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4550
User Manual
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Parr Instrument 4550 User Manual

4550
Floor Stand Reactors
Operating Instruction Manual
395M
Floor Stand Reactors
PREFACE 3
Fixed Head or Removable Head Design 6
INSTALLATION 7
HOW TO USE THE VESSEL 14
Fixed Head Vessels 14
To open the Vessel 14
Before Closing the Vessel 14
To Close the Vessel 14
Removable Head Vessels 14
To Open the Vessel 14
Before Closing the Vessel 14
To Close the Vessel 14
Sealing Vessels with PTFE Gaskets 14
Gas Connections 14
Pressurizing the Vessel 15
Do Not Overfill the Vessel 15
Releasing Pressure 15
Withdrawing Liquid Samples 15
Initial Operating Test 15
MAINTENANCE 16
General Maintenance Notes 16
Periodic Pressure Tests 17
IDENTIFY THE VALVES 10
Gas Inlet Valve 10
Gas Release Valve 10
Liquid Sampling Valve 10
OTHER VESSEL HEAD FITTINGS 11
Safety Rupture Disc 11
Type J Thermocouple 11
Pressure Gage 11
Gage and Valve Adapters 11
ACCESSORIES 12
Internal Cooling Coils 12
Variable Speed Electric Motor 12
Air Motor 12
Liners 12
Spare Parts Kit 12
Pneumatic Lift for Fixed Head Vessels 13
PARTS LISTS 18
Reaction Vessel Parts List 18
Overarm Parts List 21
Cooling Coil Parts List 22
Heaters Parts List 23
DRAWINGS 24
4553 - 1 Gallon Fixed Head Stand Assembly 24
4554 - 2 Gallon Fixed Head Stand Assembly 26
Customer Service
Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department:
1-309-762-7716 • 1-800-872-7720
Fax: 1-309-762-9453
E-mail: parr@parrinst.com
http://www.parrinst.com
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Parr Instrument Company
4550 Floor Stand Reactors

PREFACE

Scope

These instructions describe the installation, opera­tion and maintenance of Parr Series 4550 Floor Stand Reactors offered in two sizes, 1 and 2 Gallon (3.75 and 7.5 liter). They cover the basic steps to be followed when 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 that 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 included to further your understanding of this instrument and its component parts:
No. Description
201M Limited Warranty
230M Safety Precautions to be observed when
operating Pressure Reaction Equipment
231M Operating Instructions for Parr Safety
Rupture Discs
234M Operating and Maintenance Instructions
for Parr Magnetic Drives
323M Operating Instructions for Parr Pressure
Relief Valves
548M Operating Instructions for 4848 Reactor
Controllers
FX004 Health & Safety Assurance Certification

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.

Intended Usage

This system has been designed for use as a high 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 this equipment is used in a manner beyond its intended usage, the protection provided by the equipment may be impaired.
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 Reactor Controllers operate with a Type J (iron-constantan) 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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4550 Floor Stand 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.
Caution! Do not use in hazardous atmospheres.
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: 0 to 2000 meters above sea level.
Storage: -25 °C and 65 °C; 10% to 85% relative
humidity.

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. The vessel, motor, heater, and temperature controller may be packed separately for convenience in shipping, but these parts are easily reassembled. 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 4550 Floor Stand Reactor and its components are very heavy. Before moving ensure all cables are disconnected. Use proper and safe lifting techniques when installing or moving the 4550 Reactor and/ or its components.

Cleaning & Maintenance

Periodic cleaning may be performed on the exterior surfaces of the instrument with a lightly dampened cloth containing mild soap solution. All power should be disconnected 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 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
4550 Floor Stand Reactors

User’s 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 which 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 a choice between over- or 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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4550 Floor Stand Reactors

Fixed Head or Removable Head Design

Parr Series 4550 Series Reactors are furnished with two structural options in addition to the size, pressure range, stirrer motor, controller and similar options. These are:

Fixed Head or Removable Head Vessel Design

In the fixed head design, the head of the vessel may remain fixed in the reactor support stand. All attachments to the head, gas and liquid feed and discharge lines, cooling water, vapor take-off and condenser, thermocouple, and any electrical leads can remain permanently in place. The reactor is opened by removing the cover clamp sections and lowering the cylinder away from the head.
In the removable vessel design, the entire vessel must be removed from the support stand for charg­ing, product recovery, and cleaning.
There is no difference in the pressure or temperature limits or basic operating instructions based upon the fixed head or movable vessel options. There are dif­ferences in the design of the stand components which adapt the vessels to the support system.

Flat PTFE Gasket or Self Sealing O-ring Closure

The flat gasket is held in a recess in the vessel head and a machine pilot on the cylinder closes the recess to completely contain the gasket. The split ring closure used with this gasket has six cap screws which must be tightened to develop the loading on the gasket.
The self sealing design features an O-ring retained in a groove on the vessel head. This design is self seal­ing and the split ring used with this sealing system does not require nor have the cap screws used with the flat gasket.
Maximum temperatures of a given system are de­pendant upon the material of construction and type of seal. Other accessories may limit operating tem­perature. The flat PTFE gasket can be used to operat­ing temperatures as high as 350 °C. The flat flexible graphite gasket can be used to operating temperatures as high as 500 °C. The maximum temperature of the vessels equipped with O-ring seals depends upon the material used for the O-ring. The most common material is a fluoroelastomer (FKM) which has a 225 °C maximum operating temperature limit.
Fixed Head with O-ring
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Parr Instrument Company
Moveable Head with Flat Gasket

INSTALLATION

Pressure and Temperature Limits

4550 Floor Stand Reactors
The working pressure and temperature at which any reactor or pressure vessel can be used will depend upon the design of the vessel and the materials used in its construction. Since all materials lose strength at elevated temperatures, any pressure rating must be stated in terms of the temperature at which it applies. The standard material of construc­tion for Parr Instrument Company is Type 316 Stain­less Steel.
Limits for vessels made of other materials and for other operating temperatures can be obtained from Parr Customer Service. No attempt should be made to increase these limits by making alterations or by substituting components that 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 vessels will be determined by the physi­cal characteristics of the vessel material and will be prescribed on an individual basis.
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 one and two gallon reactors must not exceed the following maximum limits:
Pressure Vessel and Temperature Limits
Vessel Material Maximum Pressure Maximum Temperature
T316SS 1900 psig 350 °C PTFE Flat Gasket
T316SS 1900 psig 300 °C FFKM O-ring
T316SS 1900 psig 225 °C FKM O-ring
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4550 Floor Stand Reactors

Assemble the Reactor

These reactors require at least 10 sq. ft. of work­space in a well-ventilated area with convenient access to an electric outlet, running water, air and a drain. This unit needs to be placed at least 10 inches away from walls or flammable materials.
1. Set the stand in the workspace.
2A. Removable Vessels.
First pivot the overarm assembly to the back of the support stand.
The pressure vessel has been shipped as a complete assembly; it may be easiest on the initial setup to place the entire pressure vessel assembly into the heater. Note: The complete assembly does not need to be removed from the heater during opening and closing operations. It is designed so that the cylinder can remain in the heater while the head and split rings are attached or removed.
Once the vessel assembly is in place rotate the magnetic stirrer by hand to make sure that it turns freely. Then move the overarm back into position above the vessel. The knob on the top of the overarm will raise the upper shaft with coupling for attachment to the adapter on the top of the magnetic stirrer. Push down and rotate the upper shaft to bring these compo­nents into alignment.
Occasionally the motor housing and overarm as­sembly may vibrate out of the standard position. If the upper shaft is not in alignment with the center of the top of the magnetic stirrer it will be necessary to loosen the bolt which attaches the motor housing to the support stand. Remove the motor housing panel; there is a single bolt that runs through the lower housing support and the top shelf of the floor stand. Once the bolt is loosened, rotate the housing the required amount, connect the upper shaft to the magnetic stirrer and then tighten the motor housing bolt.
2B. Fixed Head Reactor.
Bolt the stand to the floor using the holes in the base plate.
Loosen the panel screw of the vessel retainer mounted on the midplate of the support stand and open the retainer bracket.
The pressure vessel has been shipped as a complete assembly. It is necessary to loosen the split ring bolts and remove the split ring. Lift the head assembly out of the cylinder and slide it into the midplate of the stand. Close the retainer bracket. The cylinder should be placed in the cylinder lift bracket.
Rotate the magnetic stirrer by hand to make sure that it turns freely.
Connect an air line to the 1/4” quick disconnect fitting at the base of the support stand. This pneumatic lift package will raise or lower the cylinder. It may also be used for the heater. The lever on the side panel of the support frame controls the lift motion.
The pneumatic package includes a pressure regulator with gage located inside of the support stand housing. It can be accessed by removing the back panel of the support stand. The regula­tor has been preset to 50 psi. The regulator can be adjusted by lifting up on the cap. Rotate clockwise to increase pressure, counter-clock­wise to decrease the amount of pressure sent to the pneumatic lift cylinder. Press the cap back down after setting the pressure.
The flow control valves have been preset for optimum performance. Both the speed and lifting capacity of the pneumatic lift package can be adjusted with the flow control valves located on the input and output ports of the pneumatic cylinder.
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Parr Instrument Company
4550 Floor Stand Reactors
3. Set the Reactor 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.
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:
5. Plug the motor cord into the motor socket on the rear of the controller.
Secure the clamp on the motor cord with the provided screw next to the motor socket for safety purposes.
6. Connect the thermocouple and extension wire to both the thermocouple and to the controller in the “Primary Temp Input” position on the rear panel. Insert the thermocouple in the 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 the magnetic drive. See Instruction Manual No. 234M.
9. Connect tubing to the rupture disc outlet and run to a safely vented area. See Instruction Manual 231M.
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 solid state relay located in the 4848 Controller.
Parr Motor Only:
The Motor output connector is to be used only with Parr Instrument Company motor assemblies supplied with the appropriate motor power cord.
4. Connect the heater cord from the heater into the heater socket on the rear panel of the Series 4848 Reactor Controller.
10. Note the voltage and amperage requirement stamped on the controller data plate, and then plug the power cord into an appropriate outlet. Power for these reactors should be drawn from a grounded outlet capable of carrying up to the full current rating of the reactor.
11. If an electric stirrer motor is supplied, turn the speed control knob fully counterclockwise on the Reactor Controller, turn on the motor switch and slightly increase the speed for a short run to check the stirrer drive system but do not turn on the heater, put heater toggle switch in center position (OFF). There must always be a vessel in the heater when it is turned on, and the vessel and heater sizes must match. If the heater is op­erated without proper size vessel in contact with the mantle, the mantle may overheat and fail.
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