Reaction Techniques

Materials to be treated in a Parr hydrogenator are sealed in a reaction bottle with a catalyst and connected to a hydrogen reservoir. Air is removed either by evacuating the bottle or by flushing with hydrogen. Pressure is then applied from the reservoir and the bottle is shaken vigorously to initiate the reaction. The bottle can be heated or cooled during this process, if necessary.  After the reaction reaches the desired point, the shaker is stopped, the bottle vented and the product and catalyst are recovered.

Progress of the reaction can be followed by observing the pressure drop in the system. For example, when using a 250 mL charge in a 500 mL bottle and drawing hydrogen from the standard 4-liter tank, the tank pressure will drop approximately 8 psi for each one-tenth mole of hydrogen consumed. The exact relationship between the pressure drop and the amount of hydrogen consumed can be determined by making a calibration run using a weighed amount of a compound whose hydrogen acceptance is known.

Convenient Valves and Fittings

Each apparatus is equipped with all necessary valves and fittings for admitting hydrogen to the bottle, for evacuating the bottle and for filling the hydrogen tank-all without disturbing the bottle connection. Separate gages show the bottle pressure and the tank pressure at all times. The four-liter gas tank, bottle holder and a sturdy shaker mechanism are arranged in a compact assembly on a steel base for convenient operation on a laboratory bench or in a hood.

The gas connection from the hydrogen tank to the reaction bottle is made with polypropylene tubing that extends directly into the bottle so that no metal parts come in contact with the charge. The tank itself, its valves and pressure gages are made of stainless steel. These parts are well suited for use with hydrogen. All of these valves have stainless stems, PTFE packing and replaceable PCTFE seats to ensure positive, leak-proof control in quantitative procedures. A smaller, one-liter stainless tank (A16CA2) is available for semimicro operations in which small amounts of gas must be measured. The regular valves are easily transferred to this smaller tank.

A six foot pressure hose is furnished with each apparatus for filling the hydrogen tank from a commercial gas cylinder. This can be attached easily to any gas pressure regulator or tank valve system.