Parr Instrument 4590 User Manual

4590
Micro Bench Top Reactors
Operating Instruction Manual
399M
4590 Micro Reactors
PREFACE 4
Electrical Ratings 4
INSTALLATION 8
HOW TO USE THE VESSEL 14
To open the Vessel 14
Before Closing the Vessel 14
Sealing Vessels with PTFE Gaskets 14
Sealing with Flexible Graphite Gaskets 14
O-Ring Closures 14
Gas Connections 15
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
Technical Support 17
SERIES 4590 VESSEL PARTS LISTS 18
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
ACCESSORIES AND OPTIONS 11
Liners 11
Spare Parts Kit 11
Air Motor 12
Standard Reaction Vessel Parts List 18
High Pressure Reaction Vessel Parts List 21
HP/HT Reaction Vessel Parts List 23
Overarm and Stand Parts List 24
Support Stands 25
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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4590 Micro Reactors

PREFACE

Scope

These instructions describe the installation, opera­tion and maintenance of Parr Series 4590 Bench Top Micro Reactors which are offered in three sizes 25, 50 and 100 mL. 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 below. 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 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.
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Parr Instrument Company
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.

Explanation of Symbols

II On position, full power heater switch
I On position, half power heater switch
O Off Position
~ Alternating Current (AC)
4590 Micro Reactors
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: 2,000 meters. Storage: -25 °C to 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 4590 and its components are very heavy. Before moving ensure all cables are disconnected. Use proper and safe lifting techniques when installing or moving the 4590 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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4590 Micro 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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Parr Instrument Company
4590 Micro Reactors
Parr Series 4590 Micro 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 split ring 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 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 maximum operating temperature limit.
225 °C
Fixed Head with PTFE Gasket
Moveable Head with O-ring Seal & Easy Close Split Ring
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4590 Micro 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.
All Parr reactors show the maximum safe operating pressure and temperature imprinted on the cylinder. An accompanied restricted operating limit tag and/ or supplemental manual is given when a compo­nent of the system limits the operation below the imprinted valves.
The standard material of construction for Parr Instrument Company is Type 316 Stainless Steel. The working pressure and temperature in these 25, 50 & 100 mL reactors must not exceed the following maximum limits:
Pressure Vessel and Temperature Limits
In the standard pressure and temperature setup, the system must not exceed the following:
Vessel
Material
T316SS
T316SS
T316SS
Maximum
Pressure
3000 psig
(200 bar)
3000 psig
(200 bar)
3000 psig
(200 bar)
Maximum
Temperature
350 °C PTFE
Flat Gasket
225 °C FKM
O-Ring
300 °C FFKM
O-Ring
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. The safe operat­ing pressure of any system can be no higher than that of its lowest rated component.
In the high pressure/high temperature setup, the system must not exceed the following:
Vessel
Material
T316SS (HP)
T316SS
(HPHT)
Maximum
Pressure
5000 psig
(345 Bar)
5000 psig
(345 Bar)
Maximum
Temperature
350 °C PTFE
Flat Gasket
500 °C Flexible
Graphite
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Parr Instrument Company
4590 Micro 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 stand in the workspace.
Bolt the stand to the bench top using the holes in the base plate.
2. 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:
3. Connect the heater cord from the heater into the heater socket on the rear panel of the Series 4848 Reactor Controller.
4. 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.
5. 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.
6. 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.
7. Connect cooling water to the magnetic drive. See Instruction Manual No. 234M.
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, Power-stat 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.
Parr Motor Only:
8. Connect tubing to the rupture disc outlet and run to a safely vented area. See Instruction Manual 231M.
9. 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.
10. 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 heater, the heater may overheat and fail.
The Motor output connector is to be used only with Parr Instrument Company motor assemblies supplied with the appropriate motor power cord.
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