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Series 3900 Shaker Hydrogenator 271M
311M Supplemental Instructions for 4833
Series 3900 Shaker Hydrogenator Literature
Parr shaker type hydrogenators provide compact and easily operated systems for treating chemicals with hydrogen in the presence of a catalyst at pressures up to 5 atmospheres (60 psig) and temperatures to 80ºC. They are used primarily for synthesizing or modifying organic compounds by catalytic hydrogenation, reduction or condensation, but they are equally suitable for any other laboratory procedure in which a liquid and gas must be mixed vigorously in a glass reactor at pressures up to 5 atm.
AN EIGHTY YEAR HISTORY
The basic design for these hydrogenators stems from an apparatus first described by Voorhees and Adams in 1922 and offered commercially by Parr about 1926. Since that time, Parr has added many improvements and accessories to enhance the usefulness of these reactors to the point where they have become an essential piece of equipment in almost all organic chemical laboratories.
REFERENCES
No attempt is made here to list the hundreds of references to the Parr hydrogenator which have appeared in chemical literature since Dr. Roger Adams published his first paper describing an apparatus of this kind in 1923. More than five hundred literature references are cited in Augustine's book on Catalytic Hydrogenation that is listed below. Additional references can be obtained from other books in this list. Among these, the books by Augustine, Freifelder and Rylander will be particularly helpful to those users who want additional information regarding hydrogenation techniques, catalysts and procedures for treating specific functional groups. The following references are therefore highly recommended:
- R. L. Augustine, Catalytic Hydrogenation, Marcel Dekker, Inc., New York (1965).
- Morris Friefelder, Practical Catalytic Hydrogenation, Wiley- InterscienceDiv.ofJohnWiley&Sons, Inc., NewYork(1971).
- Gilman-Blatt, Organic Synthesis, Collective Volume /, p. 65, John Wiley & Sons, Inc., New York (1948).
- H. W. Lohse, Catalytic Chemistry, Chemical Publishing Co., Inc., New York (1945).
- Paul N. Rylander, Catalytic Hydrogenation Over Platinum Metals, Academic Press, New York (1967).
- Paul N. Rylander, Catalytic Hydrogenation in Organic Synthesis, Academic Press, New York (1979).
- Biennial conferences held at the New York Academy of Sciences in even- numbered years starting in 1966 have produced excellent collections of papers under the general title, Catalytic Hydrogenation and Analogous Pressure Reactions. The initial set is published in the Annals of the New York Academy of Sciences, Vol. 145, Art. 1, pp. 1-206 (1967). Papers presented at conferences held in more recent years are published by Marcel Dekker, New York, under the general title, Catalysis of Organic Reactions.
MANY APPLICATIONS
The broad usefulness of this apparatus is best illustrated by the numerous references to it in chemical literature published during the past fifty years. Applications arise wherever low pressure catalytic reactions are used, as in the fields of teaching, research, product development and in the production of fine organic chemicals and pharmaceuticals. In addition, these reactors are frequently used in quantitative investigations to assay compounds containing hydrogensaturable double bonds and to test the activity of catalysts used in industrial processing.
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 brass or bronze. These parts are well suited for use with hydrogen, but they must be replaced with a stainless steel tank and stainless valves if ammonia or other corrosive gases are to be used in the system. All of these valves have stainless stems, PTFE packing and replaceable Kel-F seats to ensure positive, leak-proof control in quantitative procedures. A smaller, one-liter brass tank 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 6-ft 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.
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
| Apparatus No. | Bottle No. | Size mL | Bottle Type | Max.Working Pressure psig | Requires Connector No. |
| 3911 | 66CA2 | 250 | Borosilicate Glass | 60 | A122CA2* |
| 3911 | 66CA | 500 | Borosilicate Glass | 60 | A122CA |
| 3911 | 66CA3 | 500 | Borosilicate Glass Fiberglass Covered | 60 | A122CA |
| 3921 | 71CA | 1000 | Borosilicate Glass | 40 | Al23CA2* |
| 3921 | 71CA2 | 1000 | Borosilicate Glass Fiberglass Covered | 40 | Al23CA2* |
| 3921 | 72CA | 2000 | Borosilicate Glass | 30 | Al23CA |
| 3921 | 72CA3 | 2000 | Borosilicate Glass Fiberglass Covered | 30 | Al23CA |
| 3921 | 72CA4 | 2250 | Hand Blown, Heavy Wall Borosilicate Glass | 60 | Al23CA |
| 3921 | 126CA | 2500 | Stainless Steel | 65 | Al55CA Tube with 133CA2 Spacer Spool |
The standard 500 mL bottle (66CA) for the 3911 apparatus is 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 3921 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 3921 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 1700 mL bottle made of T304 stainless steel, which can be installed in any 3921 apparatus. This bottle with a stainless steel cover and O-ring seal will withstand working pressures up to 65 psig.
SAFETY CONSIDERATIONS
Parr shaker type hydrogenators are usually operated in an open laboratory without additional barricades or protective screens, but the operator must realize that additional protection may be necessary if there is any possibility that a reaction may run out of control, or if unexpected bottle breakage would produce a hazardous spill of toxic or flammable materials. Potentially explosive reactions are best handled with the apparatus located behind a suitable barricade or in a pressure test cell.
There must be no gas burners or open flames near a hydrogenation apparatus. The room must be well ventilated and any gas released from the apparatus should be discharged into an explosion proof hood or ventilating duct. Care must also be taken to prevent ignition by a static charge from an insulated object.
The hazards involved in performing pressure reactions in glass bottles is minimized in these reactors by using carefully selected and pressure tested bottles within steel shielding. In spite of these precautions, a bottle will sometimes break below its rated pressure. The user must be constantly aware of this hazard and take whatever additional precautions he considers necessary to protect himself and others from injury in case a bottle should unexpectedly fail.
All catalysts must be handled cautiously because of their highly reactive nature. Although virgin metal catalysts are generally safe themselves, care must be taken when they are brought into contact with organic liquids or combustible vapors in the presence of oxygen because of their ability to promote rapid oxidation. Any catalyst that has been exposed to hydrogen is also potentially hazardous and may ignite spontaneously as it dries. For this reason, used catalysts must always be kept wetted and out of contact with combustible vapors or solids.
BOTTLE HEATERS
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:
HEATING MANTLES
| Mantle No. | Watts | Volts | Use with Bottle No. |
| A450EEB | 100 | 115 | 66CA, 66CA2 |
| A450EEE | 100 | 230 | 66CA, 66CA2 |
| A451EEB | 200 | 115 | 71CA, 72CA, 72CA4, 126CA |
| A451EEE | 200 | 230 | 71CA, 72CA, 72CA4, 126CA |
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, or into an electric outlet. Heating mantles do not work well on bottles that have been covered with fiberglass. They work best on plain glass 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 within one degree C in the 0 to 100ºC 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 (UUCSA) grounded plugs and sockets.
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.
For supplemental Instructions for the 4833 Controller see Manual 311M.
THERMOCOUPLE ASSEMBLIES
| Assembly No. | Equipped w/Thermocouple | Fits Bottle No. | Fits Bottle Size |
| A159CAPA | A295E | 66CA2 | 250 mL |
| A159CA2PA | A295E | 66CA | 500 |
| A159CA3PA | A295E2 | 71CA | 1000 |
| A159CA4PA | A295E2 | 72CA | 2000 |
| 72CA4 | 3000 | ||
| A159CA5PA | A295E2 | 126CA | 1700 |
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.
ELECTRIC MOTORS
A 1/6 hp motor drives the bottle shaker for the 3911 hydrogenator with an enclosed vee-belt drive. On the larger, 3921 apparatus the shaker is driven by a 1/4 hp 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 will have a temporary connecting cord and switch which are not explosion proof. An explosion proof switch and wiring will have to be provided by the user.
CSA CERTIFICATION
Parr hydrogenators operating on 115 volts are certified to the electrical code of the Canadian Standards Association. CSA certification is not provided for 230 volt units.
DIMENSIONS AND WEIGHTS
| 3911 Hydrogenator | 3921 Hydrogenator | |
| Base plate | 21-1/2 x 15 in. | 26 x 20 in. |
| Overall height | 14 in. | 17 in. |
| Net weight | 58 lb. | 160 lb |
| Shipping weight | 65 lb. | 180 lb. |
OTHER PARR HYDROGENATORS
In addition to the shaker type hydrogenators described in this bulletin, Parr also offers other pressure reactors that are widely used for catalytic reactions with hydrogen. These include Stirred Reactors made of stainless steel and other corrosion resistant alloys in sizes from 300 mL to 2 gallons for use at pressures up to 2000 psig (136 atm) and temperatures to 350ºC. These are complete working units with all necessary controls and many convenient operating features.
ACE GLASS
Ace Glass offers a Parr Shaker Type Hydrogenator modified with their glassware and a solvent trap. More information may be found at:
http://www.aceglass.com
Ph: 800-223-4524
E-mail: sales@aceglass.com
Parr Shaker Type Hydrogenation Apparatus
Shaker Type Hydrogenation Apparatus 
Today's Date: 03 September 2010
Parr Instrument Company
211 Fifty Third Street
Moline, Illinois 61265-9984
1-800-872-7720 / (309) 762-7716 FAX (309) 762-9453
Email: parr@parrinst.com
OTHER PARR HYDROGENATORS
In addition to the shaker type hydrogenators described in this bulletin, Parr also offers other pressure reactors that are widely used for catalytic reactions with hydrogen. These include Stirred Reactors made of stainless steel and other corrosion resistant alloys in sizes from 300 mL to 2 gallons for use at pressures up to 2000 psig (136 atm) and temperatures to 350ºC. These are complete working units with all necessary controls and many convenient operating features.
ACE GLASS
Ace Glass offers a Parr Shaker Type Hydrogenator modified with their glassware and a solvent trap. More information may be found at:
http://www.aceglass.com
Ph: 800-223-4524
E-mail: sales@aceglass.com
Parr Shaker Type Hydrogenation Apparatus
Shaker Type Hydrogenation Apparatus
Today's Date: 03 September 2010
Parr Instrument Company
211 Fifty Third Street
Moline, Illinois 61265-9984
1-800-872-7720 / (309) 762-7716 FAX (309) 762-9453
Email: parr@parrinst.com