Parr Instrument 4540 User Manual
4540
High Pressure Reactors
Operating Instruction Manual
394M
4540 High Pressure Reactor System
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
FIXED HEAD OR REMOVABLE HEAD DESIGN 6
Vessel Head Design 6
PTFE Flat Gasket 6
INSTALLATION 7
Pressure and Temperature Limits 7
Assemble the Reactor 8
IDENTIFY THE VALVES 9
Gas Inlet Valves 9
Gas Release Valve 9
Liquid Sampling Valve 9
HOW TO USE THE VESSEL 13
Fixed Head Vessels 13
Removable Head Vessels 13
MAINTENANCE 15
General Maintenance Notes 15
Periodic Pressure Tests 16
Technical Support 16
4540 SERIES REACTION VESSEL PARTS LIST 17
Standard Vessel Fittings 17
Heaters Parts List 19
Overarm Parts List 20
4540 SERIES DRAWINGS 22
4540 Series Vessel with Fittings 22
1/4 HP Light Duty FH/RH Overarm and Motor 24
1/8 HP Light Duty FH/RH Vessel Overarm and Motor 25
4544 600 mL Removable Head Reactor 26
4545 600 mL Fixed Head Reactor 27
4544/4544A 600 mL Removable Head Reactor 28
4545/4545A 600 mL Fixed Head Reactor 29
4546 1200 mL Removable Head Reactor 30
4547 1200 mL Fixed Head Reactor 31
OTHER VESSEL HEAD FITTINGS 10
Safety Rupture Disc 10
Type J Thermocouple 10
Pressure Gage 10
Gage and Valve Adapters 10
ACCESSORIES 11
Serpentine Cooling Coil 11
Spare Parts Kit 11
Liners 11
Variable Speed Electric Motor 11
Air Motor 11
Pneumatic Lift for Fixed Head Vessels 12
2
Parr Instrument Company
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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4540 High Pressure Reactor System
PREFACE
Scope
These instructions describe the installation, operation and maintenance of Parr Series 4540 Pressure
Reactors offered in two sizes, 600 mL and 1200 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 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
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.
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 100 ohms. If the resistance of the thermocouple circuit is higher, it will reduce the sensitivity
of the control system.
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3
4540 High Pressure Reactor System
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. 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
Before moving ensure all cables are disconnected.
Use proper and safe lifting techniques when installing
or moving the 4540 Reactor and/or its components.
Cleaning & Maintenance
Periodic cleaning may be performed on the exterior
surfaces of the controller with a lightly dampened
cloth containing mild soap solution. All power
should be disconnected and the power cord should
be unplugged 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 need to 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.
4
Parr Instrument Company
4540 High Pressure Reactor System
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 a choice between over-or underdesigned 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 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
4540 High Pressure Reactor System
FIXED HEAD OR REMOVABLE HEAD DESIGN
Parr Series 4540 High Pressure Reactors are furnished with two structural options in addition to the size,
pressure range, stirrer motor, controller and similar options. These are:
Fixed Head Moveable Head
Vessel Head Design
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.
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 head vessel design, all connections to
the head are removed to allow the vessel to be opened.
PTFE Flat Gasket
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 eight compression bolts which must be tightened to develop
the loading on the 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 PTFE flat gasket can be used to
operating temperatures as high as 350 °C.
Metal gaskets can be furnished for special applications. The metal gaskets are not interchangeable
with the flat gasket design, but require special
grooves machined into the head and cylinder.
Parr recommends the PTFE flat gaskets for most
applications.
6
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.
4540 High Pressure Reactor System
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.
Pressure Vessel and Temperature Limits
The standard material of construction for Parr Instrument Company is Type 316 Stainless Steel. The working
pressure and temperature in these one and two liter reactors must not exceed the following maximum limits:
Vessel Material Maximum Pressure Maximum Temperature
T316 SS 5000 psig 350 °C PTFE Flat Gasket
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7
4540 High Pressure Reactor System
Assemble the Reactor
These reactors require at least 10 square feet of workspace in a well-ventilated area with convenient access
to an electric outlet, running water and a drain. This
unit needs to be placed at least 10 inches away from
walls or flammable materials.
1. 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 No. 548M or
follow the steps below.
Labeled connections are provided on the rear panel
of the controller.
Parr Cooling Only:
The Parr Cooling output connector is to be used
only with Parr Instrument Company cooling solenoid valve assemblies supplied with the appropriate cooling power cord.
Parr Heating Only:
2B. Vessels on stationary stand.
Bolt the stand to the bench/floor using
the holes in the base plate.
Loosen the panel screw holding the vessel retainer
to the front midplate. Open the vessel retainer to
allow the placement of the vessel assembly. If fixed
head style, position the head in the slot located in
the front midplate. If removable head style, place
vessel assembly such that the split ring rests on
midplate bracket. After installing the vessel, close
the vessel retainer and retighten the panel screw.
Pull up on the release knob located at the top of the
belt guard. This knob is attached to the upper drive
shaft and the universal coupling. Lifting the knob
will allow the alignment of the universal coupling
and the drive adapter attached to the magnetic
drive. Turn the knob to align the slot in the drive
adapter with the universal coupling.
3. Connect the power cord from the heater into the
heater socket on the rear panel of the controller.
4. Plug the motor power 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.
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,
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 sold state relay located in the 4848
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.
2A. Vessels on movable cart.
The motor is contained in the overarm assembly
attached to the cart. The overarm assembly pivots
to the rear to allow the vessel to be placed in the
heater. The overarm is then aligned atop the vessel.
Pull up on the release knob to allow the upper
drive shaft to be connected to the magnetic stirrer.
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Parr Instrument Company
5. Note the voltage requirement on the controller
identification label on the back panel, and then
plug the power cord into an appropriate outlet.
Power for these reactors should be drawn from a
3-slot, grounded outlet capable of carrying up to
the full current rating of the system.
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.
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 Reactor Controller.
8. Connect cooling water to internal cooling coil if
installed.
9. Connect cooling water to the magnetic stirrer. See
manual no. 234M.
10. Connect tubing to the rupture disc outlet and run
to a safely vented area. See manual no. 231M.
11. Using the switch on the Reactor Controller, turn on
the motor for a short run to check the stirrer drive
system.
IDENTIFY THE VALVES
4540 High Pressure Reactor System
Gas Inlet Valves
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 bomb cylinder. This is an angle valve with an
attached fitting which provides a socket for attaching
the pressure hose furnished with the reactor.
Gas Release Valve
The gas release valve is connected to a plain opening
on the underside of the bomb head. Gas released from
this valve will be drawn from the top of the reactor.
Gage Adapter
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 liquid 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
Thermocouple
Gas Inlet Valve
Gas Hose Connection
Gas Release Valve
Split Ring Assembly
Shaft Assembly
Liquid Sampling Valve
Thermowell
Dip Tube
Cooling Coil
Stirrer Bracket
Impeller
Removable Head Vessel Vessel with Standard Magnetic Drive Shown
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9
4540 High Pressure Reactor System
OTHER VESSEL HEAD FITTINGS
Safety Rupture Disc
There is a safety rupture disc attached to the head
that 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
Sheet No. 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” dia. Stainless steel
sheath is furnished with the reactor. Insert this thermocouple into the head thermowell and connect it
to the thermocouple socket on the rear panel of the
temperature controller using the A470E2 extension
wire furnished with the controller.
Pressure Gage
A pressure gage, usually 0-7500 psi with a T316
stainless steel Bourdon tube, is mounted on the
head using attachment fittings similar to those used
for the inlet/sampling valve assembly.
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 209HC4 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. Now hold the fitting
firmly in place and close the joint by tightening the
209HC4 bushing. 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: PTFE tape should be used only on all
tapered (NPT) threads, not on the straight
threads of the 209HC4.
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56HCPH
208HC15
1446HC
209HC4
PRESSURE GAGE
Parr Instrument Company
A451VB
A455VB2
491HCAD
208HC6
209HC4
INLET SAMPLING VALVE
A455VB2
208HC11
209HC4
GAS RELEASE VALVE
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