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5100
User Manual
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Parr Instrument 5100 User Manual

5100
Low Pressure Reactors
Operating Instruction Manual
378M
5100 Low Pressure Reactors
Preface 3
Installation 6
Do Not Overfill the Vessel 11
Releasing Pressure 11
Withdrawing Liquid Samples 11
Initial Operating Test 11
Maintenance 12
General Maintenance Notes 12
Periodic Pressure Tests 13
Technical Support 13
Parts List 14
Cylinders 14
Heads 14
Internal Fittings 14
External Fittings 17
Accessories 18
Heaters 18
Identify the Valves 9
Other Vessel Head Fittings 9
Accessories 10
Air Motor 10
Spare Parts Kit 10
Mantle Heaters 10
Variable Speed Electric Motor 10
Cooling Loop 10
Product Features and Part Identification 19
5100 Stand 19
Stand for 5100 20
Stand for 5110 21
5100 Overarm 22
5100 Internals 23
5111 & 5112 Internals 26
5100 Metal Vessels Internals 27
5100 Head Assembly 28
5110 Head Assembly 29
5100 Head Fittings and Valves 30
5110 Head Fittings and Valves 30
Customer Service
Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department:
How to use the Vessel 11
Gas Connections 11
Pressurizing the Vessel 11
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Parr Instrument Company
1-309-762-7716 • 1-800-872-7720
Fax: 1-309-762-9453
E-mail: parr@parrinst.com
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5100 Low Pressure Reactors

Preface

Scope

These instructions describe the installation, opera­tion and maintenance of Parr Series 5100 Fixed Head Bench Top Reactors offered in six sizes from 160 mL to 1.5 L with glass and/or metal cylinders. They cover the basic steps to be followed for installing these reactors and describe the function of all standard components. They are intended to be used in con­junction with several related instruction sheets listed on the previous page. This information describes several components which are common to most Parr pressure reaction equipment, and includes safety precautions and other related information applicable to all reaction laboratories. The users should study all of these instructions carefully before starting to use these vessels so that they will fully understand the capabilities and limitations of the equipment.

Related Instructions

The following Parr publications are also available to further your understanding of this instrument and its component parts:
No. Description of Instructions
230M Safety Precautions to be observed when
operating Pressure Reaction Equipment
231M Parr Safety Rupture Discs 548M 4848 Reactor Controllers 549M 4848 Controller CD-ROM 553M A2110E Motor Controller 234M Parr Magnetic Drives 323M Parr Pressure Relief Valves 201M Limited Warranty FX004 Health & Safety Assurance Certification

Intended Usage

This system has been designed for use as a low pressure reactor system. It has been designed, built, and tested to strict physical and electrical standards. However, it is the user's responsibility to install and operate it in conformance with local pressure and electrical codes.
If the instrument is used in a manner not specified by Parr Instrument Company, the protection pro­vided by the equipment may be impaired.

Safety Information

To avoid electrical shock, always:
1. Use a properly grounded electrical outlet of correct voltage and current handling capability.
2. Ensure that the equipment is connected to electrical service according to local national electrical codes. Failure to properly connect may create a fire or shock hazard.
3. For continued protection against possible hazard, replace fuses with same type and rating of fuse.
4. Disconnect from the power supply before maintenance or servicing.
To avoid personal injury:
1. Do not use in the presence of flammable or combustible materials; fire or explosion may result. This device contains components which may ignite such material.
2. Refer servicing to qualified personnel.
General Specifications
Electrical Ratings
Controller ratings are found in the Operating Instruc­tions for the controller supplied with your reactor and on the controller data plate.
Before connecting a controller to an electrical outlet, the user must be certain that the electrical outlet has an earth ground connection and that the line, load and other characteristics of the installation do not exceed the following limits:
Voltage: Fluctuations in the line voltage should not exceed 10% of the rated nominal voltage shown on the data plate.
Frequency: Controllers can be operated from either a 50 or 60 Hertz power supply without affecting their operation or calibration.
Current: The total current drawn should not exceed the rating shown on the data plate on the controller by more than 10 percent.
Thermocouple: Unless otherwise specified, all Series 4848 Controllers operate with a Type J (iron­constantan) thermocouple. The total resistance of the thermocouple and the lead wires should not exceed 100 ohms. If the resistance of the thermo­couple circuit is higher, it will reduce the sensitivity of the control system.
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5100 Low Pressure Reactors

Explanation of Symbols

II On position, full power heater switch
I On position, half power heater switch
O Off Position
~ Alternating Current (AC)
This CAUTION symbol may be present on the Product Instrumenta­tion and literature. If present on the product, the user must consult the appropriate part of the accompanying product literature for more information.
This CAUTION symbol indicates that the surface may be hot.
Protective Earth (PE) terminal. Provided for connection of the Protec­tive Earth (green or green/yellow) supply system conductor.
Environmental Conditions
This instrument is intended to be used indoors.
Operating: 15 ºC to 35 ºC; maximum relative humidity of 80% non-condensing.
Installation Category II (over voltage) in accordance with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Caution! Do not use in hazardous atmospheres.

Unpack Carefully

Unpack the equipment carefully and check all the parts against the packing list. If shipping damage is discovered, report it immediately to the deliver­ing carriers. Examine the components closely for any loose parts or shipping damage and be sure to check all layers of packing materials thoroughly so as not to overlook any parts which might otherwise be discarded.

Provisions for Lifting and Carrying

The Parr Series 5100 Fixed Head Bench Top Reactors and its components are very heavy. Before moving ensure all cables are disconnected. Use proper and safe lifting techniques when installing or moving the Parr Series 5100 Fixed Head Bench Top Reactors and/ or its components.

Cleaning & Maintenance

Periodic cleaning may be performed on the exterior surfaces of the controller with a lightly dampened cloth containing mild soap solution. All power should be disconnected and the power cord should be unplugged when cleaning the instrument.
There are no user serviceable parts inside the prod­uct other than what is specifically called out and discussed in this manual. Advanced troubleshooting instructions beyond the scope of this manual can be obtained by calling Parr Instrument Company in order to determine which part(s) may need to be replaced or serviced.
Ensure that any hot surfaces have had adequate time to cool before cleaning or maintaining the reactor and/or its components.
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Parr Instrument Company
5100 Low Pressure Reactors

Users Responsibility

All Parr reactors and pressure vessels are designed and manufactured with great care to assure safe operation when used within their prescribed temperature and pressure limits.
But… the basic responsibility for safety when using this equipment rests entirely with the user; who must:
1. Select a reactor or pressure vessel that has the
capability, pressure rating, corrosion resistance, and design features that are suitable for its intended use. Parr engineers will be glad to discuss available equipment and material options with prospective users, but the final responsibility for selecting a reactor or pressure vessel that will perform to the user's satisfaction in any particular reaction or test must rest with the user - not with Parr.
In exercising the responsibility for the selection of pressure equipment, the prospective user is often faced with the choice between over­or under-designed equipment. The hazards introduced by under-designed pressure vessels are readily apparent, but the penalties that must be paid for over-designed apparatus are often overlooked. Recognizing these criteria, Parr reactors and pressure vessels are offered in several different styles, each designed for convenient use in daily operation within certain temperature and pressure limits, using gaskets, closures, and other elements carefully selected for safe operation within the limits specified for that design. But in order to preserve the validity of these designs, all temperature and pressure limits must be observed, and no attempt should be made to increase these limits by making alterations or by substituting components which are not recommended by Parr Instrument Company.
2. Install and operate the equipment within a suitable barricade, if required, with appropriate safety accessories and in full compliance with
local safety codes and rules.
All standard Parr pressure vessels are provided with either a suitable relief device or a means to attach one (typically in the form of a plugged opening). When a pressure vessel is delivered without a pressure venting device, it is the cus­tomer’s responsibility to provide pressure relief in order to protect the operator and the equip­ment from destructive high pressures. If you need more information or need help in selecting a proper relief device, please contact Parr Instru­ment Company.
3. Establish training procedures to ensure that any person handling the equipment knows how to use it properly.
4. Maintain the equipment in good condition and establish procedures for periodic testing to be sure the vessel remains structurally sound.
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5100 Low Pressure Reactors

Installation

Pressure and Temperature Limits

The maximum working conditions for Parr vessels are stamped on the cylinder. No attempt should be made to increase these limits by making altera­tions or by substituting components which are not recommended by the Parr Instrument Company. It must also be understood that lower pressure and temperature limits may be required for modified reactors and for vessels made of special alloys. Limits for such vessels will be determined by the physical characteristics of the vessel material and will be prescribed on an individual basis.
Working temperatures up to 225 °C are permissible in reactors equipped with fluoroelastomer (FKM) O-ring seals, such as Viton®. The higher the operat­ing temperature above 200 °C, the shorter the life of the O-ring will be. Perfluoroelastomer (FFKM) O-ring seals such as Kalrez® have a broad chemical resis­tance. Unfortunately, they are very expensive and will generally be reserved for unique applications. Ethylene propylene (EP) O-rings can be used to 170 °C and are recommended for applications where solvents such as ammonia and amines which will rapidly destroy fluoroelastomer O-rings.
The maximum working pressure and temperature for any vessel is governed by the design of the vessel and the strength of the material from which it is constructed. There is also a close relationship between working pressure and temperature since the strength of any material will normally fall off as the temperature is increased. Temperature and pressure limits are also affected by the physical properties and temperature limits of the gaskets and seals used in the vessel, and by any valves, gages or other fittings attached to the vessel. Obviously, the safe operating pressure of any system can be no higher than that of its lowest rated component.
All Parr reactors show the maximum safe operating pressure and temperature imprinted on the cylinder. The working pressure and temperature in these 160 mL to 1.5 L reactors must not exceed the following maximum limits:
Pressure and Temperature Limits
Vessel Material
Glass 150 psi 225 °C T316 SS 1000 psi 225 °C
Maximum Pressure
Maximum Temperature

Assemble the Reactor

These reactors require at least 10 inches of work­space from walls or flammable materials on a sturdy bench, table, or floor in a well ventilated area with convenient access to an electric outlet, running water, and a drain. If the tabletop is not heat resis­tant it would be ideal to provide an insulated pad on which to set the vessel when it is hot.
Review the following instructions first, prior to as­sembling the reactor.
1. Set the stand in the workspace.
Bolt the stand to a workbench or to the floor using the holes in the base plate.
Place the head assembly in the stand. Make sure the O-ring that seals the head and the cylinder together is installed in the head groove.
Two types of glass cylinders can be used with this apparatus (jacketed and non-jacketed) If a jacketed cylinder is being used, remove the jacket connection hoses, if present. A pair of split rings, with thumbscrews, is used to join the head and the cylinder flanges. The split rings are lined at the bottom with plastic cushions that eliminate metal against glass contact that could result in dangerous point loading on the glass. Examine the plastic cushions carefully. If they are cracked or otherwise appear damaged, they should be replaced.
CAUTION! Take care when handling the glass cylinder. If any of the pressure or load bearing surfaces become chipped or scratched, the pressure rating of the cylinder will be compromised.
If a metal cylinder is also being used with this apparatus, note that the split rings differ from those provided for a glass cylinder. Split rings intended for sealing a metal cylinder to a metal head should not be used with glass cylinders. A clasp system on both ends of the split rings is used to ensure proper alignment when as­sembled. Before using the split rings to mate the head and the cylinder, make sure the three thumbscrews on each half ring are backed off so that the end of the screw is flush with the inside of the split ring. Both sets of split rings feature thumb screws to be installed finger-tight.
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Parr Instrument Company
5100 Low Pressure Reactors
Carefully bring the flange of the glass cylinder in contact with underside of the reactor head. A lab jack / cork support is provided for 1.0 and
1.5 liter glass reactors. When using the lab jack, bring the cylinder flush with the O-ring in the head, ensuring no stress is put on the glass. Align the major OD of the head with the OD of the cylinder flange. If a jacketed cylinder is being used, orient the cylinder so that the jacket connections are oriented to either side. Hold the cylinder carefully at the bottom with one hand, slide one of the half split rings onto the head/cyl­inder flanges, and rotate/slide around the head/ cylinder flanges until the latches are facing you. Use one hand to steady this half split ring to the head/cylinder flanges as you attach the other half split ring from the front. Secure the latches. If using a lab jack, now lower it so that cylinder hangs freely.
At this point, the glass cylinder will be held in place loosely and can be rotated for proper ori­entation if needed. Tighten the six thumb screws two at a time, 180 degrees apart in a criss-cross pattern rather than progressively around the circle until finger-tight and the head flange is flush with the top of the cylinder flange. Do not over-tighten.
Labeled connections are provided on the rear panel of the controller.
Parr Cooling Only:
The Parr Cooling output connector is to be used only with Parr Instrument Company cooling solenoid valve assemblies supplied with the appropriate cooling power cord.
Parr Heating Only:
The Parr Heating output connector is to be used only with Parr Instrument Company heater assemblies supplied with the appropriate heater power cord.
Note: Do not make connections to a Variac, Powerstat or the like to attempt to control the heating output. The heavy inductive load on the primary side of such devices can destroy the internal sold state relay located in the 4848 Controller.
CAUTION! Never use tools, such as pliers, to tighten the thumbscrews. Excessive loading on the cylinder flange can compromise the pressure rating of the cylinder.
CAUTION! Before applying pressure to the reactor, install the transparent Lexan safety shield onto the front of the reactor stand. Failure to do so can result in serious injury if the cylinder should break under pressure.
To remove the cylinder from the head, follow the above procedure in the reverse order. If a jack­eted cylinder is being used, drain and disconnect the jacket hoses first.
2. Set the Controller near the reactor, leaving a space of at least six inches between the controller and the base of the reactor so that the controller will not be unduly affected by radiant heat. Connect the reactor to the controller using information contained in its Instruction Manual 548M or follow the steps below.
Parr Motor Only:
3. The support and heater are shipped fully assembled. The heater raises and lowers on its support rod to permit the vessel or cylinder to be removed. Lower the heater, open the hinged retainer on the front of the support and slide the vessel into its support. Fixed head vessels have a square lip which fits into a matching groove in the support plate. Removable vessels are supported by the split rings which rest on top of the support plate. The stirrer drive connector lifts by rotating and lifting the knob above the belt guard. The universal joint contains a cross pin that slips into the groove on top of the magnetic drive.
4. Connect the heater cord from the heater into the heater socket on the rear panel of the Series 4848 Reactor Controller.
5. Plug the motor cord into the motor socket on the rear of the controller.
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5100 Low Pressure Reactors
Secure the clamp on the motor cord with the provided screw next to the motor socket for safety purposes.
6. Connect the thermocouple extension wire to both the thermocouple and to the controller in the “Primary Temp Input” position on the rear panel. Insert the thermocouple into thermowell.
7. Connect leads from accessory packages such as tachometer, pressure transducer and high temp cut-off to the designated positions on the back panel of the 4848 Controller.
8. Connect cooling water to internal cooling coil if installed.
9. Connect cooling water to the magnetic stirrer. See Instruction Manual 234M.
10. Connect tubing to the rupture disc outlet and run to a safely vented area. See Instruction Manual 231M.
11. Note the voltage requirement on the controller identification label on the back panel, and then plug the power cord into an appropriate outlet. Power for these reactors should be drawn from a 3-slot, grounded outlet capable of carrying up to the full current rating of the system.
12. Using the switch on the Reactor Controller, turn on the motor for a short run to check the stirrer drive system.
This apparatus includes a safety shield which should be used at all times. A relief valve pre-set to either 145 psi (CE certified) or 150 psi is also provided as a safety precaution to prevent over-pressurizing the glass cylinder - this also should be used at all times. Should this relief valve be inadvertently removed, the glass vessel could be over-pressurized, resulting in an explosion. The safety shield has been designed to withstand the force of this explosion. However, in the event of an explosion, some glass fragments will exhaust through the vertical slots provided in the back of the shield for the hoses.

Assembling and Connecting the Circulator Jacket Hoses

CAUTION! If a jacketed vessel is being used, the compression fittings should be pre­assembled onto the insulated hoses before attaching them to the cylinder. Failure to do so or tightening any of the compression fittings while the hoses are attached to the cylinder will likely cause the jacket nipple to break off.
Once the hoses are fixed at one end, they tend to have a preferred orientation. The following hose assembly procedure will minimize any side loading by the hoses against the jacket connection nipples.
Attach the hoses to the circulating bath first and route them through the openings at the rear of the reactor stand. Note that lower left connection is the jacket inlet. This should be connected to the circulator pump discharge. Elbows are used on the cylinder end to route the insulated hoses down and then out the rear of the stand. With the hose in its free state and not being twisted or rotated, tighten the elbows to the hoses in a manner that orients the open end of the elbow in line with the jacket nipple. This minimizes any side loading of the hose against the nipple.
Slide the brown plastic nut onto the nipple adapter so that the flange with the O-ring groove is recessed inside the nut. Tighten the tube stub onto the elbow. Place the O-ring in the groove of each of the as­sembled adapters and then screw the hose adapter onto the jacket nipple. Tighten firmly, by hand only!
No pliers!

Draining the Jacket

To drain the jacket, first lower the temperature of the jacket circulating fluid to 60 °C or less.
Note: Oil, used as the circulating fluid, drains much faster when it is hot.
Turn off the circulator and loosen the hose connec­tion at the top of the jacket. This will allow air to enter the jacket and cause to fluid to drain back into the circulator. When the draining is complete, both hoses can be disconnected from the jacket. The ends of the hoses should be supported at a level higher than that of the circulator bath to prevent siphoning and fluid loss.
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Parr Instrument Company
5100 Low Pressure Reactors

Identify the Valves

Gas Inlet Valve

The gas inlet valve is easily identified when the vessel is open by noting that it is connected to a dip tube which extends to a point near the bottom of the vessel cylinder. This is an angle valve with an attached fitting which provides a socket for attaching the A495HC pressure hose furnished with the reactor.

Gas Release Valve

The gas release valve is connected to the gage adapter on vessels with volumes of 160 – 600 mL. The gas release valve is installed in a port by itself on 1 L & 1.5 L vessels. These ports do not have a threaded connection on the underside of the head; they are always open to the gas phase of the reactor.

Liquid Sampling Valve

The liquid sampling valve is attached to the same fitting as the gas inlet valve and connected to a common dip tube. With this arrangement, incoming gas is always introduced below the surface of the liquid and the operator is provided with a means for clearing the dip tube to be sure that any sample taken during a run will be representative of the charge. This can be done by opening the upper gas inlet valve momentarily to allow the inlet gas to force any liquid in the dip tube back into the reactor before withdraw­ing a sample from the sampling valve.

Relief Valve

The relief valve is connected to the gage adapter and is pre-set to either 145 psi (CE certified) or 150 psi to ensure that the glass cylinder is not over­charged. When using a metal cylinder, a plug is provided so that the relief valve can be removed (due to higher pressure rating of metal cylinder).

Other Vessel Head Fittings

Safety Rupture Disc

There is a safety rupture disc attached to the head which is intended to rupture and release the pres­sure before it reaches a dangerous level. A metal tag wired to the safety head identifies the burst pres­sure at room temperature for that particular disc. A similar tag is furnished with each replacement disc. This tag must remain with the apparatus at all times so that both present and future operators will be aware of the disc rating. Users should read the discussion of rupture discs given in the Instruction Sheet No. 231M for a complete description of the characteristics of rupture discs and the precautions to be observed when operating pressure equipment protected by this type of safety device. The disc is rated for 1000 psi and should remain installed for both glass and metal cylinders.

Pressure Gage

A pressure gage, typically 200 psi gage for glass cylinders and 1000 psi gage for metal cylinders includes a T316 Stainless Steel Bourdon tube. It is mounted on the head using attachment fittings similar to those used for the inlet/sampling valve assembly.

Type J Thermocouple

A Type J thermocouple in a 1/8” diameter stainless steel sheath is furnished with the reactor. Insert this thermocouple into the head thermowell and con­nect it to the thermocouple socket on the rear panel of the reactor controller using the extension wire furnished with the reactor.
*See Page 30 for drawing of head fittings and valves.
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5100 Low Pressure Reactors

Accessories

Air Motor

Variable stirring speeds from 100 to 2000 rpm with no spark hazard can be obtained by replacing the standard motor with an air motor. This motor oper­ates on compressed air which must be supplied at 40 psig minimum pressure with at least 10CFM available at that pressure. It is furnished with a speed control valve and oiler, all assembled on a mounting bracket.
To operate reactors equipped with an air motor, mount the drive system firmly on the support stand and connect the air hose to a compressed air line. Fill the oiler with SAE 10 oil and adjust the oiler to feed one drop per minute into the air stream. For long continuous runs at high speeds, the oiling rate should be increased to three drops per minute. If the motor becomes sluggish, flush it with a non-flam­mable solvent in a well-ventilated area. Disconnect the air line and muffler and pour a small amount of solvent into the inlet port. Rotate the shaft by hand in both directions for a few minutes; then connect the air line and run the motor until there is no further trace of solvent in the exhaust. If the muffler felts are dirty, wash them in solvent or replace them. Relubricate the motor with a squirt of oil into the chamber and reassemble. If it becomes necessary to disassemble the motor to replace the vanes, follow directions given in the instruction sheet published by the Gast Manufacturing Corp., Benton Harbor, Michigan.

Spare Parts Kit

Parr can furnish spare parts kits for these reactors which will provide a reserve supply of parts and tools sufficient to handle most normal replacements and emergency repairs during a year of heavy usage.
These kits contain replacement gaskets, packing, O-rings, shafts, bearings, and rupture discs. They can be ordered from any Parr Dealer or direct from the Parr Instrument Company. The order must specify the reactor size and indicate type of rupture disc, stirrer drive and whether it has a flat-gasket or O-ring closure.

Mantle Heaters

Mantle heaters with high temperature fabric heating mantles housed in sturdy aluminum shells can be provided for any plain (non-jacketed) cylinder. These heaters are designed to provide uniform heat dis­tribution to the walls and bottoms of these vessels. They are attached to a support rod with a spring steel clamp and arranged so that they can be raised or lowered on the rod as desired. Each mantle must always be used with the vessel of the size for which it was designed, and must always be fully attached to the vessel before heat is turned on. Similarly, a short vessel must never be heated in a deep mantle. Without full contact with a vessel wall, a mantle will overheat and burn out.

Variable Speed Electric Motor

Reactors are normally equipped with a DC variable speed motor supplied and controlled through the Series A2110E or 4848 Controllers. Instructions for connecting and operating these motors are included in the controller’s instruction manual No. 553M or 548M. This motor is installed in a drive system designed to produce stirring speeds from 0 to 1700 rpm.

Cooling Loop

Each 5100 Reactor has a single loop cooling coil installed in the vessel (except the 160 & 215 mL units). A slow, continuous flow of cold water through a cooling loop proves a very effective means for controlling temperature overshoot in these reactors, particularly when operating at tem­peratures below 150 °C. Water flow through the loop can be controlled automatically using a solenoid valve in the cold water line, with the solenoid con­nected to the cooling socket on the rear panel of the 4848 Reactor Controller. With this arrangement, cold water will be admitted to the cooling loop whenever the controller calls for cooling.
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