Parr Instrument 4590 Instruction Manual

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399M
4590
Micro Bench Top Reactors
Operating Instruction Manual
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4590 Micro Reactors
www.parrinst.com 3
PREFACE 4
Scope 4
Related Instructions 4
Intended Usage 4
Safety Information 4
General Specifications 4
Electrical Ratings 4
Explanation of Symbols 5
Environmental Conditions 5
Unpack Carefully 5
Provisions for Lifting and Carrying 5
Cleaning & Maintenance 5
User’s Responsibility 6
Fixed Head or Removable Head Vessel Design 7
Flat Gasket or Self Sealing O-Ring Closure 7
INSTALLATION 8
Pressure and Temperature Limits 8
Assemble The Reactor 9
IDENTIFY THE VALVES 10
Gas Inlet Valve 10
Gas Release Valve 10
Liquid Sampling Valve 10
OTHER VESSEL HEAD FITTINGS 11
Safety Rupture Disc 11
Type J Thermocouple 11
Pressure Gage 11
ACCESSORIES AND OPTIONS 11
Liners 11
Spare Parts Kit 11
Air Motor 12
HOW TO USE THE VESSEL 14
To open the Vessel 14
Before Closing the Vessel 14
Sealing Vessels with PTFE Gaskets 14
Sealing with Flexible Graphite Gaskets 14
O-Ring Closures 14
Gas Connections 15
Pressurizing the Vessel 15
Do Not Overfill the Vessel 15
Releasing Pressure 15
Withdrawing Liquid Samples 15
Initial Operating Test 15
MAINTENANCE 16
General Maintenance Notes 16
Periodic Pressure Tests 17
Technical Support 17
SERIES 4590 VESSEL PARTS LISTS 18
Standard Reaction Vessel Parts List 18
High Pressure Reaction Vessel Parts List 21
HP/HT Reaction Vessel Parts List 23
Overarm and Stand Parts List 24
Support Stands 25
Customer Service
Questions concerning the installation or operation
of this instrument can be answered by the Parr
Customer Service Department:
1-309-762-7716 • 1-800-872-7720
Fax: [phone]
E-mail: [email protected]
http://www.parrinst.com
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4590 Micro Reactors
Parr Instrument Company
4
PREFACE
Scope
These instructions describe the installation, opera-
tion and maintenance of Parr Series 4590 BenchTop
Micro Reactors which are offered in three sizes 25,
50 and 100 mL.They cover the basic steps to be fol-
lowed when installing these reactors and describe
the function of all standard components.They are
intended to be used in conjunction with several
related instruction sheets listed below.This infor-
mation describes several components which are
common to most Parr pressure reaction equipment,
and includes safety precautions and other related in-
formation 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 Instruc-
tions 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 aType J (iron-
constantan) thermocouple. The total resistance of
the thermocouple and the lead wires should not
exceed 100 ohms. If the resistance of the thermo-
couple circuit is higher, it will reduce the sensitivity
of the control system.
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4590 Micro Reactors
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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 ap-
propriate part of the accompanying product literature for more infor-
mation.
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.
Caution!
Do not use in hazardous atmospheres.
Operating: 15 ºC to 35 ºC; maximum relative
humidity of 80% non-condensing.
Installation Category II (over voltage) in accordance
with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25 °C to 65 °C; 10% to 85% relative humidity.
Unpack Carefully
Unpack the equipment carefully and check all the
parts against the packing list. If shipping damage
is discovered, report it immediately to the deliver-
ing carriers.The vessel, motor, heater, and tem-
perature controller may be packed separately for
convenience in shipping, but these parts are easily
reassembled. Examine the components closely for
any loose parts or shipping damage and be sure to
check all layers of packing materials thoroughly so
as not to overlook any parts which might otherwise
be discarded.
Provisions for Lifting and Carrying
The 4590 and its components are very heavy. Before
moving ensure all cables are disconnected. Use
proper and safe lifting techniques when installing or
moving the 4590 and/or its components.
Cleaning & Maintenance
Periodic cleaning may be performed on the exterior
surfaces of the instrument with a lightly dampened
cloth containing mild soap solution. All power should
be disconnected when cleaning the instrument.
There are no user serviceable parts inside the product
other than what is specifically called out and discussed
in this manual. Advanced troubleshooting instructions
beyond the scope of this manual can be obtained by
calling Parr Instrument Company in order to determine
which part(s) may be replaced or serviced.
Ensurethat anyhot surfaceshave hadadequate
time to cool before cleaning or maintaining
the reactor and/or its components.
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Parr Instrument Company
6
4590 Micro Reactors
User’s Responsibility
All Parr Reactors and pressure vessels are designed and manufactured with great care to assure safe operation
when used within their prescribed temperature and pressure limits. But . . . the basic responsibility for safety
when using this equipment rests entirely with the user; who must:
1. Select a reactor or pressure vessel which has the
capability, pressure rating, corrosion resistance
and design features that are suitable for its in-
tended use. Parr engineers will be glad to dis-
cuss available equipment and material options
with prospective users, but the final responsi-
bility 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 intro-
duced 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 pres-
sure 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 recom-
mended 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 cus-
tomer’s responsibility to provide pressure relief
in order to protect the operator and the equip-
ment from destructive high pressures. If you
need more information or need help in selecting
a proper relief device, please contact Parr Instru-
ment 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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4590 Micro Reactors
www.parrinst.com 7
Parr Series 4590 Micro Reactors are furnished with two structural options in addition to the size, pressure
range, stirrer motor, controller and similar options.These are:
Fixed Head or Removable Head Vessel Design
In the fixed head design, the head of the vessel
may remain fixed in the reactor support stand. All
attachments to the head, gas and liquid feed and
discharge lines, cooling water, vapor take-off and
condenser, thermocouple, and any electrical leads
can remain permanently in place. The reactor is
opened by removing the split ring sections and
lowering the cylinder away from the head.
In the removable vessel design, the entire vessel
must be removed from the support stand for charg-
ing, product recovery, and cleaning.
There is no difference in the pressure or temperature
limits or basic operating instructions based upon the
fixed head or movable vessel options.There are dif-
ferences in the design of the stand components which
adapt the vessels to the support system.
Flat Gasket or Self Sealing O-Ring Closure
The flat gasket is held in a recess in the vessel
head and a machine pilot on the cylinder closes the
recess to completely contain the gasket. The split
ring closure used with this gasket has six cap screws
which must be tightened to develop the loading on
the gasket.
The self sealing design features an O-ring retained
in a groove on the vessel head. This design is self
sealing and the split ring used with this sealing
system does not require nor have the cap screws
used with the flat gasket.
Maximum temperatures of a given system are
dependant upon the material of construction and
type of seal. Other accessories may limit operating
temperature.The flat PTFE gasket can be used to oper-
ating temperatures as high as 350 °C. The flat flexible
graphite gasket can be used to operating tempera-
tures as high as 500 °C.The maximum temperature of
the vessels equipped with O-ring seals depends upon
the material used for the O-ring. The most common
material is a fluoroelastomer (FKM) which has a 225 °C
maximum operating temperature limit.
Fixed Head with PTFE Gasket Moveable Head with O-ring Seal & Easy Close Split Ring
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Parr Instrument Company
8
4590 Micro Reactors
INSTALLATION
Pressure andTemperature 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 construc-
tion for Parr Instrument Company isType 316 Stain-
less Steel.
Limits for vessels made of other materials and for
other operating temperatures can be obtained from
Parr Customer Service. No attempt should be made
to increase these limits by making alterations or by
substituting components that are not recommended
by the Parr Instrument Company. It must also be
understood that lower pressure and temperature
limits may be required for modified reactors and for
vessels made of special alloys.
Limits for vessels will be determined by the physi-
cal 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.The safe operat-
ing 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.
An accompanied restricted operating limit tag and/
or supplemental manual is given when a compo-
nent of the system limits the operation below the
imprinted valves.
The standard material of construction for Parr
Instrument Company isType 316 Stainless Steel.The
working pressure and temperature in these 25, 50
& 100 mL reactors must not exceed the following
maximum limits:
Pressure Vessel and Temperature Limits
In the standard pressure and temperature setup, the
system must not exceed the following:
Vessel
Material
Maximum
Pressure
Maximum
Temperature
T316SS 3000 psig
(200 bar)
350 °C PTFE
Flat Gasket
T316SS 3000 psig
(200 bar)
225 °C FKM
O-Ring
T316SS 3000 psig
(200 bar)
300 °C FFKM
O-Ring
In the high pressure/high temperature setup, the
system must not exceed the following:
Vessel
Material
Maximum
Pressure
Maximum
Temperature
T316SS (HP) 5000 psig
(345 Bar)
350 °C PTFE
Flat Gasket
T316SS
(HPHT)
5000 psig
(345 Bar)
500 °C Flexible
Graphite
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4590 Micro Reactors
www.parrinst.com 9
Assemble The Reactor
These reactors require at least 10 sq. ft. of workspace
in a well-ventilated area with convenient access to an
electric outlet, running water, air and a drain.
1. Set the stand in the workspace.
Bolt the stand to the bench top using the
holes in the base plate.
2. Set the Reactor Controller near the reactor, leav-
ing 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.
Note: Do not make connections to aVariac,
Power-stat or the like to attempt to control
the heating output. The heavy inductive
load on the primary side of such devices
can destroy the internal sold state relay
located in the 4848 controller.
Parr Motor Only:
The Motor output connector is to be used only
with Parr Instrument Company motor assemblies
supplied with the appropriate motor power cord.
3. Connect the heater cord from the heater into
the heater socket on the rear panel of the Series
4848 Reactor Controller.
4. Plug the motor cord into the motor socket on the
rear of the controller.
Secure the clamp on the motor cord with
the provided screw next to the motor
socket for safety purposes.
5. Connect the thermocouple and extension wire
to both the thermocouple and to the controller
in the “PrimaryTemp Input” position on the rear
panel. Insert the thermocouple in the thermowell.
6. Connect leads from accessory packages such as
tachometer, pressure transducer and high temp
cut-off to the designated positions on the back
panel of the 4848 Controller.
7. Connect cooling water to the magnetic drive.
See Instruction Manual No. 234M.
8. Connect tubing to the rupture disc outlet and run
to a safely vented area. See Instruction Manual
231M.
9. Note the voltage and amperage requirement
stamped on the controller data plate, and then
plug the power cord into an appropriate outlet.
Power for these reactors should be drawn from
a grounded outlet capable of carrying up to the
full current rating of the reactor.
10. If an electric stirrer motor is supplied, turn the
speed control knob fully counterclockwise on
the Reactor Controller, turn on the motor switch
and slightly increase the speed for a short run
to check the stirrer drive system but do not turn
on the heater, put heater toggle switch in center
position (OFF).There must always be a vessel in
the heater when it is turned on, and the vessel
and heater sizes must match. If the heater is op-
erated without proper size vessel in contact with
the heater, the heater may overheat and fail.
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4590 Micro Reactors
Parr Instrument Company
10
IDENTIFY THE VALVES
Gas Inlet Valve
The gas inlet valve is easily identified when the
vessel is open by noting that it is connected to a dip
tube which extends to a point near the bottom of
the cylinder. With this arrangement, incoming gas is
always introduced below the surface of the liquid.
This valve includes a coupling with an “A” socket
connection for attachment of the pressure hose.
Gas Release Valve
The gas release valve is typically connected to a side
opening on the gage adapter. Gas released from
this valve will be drawn from the top of the reactor.
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 clear-
ing 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.
Thermocouple
Magnetic Drive
Gas Release Valve
Liquid Sampling Valve
Gas Inlet Valve
Safety Rupture Disc
Pressure Gage
Standard Head Fittings for Micro Reactor
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4590 Micro Reactors
www.parrinst.com 11
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 pres-
sure at stated 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 mate-
rial 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
AType J thermocouple in a 1/8” dia. stainless steel
sheath is furnished with the reactor. Insert this ther-
mocouple 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.
Pressure Gage
The pressure gage furnished with this reactor has
aT316 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 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 materi-
als. These isolators with their internal piston isolate
the vapors from the gage.
The gage adapter may include 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.
ACCESSORIES AND OPTIONS
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 reac-
tants, 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 Cylinder
Size
Glass
Liner
PTFE
Liner
1.3” 50 mL 1431HC 1431HCHA
1.3” 100 mL 1431HC2 1431HC2HA
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.
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4590 Micro Reactors
Parr Instrument Company
12
Air Motor
Variable stirring speeds from 100 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 10CFM
available at that pressure. It is furnished with a
speed control valve and oiler, all assembled on a
mounting bracket.
To operate reactors equipped with an air motor,
mount the drive system firmly on the stand and con-
nect 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 con-
tinuous 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 felts are dirty, wash them in solvent or
replace them. Relubricate 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 directions given in the
instruction sheet published by the Gast Manufactur-
ing Corp., Benton Harbor, Michigan.
Air Motor Option
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Notes
www.parrinst.com 13
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4590 Micro Reactors
Parr Instrument Company
14
HOW TO USE THE VESSEL
Removable Vessels
Always remove removable vessels from the support
stand before attempting to open or close them.
To open the Vessel
Open the gas release valve to discharge any internal
pressure. For the bolted closure, loosen the six cap
screws in the split ring sections. Loosen the cone
pointed screw in the outer band and lower the band
to rest on the table. The ring sections can now be
removed, and the head with all attached fittings is free
to be lifted from the cylinder. Handle the head care-
fully so as not to damage the stirring shaft and other
internals when they are outside of the cylinder.
Before Closing the Vessel
Examine the head gasket or o-ring carefully to be
sure that it is in good condition. After considerable
use, some of the PTFE gasket may extrude into a
thin, ragged edge around the inside and outside
diameters. This does not necessarily mean that the
gasket must be replaced, but the extruded portion
should be removed with a sharp knife. Examine the
mating surfaces on the cylinder and head to be sure
they are clean and free from burrs; then set the head
on the cylinder.
Sealing Vessels with PTFE Gaskets
Tighten each of the cap screws with the wrench
furnished with the apparatus. Apply a firm but hard
pull to each screw. If a torque wrench is available,
apply 15 ft-lbs to each screw. DO NOT apply more
than 25 ft-lbs of torque to these bolts as this can
deform the head of the reactor. Tightening should
proceed in a criss-cross pattern rather than progres-
sively around the circle. Let the vessel stand for
about five minutes after the initial tightening; then
tighten the cap screws again. This will compensate
for any tendency of the PTFE gasket to flow under
the loading pressure.
Routinely inspect cap screws on the split ring closure
for lubrication and cleanliness. It is important to clean
and lubricate them periodically so that the required
torque is achieved when tightening the bolts.
Sealing with Flexible Graphite Gaskets
Tighten the cap screws with enclosed wrench in
same criss-cross pattern as the PTFE gasket. Initially
tighten the screws to 15 ft-lbs then increase to 20-25
ft-lbs for proper seal.
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.
Recommended Bolt Torque
PTFE 0-3000 psig
(0-200 bar)
15-20 ft-lbs
PTFE or
Flexible Graphite
3000-5000 psig
(200-345 bar)
20-25 ft-lbs
O-Ring Closures
The split rings used with an o-ring seal do not
include any compression bolts.
With the easy close split ring, the o-ring is attached
to the pilot on the underside of the head. When
closing the vessel, set the head on the cylinder and
press down on the head until the bottom of the head
meets with the cylinder flange. Then install the two
split ring halves and attach the outer drop band.
Fixed Head Vessels
Fixed head vessels are opened and closed with the
same procedure used for removable vessels except
that they are opened and closed with the head in
place. Before opening the vessel lower the heater
and swing it well to the side so that it will not be
damaged by any materials that drip from the vessel
as it is opened. When closing the vessel always
hold the cylinder until both split ring sections are in
place to lock the cylinder to the head.
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4590 Micro Reactors
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Gas Connections
For a gas connection to the vessel, use the A495HC
pressure hose (A506HC in high pressure reactors)
furnished with the reactor. Attach the hose to a pres-
sure regulator or flow control valve on a commercial
gas cylinder using PTFE tape or other thread sealant
on the 1/8” NPT male nipple and on the 1/4” NPT
bushing, if used.Then screw theType A coned pres-
sure fitting into the adapter attached to the gas inlet
valve and tighten the compression nut firmly. Do not
use any thread dope or tape on the coned fitting.The
A495HC pressure hose is made of reinforced Nylon
which can be used for all non-corrosive gases at
pressures up to 2500 psig. For operations involving
corrosive gases, this hose should be replaced with
an A490HC hose (optional) which has a PTFE lining
and a braided stainless steel outer covering.These
hoses have the same fittings as in the A495HC.
Alternately the A506HC for high pressure systems is
made ofT316 Stainless Steel tubing.
Note: For high pressure applications involving cor-
rosive gases please contact Parr Customer Service.
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
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 regula-
tor 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 discon-
nect the hose at the vessel end.
Do Not Overfill the Vessel
Always watch the pressure gage closely when admit-
ting 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 provid-
ed for expansion when the liquid is heated. This hazard
is explained in greater detail in a warning statement
included in the Instruction Manual No. 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 tem-
perature controller.
Note: The following steps are common to both head configurations.
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4590 Micro Reactors
Parr Instrument Company
16
MAINTENANCE
General Maintenance Notes
1. Periodically inspect all electrical wiring and pres-
sure connections for excessive corrosion. Sus-
pect 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 HighTempera-
ture 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 PipeTaper) 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.
7. If your vessel is equipped with a loose compres-
sion ring be sure that it is in place on the head
before attaching any head fittings.The compres-
sion ring cannot be installed after fittings have
been screwed into the head.
8. Clean all threads and gas passages thoroughly
and remove all tape fragments when overhaul-
ing a vessel. An ultrasonic bath is excellent for
cleaning metal parts, but do not place a thermo-
couple 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 clo-
sure for lubrication and cleanliness. These
screws should not be allowed to dry because
the threads will seize. Regularly apply Parr
HighTemperature Anti-Seize Lubricant (Parr No.
424HC2) before this happens.
10. To operate reactors equipped with an air motor,
connect the 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 oil-
ing rate should be increased to three drops per
minute. If the motor becomes sluggish, flush
it with a non-flammable solvent in a well venti-
lated 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. Relubricate the motor with a squirt of
oil into the chamber and reassemble.
11. If servicing assistance is needed, contact Parr
Instrument Company directly at the address
shown on the back of these instructions.
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4590 Micro Reactors
www.parrinst.com 17
Periodic Pressure Tests
Each cylinder used in a Parr stirred reactor is tested
under hydrostatic pressure to the higher of 1.43
times the rated working pressure at room tem-
perature or 1.30 times the rated working pressure
corrected for temperature before it is released from
the factory. Micrometer caliper measurements are
taken during this test to check the deflection of the
walls under pressure. Excessive deflection or failure
of the metal to resume its original dimensions after
pressure is released indicates that a cylinder is po-
tentially 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 that 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 hy-
drostatic 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 (RMA).
Apparatus returned for testing and overhaul should
be shipped prepaid to the following address:
Ship repair to:
Parr Instrument Company
Attn: Service Department
RMA # XXXXXX
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 (FX004) signed by a
responsible user.
Technical Support
Parr Instrument Company strives to provide our
customers with world class support. When contact-
ing Parr for technical support, please provide the
complete serial number etched on the side of the
cylinder. Serial numbers are a long string of letters
and numbers. See highlighted text in figure below
for an example of a complete serial number.
PARR INSTRUMENT COMPANY
MOLINE, IL. USA
2430HC3 222315 T316 112409 4600-1003-14106
MAWP 1900 PSI AT 350C 2010
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: [phone]
E-mail: [email protected]
www.parrinst.com
Each Parr operating instruction manual binder
includes a customized Parts List that contains a list
of the parts in the major components of your Parr
Reactor. Do not discard this Parts List. You should
use this parts list for reordering consumable and
replacement parts to ensure that you order the cor-
rect items for your reactor system.
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4590 Micro Reactors
Parr Instrument Company
18
SERIES 4590 VESSEL PARTS LISTS
Standard Vessel Fittings
(3000 psig / 350 °C)
Standard 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:
FH - Fixed Head OR - O-Ring Seal
RV - Removable Head SC - Screw Cap
FG - Flat Gasket SR - Split Ring
* 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 CA - Titanium G2 or G4
CG - Alloy B-2 CH - Alloy C-276
CX - Zirconium
Cylinders*
Part No. Description Code
2430HC Cylinder, 25 mL SR FG
2430HC2 Cylinder, 50 mL SR FG
2430HC3 Cylinder, 100 mL SR FG
2900HC Cylinder, 25 mL SR OR
2900HC2 Cylinder, 50 mL SR OR
2900HC3 Cylinder, 100 mL SR OR
1430HC Cylinder, 25 mL SC OR
1430HC2 Cylinder, 50 mL SC OR
1430HC3 Cylinder, 100 mL SC OR
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4590 Micro Reactors
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Heads*
Part No. Description Code
2432HC Head RV FG
2902HC Head RV OR
2772HC Head FH FG
2774HC Head FH OR
1432HC Head SC OR
Split Rings and Accessories
Part No. Description
1379HC Screw Cap SC OR
2195HC Split Ring SR RV OR
A455HC Split Ring, with six bolts SR RV
232HCFDE Compression Bolt SR RV
A456HC Drop Band SR RV
456HCF2 Drop Band Bolt SR RV
454HC Compression Ring SR RV
A2345HC3 Split Ring w/bolts SR FH FG
232HCF3DE Compression Bolt SR FH
A2193HC Split Ring SR FH OR
1433HCJV Head Seal, O-Ring, FKM SC OR
Gaskets & Seals
Part No. Description Code
48HC Gasket, silver, mag drive
48HCFG Gasket, gold plated, mag drive
2901HCJK Head Seal, O-Ring, FFKM SR OR
2901HCJV Head Seal, O-Ring, FKM SR OR
429HC2 Flat Head Gasket, PTFE SR FG
429HC2KL Flat Head Gasket, Flexible
Graphite
SR FG
1433HCJK Head Seal, O-Ring, FFKM SC OR
1433HCJV Head Seal, O-Ring, FKM SC OR
Thermowell*
Part No. Description Code
1467HC Thermowell, 25/50 mL RV
1467HC2 Thermowell, 100 mL RV
1467HC4 Thermowell, 25/50mL FH
1467HC5 Thermowell, 100mL FH
Dip Tube*
Part No. Description
1443HC DipTube, 25 mL
1443HC2 DipTube, 50 mL
1443HC3 DipTube, 100 mL
Shaft/Impeller Assembly
Part No. Description Code
A1987HC Shaft/Impeller, 25/50 mL SC
A1987HC2 Shaft/Impeller, 100 mL SC
A1987HC3 Shaft/Impeller, 25/50 mL RV
A1987HC4 Shaft/Impeller, 100 mL RV
A1987HC5 Shaft/Impeller, 25/50mL FH
A1987HC6 Shaft/Impeller, 100mL FH
Gages
Part No. Description
593HCP1AD Gage, 3-1/2” 100 psi/bar
593HCP2AD Gage, 3-1/2” 200 psi/bar
593HCP6AD Gage, 3-1/2” 600 psi/bar
593HCPD Gage, 3-1/2” 1000 psi/bar
593HCPF Gage, 3-1/2” 2000 psi/bar
593HCPG Gage, 3-1/2” 3000 psi/bar
593HCP40AD Gage, 3-1/2” 4000 psi/bar
593HCP50AD Gage, 3-1/2” 5000 psi/bar
External Fittings
Part No. Description
A122VB Straight Valve 1/8 NPTM
A146VB Angle Valve 1/8 NPTM
420HC Adapter “A” Socket x 1/8 NPT(F)
195VBAD Tee, Branch 1/8 NPT MFF
836HC Gage Adapter, ¼” NPT (top), 1/8” (side)
836HC6 Gage Adapter, ¼” NPT (top), (2) ¼”
NPT (side), 1/8” (side)
836HC7 Gage Adapter, ¼” NPT (top), (1) ¼”
NPT (side), 1/8” (side)
A833HC Male Connector forThermocouple 1/8T
A138CA* Male Connector forThermowell ¼T
A472E Thermocouple, SS, 7-1/2” L
A472E4 Thermocouple, SS, 5-1/2” L
A490E Thermocouple, SS, dual 7-1/2” L
A888HC2 Safety Rupture Disc Assembly
(See 231M)
49HC2 Orifice Cone
527HC Orifice Ring
433HC4 Safety Head
366VB Hex Coupling
288VBAD Male Connector
526HC_ /
581HC_ Rupture Disc series for the A888HC2
A1120HC6* Magnetic Drive Assembly
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