Parr Instrument 4590 User Manual
4590
Micro Bench Top Reactors
Operating Instruction Manual
399M
4590 Micro Reactors
PREFACE 4
Scope 4
Related Instructions 4
Intended Usage 4
Safety Information 4
General Specifications 4
Electrical Ratings 4
Explanation of Symbols 5
Environmental Conditions 5
Unpack Carefully 5
Provisions for Lifting and Carrying 5
Cleaning & Maintenance 5
User’s Responsibility 6
Fixed Head or Removable Head Vessel Design 7
Flat Gasket or Self Sealing O-Ring Closure 7
INSTALLATION 8
Pressure and Temperature Limits 8
Assemble The Reactor 9
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
www.parrinst.com
3
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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7
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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