Parr Instrument 4520 User Manual

383M

4520

BenchTop Reactors

Operating Instruction Manual

Parr Instrument Company

4520 Bench Top Reactors

TABLE OF CONTENTS
Related Instructions............................	2
Customer Service...............................	2
Preface ....................................................	3
Scope .................................................	3
Safety Information ..............................	3
General Specifications .......................	3
Explanation of Symbols......................	4
Environmental Conditions ..................	4
Provisions for Lifting and
Carrying..............................................	4
Cleaning and Maintenance………......4
Intended Usage ..................................	5
User’s Responsibility ..........................	5
Unpack Carefully ................................	5
Installation ..............................................	6
Pressure and Temperature
Limits ..................................................	6
Assemble the Reactor............................	7
Fixed Head or Removable Head
Vessel Design ....................................	9
Flat PTFE Gasket or Self Sealing
O-ring Closure ....................................	9
Identify the Valves..................................	10
Gas Release Valve.............................	10
Gas Inlet Valve ...................................	10
Liquid Sampling Valve........................	10
Other Head Fittings................................	12
Safety Rupture Disc ...........................	12
Type J Thermocouple.........................	12
Pressure Gage ...................................	12
Gage and Valve Adapters ..................	12
How to Use the Vessel...........................	13
PTFE Gasket or O-ring Seal ..............	13
Fixed Head Vessel Installation ...........	13
Moveable Head Vessel Installation ....	13
Sealing Vessels with PTFE Gaskets ..	13
Sealing Vessels with O-ring Seals .....	13
Gas Inlet / Liquid Sampling Valves.....	13
Gas Connections................................	13
Pressurizing the Vessel .....................	14
Do Not Overfill the Vessel ..................	14
Withdrawing Liquid Samples ..............	14
Releasing Pressure ............................	14
To Open the Vessel at Completion
of a Test .............................................	15
Initial Operating Test ..........................	15
Variable Speed Electric Motor............	15

Accessories............................................	16
Internal Cooling Coils.........................	16
Liners .................................................	16
Spare Parts Kit...................................	16
Air Motor ............................................	17
Explosion Proof Operation ...................	18
Periodic Pressure Tests ........................	19
General Maintenance Notes..................	20
Parts Lists...............................................	21
Reaction Vessel Parts List .................	21
Removable Head Style Parts Lists ....	23
Fixed Head Style Parts Lists..............	25
Overarm Parts List .............................	28
Cooling Coil Parts List........................	30
Vessel Heaters Parts List...................	31
Related Instructions

The following Parr publications can be ordered to further your understanding of this instrument and its component parts:

No. Description

230M Safety Precautions to be observed when operating Pressure Reaction Equipment

231M Operating Instructions for Parr Safety Rupture Discs

548M Operating Instructions for 4848 Reactor Controllers

234M Operating and Maintenance Instructions for Parr Magnetic Drives

323M Operating Instructions for Parr Pressure Relief Valves

201M Limited Warranty

F0042 Health & Safety Assurance Certification

Customer Service

Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department:

309-762-7716

800-872-7720 Fax: [phone] www.parrinst.com [e-mail]

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Parr Instrument Company	4520 Bench Top Reactors

PREFACE

Scope

These instructions describe the installation, operation and maintenance of Parr Series 4520 Bench Top Reactors offered in one and two liter sizes. 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.

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 (iron-constantan) thermocouple. The total resistance of the thermocouple and the lead wires should not exceed 20 ohms. If the resistance of the thermocouple circuit is higher, it will reduce the sensitivity of the control system.

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Parr Instrument Company	4520 Bench Top 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 apparatus is to be used indoors. Operating: 15 °C to 35 °C; maximum relative humidity of 80% non-condensing. Installation Category II (overvoltage) in accordance with IEC 664. Pollution degree

2 in accordance with IEC 664.

Altitude Limit: 2,000 meters.

Storage: -25 °C and 65 °C; 10% to 85% relative humidity.

Provisions for Lifting and Carrying

The Series 4520 Bench Top Reactors and their components are very heavy. Before moving ensure all cables are disconnected. Use proper and safe lifting techniques when installing or moving the reactor and/or its components.

Caution!

Do not use in hazardous atmospheres.

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	4520 Bench Top Reactors

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.

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 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 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.

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.

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Parr Instrument Company

4520 Bench Top Reactors

INSTALLATION

Pressure and Temperature Limits

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 liter reactors must not exceed the following maximum limits:

Pressure and Temperature Limits

Vessel	Maximum	Maximum
Material	Pressure	Temperature
T316SS	1900 psig	350	C PTFE Flat
		Gasket
T316SS	1900 psig	225	C FKM O-ring
T316SS	1900 psig	275	C FFKM O-ring

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Parr Instrument Company	4520 Bench Top 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.

1.Set the Temperature 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 No. 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:

The Parr Heating output connector is to be used only with Parr Instrument Company heater assemblies supplied with the appropriate heater power cord.

Motor:

Secure the clamp on motor cord to the controller with the provided screw next to the motor socket for safety purposes.

The Motor output connector is to be used only with Parr Instrument Company motor assemblies supplied with the appropriate motor power cord.

2. For Fixed Head Reactors

Bolt the stand to the bench, table, or floor using the holes in the base plate.

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 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.

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.

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Parr Instrument Company

4520 Bench Top Reactors

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.

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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Parr Instrument Company	4520 Bench Top Reactors

Parr Series 4520 1 & 2 Liter 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.

The flat PTFE gasket can be used to operating temperatures as high as 350 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

Moveable Head with Flat Gasket

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Parr Instrument Company	4520 Bench Top Reactors

IDENTIFY THE VALVES

Gas Release Valve

The gas release valve is mounted on an extension in a 1/8” NPT port. This valve is open to the gas head space of the cylinder.

This position also includes a 1/8” NPT thread on the underside of the head which may be used for a second dip tube or an alternate accessory such as a catalyst addition device.

Note: If a fitting is added to the underside of the head in this location it will be necessary to install an additional valve on the gage adapter open to the gas space of the vessel for pressure release.

Gas Inlet Valves

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 cylinder. This is an angle pattern valve with an attached coupling which provides a socket for attaching the A495HC gas hose furnished with the reactor.

Liquid Sampling Valve

The liquid sampling valve is attached to the same adapter as the gas inlet valve combined with the 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 gas valve momentarily to force any liquid in the tube back into the reactor before withdrawing a sample from the sampling valve.

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