Parr Instrument 6100 User Manual

6100
Compensated Jacket Calorimeter
Operating Instruction Manual
For models produced after October 2010
584M
Table of Contents6100
Scope 3
Related Instructions 3
Explanation of Symbols 4
Safety Information 4
Intended Usage 4
General Specifications 4
Environmental Conditions 5
Provisions for Lifting and Carrying 5
Cleaning & Maintenance 5
Getting Started 5
Concept of Operation 6
Overview 6
Compensated Jacket Operation 6
Dynamic Operation 7
Full Microprocessor Based Process Control 7
Full Microprocessor Based Data Acquisition and Handling 7
Flexible Programming 7
Chapter 4 14
Program Installation & Control 14
Software Installation 14
Default Settings 14
Revising Default Settings 14
Chapter 5 18
Operating Instructions 18
Operating the 1108P Oxygen Combustion Vessel 18
Operating the Filling Connection 18
Operating the Calorimeter 18
Samples and Sample Holders 20
Combustion Aids 20
Oxygen Charging Pressure 20
Combustion Capsules 20
Foodstuffs and Cellulosic Materials 21
Coarse Samples 21
Corrosive Samples 21
Explosives and High Energy Fuels 22
Volatile Sample Holders 22
Poor Combustion 23
Installation 8
Environmental Conditions 8
Required Consumables, Utilities and Power Requirements 8
Oxygen Filling Connection 8
Printer and Balance Connections 8
Standardizing the Calorimeter 8
Swagelok Tube Fittings 9
Retightening Swagelok Tube Fittings 9
Chapter 3 12
Instrument Description 12
Types of Controls 12
Menu Keys 13
Control Keys 13
Chapter 6 24
Corrections & Final Reports 24
Entering Corrections and Obtaining the Final Report 24
Manual Entry 24
Fixed Corrections 24
Chapter 7 26
Reporting Instructions 26
Report Option Section 26
Report Generation 26
Net Heat of Combustion 27
Chapter 8 28
File Management 28
Clearing Memory 28
Removable SD Memory Cards 28
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Table of Contents
Chapter 9 30
Maintenance & Troubleshooting 30
Oxygen Bomb 30
Fuses 30
6100 Calorimeter Error List 31
Appendix A 32
Menu Operating Instructions 32
Calorimeter Operation Menu 32
Temperature vs. Time Plot Screen 32
Temperature Plot Setup Menu 33
Operating Controls Menu 34
Spiking Correction 34
Program Information and Control Menu 35
User/Factory Settings 35
Bomb 1 37
Bomb Control Chart 37
Thermochemical Calculations Menu 38
Calculation Factors 38
Net Heat/Dry Heat Factors 39
Data Entry Controls Menu 40
Net Heat Data Entry Controls 40
Auto Sample ID Controls 40
Moisture Data Entry Controls 41
Auto Preweigh Controls 41
Reporting Controls Menu 42
Communication Controls Menu 42
Balance Port Communications 43
File Management 44
Diagnostics Menu 44
ASTM Treatment for Acid and Sulfur 49
ISO Calculations 50
Spiking Samples 50
Conversion to Other Moisture Bases 51
Conversion to Net Heat of Combustion 51
Appendix C 52
Standardization 52
Standardizing the Calorimeter 52
Standard Materials 52
Automatic Statistical Calculations 52
Appendix D 56
Communications Interfaces 56
USB Port for Connection 56
Balance and Port Input Driver Specifications 56
Mettler 011/012 Balance Interface 56
Sartorius Balance Interface 56
Generic Interface 57
Network Interface 58
Samba Server Feature (Optional) 59
Bar Code Port 67
Network Data Devices 67
Appendix E 68
Technical Service 68
Contact Technical Service 68
Return for Repair 68
Appendix B 46
Calculations 46
Calculating the Heat of Combustion 46
General Calculations 46
Thermochemical Corrections 46
ASTM and ISO Methods Differ 47
Fuse Correction 47
Acid and Sulfur Corrections 48
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Appendix F 70
Parts Lists & Drawings 70
Principal Assemblies in Calorimeter 70
Parts List for A1279DD2 Controller Assembly 70
Parts List for A1284DD2 Stirrer Hub Assembly 70
Parts List for Oxygen Filling System 71
6100 Stirrer Motor and Drive Parts List 71
Printer and Supplies 71
Spare and Installation Parts List 71
6100

Preface

Figures
Swagelok Tube Fittings 10
6100 Compensated Jacket Calorimeter Back Panel 11
2811 Pellet Press 20
3601 Gelatin Capsules 21
43A6 Combustion Capsule with Adhesive Tape Seal 21
43AS Combustion Capsules 21
Combustion Capsule with Adhesive Tape Seal 22
6100 Compensated Jacket Calorimeter Cutaway Front 72
6100 Compensated Jacket Calorimeter Cutaway Rear 73
A1279DD2 Control Schematic 74
A1278DD Oxygen Solenoid Assembly 75
A1284DD2 Stirrer Hub Assembly 76
Stirrer Motor Assembly 77
Customer Service
Questions concerning the installation or operation of this instrument can be answered by the Parr Customer Service Department:
Tables
Factory Default Settings 16
Settings for ISO & BSI Methods 49 Calorimeter Control Limit Values in J/g When Benzoic
Acid is Used as a Test Sample 53 Calorimeter Control Limit Values in cal/g When Benzoic
Acid is Used as a Test Sample 54 Calorimeter Control Limit Values in BTU/lb When Benzoic
Acid is Used as a Test Sample 55
6100 Data File Naming Convention 57
6100 Calorimeter Run Data Template 57
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
Preface

Scope

This manual contains instructions for installing and operating the Parr 6100 Calorimeter. For ease of use, the manual is divided into nine chapters.
Concept of Operation Installation Instrument Description Program Installation & Control Operating Instructions Corrections & Final Reports Reporting Instructions File Management Maintenance & Troubleshooting
Subsections of these chapters are identified in the Table of Contents.
To assure successful installation and operation, the user must study all instructions carefully before starting to use the calorimeter to obtain an under­standing of the capabilities of the equipment and the safety precautions to be observed in the operation.

Related Instructions

Additional instructions concerning the installation and operation of various component parts and pe­ripheral items used with the 6100 Calorimeter have been included and made a part of these instructions.
No. Description
201M Limited Warranty 483M Introduction to Bomb Calorimetry 418M 1108P Oxygen Combustion Vessel 207M Analytical Methods for Oxygen Bombs
Additional instructions for the printer are found in the respective package and should be made a part of this book.
Note: The unit of heat used in this manual is the International Table calorie, which is equal to 4.1868 absolute joules.
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Preface

Explanation of Symbols

I On Position
O Off Position
~ Alternating Current
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.
ATTENTION, Electrostatic Discharge (ESD) hazards. Observe precau­tions for handling electrostatic sensitive devices.
Protective Earth (PE) terminal. Provided for connection of the protec-
tive earth (green or green/yellow) supply system conductor.
Chassis Ground. Identifies a connection to the chassis or frame of the equipment shall be bonded to Protective Earth at the source of supply in accordance with national and local electrical code requirements.
Earth Ground. Functional earth connection. This connection shall be bonded to Protective earth at the source of supply in accordance with national and local electrical code requirements.

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 com-
bustible materials; re or explosion may result.
This device contains components which may ignite such material.

Intended Usage

If the instrument is used in a manner not specified by Parr Instrument Company, the protection pro­vided by the equipment may be impaired.
General Specifications
Electrical Ratings
115VAC, 2.0 Amps. 50/60 Hz 230VAC, 2.0 Amps, 50/60 Hz
Before connecting the calorimeter 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: Calorimeters can be operated from either a 50 or 60 Hertz power supply without affect­ing their operation or calibration.
2. Refer servicing to qualified personnel.
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Current: The total current drawn should not exceed
the rating shown on the data plate on the calorim­eter by more than 10 percent.
6100
Preface

Environmental Conditions

Operating: 15 ºC to 30 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 ºC and 65 ºC; 10% to 85% relative
humidity.

Provisions for Lifting and Carrying

Before moving the instrument, disconnect all con­nections from the rear of the apparatus. Lift the instrument by grabbing underneath each corner.

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.

Getting Started

These steps are offered to help the user become familiar with, install, operate and develop the full capabilities of the Parr 6100 Calorimeter.
1. Review the Concept of Operations, Chapter 1, to get an understanding of the overall capabilities of the calorimeter and microprocessor control.
2. Unpack and install the calorimeter in accordance with the Installation Instructions, Chapter 2. This simple, step-wise procedure will acquaint the user with the various parts of the calorimeter and make it easier to understand the operating
instructions which follow.
3. Turn the power switch ON (located on the back). Turn to the Instrument Description, Chapter 3, to review the touch screen controls.
4. Review the Program Installation and Control, Chapter 4, to match the factory settings to the in­tended mode of operation. Any required changes can be made to the program parameters located in the Main Menu.
5. Review the Reporting Instructions, Chapter 7, to become familiar with the manner in which calo­rimetry corrections are entered. Also discussed are generating final reports, editing and clearing memory.
6. Turn to the Menu Operating Instructions, Ap-
pendix A, to review the menu functions used
to modify the program contained in the 6100 Calorimeter. A review of the menus will provide
a good idea of the capabilities and exibility
designed into this instrument.
7. Review the Calculations, Appendix B. This pro- vides information about calculations performed by the 6100 Calorimeter.
8. Review Standardization, Appendix C. This will serve two important functions. First, it provides instructions on generating the energy equivalent factor required to calculate the heat of combus­tion of unknown samples. Secondly, it will give the user the opportunity to run tests on a mate­rial with a known heat of combustion to become familiar with the instrument and confirm that the instrument and operating procedures are pro­ducing results with acceptable precision. Most 6100 Calorimeters will have an energy equiva-
lent of approximately 2400 calories per ºC. The
runs for standardization and determinations are
identical, except for the setting of the instrument
to the standardization or determination mode.
9. Review the Communication Interfacing, Appen­dix D, for the correct installation of any peripher­als connected to the 6100 Calorimeter.
10. After successful standardization, the 6100 Calo­rimeter should be ready for testing samples.
Note About Nomenclature:
Historically, burning a sample enclosed in a high pressure oxygen environment is known as Oxygen Bomb Calorimetry and the vessel containing the sample is known as an Oxygen Bomb. The terms bomb and vessel are used interchangeably.
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1
Concept of Operation

chaPter 1

Concept of Operation

Overview

The 6100 Calorimeter has been designed to provide the user with:
The Model 6100 can also be equipped with a vari-
ety of special purpose oxygen bombs for unusual samples and/or applications. The 1104 High Strength Oxygen Combustion Vessel is designed for testing explosives and other potentially hazardous materials. The 1109A Semimicro Oxygen Combustion Vessel can
be fitted along with its unique bucket to test samples ranging from 25 to 200 mg.
A traditional design calorimeter with removable
oxygen bomb and bucket.
A moderately priced calorimeter which uses real
time temperature measurements to determine heat leaks without using a controlled calorimeter jacket.
A full featured calorimeter that does not require circulating water.
A compact calorimeter requiring minimum laboratory bench space.
A modern intuitive graphical user interface for ease of operation and training.
A calorimeter with up to date digital hardware, software and communications capabilities.
A calorimeter that is cost effective and which can incorporate a user’s current bombs, buckets, and accessories.
Removable Bomb
The Model 6100 Calorimeter utilizes the Parr 1108P
Oxygen Combustion Vessel. More than 20,000 of the 1108 style oxygen combustion vessels have been
placed in service on a world wide basis. This bomb features an automatic inlet check valve and an adjust­able needle valve for controlled release of residual gasses following combustion. They are intended for samples ranging from 0.6 to 1.2 grams with a maxi­mum energy release of 8000 calories per charge.
The 1108P Oxygen Combustion Vessel is made of
high-strength, high nickel stainless steel designed to resist the corrosive acids produced in routine fuel testing. An alternative 1108PCL vessel is available, constructed of an alloy containing additional cobalt and molybdenum to resist the corrosive conditions produced when burning samples containing chlori­nated compounds.
Removable Bucket
The A391DD removable bucket has been designed to hold the bomb, stirrer and thermistor with a mini­mum volume of water and to provide an effective circulating system which will bring the calorimeter to rapid thermal equilibrium both before and after firing.

Compensated Jacket Operation

The 6100 Calorimeter is intended for the user who wants a calorimeter with the convenient automatic features provided in a modern isoperibol calorimeter, but whose precision requirements can be met with a static system. To meet these criteria, the temperature controlled water jacket and its accessories have been removed from the 6200 Isoperibol Calorimeter and replaced with an insulating jacket around the bucket chamber. This eliminates all water and water connections, resulting in a significant saving in cost. To obtain the best precision with an uncontrolled jacket, the 6100 Calorimeter has temperature moni­toring capability built into the jacket. This allows the calorimeter to measure the actual jacket temperature and apply the appropriate heat leak corrections in real time. While, not equal to a controlled jacket, the 6100 method offers a significant improvement over the traditional static jacket and makes it possible to obtain reasonable precision without the long pre­and post-periods normally required for static jacket calorimetry. It also makes it possible to use the Parr Dynamic Method for rapid testing. As with all static jacket calorimeters, best results are obtained when the instrument is operated in a location where it is not subject to air drafts and fluctuating tempera­tures. The preferred operating environment is in a
temperature controlled room (+/- 1 C). It is a well
accepted principle of reliable analysis that any instru­ment calibration be checked regularly. The optimum frequency for checking the 6100 Calorimeter depends largely on the temperature stability of the operating environment. As general rule, the instrument calibra­tion should be evaluated at least every tenth test. The calorimeter controller software conveniently offers both a graphical control chart approach in addition to
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6100
Concept of Operation
1
an automatic rolling average calculation to support calibration maintenance and verification. Following the aforementioned guidelines and using reference samples, such as benzoic acid, the process sigma (precision classification) of the 6100 Calorimeter can
be taken as 0.1%.

Dynamic Operation

In its Dynamic Operating Mode, the calorimeter uses a sophisticated curve matching technique to compare the temperature rise with a known thermal curve to extrapolate the nal temperature rise without actu­ally waiting for it to develop. Repeated testing, and over 20 years of routine use in fuel laboratories, has demonstrated that this technique can significantly cut the time required for a test by one-half without significantly affecting the precision of the calorimeter.

Full Microprocessor Based Process Control

The microprocessor controller in this calorimeter has been pre programmed to automatically prompt the user for all required data and control input and to:
Generate all temperature readings in the calorim­eter.
Monitor jacket as well as bucket temperature.
Collect and store all required test data.
Apply all required corrections for combustion
characteristics.
Compute and report the heat of combustion for the sample.

Flexible Programming

The fifth generation software built into this calorim­eter and accessed through the screen menus permit the user to customize the operation of the calorimeter to meet a wide variety of operating conditions includ­ing:
A large selection of printing options.
Choice of accessories and Peripheral equipment.
Multiple options in regard to handling
thermochemical corrections.
Choice of ASTM or ISO Correction procedures.
A variety of memory management and reporting
procedures.
Complete freedom for reagent concentrations and calculations.
Confirm equilibrium conditions.
Fire the bomb.
Confirm that ignition has occurred.
Determine and apply all necessary heat leak cor-
rections.
Perform all curve matching and extrapolations
required for dynamic operation.
Terminate the test when it is complete.
Monitor the conditions within the calorimeter and
report to the user whenever a sensor or operating condition is out of normal ranges.

Full Microprocessor Based Data Acquisition and Handling

In addition to its process control functions, the mi­croprocessor in the calorimeter has been pre pro­grammed to:
Unlimited choice of reporting units.
Automatic bomb usage monitoring and reporting.
A choice of Equilibrium or Dynamic test methods.
Automatic statistical treatment of calibration runs.
Enhanced testing and trouble shooting procedure.
The 6100 Calorimeter is equipped with a universal serial bus (USB) connection for communication with a printer, balance, or other device. If more than one device is to be used at the same time a USB hub will need to be used. It is also equipped with an Ethernet network connection for connections to laboratory computers.
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2
Installation

chaPter 2

Installation

Environmental Conditions

The 6100 Calorimeter is completely assembled and given a thorough test before it is shipped from the factory. If the user follows these instructions, instal­lation of the calorimeter should be completed with little or no difficulty. If the factory settings are not disturbed, only minor adjustments will be needed to adapt the calorimeter to operating conditions in the user’s laboratory.
This apparatus is to be used indoors. It requires at least 4 square feet of workspace on a sturdy bench or table in a well-ventilated area with convenient access to an electric outlet, running water and a drain.

Required Consumables, Utilities and Power Requirements

The 6100 Calorimeter System requires availability of
Oxygen, 99.5% purity, 2500 psig maximum.
The power requirements for the subassemblies of the 6100 Calorimeter are:
Calorimeter
115VAC, 2.0 Amps. 50/60 Hz 230VAC, 2.0 Amps, 50/60 Hz
Printer
100 to 240 VAC, 0.35 Amps 50/60 Hz
Plug the power line into any grounded outlet provid­ing proper voltage that matches the specification on the nameplate of the calorimeter. The calorimeter will
draw approximately 100 watts of power. Grounding is
very important not only as a safety measure, but also to ensure satisfactory controller performance. If there is any question about the reliability of the ground connection through the power cord, run a separate earth ground wire to the controller chassis.
Turn the power switch to the on position. After a short time, the Parr logo will appear on the LCD display followed by a running description of the instrument boot sequence. When the boot sequence is complete, the calorimeter Main Menu is displayed.

Oxygen Filling Connection

The 6100 Calorimeter is equipped with an automatic
bomb oxygen lling system. This system consists of an oxygen pressure regulator with a relief valve that mounts on an oxygen tank and a controlled solenoid
inside the calorimeter. To install the regulator on the
oxygen supply tank, unscrew the protecting cap from the oxygen tank and inspect the threads on the tank
outlet to be sure they are clean and in good condi­tion. Place the ball end of the regulator in the outlet and draw up the union nut tightly, keeping the gages tilted slightly back from an upright position. Connect
the regulator to the oxygen inlet tting on the back of
the calorimeter case. This hose should be routed so that it will not kink or come in contact with any hot surface. Connect the high-pressure nylon hose with
the push on connector to the oxygen bomb outlet
connection on the back of the calorimeter.
All connections should be checked for leaks. Any leaks detected must be corrected before proceeding. Instructions for operating the filling connection are in the Operating Instructions chapter. Adjust the pres­sure regulator to deliver 450 psi of O2. Assemble the
oxygen bomb without a charge and attach the lling
hose to the bomb inlet valve. Press the O2 Fill key on the Calorimeter Operation page and observe the delivery pressure on the 0 – 600 psi gage while the oxygen is owing into the bomb. Adjust the regula­tor, if needed, to bring the pressure to 450 psi. If there is any doubt about the setting, release the gas from the bomb and run a second check.

Printer and Balance Connections

Connect the printer to the calorimeter at this time. The Parr 1758 Printer is configured and furnished with a cord to connect directly to the USB port on the back of the calorimeter.
The balance port connection, if needed, should be made at this time. If both a printer and a balance will be used then a USB hub will need to be installed. Contact Parr to determine the correct cable to connect the balance to the calorimeter.

Standardizing the Calorimeter

The calorimeter must be accurately standardized prior to actually performing calorimetric tests on sample materials. Review Appendix C - Standardiza­tion, in order to become familiar with the general
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6100
Installation
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procedure and calculations. The user should config­ure the calorimeter at this time to accommodate the desired sample weight entry mode. The calorimeter can be placed into standardization mode on the Calorimeter Operation Page, with the operating mode key. If multiple bombs and buckets are being used with the calorimeter to maximize sample through­put, the calorimeter can be configured to prompt for a Bomb ID at the start of each test. The Bomb ID can also be selected on the Calorimeter Operations
Page, using the Bomb/EE key. Both bomb and bucket
combinations will need to be standardized separately. The end result of a standardization test is an energy equivalent value, or the amount of energy required to raise the temperature of the calorimeter one degree. Repeated standardization with any given bomb and bucket combination should yield an energy equiva­lent value with a range of 14 calories per degree, centered around the mean value for all tests using that bomb bucket combination. The calorimeter is ready for testing samples after an energy equivalent value has been obtained.

Swagelok Tube Fittings

When Swagelok Tube Fittings are used, the instruc­tions for installation are:
original position with a wrench. An increase in re­sistance will be encountered at the original posi­tion. Then tighten slightly with a wrench. Smaller tube sizes (up to 3/16” or 4mm) take less tighten­ing to reach the original position than larger tube sizes. The type of tubing and the wall thickness also has an effect on the amount of tightening re­quired. Plastic tubing requires a minimal amount of additional tightening while heavy wall metal tubing may require somewhat more tightening. In general, the nut only needs to be tightened about
1/8 turn beyond nger tight where the ferrule
seats in order to obtain a tight seal.
Over tightening the nut should be avoided. Over
tightening the nut causes distortion (flaring) of the lip of the tube fitting where the ferrule seats. This in turn causes the threaded portion of the body to deform. It becomes difficult to tighten the nut by hand during a subsequent re-tightening when the fitting body becomes distorted in this manner.
Figure 2-1
Swagelok Tube Fittings
1. Simply insert the tubing into the Swagelok Tube Fitting. Make sure that the tubing rests firmly on the shoulder of the fitting and that the nut is finger-tight.
2. Before tightening the Swagelok nut, scribe the nut at the 6 o’clock position.
3. While holding the fitting body steady with a back-
up wrench, tighten the nut 1-1/4 turns. Watch the
scribe mark, make one complete revolution and continue to the 9 o’clock position.
4. For 3/16” and 4mm or smaller tube ttings, tight-
en the Swagelok nut 3/4 turns from nger-tight.

Retightening Swagelok Tube Fittings

Swagelok tubing connections can be disconnected and retightened many times. The same reliable leak­proof seal can be obtained every time the connection is remade using the simple two-step procedure.
1. Insert the tubing with pre-swaged ferrules into the fitting body until the front ferrule seats.
2. Tighten the nut by hand. Rotate the nut to the
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Installation
Figure 2-2
6100 Compensated Jacket Calorimeter Back Panel
Note: The Cooling Water Outlet, Cooling Water Inlet, Tank Fill and Tank Drain ports are not used on the 6100 Calorimeter.
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6100
Notes
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3
Instrument Description

chaPter 3

Instrument Description

Types of Controls

All calorimeter configurations and operations are handled by a menu-driven system operated from the bright touch screen display. The settings and controls are organized into nine main sections or pages which comprise the MAIN MENU.
12
Note: Keys with a “double box” in the upper left hand corner lead to sub-menus.
Parr Instrument Company
6100

Menu Keys

The controls that change the data field information in the menus will be one of the following:
1. Toggles: These data elds contain ON/OFF or YES/NO choices. Simply touching the key
2. Option Selection: These data fields contain a list of options. Touching the key on the
3. Value Entry Fields: These data fields are used to enter data into the calorimeter. Touching
4. Data Displays: Most of these keys display values that have been calculated by the calorim-
Instrument Description
on the screen toggles the choice to the other option. The current setting is displayed in the lower right corner of the key.
screen steps the user through the available choices. The current setting is displayed in the lower right corner of the key.
the key on the screen brings up a sub menu with a key pad or similar screen for entering the required value. Some keys lead to multiple choices. Always clear the current value be­fore entering a new value. Once entered the screen will revert to the previous menu and the new value will be displayed in the lower right corner of the key.
eter and are informational only. Certain ones can be overridden by the user entering a de­sired value through a sub-menu. The value is displayed in the lower right corner of the key.
3
Note: Some keys will respond with an opportunity for the user to confirm the speci­fied action to minimize accidental disruptions to the program and/or stored data.

Control Keys

There are five control keys which always appear in the right column of the primary displays. These keys are unavailable when they are gray instead of white.
1. Escape: This key is used to go up one level in the menu structure.
2. Main Menu: This key is used to return to the main menu touch screen from anywhere in
the menu structure.
3. Start: This key is used to start a calorimeter test.
4. Report: This key is used to access the test results stored in the calorimeter, to enter ther-
mochemical corrections and to initiate a report on the display or printer.
5. Help: This key is used to access help screens related to the menu currently displayed on
the touch screen.
6. Abort: This key appears in the start key location while the test is running. Pressing this
key will abort the test in progress.
7. This key appears on the main menu only and is used to prepare the calorimeter for turning off the power.
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4
Program Installation & Control

chaPter 4

Program Installation & Control

Software Installation

The program in the 6100 Calorimeter can be exten­sively modified to tailor the unit to a wide variety of operating conditions, reporting units, laboratory techniques, available accessories and communica­tion modes.
In addition, the calculations, thermochemical cor­rections and reporting modes can be modified to conform to a number of standard test methods and procedures.
Numerous provisions are included to permit the use of other reagent concentrations, techniques, combustion aids and short cuts appropriate for the user’s work.
Note: Changes to the program are made by use of the menu structure described in Ap­pendix A of this manual. Any of these items can be individually entered at any time to revise the operating program.

Revising Default Settings

The default parameters of the 6100 Calorimeter can be changed to guarantee that the 6100 Calorimeter, when cold restarted, will always be in the desired configuration before beginning a series of tests.
Users who wish to permanently revise their default settings may do so using the following procedure:
1. Establish the operating parameters to be stored as the user default settings.
2. Go to the Program Information and Control
Menu, User/Factory Settings, User Setup ID, and
enter the desired User Setup ID.
3. Select Save User Default Settings.
To re-load the user default setting, go to the Pro-
gram Information and Control Page, User/Factory, Re-load User Default Settings, and YES.

Default Settings

Units are pre programmed with DEFAULT SET­TINGS. See Pages 16 and 17 for a listing of the factory default settings.
These default settings remain in effect until changed by the user. Should the user ever wish to return to the factory default settings, go to the Program In-
formation and Control Menu, User/Factory Settings
and Reload Factory Default Settings.
Non-volatile memory is provided to retain the date and time; even if power is interrupted or the unit is turned off.
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Notes
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4
Program Installation & Control
Table 4-1

Factory Default Settings

Calorimeter Operations
Operating Mode Determination
Bomb Installed/EE 1/2400.0
Operating Controls
Method of Operation Dynamic
Reporting Units BTU/lb
Use Spiking Correction OFF
“OTHER” Multiplier 4.1868
Calibrate Touchscreen
LCD Backlight Timeout(s)
LCD Backlight Intensity 70%
Print Error Messages ON
Language English
1200 s
Spike Controls
Use Spiking OFF
Heat of Combustion of Spike 6318.4
Use Fixed Spike OFF
Weight of Fixed Spike 0.0
Prompt for Spike before Weight OFF
Program Information and Controls
Date & Time Settings
Software and Hardware Info
Settings Protect OFF
User/Factory Settings
Feature Key
Bomb Type Select
User Function Setup
Cold Restart
User/Factory Settings
User Setup ID 61-1108
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Calibration Data & Controls
Calibration Run Limit
EE Max Std Deviation 0.0
Heat of Combustion of Standard 6318.4
Bomb Service Interval 500
Control Chart Parameters
Use Bomb 1
10
Bomb 1 Through 4
EE Value 2400.0
Protected EE Value OFF
Thermochemical Corrections Standardization
Fixed Fuse Correction ON 50
Acid Correction Fixed HNO3 10.0
Fixed Sulfur Correction ON 0.0
Heat of Formation Sulfuric Acid
Heat of Formation Nitric Acid 14.1
36.1
Determination
Fixed Fuse Correction ON 50
Acid Correction Fixed HNO3 10.0
Fixed Sulfur Correction OFF 0.0
Calculation Factors
Nitric Acid Factor 1.58
Acid Multiplier 0.0709
Sulfur Value is Percent ON
Sulfur Multiplier 0.6238
Fuse Multiplier 1.0
Use Offset Correction (ISO) OFF
Offset Value 0.0
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Parr Instrument Company
6100
Program Installation & Control
4
Net Heat/Dry Factors
Fixed Hydrogen OFF 0.0
Fixed Oxygen ON 0.0
Fixed Nitrogen ON 0.0
Calculate Net Heat of Combustion OFF
Fixed Moisture as Determined OFF 0.0
Fixed Moisture as Received OFF 0.0
Dry Calculation OFF
Data Entry Controls
Prompt for Bomb ID ON
Weight Entry Mode Touch Screen
Acid Entry Mode Touch Screen
Net Heat Entry Values Touch Screen
Auto Sample ID Controls ON
Sample Weight Warning above 2.0
Spike Weight Entry Mode Touch Screen
Sulfur Entry Mode Touch Screen
Moisture Entry Modes Touch Screen
Auto Preweigh Controls ON
Auto Sample ID Controls
Automatic Sample ID ON
Automatic Sample ID Increment 1
Automatic Sample ID Number 1
Auto Preweigh Controls
Automatic Preweigh ID ON
Automatic Preweigh ID Increment 1
Automatic Preweigh ID Number 1
Communication Controls
Printer Type Parr 1758
Balance Port
Network Interface
Printer Destination Local (USB)
Bar Code Port
Network Data Devices
Balance Port Communications
Balance Type Generic
Balance Port Device /dev/ttyUSB0
Customize Balance Settings
Balance Port Settings
Number of Data Bits 8
Parity None
Number of Stop Bits 1
Handshaking None
Baud Rate 9600
Data Characters from Balance 8
Data Precision 4
Transfer Timeout (seconds) 10
Balance Handler Strings
Data Logger
Data Logger OFF
Data Log Interval 10s
Data Log Destination Log File and Printer
Select Data Log Items
Data Log Format Text Format
Reporting Controls
Report Width 40
Automatic Reporting ON
Auto Report Destination Printer
Individual Printed Reports OFF
Edit Final Reports OFF
Recalculate Final Reports OFF
Use New EE Values in Recalculation OFF
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5
Operating Instructions

chaPter 5

Operating Instructions

Operating the Calorimeter

All operations required to standardize the 6100 Calo­rimeter, or test an unknown sample, should proceed step-wise in the following manner:

Operating the 1108P Oxygen Combustion Vessel

Detailed instructions for preparing the sample and
charging the 1108P Oxygen Combustion Vessel are
given in Operating Instructions No. 418M. Follow these instructions carefully, giving particular atten­tion to the precautions to be observed in charging and handling the bomb.

Operating the Filling Connection

To fill the bomb, connect the hose to the bomb inlet valve and push the O2 Fill button on the calorimeter control panel. The calorimeter will then fill the bomb to the preset pressure and release the residual pressure in the connecting hose at the end of the
lling cycle. It will take approximately 60 seconds to
fill the bomb. During this time a countdown timer on the O2 fill button will display the remaining fill time. Pushing the O2 key a second time will stop the
ow of oxygen at any time. Once the display returns
to its normal reading, the user can disconnect the coupling and proceed with the combustion test.
If the charging cycle should be started inadvertently, it can be stopped immediately by pushing the O2 fill key a second time.
During extended periods of inactivity, overnight
or longer, close the tank valve to prevent leakage.
When changing oxygen tanks, close the tank valve and push the O2 FILL key to exhaust the system. Do
not use oil or combustible lubricants on this filling
system or on any devices handling oxygen under
pressure. Keep all threads, fittings, and gaskets clean and in good condition. Replace the two 394HCJE O-rings in the slip connector if the connec­tor fails to maintain a tight seal on the bomb inlet valve.
The recommended filling pressure is 450 psig (3 MPa or 30 bar). This pressure is prescribed by most of the standard bomb calorimetric test methods.
Higher or lower lling pressures can be used, but
the bomb must never be filled to more than 600 psig (40 atm).
1. Allow at least 20 minutes for the calorimeter to warm up. The bomb parts should be wetted and then dried in the manner used at the conclusion of a test. This serves to wet all sealing parts as well as leaving the bomb with the same amount of residual water which will exist in all subse­quent testing.
2. Prepare and weigh the sample to 0.0001g.
Charge the oxygen bomb as described in the Operating the Filling Connection Section. Using
an additional bomb and bucket can increase the throughput of the 6100 Calorimeter. With this arrangement, the calorimeter can operate almost continuously since the operator will be able to empty a bomb and recharge it while a run is in
progress. A bomb and bucket for the next run will
be ready to go into the calorimeter as soon as it is opened. Each bomb and bucket combination will have to be standardized separately and the proper energy equivalent for each set must be used when calculating the heat of combustion.
3. Fill the calorimeter bucket by first taring the dry bucket on a solution or trip balance; then add
2000 (+/- 0.5) grams of water. Distilled water is
preferred, but demineralized or tap water con­taining less than 250 ppm of dissolved solids is satisfactory. The bucket water temperature should be at or slightly below (1-2 degrees) be­low the room temperature. It is not necessary to
use exactly 2000 grams, but the amount selected must be duplicated within +/- 0.5 gram for each
run. Instead of weighing the bucket, it can be filled from an automatic pipet, or from any other volumetric device if the repeatability of the filling
system is within +/- 0.5 mL.
To speed and simplify the bucket filling process, and to conserve water and energy, Parr offers a
closed circuit Water Handling System (No. 6510).
This provides a water supply, cooled to the starting temperature and held in an automatic pipet ready
for delivery in the exact amount needed to ll the
bucket, at a repeatable temperature. Instructions for this automatic system are given in Operating Instruction No. 454M.
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Parr Instrument Company
6100
Operating Instructions
5
4. Set the bucket in the calorimeter. Attach the lifting handle to the two holes in the side of the screw cap and partially lower the bomb in the water. Handle the bomb carefully during this op­eration so that the sample will not be disturbed. Push the two ignition lead wires into the termi­nal sockets on the bomb head. Orient the wires away from the stirrer shaft so they do not be­come tangled in the stirring mechanism. Lower the bomb completely into water with its feet spanning the circular boss in the bottom of the bucket. Remove the lifting handle and shake any drops of water back into the bucket and check for gas bubbles.
5. Close the calorimeter cover. This lowers the stir­rer and thermistor probe into the bucket.
6. Select determination or standardization as ap­propriate on the Calorimeter Operation page, by toggling the operating mode key. Press the START key. The calorimeter will now prompt the operator for Bomb ID number, sample ID num­ber, sample weight and spike weight in accor­dance with the instructions set into the Operat­ing Controls page.
7. The calorimeter will now take over and conduct the test. During the time it is establishing the initial equilibrium, it will display PREPERIOD on
the status bar. Just before it res the bomb, it
will sound a series of short beeps to warn the user to move away from the calorimeter. Once the bomb has been fired, the status bar will dis­play POSTPERIOD. The calorimeter will check to make certain that a temperature rise occurs and will then look for the final equilibrium conditions to be met. If it fails to meet either the initial or final equilibrium conditions, or if it fails to detect a temperature rise within the allotted time, the calorimeter will terminate the test and advise the user of the error.
one minute to avoid entrainment losses. After all pressure has been released, unscrew the cap;
lift the head out of the cylinder and examine the
interior of the bomb for soot or other evidence of incomplete combustion. If such evidence is found, the test will have to be discarded. Oth­erwise, wash all interior surfaces of the bomb, including the head, with a jet of distilled water and collect the washings in a beaker.
10. Titrate the bomb washings with a standard sodium carbonate solution using methyl orange, red or purple indicator. A 0.0709N sodium car­bonate solution is recommended for this titra­tion to simplify the calculation. This is prepared by dissolving 3.76 grams of Na2CO3 in the water
and diluting to one liter. NaOH or KOH solutions
of the same normality may be used.
11. Analyze the bomb washings to determine the
sulfur content of the sample if it exceeds 0.1%.
Methods for determining sulfur are discussed in Operating Instructions No. 207M.
12. At the end of the testing period, go to the main menu and press the key. Press YES to con-
firm System Shutdown. Turn off the calorimeter at the power switch when prompted by the display.
8. At the conclusion of the test, the calorimeter will signal the user.
9. Open the cover and remove the bomb and bucket. Remove the bomb from the bucket and open the knurled valve knob on the bomb head to release the residual gas pressure before at­tempting to remove the cap. This release should proceed slowly over a period of not less than
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5
Operating Instructions

Combustion Aids

Some samples may be difficult to ignite or they may burn so slowly that the particles become chilled below the ignition point before complete combus­tion is obtained. In such cases benzoic acid, white oil or any other combustible material of known purity
can be mixed with the sample. Ethylene glycol,
butyl alcohol or decalin may also be used for this purpose.
Note: It must be remembered, however, that a combustion aid adds to the total energy released in the bomb and the amount of sample may have to be reduced to compen­sate for the added charge.
Figure 5-1

2811 Pellet Press

Samples and Sample Holders

Particle Size and Moisture Content. Solid samples
burn best in an oxygen bomb when reduced to 60
mesh, or smaller, and compressed into a pellet with a Parr 2811 Pellet Press.
Large particles may not burn completely and small particles are easily swept out of the capsule by turbulent gases during rapid combustion.
Note: Particle size is important because it influences the reaction rate. Compression into a pellet is recommended because the pres­sure developed during combustion can be reduced as much as 40% when compared to the combustion of the material in the powder form. In addition to controlling burn rates, the pelletizing of samples keeps the sample in the fuel capsule during combustion.
Materials, such as coal, burn well in the as-received or air-dry condition, but do not burn completely dry samples. A certain amount of moisture is desirable in order to control the burning rate. Moisture con-
tent up to 20% can be tolerated in many cases, but
the optimum moisture is best determined by trial combustions.
If moisture is to be added to retard the combustion rate, drop water directly into a loose sample or onto a pellet after the sample has been weighed. Then let the sample stand for awhile to obtain uniform distribution.
Also, when benzoic acid is combusted for stan­dardization runs or for combustion aid purposes, it should be in the form of a pellet to avoid possible damage to the bomb which might result from rapid combustion of the loose powder.

Oxygen Charging Pressure

The 6100 Calorimeter has been designed to operate with an oxygen lling pressure of 30 atm. Signi­cant changes from this value are not recommended.

Combustion Capsules

Non-volatile samples to be tested in Parr oxygen
combustion vessels are weighed and burned in
steel, fused silica, fused quartz, and platinum al-
loyed with 3-1/2% rhodium.
Stainless steel capsules (43AS) are furnished with each calorimeter. When combusting samples that contain metal particles such as aluminum or magne­sium, the non-metallic fused silica 43A3 Capsule or fused quartz 43A3KQ is required. When superior cor­rosion resistance is needed, the Platinum Rhodium 43A5 Capsule is required.
The stainless steel capsules will acquire a dull gray
nish after repeated use in an oxygen bomb due to the formation of a hard, protective oxide lm. This
dull finish not only protects the capsule, but it also promotes combustion and makes it easier to burn the last traces of the sample.
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Parr Instrument Company
6100
Operating Instructions
5
Figure 5-2

3601 Gelatin Capsules

Capsules should be monitored for wear. Do not use the capsule if the wall or base thickness is less than
0.025”.
New capsules are heated in a muffle furnace at 500 ºC for 24 hours to develop this protective coating uniformly on all surfaces. This treatment should be repeated after a capsule has been polished with an abrasive to remove any ash or other surface depos-
its. Heating in a mufe is also a good way to destroy
any traces of carbon or combustible matter which might remain in the capsule from a previous test.
Note: After heating, place the capsules in a clean container and handle them only with forceps when they are removed to be weighed on an analytical balance.

Foodstuffs and Cellulosic Materials

Fibrous and fluffy materials generally require one of three modes of controlling the burn rate. Fibrous materials do not pelletize readily and generally require either moisture content or a combustion aid such as mineral oil to retard the burn rate and avoid development of high pressures.
43A6 Combustion Capsule with
Figure 5-3
Adhesive Tape Seal
Figure 5-4

43AS Combustion Capsules

Coarse Samples

In most cases it may be necessary to burn coarse samples without size reduction since grinding or drying may introduce unwanted changes. There is no objection to this if the coarse sample will ignite and burn completely.
Whole wheat grains and coarse charcoal chunks are typical of materials which will burn satisfactorily without grinding and without additives or a special procedure.

Corrosive Samples

The 1108P Oxygen Combustion Vessel is made of a
corrosion resistant alloy designed to withstand the corrosive mixture of sulfuric and nitric acids pro­duced in normal fuel testing operations. Samples containing chlorine and particular samples contain­ing more than 20 mg of chlorine samples with high sulfur contents will greatly accelerate corrosion of the bomb. An alternate 1108PCL vessel is available constructed of an alloy selected to specifically resist the corrosive effects of samples with high chlorine or other halogens.
Partial drying may be necessary if the moisture con­tent is too high to obtain ignition, but if the sample is heat sensitive and cannot be dried, a water soluble combustion aid such as ethylene glycol can be added to promote ignition.
While no material will offer complete corrosion resistance to these samples, the 1108PCL vessel offers significantly enhanced corrosion resistance for this service.
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5
Operating Instructions

Explosives and High Energy Fuels

The 1108P and 1108PCL vessels used in the 6100 Calorimeter have been designed to provide highly automated testing of routine samples. Materials which release large volumes of gas which detonate
with explosive force or burn with unusually high
energy levels should not be tested with these bombs.
Rather, they should be tested in a model 1104 High Pressure Oxygen Combustion Vessel designed
specifically for these types of samples.

Volatile Sample Holders

Volatile samples can be handled in a Parr 43A6 Platinum Capsule with a spun rim, or in a Parr 43AS Alloy Capsule which has a sturdy wall with a flat top rim. These holders can be sealed with a disc of plastic adhesive tape prepared by stretching tape
across the top of the cup and trimming the excess
with a sharp knife. The seal obtained after pressing this disc firmly against the rim of the cup with a flat blade will be adequate for most volatile samples.
The tape used for this purpose should be free of chlorine and as low in sulfur as possible. Borden Mystic Tape, No. M-169-C or 3M Transparent Tape, No. 610, are recommended for this purpose. The 3M Transparent Tape can be ordered through Parr, Part No. 517A.
Figure 5-5

Combustion Capsule with Adhesive Tape Seal

Use the following procedure when filling and handling any of these tape-sealed sample holders:
Weigh the empty cup or capsule; then cover the top with tape, trim with a knife and press the trimmed edge firmly against the metal rim. Also cut and attach a small flag to the disc (see Figure 5-5).
Puncture the tape at a point below the flag, then re-weigh the empty cup with its tape cover.
Add the sample with a hypodermic syringe; close the opening with the flag and re-weigh the filled cup.
The weight of the tape disc must be determined separately and a correction applied for any elements in the tape which might interfere with the deter-
mination. The approximate Heat of Combustion of the tape is 6300 cal/g. An actual amount should be
determined by running a blank test with tape alone using a sample weighing 1.0 gram. The compensa­tion for heat of tape may be done through the spike option; see Spike Controls, Line 2 - Heat of Combus­tion of Spike.
Note: Tape should always be stored in a sealed container to minimize changes in its moisture and solvent content.
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Parr Instrument Company
Set the cup in the capsule holder and arrange the auxiliary fuse so that it touches the center of
the tape disc.
Just before starting the test, prick the disc with
a sharp needle to make a small opening which is needed to prevent collapse of the disc when pressure is applied.
Fill the bomb with the usual oxygen charging
pressure.
The calorimeter will fire the bomb and complete the test in the usual manner.
6100
Operating Instructions
5
Volatile samples are defined as one with an initial boiling point below 180 ºC per ASTM D-2.
Low volatile samples with a high water content, such as urine or blood, can be burned in an open capsule by absorbing the liquid on filter paper pulp or by adding a combustion aid, such as ethylene glycol.

Poor Combustion

Because of the difference in combustion char­acteristics of the many different materials which
may be burned in an oxygen bomb, it is difcult to
give specific directions which will assure complete combustions for all samples.
The following fundamental conditions should be considered when burning samples:
Some part of the sample must be heated to its ignition temperature to start the combustion and, in burning, it must liberate sufficient heat to support its own combustion regardless of the chilling effect of the adjacent metal parts.
Insufficient space between the combustion cup and the bottom of the bomb. The bottom of the cup should always be at least one-half inch above the bottom of the bomb or above the liquid level in the bomb to prevent thermal quenching.
Excessive moisture or non-combustible material
in the sample. If the moisture, ash and other non combustible material in the sample amounts to
approximately 20% or more of the charge, it may
be difficult to obtain complete combustion. This condition can be remedied by adding a small amount of benzoic acid or other combustion aid.
The combustion must produce sufficient tur- bulence within the bomb to bring oxygen into
the fuel cup for burning the last traces of the sample.
Loose or powdery condition of the sample which will permit unburned particles to be ejected dur­ing a violent combustion.
The use of a sample containing coarse particles which will not burn readily. Coal particles which are too large to pass a 60 mesh screen may not burn completely.
The use of a sample pellet which has been made too hard or too soft. Either condition can cause spalling and the ejection of unburned fragments.
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