Parr Instrument 4530 User Manual
4530
Floor Stand Reactors
Operating Instruction Manual
388M
Floor Stand Reactors
Table of Contents
PREFACE
Scope — 3
Related Instructions — 3
Safety Information — 3
General Specifi cations — 3
Electrical Ratings— 3
Explanation of Symbols — 4
Environmental Conditions — 4
Provisions for Lifting and Carrying — 4
Intended Usage — 4
Cleaning & Maintenance — 4
User’s Responsibility — 5
Unpack Carefully — 5
INSTALLATION
Pressure and Temperature Limits — 6
ASSEMBLE THE REACTOR — 6
IDENTIFY THE VALVES
Gas Inlet Valve — 8
Gas Release Valve — 8
Liquid Sampling Valve — 8
OTHER VESSEL HEAD FITTINGS
Safety Rupture Disc — 9
Type J Thermocouple — 9
Gage and Valve Adapters — 9
HOW TO USE THE VESSEL
Fixed Head Vessels — 10
To open the Vessel — 10
Before Closing the Vessel— 10
To Close the Vessel— 10
Removable Head Vessels — 10
To Open the Vessel— 10
Before Closing the Vessel— 10
To Close the Vessel— 10
Sealing Vessels with PTFE Gaskets— 10
Gas Connections— 10
Pressurizing the Vessel — 11
Do Not Overfi ll the Vessel— 11
Releasing Pressure— 11
Withdrawing Liquid Samples— 11
Initial Operating Test— 11
ACCESSORIES
Internal Cooling Coils — 12
Variable Speed Electric Motor — 12
Air Motor — 12
Liners — 12
Spare Parts Kit — 12
EXPLOSION PROOF OPERATION — 13
PERIODIC PRESSURE TESTS — 13
GENERAL MAINTENANCE NOTES — 14
PARTS LISTS
Internal Fittings — 16
External Fittings — 17
Removable Head Style Parts Lists — 18
Fixed Head Style Parts Lists — 20
OVERARM PARTS LIST — 23
COOLING COIL PARTS LIST — 25
HEATERS PARTS LIST — 26
Customer Service
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
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Parr Instrument Company
Floor Stand Reactors
PREFACE
Scope
These instructions describe the installation, operation and maintenance of Parr Series 4530 Floor
Stand Reactors offered in one and two liter sizes.
They cover the basic steps to be followed 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
575M Operating Instructions for 4848B Reac-
tor Controllers
F0042 Health & Safety Assurance Certifi cation
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 fi re 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 fl ammable or combustible materials; fi re or explosion may result.
This device contains components which may
ignite such material.
2. Refer servicing to qualifi ed personnel.
General Specifi cations
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 specifi ed, 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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Floor Stand 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 Protec-
tive Earth (green or green/yellow) supply system conductor.
Environmental Conditions
This instrument is intended to be used indoors.
Operating: 5 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:
Storage: -25 °C and 65 °C; 10% to 85% relative hu-
midity.
Provisions for Lifting and Carrying
The 4530 Floor Stand 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 4530 Reactor and/ or
its components.
0 to 6000 feet above sea level.
Caution!
Do not use in hazardous atmospheres.
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.
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 specifi cally 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
Floor Stand 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 fi nal 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.
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
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 specifi ed 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.
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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Floor Stand Reactors
INSTALLATION
Pressure and Temperature Limits
The working pressure and temperature at which any
reactor or pressure vessel can be used will depend
upon the design of the vessel and the materials
used in its construction. Since all materials lose
strength at elevated temperatures, any pressure
rating must be stated in terms of the temperature at
which it applies. The standard material of construction for Parr Instrument Company is Type 316 Stainless Steel.
Limits for vessels made of other materials and for
other operating temperatures can be obtained from
Parr Customer Service. No attempt should be made
to increase these limits by making alterations or by
substituting components that are not recommended
by the Parr Instrument Company. It must also be
understood that lower pressure and temperature
limits may be required for modifi ed 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. 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 fi ttings attached to the vessel. Obviously,
the safe operating pressure of any system can be no
higher than that of its lowest rated component.
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:
Pressure Vessel and Temperature Limits
Vessel
Material
T316SS 1900 psig 350 °C PTFE Flat Gasket
T316SS 1900 psig 275 °C FFKM O-ring
T316SS 1900 psig 220 °C FKM O-ring
Maximum
Pressure
Maximum
Temperature
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 fl ammable materials.
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 Parr Cooling output connector is to be used
only with Parr Instrument Company cooling solenoid valve assemblies supplied with the appropriate
cooling power cord.
All Parr reactors show the maximum safe operating
pressure and temperature imprinted on the cylinder.
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Parr Instrument Company
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.
Floor Stand Reactors
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.
2.
3. Connect the power cord from the heater into the
heater socket on the rear panel of the controller.
Motor:
Secure the clamp on motor cord to the
controller with the provided screw next to
the motor socket for safety purposes.
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.
2B. Vessels on stationary stand.
Bolt the stand to the fl oor using the
holes in the base plate.
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.
5. Note the voltage requirement on the controller
identifi cation 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 Controller.
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 fi xed 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.
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 Temperature Controller,
turn on the motor for a short run to check the
stirrer drive system.
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Floor Stand Reactors
IDENTIFY THE VALVES
Gas Inlet Valve
The gas inlet valve is easily identifi ed when the
bomb is open by noting that it is connected to a dip
tube that extends to a point near the bottom of the
bomb cylinder. This is an angle valve with an attached fi tting which provides a socket for attaching
the A495HC pressure hose furnished with the reactor.
Gas Release Valve
The gas release valve is connected to an opening
that will not have any fi tting installed on the underside of the head. Gas released from this valve
will be drawn from the top of the reactor. The gas
release port does include a 1/8
th
NPT thread on the
Pressure Gage
underside of the head where an additional dip tube
or catalyst addition device may be added. If one of
these additions is made to this port then an additional valve must be added to the gage adapter to
be used as a gas release valve.
Liquid Sampling Valve
The liquid sampling valve is attached to the same
fi tting 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 gas valve momentarily to force any liquid in the dip tube back into
the reactor before withdrawing a sample from the
sampling valve.
Plug (extra port)
Gas Release Valve
Stirrer Shaft Assembly
Adjustable Impeller
Thermocouple
Gas Inlet Valve
Coupling for Gas Hose Connection
Liquid Sampling Valve
Adapter Bushings
Thermowell
Dip Tube with Nut
Stirrer Support Bracket
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Parr Instrument Company
Floor Stand Reactors
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 identifi es 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, fl ammable 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 reactor.
nished 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 fail-safe 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 fi ttings 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 fi ttings to be drawn up
tightly when facing in any direction. To attach these
fi ttings to the head, screw the gage or valves fi rmly
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 fi tting fi rmly 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.
Pressure Gage
The pressure gage furnished with this reactor has a
T316 Stainless Steel Bourdon tube. Gages are fur-
Note: Do not use PTFE tape on the straight thread
connections of the coned adapters and mating bushings. PTFE tape should only be used on the (NPT)
threads such as the needle valves or gage connection.
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