Parr Instrument 4575, 4576 HP-HT User Manual

416M

4575/76

HP/HT Pressure Reactors

Operating Instruction Manual

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
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

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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
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: [phone] E-mail: [e-mail] http://www.parrinst.com

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.

4575/76 HP/HT Pressure Reactors

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 aType 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 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 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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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 overor un- der-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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4575/76 HP/HT Pressure 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 construction for Parr Instrument Company Vessels isType 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.

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:

Pressure and Temperature Limits

	Vessel	Maximum	MaximumTemperature
	Material	Pressure
	T316SS	5000 psi	500 °C Flexible Graphite
			Gasket
	T316SS	5000 psi	350 °C PTFE 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.

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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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.

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 “PrimaryTemp Input” position on the rear panel. Insert the thermocouple into thermowell.

4575/76 HP/HT Pressure Reactors

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.

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4575/76 HP/HT Pressure Reactors

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.

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

Gas Inlet Valve

	Magnetic Drive
	Thermocouple
	/ Thermowell
Liquid
Sampling	Gas Release Valve
Valve

Head

Dip Tube	Thermocouple /
Stirring Shaft	Thermowell

Propellers	Cooling Loop

Fixed Head

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