Parr Instrument 4520 User Manual
4520
Bench Top Reactors
Operating Instruction Manual
383M
Parr Instrument Company
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
4520 Bench Top Reactors
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: 309-762-9453
www.parrinst.com
parr@parrinst.com
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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
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
4520 Bench Top Reactors
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
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.
4520 Bench Top Reactors
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
Material
T316SS 1900 psig
T316SS 1900 psig
T316SS 1900 psig
Maximum
Pressure
Maximum
Temperature
350 C PTFE Flat
Gasket
225 C FKM O-ring
275 C FFKM O-ring
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Parr Instrument Company
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
be used only with Parr Instrument Company
cooling solenoid valve assemblies supplied
with the appropriate cooling power cord.
The
be used only with Parr Instrument Company
heater assemblies supplied with the
appropriate heater power cord.
Parr Cooling
Parr Heating Only:
Parr Heating
Motor:
Secure the clamp on motor cord
to the controller with the
provided screw next to the motor
socket for safety purposes.
output connector is to
output connector is to
4520 Bench Top Reactors
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
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.
4520 Bench Top Reactors
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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.
Fixed Head with O-ring
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 Oring 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.
Moveable Head with Flat Gasket
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Parr Instrument Company
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
4520 Bench Top Reactors
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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