4575/76
HP/HT Pressure Reactors
Operating Instruction Manual
416M
4575/76 HP/HT Pressure Reactors
Preface 3
Scope 3
Related Instructions 3
Intended Usage 3
Safety Information 3
General Specifications 3
Explanation of Symbols 4
Environmental Conditions 4
Unpack Carefully 4
Provisions for Lifting and Carrying 4
Cleaning & Maintenance 4
User’s Responsibility 5
Installation 6
Pressure and Temperature Limits 6
Assemble the Reactor 6
Moveable Head Vessels 12
To open the Vessel 12
Before closing the Vessel 12
To Close the Vessel 12
Gas Connections 12
Pressurizing the Vessel 12
Do Not Overfill the Vessel 13
Releasing Pressure 13
Withdrawing Liquid Samples 13
Initial Operating Test 13
Explosion Proof Operation 14
Periodic Pressure Tests 14
General Maintenance Notes 15
Reaction Vessel Parts List 16
Identify the Valves 8
Gas Inlet Valve 8
Gas Release Valve 8
Liquid Sampling Valve 8
Other Vessel Head Fittings 9
Safety Rupture Disc 9
Type J Thermocouple 9
Pressure Gage 9
Gage and Valve Adapters 9
Accessories 10
Internal Cooling Loop 10
Liners 10
Spare Parts Kit 10
Variable Speed Electric Motor 10
Air Motor 11
How to Use the Vessel 12
Fixed Head Vessels 12
Cylinders 17
Heads 17
Split Rings and Accessories 17
Vessel Heaters 17
Internal Fittings 18
External Fittings 19
Overarm Parts List 20
Drawings 22
4575A/76A 500/250 mL Fixed Head 22
4575B 500 mL Moveable Head 23
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
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Parr Instrument Company
4575/76 HP/HT Pressure Reactors
Preface
Scope
These instructions describe the installation, operation and maintenance of Parr Series 4575/4576 HP/
HT Pressure Reactors offered in two sizes, 500 mL
and 250 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 in the following
section. 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 available 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 Controller
549M 4848 Controller CD-ROM
668M 1358 Grafoil® Tape General Guidelines
F0042 Health & Safety Assurance Certification
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.
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 (ironconstantan) 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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4575/76 HP/HT Pressure 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: 2,000 meters.
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. 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 4575/4576 HP/HT Pressure Reactors and its components are very heavy. Before moving ensure all
cables are disconnected. Use proper and safe lifting
techniques when installing or moving the 4575/4576
HP/HT Pressure Reactors 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
4575/76 HP/HT Pressure 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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5
4575/76 HP/HT Pressure 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 Vessels 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 which are not recommended by 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.
Pressure and Temperature Limits
Vessel
Material
T316SS 5000 psi 500 °C Flexible Graphite
T316SS 5000 psi 350 °C PTFE Gasket
Maximum
Pressure
Maximum Temperature
Gasket
Assemble the Reactor
These reactors require at least 10 square feet of
workspace on a sturdy bench, table, or floor in a
well ventilated area with convenient access to an
electric outlet, running water, and a drain. If the
tabletop is not heat resistant it would be ideal to
provide an insulated pad on which to set the vessel
when it is hot.
1. Set the stand in the workspace.
Bolt the stand to the bench top using the
holes in the base plate.
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 250
mL and 500 mL reactors must not exceed the following maximum limits:
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:
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.
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Parr Instrument Company
4575/76 HP/HT Pressure Reactors
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.
3. Connect the heater cord from the heater into
the heater socket on the rear panel of the Series
4848 Reactor 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. 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 top of 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.
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 internal cooling coil if
installed.
9. Connect cooling water to the magnetic stirrer.
See Instruction Manual 234M.
10. Connect tubing to the rupture disc outlet and run
to a safely vented area. See Instruction Manual
231M.
11. 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.
12. 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.
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 extension wire to
both the thermocouple and to the controller in
the “Primary Temp Input” position on the rear
panel. Insert the thermocouple into thermowell.
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4575/76 HP/HT Pressure Reactors
Magnetic Drive
Thermowell
Propellers
Valve
Valve
Identify the Valves
Gas Inlet Valve
The gas inlet valve is easily identified when the
bomb is open by noting that it is connected to a dip
tube which extends to a point near the bottom of
the cylinder. This valve has an attached fitting which
provides a socket for attaching the A506HC pressure
hose furnished with the reactor.
Gas Release Valve
The gas release valve is installed on the gage adapter. Gas released from this valve will be drawn from
the head space of the vessel.
Gas Inlet
Liquid Sampling Valve
The liquid sampling valve is attached to the same
fitting as the gas inlet valve and connected to the
same 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 upper gas inlet
valve momentarily to allow the inlet gas to force any
liquid in the dip tube back into the reactor before
withdrawing a sample from the sampling valve.
Pressure Gage
Liquid
Sampling
Thermocouple
/ Thermowell
Gas Release Valve
Head
Dip Tube
Thermocouple /
Stirring Shaft
8
Cooling Loop
Fixed Head
Parr Instrument Company
4575/76 HP/HT Pressure Reactors
Other Vessel Head Fittings
Safety Rupture Disc
There is a safety rupture disc attached to the head
which is intended to rupture and release the pressure before it reaches a dangerous level. A metal
tag wired to the safety head identifies the burst
pressure at room temperature for that particular
disc. A similar tag is furnished with each replacement disc. This tag must remain with the apparatus
at all times so that both present and future operators will be aware of the disc rating. Users should
read the discussion of rupture discs given in the
Instruction Manual 231M for a complete description
of the characteristics of rupture discs and the precautions to be observed when operating pressure
equipment protected by this type of safety device.
A typical pre-bulged disc can be used to 90% of the
rating on the tag. For additional protection, the user
should install an adequate and safe venting system
for removing any toxic, flammable or volatile material which would be released if the rupture disc
should burst. A connector for attaching 3/8” OD
tubing to the discharge port of the rupture disc is
provided for this purpose.
Type J Thermocouple
A Type J thermocouple in a 1/8” diameter Stainless
Steel sheath is furnished with the reactor. Insert
this thermocouple into the thermowell, connect the
A470E2 extension wire to both the thermocouple
and the receptacle on the back panel of the controller. For a single thermocouple connect to the "Primary Temp Input". (If a high temp cut off package
is part of the system a second thermocouple may
be inserted in the thermowell or alternately in the
heater to the vessel wall.)
Pressure Gage
The pressure gage furnished with this reactor has
a T316 Stainless Steel Bourdon tube. Gages are
furnished in a variety of ranges to meet individual
needs. Typically, the gage and the rupture disc are
furnished as matched ranges. For applications
where a gage is selected with a range under 1000
psi, a relief valve is added and set to protect the
gage. A 1000 psi rupture disc is installed as the failsafe vessel protection.
For highly corrosive applications where the vapor
phase might corrode the stainless Bourdon tube,
Parr offers isolator assemblies in a variety of materials. These isolators with their internal piston isolate
the vapors from the gage.
The gage adapter includes a ¼” NPT side port with
a plug installed. This position may be used for a
variety of fittings such as a needle valve, pressure
transducer or relief valve.
Gage and Valve Adapters
The pressure gage and the combined gas inlet and
sampling valves are attached to the head with an
adapter which allows these fittings to be drawn up
tightly when facing in any direction. To attach these
fittings to the head, screw the gage or valves firmly
into the adapter, then run the 366HC bushing onto
the threaded stem as far as it will go. Screw this
assembly into the head through the 326HC compression nut until the nose of the adapter is seated;
then back it off until the valve or gage is facing in
the desired direction. Now hold the fitting firmly in
place and close the joint by tightening the 326HC
compression nut. This connection can be made and
broken repeatedly without destroying the sealing
faces. A light coating of thread lubricant, such as
Parr No. 424HC2 High Temperature Anti-Seize Lube,
applied to the threads and to the nose of the adapter
will help to obtain a tight joint.
Note: Do not use Grafoil® tape on the straight
thread connections of the coned adapters
and mating bushings. Grafoil® tape should
only be used on the (NPT) threads such as the
needle valves or gage connection. Refer to
instruction manual no. 668M 1358HC Grafoil
Tape General Guidelines for use.
®
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9
4575/76 HP/HT Pressure Reactors
Accessories
Internal Cooling Loop
A cooling loop is mounted to the underside of the
head and sealed with a ferrule and compression nut
arrangement.
A slow continuous flow of cold water through the
cooling loop is an effective means for controlling
temperature overshoot, particularly when operating
at temperatures below 150 °C. Alternately the cooling loop is used to effectively cool the system at the
completion of a reaction.
An optional solenoid valve package is available to
automate the cooling process. This package coordinates with the internal coil, with the water supply
and connects to the temperature control.
If the internal cooling is not required, the coil may
be removed and the alternate plugs installed.
Liners
Glass or PTFE liners can be furnished to fit most
Parr reactors. These liners slide into the cylinder.
Although they will not keep corrosive vapors from
reaching the surfaces of the cylinder and head, they
make it much easier to add and remove liquid reactants, and they give some protection to the cylinder
when working with corrosive solutions. It must be
noted, however, that adding a PTFE liner will slow
the heat transfer rate into the vessel, and it may be
necessary to adjust the temperature control method
to prevent overheating.
Liner Part Numbers
Fits ID
2.5” 250 mL 762HC10
2.5” 500 mL 762HC2 762HC11HA
Cylinder
Size
Glass
Liner
PTFE Liner
Spare Parts Kit
Spare parts kits are available for these reactors. The
kits will provide a reserve supply of parts and tools
sufficient to handle most normal replacements and
emergency repairs during a year of heavy usage.
The kits contain small perishable items required for
continuous operation including gaskets, bushings,
rupture discs and seals. They can be ordered from
any Parr Dealer or direct from the Parr Instrument
Company. The order must specify the reactor size
and indicate type of rupture disc, stirrer drive and
whether it has a flat-gasket or O-ring closure. It is
most advantageous to provide the complete vessel
number from the head or cylinder.
Variable Speed Electric Motor
Reactors are normally equipped with a DC variable
speed motor supplied and controlled through the
Series 4848 Reactor Controller. Instructions for connecting and operating these motors are included in
the controller Instruction Manual 548M. This motor
is usually installed in a drive system designed to
produce stirring speeds from 0 to 600 rpm. Higher
speeds up to 1700 rpm can be obtained by substituting a larger diameter motor drive pulley.
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Parr Instrument Company
4575/76 HP/HT Pressure Reactors
Air Motor
Variable stirring speeds from 300 to 2000 rpm with
no spark hazard can be obtained by replacing the
standard motor with an air motor. This motor operates on compressed air which must be supplied
at 40 psig minimum pressure with at least 20CFM
available at that pressure. It is furnished with a
speed control valve, oiler, and muffler.
To operate reactors equipped with an air motor, connect the air hose to a compressed air line. Fill the
oiler with SAE 10 oil and adjust the oiler to feed one
drop per minute into the air stream. For long continuous runs at high speeds the oiling rate should
be increased to three drops per minute.
If the motor becomes sluggish, flush it with a nonflammable solvent in a well ventilated area. Disconnect the air line and muffler and pour a small
amount of solvent into the inlet port. Rotate the
shaft by hand in both directions for a few minutes;
then connect the air line and run the motor until
there is no further trace of solvent in the exhaust.
If the muffler felts are dirty, wash them in solvent or
replace them. Re-lubricate the motor with a squirt of
oil into the chamber and reassemble.
If it becomes necessary to disassemble the motor to
replace the vanes, follow the directions given in the
instruction sheet published by the Gast Manufacturing Corporation, Benton Harbor, Michigan.
2563HC2
Air Motor Option
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4575/76 HP/HT Pressure Reactors
How to Use the Vessel
Fixed Head Vessels
First, lower the heater and push it to the side. Before attempting to remove the split ring open the
gas release valve to discharge any internal pressure.
Raise the cylinder support holder to the bottom of
the cylinder. The head with any attached connection
lines will remain in place.
Moveable Head Vessels
First, open the gas release valve to discharge any
internal pressure. Remove the complete vessel assembly from the support stand.
To open the Vessel
Loosen the bolts in a criss-cross pattern reversing
the tightening procedure, gradually decreasing the
torque on each bolt. The head assembly can be removed from the cylinder. Handle the head carefully
so that no damage will occur to any of the internal
fittings.
Before closing the Vessel
Examine the head seal carefully to be sure that it
is in good condition. The seal should not have any
nicks, be hardened or deformed. Also examine the
mating surfaces on the head and cylinder to be sure
they are clean and free from burrs.
To Close the Vessel
Place the two split ring halves around the head and
cylinder flanges. Close the latches on the fixed head
split ring. Install the drop band on the movable
head split ring.
A torque wrench is furnished with these vessels
and it includes an adapter for the 12 point heads of
the bolts used in these split rings. The amount of
torque to be applied will depend upon the intended
maximum operating pressure. To ensure a good
seal over the full operating range apply the recommended bolt torque per the table below.
Recommended Bolt Torque
Material Pressure (psi) Torque (ft-lb)
PTFE 0 - 3000 35 ft-lbs
Flexible Graphite 0 - 3000 35 ft-lbs
PTFE or Flexible
Graphite
Pick a starting bolt and tighten it to approximately
15 ft-lbs. Then by-pass the adjacent bolts and move
around the closure to a bolt approximately 180 degrees from the starting bolt. Torque all bolts to the
initial 15 ft-lbs. Then proceed with the same pattern
increasing the torque in 10 ft-lbs increments.
Note: Flexible graphite gaskets tend to be
somewhat flakey. To extend the useful life
of these gaskets, first rough up the sealing
surface of the cylinder with 120 grit sand paper to ensure the gasket remains in the head
groove and does not stick to the cylinder.
Secondly, coat both sealing surfaces with
a silicone lubricant. This process will aid in
compressing the gasket so it does not break
apart after one use.
4000 - 5000 40 ft-lbs
Gas Connections
Gas connections are dependent on applications.
For most applications the stainless steel hose furnished with the system is sufficient. Attach the Type
“A” coned pressure fitting into the adapter attached
to the gas inlet valve and tighten the compression nut firmly. Do not use any thread dope on the
coned fitting.
Pressurizing the Vessel
Check all valves carefully before admitting gas into
the system. The liquid sampling valve must remain
closed throughout the charging procedure. The gas
release valve must also be closed unless the vessel
is to be purged, or unless there is to be a continuous
flow through the reactor during a run. Always make
certain that the pressure in the gas tank is greater
than the pressure in the vessel; otherwise liquid
will be forced out of the vessel and into the gas
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Parr Instrument Company
4575/76 HP/HT Pressure Reactors
tank when the inlet valve is opened. If there is any
possibility that the tank pressure might not be high
enough to force gas into the reactor, install a one
way check valve (optional) in the gas line to prevent
any reverse flow. With the inlet valve open and the
flow control valve on the gas tank closed, open the
main valve on the gas tank only about one-quarter
turn; then use the flow control valve or the valve
on a pressure regulator to control the flow of gas
into the vessel. After the desired pressure has been
reached, close the tank valves and the vessel inlet
valve and disconnect the hose at the vessel end.
Do Not Overfill the Vessel
Always watch the pressure gage closely when admitting gas so as not to exceed the maximum working limit. Remember that any subsequent increase
in temperature will raise the pressure. Also, be
sure that the amount of liquid placed in the vessel
is carefully controlled. As a general rule, the liquid
charge should not exceed two-thirds of the capacity of the cylinder. Too much liquid in the vessel can
lead to development of dangerous pressures if sufficient space is not provided for expansion when the
liquid is heated. This hazard is explained in greater
detail in a warning statement included in the Instruction Manual 230M.
Releasing Pressure
Use the gas release valve to reduce the pressure in
the vessel if the reactor is accidentally overcharged
when filling. Use this valve also to release any
excess pressure during a run and to exhaust the
vessel at the end of a run. If the discharge gases are
flammable or toxic, discharge to an exhaust hood or
to any other safe release point.
Withdrawing Liquid Samples
Liquid samples may be withdrawn from the sampling valve attached to the same adapter as the gas
inlet valve whenever the vessel is pressurized. Always close the inlet valve before withdrawing a liquid sample and open the sampling valve cautiously
because liquid will be discharged with considerable
force. Be particularly careful if the temperature of
the sample is above its boiling point at atmospheric
pressure. If so, it will “flash” and be lost as soon
as it is released from the vessel. This problem can
be avoided by connecting an optional 4351 Sample
Collection Vessel to the sampling valve to collect the
liquid into an appropriate receiver. The addition of
a small amount of gas can be used to clear the dip
tube between liquid samples so that the next sample drawn through the tube will truly be representative of the mixture.
Initial Operating Test
Read all operating instructions carefully so as to be
well acquainted with the correct procedures for handling the vessel and for operating the controller and
other accessories. An initial operating test should
be made, with only water, to check the apparatus
before starting the first experimental runs. For this
initial test, fill the cylinder not more than half full of
water and run the temperature up to 150 ºC while
checking the apparatus for leaks and observing the
performance of the reactor controller.
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13
4575/76 HP/HT Pressure Reactors
Explosion Proof Operation
If the local safety code requires that equipment
installed in the user’s laboratory must be explosion
proof, there are four possible ignition hazards to be
considered:
1. The Motor
The standard adjustable speed motor is not
explosion proof, yet these motors are not unduly hazardous if operated in a well ventilated
location where care is taken to prevent the
accumulation of explosive gases or vapors. To
eliminate any possible spark hazard originating at the motor, Parr can furnish an air motor as described previously, or the reactor can
be equipped with a variable speed, explosion
proof motor that is approved for use in Class
1, Groups C & D, and Class 2, Groups E, F, & G
atmospheres. Explosion proof motors are furnished with a temporary power cord and plug
which are not explosion proof. The user should
remove this temporary wiring and replace
it with an explosion proof switch and wiring
which will comply with the local electrical code.
2. The Reactor Controller
The Series 4848 Reactor Controllers furnished
with these reactors contain switches and other
elements that are not explosion proof. The
minimal spark hazard associated with these
units can be resolved by installing the controller in a remote location outside of the hazardous area or by enclosing it in an approved
explosion proof housing. If enclosed within a
positive pressure, clean air housing, the discharge from the housing must be directed into
a safe area. If requested, Parr will furnish the
long lead wires needed to mount the controller in a remote location. If the controller is to
be installed in an explosion proof housing, the
user must provide the necessary housing and
installation.
3. The Heater
The elements in the heater could be dangerous
in an explosive atmosphere if the surface temperature of the element becomes high enough
to ignite flammable vapors. This hazard must
be evaluated for each individual installation
since major modifications are required if the
heater must be isolated from the surrounding
atmosphere. Users who consider this a significant hazard are urged to contact the Parr
Instrument Company for further discussion and
suggestions that might be helpful.
4. The Wiring
The wiring provided with the standard reactor
systems does not meet the standards prescribed for explosion proof operation. Optional,
intrinsically safe barriers are available.
Periodic Pressure Tests
Each cylinder used in a Parr stirred reactor is
tested under hydrostatic pressure to 1.3 times its
maximum rating before it is released from the factory. Micrometer caliper measurements are taken
during this test to check the deflection of the walls
and bottom of the cylinder under pressure. Excessive deflection or failure of the metal to resume
its original dimensions after pressure is released
indicates that a cylinder is potentially unsafe and
it will be rejected. Similar tests should be made
at regular intervals during the life of each cylinder,
and particularly whenever the user suspects that
the equipment has been over-stressed or damaged.
Some laboratories maintain hydraulic test facilities
and make it a rule that all pressure vessels must
be tested at regular intervals. Records are kept of
deflections at specific test pressures so that any
increase in deflection becomes a warning that the
metal has lost strength. Any cylinder which fails to
return to its original dimensions after application of
the prescribed hydrostatic test should be discarded
as unsafe for further use.
Users who do not have pressure test facilities can
return any Parr pressure vessel to the factory for
hydrostatic testing and overhaul. This should be
done whenever the metal shows excessive damage from corrosion or whenever an over-pressure
or other unusual occurrence raises any safety
questions. To return a vessel for repair contact Parr
Instrument Company for a return authorization
number. Apparatus returned for testing and overhaul should be shipped prepaid to Parr Instrument
Company, 211-53rd Street, Moline, Illinois 61265.
An order or letter of instructions should be mailed
to the same address, as no repair work will be
started without specific instructions and a Health &
Safety Assurance Certification form (F0042) signed
by a responsible user.
14
Parr Instrument Company
4575/76 HP/HT Pressure Reactors
General Maintenance Notes
1. Periodically inspect all electrical wiring and
pressure connections for excessive corrosion.
Suspect parts should be replaced by components only supplied by Parr Instrument Company.
2. Always use appropriate wrenches on all fittings
and valves. Never use pliers or pipe wrenches.
3. Head and cylinder service fixtures are available
for convenience and protection of components
during maintenance of your reactor.
4. To reinstall straight thread (NPS) fittings to the
head, screw the gage or valves firmly into the
adapter. Run the bushing onto the threaded
stem as far as it will go. Screw this assembly
into the head until the nose of the adapter is
seated; then back it off until the valve or gage
is facing in the desired direction (no more than
one full turn). Hold the fitting firmly in place
and close the joint by tightening the bushing.
This connection can be made and broken repeatedly without destroying the sealing surfaces. A light coating of thread lubricant, such
as Parr High Temperature Anti-Seize Lubricant,
applied to the straight threads and to the nose
of the adapter will help to obtain a tight joint.
Note: PTFE tape should not be used
on this joint.
5. NPT (National Pipe Taper) threads should not
be disassembled any more than necessary. It
will become increasingly difficult to maintain a
tight seal with these tapered threads if the joint
is made and broken repeatedly. Grafoil tape or
PTFE tape (if temp allows) should be used on
all NPT threads.
6. Do not use oil or anti-seize lubricant on threads
or fittings if the vessel is to be used with oxygen.
8. Clean all threads and gas passages thoroughly
and remove all tape fragments when overhauling a vessel. An ultrasonic bath is excellent
for cleaning metal parts, but do not place a
thermocouple probe, pressure gage, face seals
or ball bearings in an ultrasonic bath. Periodic
cleaning may be performed on the exterior surfaces of the reactor stand with a lightly dampened cloth containing mild soap solution. All
power should be disconnected when cleaning.
9. Routinely inspect cap screws on split ring
closure for lubrication and cleanliness. These
screws should not be allowed to dry because
the threads will seize. Regularly apply Parr
High Temperature Anti-Seize Lubricant (Parr No.
424HC2) before this happens.
10. To operate reactors equipped with an air motor,
connect air hose to a compressed air line. For
best torque and speed control the piping to the
motor should be at least 3/8” IPS or larger. Fill
the oiler with SAE 10 oil and adjust the oiler
feed one drop per minute into the air stream.
For long continuous runs at high speeds the
oiling rate should be increased to three drops
per minute. If the motor becomes sluggish,
flush it with a non-flammable solvent in a well
ventilated area.
Disconnect the air line and muffler and pour
a small amount of solvent into the inlet port.
Rotate the shaft by hand in both directions for
a few minutes; then connect the air line and
run the motor until there is not further trace of
solvent in the exhaust. If the muffler is dirty,
replace it. Re-lubricate the motor with a squirt
of oil into the chamber and reassemble.
11. If servicing assistance is needed, contact Parr
Instrument Company directly at 800-872-7720
or at the address shown on the back of these
instructions.
7. If your vessel is equipped with a loose compression ring be sure that it is in place on the
head before attaching any head fittings. The
compression ring cannot be installed after fittings have been screwed into the head.
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15
4575/76 HP/HT Pressure Reactors
Reaction Vessel Parts List
Consult the itemized list for your reactor, provided
along with this manual. For purpose of reactor identification, the following abbreviation codes are used:
RV - Removable Vessel FMD- Footless Mag Drive
FG - Flat Gasket Seal FH - Fixed Head
SS - T316 Stainless Steel LD - Light Duty Stirrer
GE - Gas Entrainment B DV- Bottom Drain Valve
* For parts made from alternate materials use the
codes shown below as a suffix to the standard part
number.
CM - Alloy 400 CC - Alloy 20Cb3
CT - Alloy 600 CAD - Titanium Grade 2
CX - Zirconium CAA - Titanium Grade 4
CH - Alloy C-276 CG - Alloy B-2
A888HC2 RUPTURE DISC ASSY
(OPPOSITE GAGE ASSEMBLY)
288VBAD MALE CONNECTOR
366VB HEX COUPLE
433HC4 SAFETY HEAD
49HC2 ORIFICE CONE
527HC ORIFICE RING
526HC/581HC RUPTURE DISC
2965HC2
HEAD
265HC9
THERMOWELL
2996HC COLLAR
1133HC BUSHING
1459HC4
COOLING LOOP
2141HC53
SHAFT
(2) A2148HC
IMPELLERS
WITH SCREWS
Head Assembly with A2140HC2
Footless Magnetic Stirrer
1446HC ADAPTER
(2) A176VB VALVES
197VBAD MALE TEE
326HC COMPRESSION NUT
A3314HC STIRRER BRACKET
1452HC ADAPTER
366HC BUSHING
1461HC INLET TUBE
A837HC3 IMPELLER
A837HC IMPELLER
WITH NUT
822HC40 SHAFT
WITH SCREW
WITH BUSHING
WITH SCREW
Head Assembly with A1120HC6
Magnetic Stirrer
56HC PRESSURE GAGE
1452HC3 APDAPTER
491HCAD NIPPLE
A176VB VALVE
94CA PLUG
326HC COMPRESSION NUT
366HC BUSHING
A472E3 THERMOCOUPLE
(2) A92HW MALE CONNECTOR
2965HC HEAD
457HC3KL GASKET
265HC6 THERMOWELL
48HC GASKET
1459HC COOLING LOOP
(2) 1359HC2 NUT, LONG HP/HT
(2) 1360HC FERRULE
16
Parr Instrument Company
4575/76 HP/HT Pressure Reactors
Cylinders*
Part No. Description Code
500 mL Models
1834HC2 Cylinder, 500 mL
1834HC7 Cylinder, 500 mL BDV
250 mL Models
1834HC Cylinder, 250 mL
1834HC6 Cylinder, 250 mL BDV
Heads*
Part No. Description Code
Removable Head Models
1836HC Head, stirred RV (LD)
1836HC5 Head for catalyst basket RV (LD)
1836HC6 Head, FMD RV (FMD)
Fixed Head Models
2965HC Head, stirred FH (LD)
2965HC2 Head, stirred, FMD FH (FMD)
2965HC3 Head, stirred, for catalyst
FH (LD)
basket
Split Rings and Accessories
Part No. Description Code
A246HC2 Split ring, 4140 alloy steel RV
A246HC2-T Split ring, T316SS
RV
(PED vessels)
248HC Compression ring RV
A247HC Drop Band RV
A2966HC Split ring, with latches
FH
captive compression ring,
4140 alloy steel
A2966HC-T Split ring, with latches,
FH
captive compression ring,
T316SS (PED vessels)
Vessel Heaters
Part No. Description Code
Fixed Head Models
A2952HC11EB Heater Assembly, 250/500 mL,
1400W, 115V
A2952HC11EE Heater Assembly, 250/500 mL,
1800W, 230V
A2952HC12EB Heater Assembly, 250/500 mL,
Open Bottom, 1400W, 115V
A2952HC12EE Heater Assembly, 250/500 mL,
Open Bottom, 1800W, 230V
Removable Head Models
A2952HC13EB Heater Assembly, 250/500 mL,
1400W, 115V
A2952HC13EE Heater Assembly, 250/500 mL,
1800W, 230V
A2952HC14EB Heater Assembly, 250/500 mL,
Open Bottom, 1400W, 115V
A2952HC14EE Heater Assembly, 250/500 mL,
Open Bottom, 1800W, 230V
Both Removable & Fixed Head Models
2144E3EB Heating Element, 250/500 mL,
1400W, 120V
2144E3EE Heating Element, 250/500 mL,
1800W, 240V
FH
FH
FH
FH
RV
RV
RV
RV
FH RV
FH RV
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17
4575/76 HP/HT Pressure Reactors
Internal Fittings
(Common to all models)
Cooling*
Part No. Description Code
1459HC Cooling loop, 500 mL
1459HC2 Cooling loop, 250 mL
1459HC3 Cooling loop 250 mL GE
1459HC4 Cooling loop 500 mL GE
1360HC Ferrule for cooling loop
1359HC2 Nut for cooling loop
A92HWAD External male connector,
T316SS
Dip Tubes*
Part No. Description Code
1461HC Dip tube with nut, 500 mL
1461HC2 Dip tube with nut, 250 mL
1461HC3 Dip tube 500 mL for use
with catalyst basket
Stirrer Shafts*
Part No. Description Code
822HC17 Stirrer shaft, 500 mL RV (LD)
822HC39 Stirrer shaft, 250 mL RV (LD)
2141HC41 Stirrer shaft, 500 mL RV (FMD)
2141HC40 Stirrer shaft, 250 mL RV (FMD)
Propellers*
Part No. Description Code
822HC17 Stirrer shaft, 500 mL RV (LD)
822HC39 Stirrer shaft, 250 mL RV (LD)
2141HC41 Stirrer shaft, 500 mL RV (FMD)
2141HC40 Stirrer shaft, 250 mL RV (FMD)
Thermowells*
Part No. Description Code
265HC6 Thermowell, 6”, 500 mL
265HC9 Thermowell, GE stirrer, 5.25”, 500 mL
265HC28 Thermowell, 3”, 250 mL
265HC29 Thermowell, 2.3”, 250 mL GE
265HC13 Thermowell plug
A472E Thermocouple, 250 mL RV
A472E2 Thermocouple, 500 mL RV
A427E3 Thermocouple, 500 mL FH
A472E2 Thermocouple, 250 mL FH
A2067HC2 Thermowell 500 mL for use
with catalyst basket
A2067HC3 Thermowell 500 mL for use
with catalyst basket
For use with A2067HC Thermowells:
1359HC Nut for thermowell
1360HC Ferrule for thermowell
A1357E3 1/16” OD thermocouple, 11 ½" RV
A1357E 1/16” OD thermocouple, 15 ½” FH
RV
FH
822HC40 Stirrer shaft, 500 mL FH (LD)
822HC41 Stirrer shaft, 250 mL FH (LD)
2141HC52 Stirrer shaft, 250 mL FH (FMD)
2141HC53 Stirrer shaft, 500 mL FH (FMD)
Gas Entrainment Shafts*
Part No. Description Code
2027HC2 Upper shaft, 250 & 500 mL RV (LD)
2027HC4 Upper shaft, 250 & 500 mL FH (LD)
2028HC Lower shaft, 250 mL RV (LD)
2028HC4 Lower shaft, 500 mL RV (LD)
2141HC42 Gas Entrainment 250 mL RV (FMD)
2141HC43 Gas Entrainment 500 mL RV (FMD)
2141HC54 Gas Entrainment 250 mL FH (FMD)
2141HC55 Gas Entrainment 500 mL FH (FMD)
18
Parr Instrument Company
Gaskets and Seals
Part No. Description Code
457HC3KL Head gasket, graphite
457HC2 Head gasket, PTFE (up to
350 °C)
48HC Thermowell gasket, silver
48HCFG Thermowell gasket, gold
plated
48HCKL Thermowell gasket, grafoil
1261HC2KF Graphite bushing for
A1871HC Stirrer bracket
1869HC2KF Graphite bushing GE
A1871HC Stirrer support bracket
1967HC Graphite bushing, catalyst
basket
4575/76 HP/HT Pressure Reactors
External Fittings
(Common to all models)
Gage Port Fittings
Part No. Description
56HCPD Pressure gage, 1000 psi
56HCPF Pressure gage, 2000 psi
56HCPG Pressure gage, 3000 psi
56HCPH Pressure gage, 5000 psi
56HCPK Pressure gage, 10000 psi
A176VB Valve, straight 1/4 NPT (F)
491HCAD Nipple, 1/4" NPT
1452HC3 Gage adapter, 3 -1/4” NPT (F)
Connections
326HC Compression nut
366HC Bushing
154VB2 Elbow, 45°, 1/4” NPT (M/F)
Double Valve Assembly
Part No. Description
1452HC Valve adapter
326HC Compression nut
366HC Bushing
197VBAD Tee, 1/4" NPT
A176VB Valve, straight 1/4 NPT (F)
1446HC Adapter, A-skt x 1/4” (M)
(hose connection)
Magnetic Drive
See manual 234M for a full list of magnetic stirrers and parts.
Rupture Disc Port
See manual 231M for a full list of rupture discs.
Part No. Description
A888HC2 Rupture disc assembly consists of:
433HC4 Safety head outlet, 1/4 NPT(M)
49HC2 Orifice cone
527HC Orifice ring
366VBAA Coupling, 1/4" NPTF
288VBAD Male connector, 1/4" NPT x 3/8" T
526HCPD Rupture disc, 1000 psi
526HCPF Rupture disc, 2000 psi
526HCPG Rupture disc, 3000 psi
526HCPH Rupture disc, 5000 psi
581HCPD Rupture disc, 1000 psi, gold faced
581HCPF Rupture disc, 2000 psi, gold faced
581HCPG Rupture disc, 3000 psi, gold faced
581HCPH Rupture disc, 5000 psi, gold faced
433HC4
Safety
Head
Outlet
526HC/
581HC
Rupture
Disc
527HC
Orifice
Ring
**49HC2
Orifice
Cone
288VBAD
366VBAA
A888HC2
A888HC2
Rupture
Disc
Assembly
shown with
1/4 NPT
female hex
coupling
and 1/4
NPT male
connector
to 3/8” OD
tubing
Gasket Seals for Magnetic Stirrers
Part No. Description
48HC Silver gasket A1120HC6
48HCFG Gold plated gasket A1120HC6
48HCKL Graphite gasket A1120HC6
2142HC Silver gasket A2140HC2
2142HCFG Gold plated gasket A2140HC2
2142HC2KL Graphite gasket A2140HC2
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19
4575/76 HP/HT Pressure Reactors
Overarm Parts List
1/8 hp Motor and Overarm Assembly
Part No. Description Code
1355EES Motor, 1/8 hp
A1554EES Motor, 1/8 hp, EMC
857HC Pulley, 600 rpm
857HC5 Pulley, 1700 rpm
847HC9 Belt for 600 rpm pulley
847HC10 Belt for 1700 rpm pulley
A2562HC3 Upper Drive Shaft, 7.58" LD
A2562HC4 Upper Drive Shaft, 5.68" FMD
Driven Pulley for 1/8 hp Motor and Overarm Assembly
Part No. Description
A2179HC Driven Pulley assembly consists of:
858HC2 Pulley
841HC Snap ring, external
839HC Ball bearing
862HC Support hub
842HC Snap ring, internal
299HC2 PTFE bushing
845HC2 Release knob
732HC Snap ring, extl, 1" dia
Removable Style Vessel, 1/8 hp Motor
20
Parr Instrument Company
Overarm Assembly for 4575/4576
4575/76 HP/HT Pressure Reactors
1/4 hp Motor and Overarm Assembly
Part No. Description Code
A388EES Motor, 1/4hp, 90VDC
A388EEQ Motor, 1/4hp, 90VDC, XP
A388EET Motor, 1/4hp, 180VDC
A388EER Motor, 1/4hp, 180VDC, XP
695HC5 Pulley, 600 rpm
695HC2 Pulley, 1700 rpm
728HC5 Belt for 600 rpm pulley
728HC6 Belt for 1700 rpm pulley
A2564HC7 Upper Drive Shaft, 9.56" LD
A2564HC8 Upper Drive Shaft, 7.66" FMD
Driven Pulley for 1/4 hp Motor and Overarm Assembly
Part No. Description
A2519HC Driven pulley assembly consists of:
706HC2 Pulley
725HC Support hub
732HC Snap ring
730HC Ball bearing
731HC Snap ring internal, 2”
2429HC PTFE bushing
726HC Release knob
Fixed Head Style Mounting, 1/4 hp Motor
Overarm Assembly for 4575A/4576A
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21
4575/76 HP/HT Pressure Reactors
Drawings
4575A/76A 500/250 mL Fixed Head
22
Parr Instrument Company
4575B 500 mL Moveable Head
2350HC5
2563HC
BACKPLATE, UPPER
ENCASEMENT
ENCASEMENT, UPPER
4575/76 HP/HT Pressure Reactors
HC4
2552
PANEL, REAR
2551HC4
ENCLOSURE, LOWER
2543HC
BASEPLATE, BENCH TOP
2359HC
2207HC
2208HC
1374HCJV
(5X) 2561HC3
(5X) TB3724FS12
3/8-24 X .75L FHSCS
SPACER, MOVABLE; 4575B/76B
4575B
(500mL SHOWN)
VESSEL ASSEMBLY
RETAINER, VESSEL
PANEL SCREW 6-32 THD
HUB, SCREW;
ALUM 1/2-13 THD
2569HC2
2555HC4
2554HC34
SUPPORT PLATE
SC1932SC10
10-32 X 5/8 SHSS
O-RING FKM 1/8 ID
WASHER, SPLIT 6-32 PNL SCR
1990HC13
A2952HC13
SUPPORT ROD
SUPPORT ROD, HEATER
HT REMOVABLE HEAD
HEATER ASSY, 250/500mL
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23
416M R01 Revision 10/18/13
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