Glass-lined equipment attachment

Solid samples are typically loaded in a glove box or glove bag into a short section of 8 mm glass tubing which has been sealed at one end, the tube is then attached to a 6 mm high vacuum stopcock, and the sample is sealed off with a 3 point seal under vacuum. The vacuum provided by a rotary pump is sufficient for this manipulation, but it is often convenient to have one line equipped with an oil diffusion pump to provide somewhat higher vacuum conditons which will more efficiently remove traces of hydrocarbon solvents from analytical samples. 

The assembly (Fig. 5) is attached to a conventional vacuum line equipped with a distillation train.8"10 All stopcocks and ground-glass joints are lubricated with an inert, self-thickened, halocarbon grease, which is unaffected by bromine. Germane is best prepared... 

Gases are transferred in a standard Pyrex glass vacuum line equipped with high-vacuum stopcocks (lubricated with a fluorocarbon grease [Halocarbon]) to which is attached a four-trap system used for low-temperature trap-to-trap distillation (Fig. 1). Because of the reactivity of the compounds, a Heise-Bourdon tube gauge [Dresser Ind.], is used for PVT measurements. 

Today, the glassware required consists of either a round-bottom flask or a Schlenk tube serving as the reaction chamber. This chamber is equipped with a magnetic stirbar and a Teflon high-vacuum valve (or glass stopcock) which provides for easy vacuum control after attachment to a vacuum line (Fig. 8.7). 

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