Pressure Tested Bottles
Reaction bottles for these hydrogenators are offered in several sizes as listed in the table below. All are made of borosilicate glass and individually pressure tested to twice their specified maximum working pressure. Several of these bottles can be furnished with a tough outer fiberglass coating. These coated bottles are no stronger than the plain ones, but the fiberglass envelope will usually retain any broken glass and prevent the loss of valuable reactants in case of accidental breakage.
When considering the listed bottle sizes it must be remembered that in most catalytic procedures the reaction bottle is filled only about half full to leave sufficient space for effective mixing.
|Reaction Bottles for Parr Hydrogenators|
|Model No.||Bottle No.||Size, mL||Bottle Type||Max. Working Pressure, psi||Requires Tube Assembly No.|
|3911||66CA3||500||Borosilicate Glass Fiberglass Covered||60||A122CA|
|3921||71CA2||1000||Borosilicate Glass Fiberglass Covered||40||A123CA2|
|3921||72CA3||2000||Borosilicate Glass Fiberglass Covered||30||A123CA|
|3921||72CA4||2250||Hand Blown, Heavy Wall Borosilicate Glass||60||A123CA3|
|3921||A129CA3||1825||Stainless Steel||65||A155CA Tube with 133CA2 Spacer Spool|
The standard 500 mL bottle (66CA) for the 3910 Series Apparatus are made with a heavy wall and a rounded bottom, which reduces its actual capacity to about 470 mL. This bottle fits tightly inside a wrap around metal screen that will restrain flying glass in case of accidental breakage. Smaller charges can be treated in an alternate 250 mL bottle (66CA2) which fits into the same bottle holder but requires an additional spacer spool to compensate for the differences in bottle heights. Special bottles with smaller capacities down to 50 mL or less can be constructed for treating micro samples. (Augustine describes a micro hydrogenation bottle that can be made by sealing a 50 mL or smaller heavy walled flask inside a larger bottle.)
Bottles for the larger 3920 Series Apparatus are made in several sizes from 1000 to 2500 mL all of which fit into the same bottle holder. One each of the plain 1000 and 2000 mL bottles is furnished with each 3920 Series Hydrogenator. These are carefully selected, machine blown bottles which, because of their large size, are restricted to 40 and 30 psig working pressures. If higher pressures up to 60 psig are required for treating large amounts of reactants, users are urged to purchase the special 2500 mL heavy duty bottle (72CA4) which is made specifically for this purpose. This is a hand blown, borosilicate glass bottle with an extra heavy wall that is much stronger than the standard machine-made bottles. Or, for reactions that can be handled satisfactorily in stainless steel, there is a 1825 mL bottle made of T316 Stainless Steel, which can be installed in any 3920 Series Apparatus. This bottle with a stainless steel cover and O-ring seal will withstand working pressures up to 65 psig.
Although a heater is not required for many of the reactions conducted in these hydrogenators, wrapping an electric heating mantle around the bottle can develop bottle temperatures up to 80 °C. Glass fabric mantles for this purpose are available in two sizes:
|Mantle No.||Watts||Volts||Use with Bottle No.|
|A451EEB||200||115||71CA, 72CA, 72CA4, A129CA3|
|A451EEE||200||230||71CA, 72CA, 72CA4, A129CA3|
These mantles have an adjustable strap so that a tight fit can be secured around any of the listed bottle sizes. A heater cord and plug are provided so that the electrical connection can be made by simply running the cord through the top of the bottle holder and plugging it into a Parr 4833 Temperature Controller. Heating mantles do not work well on bottles that have been covered with fiberglass. They work best on plain glass and stainless steel bottles.
Temperature Measurement and Control
Temperature measurement and automatic bottle temperature control can be added to any Series 3900 Shaker Type Hydrogenator with a Parr 4833 Temperature Controller. This compact, microprocessor-based controller will measure and control the bottle temperature in the 25 to 80 ºC range without a large investment in automatic control equipment, while providing several features usually available only in more expensive temperature control systems.
The 4833 Controller operates with a Type J (iron-constantan) thermocouple in a 1/8″ diameter stainless steel probe held in an A159CA Thermocouple Assembly which carries both the probe and the gas passage through a single opening in the bottle stopper. Assemblies are provided with thermocouples of different lengths to fit various bottle sizes.
The user can program the controller to operate in either a simple ON/OFF mode or in a more robust PID (Proportional-Integral-Derivative) mode in which the system evaluates and uses the time dependency of the set point/process temperature relationship to augment the proportional action of the controller. The controller can be instructed to automatically tune the PID parameters to fit the characteristics of the system. Dual, four digit displays show the set point and the bottle temperature. An illuminated heater switch shows that power is being applied to the heater. Overheating or a break in the thermocouple circuit will activate an alarm and shut off the heater.
Simply plugging the heater and thermocouple cords into sockets on the rear panel makes electrical connections to the 4833 Controller. Heater loads up to 3 amperes can be handled by a built-in solid state relay. Units can be furnished for either 115 or 230 volt operation, equipped with standard grounded plugs and sockets, specifically for country of destination.
Users who do not require the automatic control features provided by a 4833 Controller can measure the bottle temperature with any laboratory or industrial temperature indicator suitable for use with a Type J thermocouple, purchasing only an A159CA bottle connector assembly with an A295E thermocouple. Glass thermometers cannot be used in these hydrogenators as they are too fragile to withstand the vigorous shaking action of the bottle shaker.
|Assembly No.||Equipped w/|
|Fits Bottle No.||Fits Bottle Size|
Water Cooling Jacket
Cooling can be provided for the standard 500 mL bottle in the 3911 Hydrogenator by adding an A103CA water jacket. This jacket fits into the bottle clamp in place of the bottle guard, using a soft rubber ring to seal the neck of the bottle. Nipples are provided for hose connections to a cold water line and to a drain. This jacket is made only for the 500 mL bottle. It is not offered in larger sizes.
An electric motor drives the bottle shaker for the 3911 Hydrogenator with an enclosed belt drive. On the larger, 3921 Apparatus the shaker is driven by a geared head motor with a crank mechanism. These are constant speed motors that oscillate the shaker at approximately 175 cycles per minute. They are not explosion proof, yet they are not considered unduly hazardous if operated in a well ventilated location where care is taken to prevent the accumulation of explosive gases or vapors. If an explosion proof motor is required, it can be furnished at extra cost. Units equipped with an explosion proof motor are supplied with a connecting cord and switch and wiring option can be provided by Parr Instrument Company.