter of 98% formic acid is added and the mixture is stirred until the evolution of carbon monoxide is rapid (about 5 minutes). A solution of 29.6 g (38 ml, 0.40 mole) of t-butyl alcohol in 55 g (1.2 mole) of 98-100% formic acid is then added dropwise to the stirred mixture over 1-2 hours, the temperature being maintained at 15-20°. After stirring for an additional 30 minutes, the mixture is poured onto 700 g of ice, the layers are separated, and the aqueous (upper) layer is extracted three times with lOO-ml portions of carbon tetrachloride. The combined carbon tetrachloride solutions are shaken with 110 ml of 15 A ammonium hydroxide, whereupon ammonium 1-adamantanecarboxylate forms as a crystalline solid. This precipitate is collected by filtration through a fritted glass funnel and washed... 

The precipitate that forms during ozonolysis sometimes impedes stirring, and in some cases it may be necessary to dilute the slurry with another 100 ml. of methanol after the first hour. Solid can also clog the gas-dispersion tube. The submitters scraped the fritted-glass tip occasionally to maintain a constant flow rate, whereas the checkers prepared a more dilute solution of nitronate anion (Note 3). 

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