Parr Instrument 6100 User Manual

Page 1
6100
Compensated Jacket Calorimeter
Operating Instruction Manual
For models produced after October 2010
584M
Page 2
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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
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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.
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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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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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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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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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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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Notes
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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.
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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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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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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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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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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.
Page 25
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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6
Corrections & Final Reports

chaPter 6

Corrections & Final Reports

Entering Corrections and Obtaining the Final Report

Final reports for each test can be obtained whenever the operator is prepared to enter any required cor­rections for fuse, acid and sulfur.
When entering corrections, the user can choose either of two methods. These are:
Manual Entry
Fixed Corrections
Program and Installation, Chapter 4. provides the default settings used to setup the method preferred by the user.
Refer to the Reporting Instructions, Chapter 7, for the steps necessary to initiate a report from the controller.

Manual Entry

During the reporting process, the controller will prompt the user to enter the following values:
Fuse Correction: Key in the Fuse Wire Correction and press the ENTER key. The default setting for this value is to be entered in calories. The fuse correction
has two components and these are explained in Appendix B.
If xed values for fuse, acid and sulfur are turned
OFF on the Thermochemical Corrections Page, then the user must manually enter the values at the prompt.
If the Spiking Correction is used, a spiking correction must be entered before obtaining a Final Report.
After the last entry has been made, the calorimeter will automatically produce a Final Report.
If values for these corrections are not available, the operator can use the SKIP key to bypass any of the corrections; however, a Final Report will not be printed until an entry is made for fuse, acid and sulfur.

Fixed Corrections

In many cases, xed values for fuse and acid can be
used without introducing a significant error since the corrections are both relatively small and con­stant.
Fixed sulfur corrections can also be used whenever
a series of samples will be tested with a reasonably constant sulfur content.
Details for applying xed corrections are found in Appendix B, Thermochemical Calculations.
Acid Correction: Key in the Acid Correction and press the ENTER key. The default setting for this value is to be entered in milliliters of standard alkali required to titrate total acid or calories.
Sulfur Correction: Key in the Sulfur Correction and press the ENTER key. The default setting for this value is to be entered as percent sulfur in the sample.
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Parr Instrument Company
Any value set-up as a xed correction will be auto­matically applied and the controller will not prompt the user for this value.
Page 27
6100
Notes
6
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7
Reporting Instructions

chaPter 7

Reporting Instructions

Report Option Section

The 6100 Calorimeter can transmit its stored test data in either of two ways. The REPORT DESTINA- TION key on the Reporting Controls Page toggles the report destination between the display and an optional printer connected to the USB port of the calorimeter. This page also selects the type of reports that are generated automatically by the calorimeter.

Report Generation

There are two kinds of calorimeter reports: Prelimi­nary and Final.
Select From List: This key displays the stored results specified with the following two keys:
Preliminary Reports are generated at the conclusion of a test. They will not contain the final thermochem­ical corrections for sulfur, fuse, or acid. They are intended to confirm to the operator that the results
of the test fell within the expected range.
Final reports are generated once all of the thermo­chemical corrections have been entered into the file. If xed corrections are used for all of the thermo­chemical corrections a preliminary report will not be generated.
Thermochemical corrections are entered by using the following steps to select and edit preliminary reports.
Test results are stored as files using the sample ID number as the file name. A listing of the stored results is accessed by pressing the REPORT com­mand key. The REPORT command key brings up a sub-menu on which the operator specifies.
Run Data Type: This key enables the opera­tor to display only determination runs, only standardization runs and all runs. (The choice of solution data type is not applicable to this calorimeter.)
Run Data Status: This key enables the opera­tor to display only preliminary reports, only fi­nal reports, both preliminary and final reports, only pre weighed sample reports or all stored reports.
Prompt For Final Values: When turned on, the controller will prompt the operator to enter any missing corrections for fuse, sulfur and acid in any selected preliminary reports. When turned off preliminary reports will be displayed as entered.
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6100
The displayed files can be sorted by sample ID num­ber, by type, by status or by date of test by simply touching the appropriate column.
Individual files can be chosen by highlighting them using the up and down arrow keys to move the cursor. Press the SELECT key to actually enter the selection. Once selected the highlight will turn from dark blue to light blue. A series of tests can be selected by scrolling through the list and selecting individual files.
The double up and down keys will jump the cursor to the top or bottom of the current display.
If a range of tests is to be selected, select the first test in the series, scroll the selection bar to the last test in the series and press EXTEND SEL to select the series.
The DESEL ALL key is used to cancel the current selection of files.
To bring the selected report or series of reports to the display, press the DISPLAY key. To send the re- ports to the printer press the PRINT key.
Reporting Instructions

Net Heat of Combustion

To have the Net Heat of Combustion print as part
of preliminary and final reports, go to the Thermo-
chemical Corrections Page, Net Heat/Dry Factors, and turn ON Calculate Net Heat of Combustion. Dur-
ing the reporting process, the controller will prompt
for the hydrogen (H) value.
7
The EDIT key brings up a sub-menu which enables the operator to edit any of the data in the report or add thermochemical corrections to convert prelimi­nary reports to final reports. Final reports can only be edited if EDIT FINAL reports on the reporting control page is turned on.
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Page 30
8
File Management

chaPter 8

File Management
The 6100 Calorimeter will hold data for 1000 tests in its memory. These tests may be pre weights, preliminary or final reports for either standardization or determination runs. Once the memory of the controller is filled, the controller will not start a new analysis until the user clears some of the memory.

Clearing Memory

The FILE MANAGEMENT key on the main menu leads to the file management sub-menu. The RUN DATA FILE MANAGER key leads to a listing of the files.
Single files can be deleted by highlighting the file and pressing the DELETE key. The controller will then ask the user to confirm that this file is to be deleted.
A series of files can be deleted by selecting the first file in the series and then the last file in the series using the EXTEND SEL key and then pressing the DELETE key.

Removable SD Memory Cards

The controller of the 6100 Calorimeter can accept SD memory cards. These cards can be used to:
Copy test file data for transfer to a computer.
Copy user settings for back up.
Reload user settings to the controller.
Restore or update the controller’s operating
system.
SD memory cards are inserted into one of the slots on the back of the control section of the calorimeter. Keys are provided on the FILE MANAGEMENT sub­menu to initiate each of the above three actions with the exception of restoring or updating the control­ler’s operating system.
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Page 31
6100
Notes
8
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9
Maintenance & Troubleshooting

chaPter 9

Maintenance & Troubleshooting

Oxygen Bomb

Under normal usage the 1108P Parr Oxygen Com­bustion Vessel will give long service if handled with
reasonable care. However, the user must remember
these bombs are continually subjected to high tem­peratures and pressures that apply heavy stresses to the sealing mechanism. The mechanical condition of the bomb must therefore be watched carefully and any signs of weakness or deterioration should be replaced before they fail.
It is recommended the 1108P Oxygen Combustion
Vessel have O-rings and valve seats replaced after 6 months, 500 firings or at more frequent intervals if the bomb has been subject to heavy usage or if it
Parr Part No. Description Type Ratings
139E23 Lines Protective Fuses Fast-Acting 15 Amps, 250Vac
shows any evidence of damage. Detailed informa­tion can be found in Manual 418M supplied as a
part of this manual. This 1108P Oxygen Combustion
Vessel is the only part of the calorimeter system that requires routine maintenance. All other problems will require diagnosis and parts replacement.

Fuses

The replacement of protective fuses for the 6100 Calorimeter should be performed by qualified personnel.
Note: Check the labels on the instrument for correct fuse rating.
Caution! For continued protection against possible hazard, replace fuses with same type and rating of fuse.
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6100

6100 Calorimeter Error List

The calorimeter will run a number of diagnostic checks upon itself and will advise the operator if it detects any
error conditions. Most of these errors and reports will be self-explanatory. The following list contains errors
that are not necessarily self-evident and suggestions for correcting the error condition.
Maintenance & Troubleshooting
9
A Misfire Condition Has Been Detected
This error will be generated in the event the total
temperature rise fails to exceed 0.5 °C after the rst
minute of the post-period.
A Preperiod Timeout Has Occurred
The calorimeter has failed to establish an acceptable initial temperature, prior to firing the bomb, within the time allowed. Possible causes for this error are listed below:
A bomb leak
Poor bucket stirring
Metal to metal contact between the bucket and
the jacket
Lid not tight
Foam seal has deteriorated
Starting bucket temperature is too low or too
high
Unstable room temperature
A Postperiod Timeout has Occurred
The calorimeter has failed to establish an acceptable final temperature within the time allowed. Possible causes for this error are listed below:
A bomb leak
Poor bucket stirring
Unstable room temperature
There Is A Problem With The Bucket Thermistor
Possible electrical open or short. These errors will result if the temperature probe response is not within
the expected range. Probe substitution can be useful
in determining the cause of the problem (probe or electronics). The valid working range of the probe resistance is 1000 to 5000 ohms.
There Is A Problem With The Jacket Thermistor
Possible electrical open or short. These errors will result if the temperature probe response is not within
the expected range. Probe substitution can be useful
in determining the cause of the problem (probe or electronics). The valid working range of the probe resistance is 1000 to 5000 ohms.
Check connection to board
Check quick disconnect between cables
Replace probe
Room temperature is below 10 °C (50 °F)
A/D Initialization Failed
Shortly after power is applied to the calorimeter controller and the operating system has started, the CPU attempts to read the unique IO board calibra­tion information from the IO board. If the IO board is not connected to the CPU, or the information on the board is not valid, this error will be issued.
Bomb ID – Has Been Fired – Times Which Exceeds The Bomb Service Interval
The calorimeter controller keeps track of how many times the bomb has been red. When this count ex­ceeds a preset limit (usually 500) this message will be issued each time the bomb is used for a test. Perform bomb maintenance and reset the bomb fire count on the Calibration Data and Control page for the appro­priate bomb number.
You Have Exceeded The Run Data File Limit (1000 Files)
The memory set aside for test runs has been filled. Use the memory management techniques to clear out non-current tests. See page 31.
Bomb EE Standard Deviation Warning
The relative standard deviation for the calibration
runs in memory for the indicated bomb exceeds the
preset limit.
Check connection to board
Check quick disconnect between cables
Replace probe
Room temperature is below 10 °C (50 °F)
Sample Weight Warning
The entered sample mass exceeds the value entered
via the [Sample Weight Warning Above] key on the Data Entry Controls page. This warning threshold is normally 2 grams.
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Page 34
A
Menu Operating Instructions

aPPendix a

Menu Operating Instructions
When the START key is pressed, the calorimeter will prompt the user for the Sample ID, sample weight, Bomb ID and spike weight as programmed by the user in the Operating Controls and Data Entry Con­trol menu screens.
The settings and controls are organized into ten main sections or pages which comprise the Main
Menu. This appendix describes all pages of the
menu-based operating system of the 6100 Calorim­eter.
Operating Mode: Sets the operating mode by tog­gling between standardization and determination.
Bomb/EE: Used to identify the bomb presently installed in the calorimeter and its EE value.
Start Preweigh: This key is used to start the sample preweigh process. The user is presented with or
prompted for a sample ID. Next, the user is asked to
key in the associated sample mass or alternatively the mass is retrieved from a connected balance.
O2 Fill: This key is used to activate the oxygen lling
system used to fill the bomb. Pressing this same key while the bomb is filling will abort the process.
Note: Keys which make global changes to the setup of the calorimeter contain a YES or NO response to make certain that the user wishes to proceed. This two step entry is intended to prevent inadvertent global pro­gram changes.

Calorimeter Operation Menu

The calorimeter will normally be operated from the Calorimeter Operating Page, although tests can always be started from any menu page.
Temperature Graph: Press this key to view the Temperature vs. Time Plot Screen.

Temperature vs. Time Plot Screen

Setup: Press this key to access the Temperature Plot Setup Menu, which has many keys that
permit the user to fully customize both the x (time) axis and the scaling of the y axis.
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Temperature Plot Setup Menu

Enable Bucket: Toggles ON/OFF.
Bucket Autoscale: Toggles ON/OFF.
Enable Jacket: Toggles ON/OFF.
Jacket Autoscale: Toggles ON/OFF.
Time Mode: Toggles between Autoscale, Win-
dow, and Range.
Bucket Plot Symbol: Toggles between:
» No Point
» Small Dot
» Round
» Square
» Up Triangle
» Down Triangle
» Diamond
Bucket Min Value: Press this key to access its
numeric dialog box to set a minimum bucket
value.
Jacket Min Value: Press this key to access its
numeric dialog box to set a minimum jacket
value.
Time Window: Sets the time scale for the X-
axis.
Time Units: Toggles between minutes and seconds.
Bucket Plot Color: Toggles between:
» Red
» Green
» Yellow
» Blue
» Magenta
» Cyan
» White
» Black
Bucket Max Value: Press this key to access its
numeric dialog box to set a maximum bucket
value.
Jacket Plot Color: Toggles between (same as Bucket Plot Color, above).
Jacket Max Value: Press this key to access its
numeric dialog box to set a maximum jacket
value.
Time Minimum: Press this key to access its
numeric dialog box to set the least amount of
time for the run.
Time Maximum: Press this key to access its
numeric dialog box to set the greatest amount
of time for the run.
Jacket Plot Symbol: Toggles between (same as Bucket Plot Symbol, above).
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Operating Controls Menu

Method of Operation: Offers an operating mode of either dynamic or equilibrium. In most cases, the dynamic mode with its curve matching capability
will save approximately 3-4 minutes per test and will
produce the same operating precision as the slower equilibrium mode.
Reporting Units: Toggles between BTU/lb, cal/g, J/ kg. Other, and MJ/kg. A user selected set of report­ing units may be programmed by selecting “Other”.
Spike Correction: This key accesses sub-menu, Spike Controls. Spiking is the material addition, such as benzoic acid or mineral oil, to samples which are difficult to burn in order to drive the combustion to completion.

Spiking Correction

Use Spiking: When set to ON, the calorimeter will prompt for the weight of the spike added and will compensate for the heat of combus­tion in the calculations.
Heat of Combustion of Spike: The heat of combustion of spike is entered on sub-menu
keyboard in cal/g.
Use Fixed Spike: When set to ON, a constant amount of spike is to be added to each test.
Weight of Fixed Spike: The weight of the fixed
spike is entered on a sub-menu keyboard.
Prompt for Spike before Weight: When set to ON, the calorimeter will prompt the user for the weight of the spike and the weight of the sample. Normally the calorimeter will prompt the user for the weight of the sample and then the weight of the spike.
Note: The precision of tests with fixed spikes can be no better than the repeatability of the spike weight.
Other Multiplier: This button allows the user to enter a final multiplier that is used when the report-
ing units are set as “Other”.
Calibrate Touchscreen: This key prompts the user to touch the screen at predefined points in order to facilitate touchscreen calibration.
LCD Backlight Time Out: The unit is equipped with an automatic circuit to shut-off the backlight when it is not being used. The back light will shut-off if there is no keyboard activity for the number of seconds entered. Pressing any key will automatically turn the back lighting ON. A setting of 0 will keep the back­light ON at all times.
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LCD Backlight Intensity: This key accesses a sub-
menu with a slide control which adjusts the contrast on the LCD display for optimum viewing.
Print Error Messages: When turned ON, all error messages will be printed on the printer as well as displayed on the screen.
Language: Steps the calorimeter through the in­stalled operating languages.
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Program Information and Control Menu

Date & Time: Accesses a sub-menu to set the cur­rent date and time.
Date: Displays current date and accesses
sub-menu on which date is set in (YY/MM/DD)
format.
Time: Displays current time and accesses sub-
menu on which time is set in (HH:MM) format.
Time Zone: Displays the selected time zone in relation to Greenwich Mean Time. Pressing this key will step through the time zones and automatically adjust the time setting.
Volume Level Adjust: Opens a window with a slide adjustment to set the volume of the key clicks and
alarms of the calorimeter. Default is 85%.
Software and Hardware Info: This screen displays important information such as the main software
version, I/O board hardware information, CPU type,
IO firmware revision, and Controller IP address.
Settings Protect: Provides protection for the pro­gram options and settings on the menus. If this is turned ON, the user will be warned that enumera­tion keys are locked when a key is pressed. Enumer-
ation Keys either toggle a value (ON/OFF) or select
from a predefined list. This feature is used primarily to protect the instrument settings from accidental changes if one were to inadvertently touch or bump up against the touch screen.
User/Factory Settings: This key leads to a sub­menu that allows the user to save or recall user defined instrument settings. Additionally, factory pre installed settings supporting different bombs or special operating modes can also be recalled.

User/Factory Settings

User Setup ID: Used to enter a unique identi­fier for recalling user settings.
Reload Factory Default Settings: Used to erase all of the settings and restore the factory de­fault settings.
Reload User Default Settings: Used to restore the last saved user’s setup should the program in the instrument be corrupted for any reason.
Save User Default Settings: Used to record the setup to the memory once the user has config­ured the instrument to their operating require­ments.
Compare Settings With Factory Defaults: This button will bring up a screen that will show the differences in the current settings of the calo­rimeter with the factory defaults.
Feature Key: Unique Feature Keys obtained from Parr allow the user to access capabilities on the instrument such as bar code interfacing or remote operation of the calorimeter, or Samba Server.
Bomb Type Select: This key toggles through the different bomb models available for the calorimeter. When the user chooses a bomb, the instrument must be re-booted to load the correct version of the software.
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User Function Setup: This key leads to sub menus
that support the conguration of ve factory/user
definable function keys. The function keys are acces­sible from the Diagnostics page.
Cold Restart: This is essentially the same as cycling power on the unit. All valid test data will be retained during this cold restart procedure.
Calibration and Data Controls Menu
Calibration Run Limit: Displays the maximum
number of runs that will be included in determining the EE value of a bomb and bucket combination and accesses the sub-menu on which this limit is set.
Most test methods suggest 10 tests. Tests in excess
of the most recent ones used are still available but are not used in the calculation of the EE value. For
example if 11 standardization tests have been run, the
calorimeter will only use the most recent 10. The 11th is still stored in the memory and is available for view or printing.
EE Max Standard Deviation: Displays the maximum
relative standard deviation in percent that will be per­mitted for any EE value calculated by the calorimeter and accesses the sub-menu on which this limit is set.
If this value is exceeded, the user will be warned to
take corrective action before proceeding with testing. This calorimeter is capable of achieving a value of
0.33 or better for 10 tests. A setting of zero disables
this check.
Heat of Combustion of Standard: Displays the heat of combustion in calories per gram for the material used to standardize the calorimeter and accesses the sub-menu on which this value is set. For benzoic acid, this value is 6318.4 calories per gram.
Bomb Service Interval: Displays the maximum
number of times a bomb may be fired before it is flagged as due for service and accesses the sub­menu on which this limit is set. Parr recommends 500 firings for this service interval.
Control Chart Parameters: A control chart is a graphi­cal tool which can assist the user in determining whether or not their process is in control. Many standard methods will dictate that a reference sample be measured periodically and the results plotted on a graph. Limits for acceptable values are defined and the process is assumed to be in control as long as the results stay within these limits. Since results are
expected to scatter with a normal distribution within
established limits, systematic trends or patterns in the data plots may also be an early warning of prob­lems.
Charted Value: Toggles the charted value be-
tween the HOC Standard (Heat Of Combustion
of Standard) and Energy Equivalent.
Process Sigma: In relation to calorimetry, sig­ma is used as the classification of the instru­ment. The higher the process sigma the higher the limits for acceptable values for precision control.
Note: The 6100 is a .2 Process Sigma calorimeter.
Temp. Rise High Warning: Sets a limit for the
temperature rise during a test. If the tempera-
ture rise exceeds the limit the user will be
warned.
Temp. Rise Low Warning: Sets a lower limit warning for the temperature rise during a test. If the temperature rise is lower than this set­ting the user will be warned.
Use Bomb: Displays the bomb number of the bomb currently installed in the calorimeter and toggles through the four possible bomb numbers. The left and right arrow keys are used to toggle through the bomb identification numbers available for each bomb.
Bomb 1 - Bomb 4: Leads to sub-menus for Bomb 1 - Bomb 4. Displays standardization information for bomb and bucket combinations. While only one bomb and bucket is installed in the calorimeter at a time, a spare may be used for servicing and for more rapid turn-around. The respective EE values for each bomb can be stored in memory.
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Note: For rapid turn around between tests, user may wish to use two bombs. Each bomb should be assigned a bomb number. Set prompt for bomb ID to “ON”.

Bomb 1

EE Value: Displays the calculated EE value for the corresponding Bomb 1.
Manual EE Entry: This key allows the user to manually enter an EE or calibration factor for a given calorimeter ID or bomb head. If an EE value is manually entered, it is necessary to turn the Protect EE Value ON in order to prevent this value from being overwritten by an automatic update.
Print Standardization Runs: Will print all of the tests that have been incorporated into the calcu­lated EE value. This will be helpful in evaluating a series of tests which fail to produce a satisfactory EE value and relative standard deviation.
Reset Bomb Fire Count: After bomb service, press this button to reset the fire count to zero
Control Chart Plot: Displays the current standard­ization runs being used to calculate the Bomb EE Value. The display will either chart the value of
the Heat of Combustion (HOC) of the Standard
or the Energy Equivalent (EE) depending on the selection on the Control Chart Parameters menu (see Calibration Data and Controls menu).
You can display the information used for each test by
selecting the appropriate green dot.
Number of Runs: Displays how many runs have been used to determine the EE value.
Relative Standard Deviation: Displays the rela­tive standard deviation for the series of tests used to determine the current EE value in percent of the EE value.
Bomb Fire Count: Displays the current bomb firing count or the number of times the bomb has been fired since it was last serviced. When this count matches the limit set by Bomb Service Interval, the user will be informed that the bomb is ready to be service.
Name: Enables the operator to assign a unique alpha-numeric label for the bomb ID. The ID can be up to 8 characters.
Protect EE Value: When set to ON, protects the EE value iwf the user does not wish to have the calo­rimeter automatically update its own EE value.
Update Statistics: This key will cause the EE value for this bomb ID to be updated using the most recent standardization runs; if the EE value is not protected. (The number of standardization runs used is equal to the value entered into the Calibration Data and Controls Menu under Cali­bration Run Limit. If less runs are available than the number specified, all runs will be used.)

Bomb Control Chart

Bomb 2: Accesses sub-menu, Bomb 2. Provides the same controls as described for Bomb 1.
Bomb 3: Accesses sub-menu, Bomb 3. Provides the same controls as described for Bomb 1.
Bomb 4: Accesses sub-menu, Bomb 4. Provides the same controls as described for Bomb 1.
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Thermochemical Calculations Menu

Standardization Correction
Fixed Fuse Correction: Displays both the ON/OFF of the xed fuse corrections for standardization runs
and the value of the correction. This key toggles
the correction ON/OFF and accesses a sub-menu on which the value is set. An appropriate xed fuse
value is 50 calories.
Acid Correction: Press this key on the LEFT side
to toggle between Fixed HNO3, Calculated HNO3, Entered Total, Entered HNO3, and Fixed Total for the
acid correction for determination runs. Press it on
the RIGHT side to access the Acid Correction nu­meric dialog box on which the value can be set.
the RIGHT side to access the Acid Correction nu­meric dialog box on which the value can be set.
Fixed Sulfur Correction: Displays both the ON/OFF of the xed sulfur corrections for determination runs
and the value of the correction. This key toggles the
correction ON/OFF and accesses a sub-menu on
which the value is set.
Note: When fixed corrections are turned ON, the value in the specified field will be used in both the preliminary and final reports. The calorimeter will not prompt for actual correc­tions. If all corrections are fixed, a prelimi­nary report will not print, rather only a final report will be generated. If values for these corrections are entered into these lines, and the toggle is set to OFF, then the fixed value will be used in the preliminary report, but not in the final report.
Calculation Factors: Accesses the Calculation Fac­tors sub-menu, which provides for setting a number of options for the way the thermochemical correc­tions are applied.

Calculation Factors

Fixed Sulfur Correction: Displays both the ON/OFF of the xed sulfur corrections for standardization
runs and the value of the correction. This key toggles
the correction ON/OFF and accesses a sub-menu on
which the value is set. When benzoic acid is used as
the calibrant, a xed sulfur value of zero should be
used.
Determination Correction
Fixed Fuse Correction: Displays both the ON/OFF of the xed fuse corrections for determination runs
and the value of the correction. This key toggles the
correction ON/OFF and accesses a sub-menu on
which the value is set.
Acid Correction: Press this key on the LEFT side
to toggle between Fixed HNO3, Calculated HNO3, Entered Total, Entered HNO3, and Fixed Total for the
acid correction for determination runs. Press it on
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Nitric Acid Factor: The default is 1.58 calories per 1000 calories of released energy.
Acid Multiplier: This multiplier is the normality of the sodium carbonate used during the acid correction titration. The default value of 0.0709 allows for direct entry of the acid correction in calories. If the bomb rinses are titrated in order to determine the acid correction, press this key to display the Acid Multiplier numeric
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dialog box, where you can change the multi­plier to represent the concentration of the base
(equivalents/L) or normality used for titration.
If this is the case, the acid correction is entered as milliliters of base used to titrate the bomb rinses.
Sulfur Value is Percent: When set to ON, the sulfur value is being entered as weight percent sulfur. If another system is to be used, this must be turned OFF and the sulfur multiplier set accordingly.
Sulfur Multiplier: Values entered by the user to be used for the sulfur correction are multiplied by this value to get the product into units of milliequivalents. The default number (0.6238) requires that the sulfur value be entered in weight percent.
Fuse Multiplier: The fuse corrections repre­sent the number of calories liberated by the burning fuse wire used to ignite the sample. If another measurement is used, the correction factor must be entered here. Press this key to
access the Fuse Multiplier numeric dialog box
and enter this multiplier value.
Net Heat/Dry Factors: Accesses the Net Heat/Dry
Factors sub-menu, which provides for setting the net heat of combustion and Dry Factors Thermochemical Corrections.

Net Heat/Dry Heat Factors

Fixed Hydrogen: Press the LEFT side to toggle
this setting ON/OFF. Press the RIGHT side to display the Fixed Hydrogen numeric dialog box and change its value.
Use Offset Correction (ISO): The thermochemi­cal calculations used for treatment of nitric acid and sulfuric acid corrections in the ISO and B. S. methods require an offset correc­tion to compensate for the back titration that is made. To use these calculations, toggle this to ON and enter the appropriate value as the offset value.
Offset Value: The value used when Offset Correction is turned ON. Press this key to ac-
cess the Offset Value numeric dialog box and
change its value.
Heat of Formation Sulfuric Acid: Different methods use different values for the heat of formation of sulfuric acid. The value can be set to match the specific method being followed. Default = 36.1.
Heat of Formation Nitric Acid: Different methods use different values for the heat of formation of nitric acid. The value can be set to match the specific method being followed. Default = 14.1.
Fixed Oxygen: ON/OFF and value entry.
Fixed Nitrogen: ON/OFF and value entry.
Calculate Net Heat of Combustion: ON/OFF.
Turn On to have the calorimeter calculate the net heat of combustion.
Fixed Moisture as Determined: Press the LEFT side to toggle ON or OFF whether to use the
entered moisture correction. Press the RIGHT side to access the Fixed Moisture as Deter­mined numeric dialog box and set the value. Units are weight %.
Fixed Moisture as Received: Press the LEFT side to toggle ON or OFF whether to use the
entered moisture correction. Press the RIGHT side to access the Fixed Moisture as Received numeric dialog box and set the value. Units are weight %.
Dry Calculation: Toggles the dry calculation ON or OFF.
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Data Entry Controls Menu

Prompt for Bomb ID: In the ON position the control­ler will prompt for a Bomb ID (1-4) when a test is started.
Weight Entry Mode: This key steps through the options for entering sample weights either manually through the touch screen, network or through the balance (USB) port.
Hydrogen Entry Mode: This key steps through the options for entering hydrogen content for calculating the net heat of combustion either manually through the touch screen or auto­matically through the balance (USB) port.
Oxygen Entry Mode: This key steps through
the options for entering oxygen content for
calculating the net heat of combustion either manually through the touch screen or auto­matically through the balance (USB) port.
Nitrogen Entry Mode: This key steps through the options for entering nitrogen content for calculating the net heat of combustion either manually through the touch screen or auto­matically through the balance (USB) port.
Automatic Sample ID Controls: Accesses sub-menu for controlling the automatic assignment of sample identification numbers.

Auto Sample ID Controls

Acid Entry Mode: This key steps through the op­tions for entering acid correction value either manually through the touch screen or automatically through the balance (USB) port.
Net Heat Entry Modes: This key accesses a menu
listing options for entering hydrogen, oxygen, and
nitrogen content for calculating the net heat of com­bustion either manually through the touch screen or automatically through the balance (USB) port.

Net Heat Data Entry Controls

Automatic Sample ID: When set to ON will automatically assign sample identification numbers in accordance with instructions set in the other two keys on this menu.
Auto Sample ID Prefix: An entry here will be
used as a prefix for all sample IDs.
Next Auto Sample ID Number: Establishes the initial sample number for a series of tests and
then shows the next sample ID which will be
assigned.
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Auto Sample ID Increment: Establishes the increment between sample numbers.
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Sample Weight – Warning Above: This key displays
and leads to a sub-menu used to set the maximum
allowable sample weight (including spike) in grams. A warning will be given if sample weights above this value are entered.
Spike Weight Entry Mode: This key steps through the options for entering spike weights either manu­ally through the touch screen, automatically through the balance (USB) port or through a network.
Sulfur Entry Mode: This key toggles steps through the options for entering sulfur correction value either manually through the touch screen or through the balance (USB) port.
Moisture Entry Mode: This key steps through the options for entering the moisture percentage wheth­er manually through the touch screen or automati­cally through the balance (USB) port.

Moisture Data Entry Controls

Auto Preweigh ID Controls: Accesses sub-menu, used to automatically assign sample identification numbers when a series of samples are pre weighed ahead of the time they are actually tested.

Auto Preweigh Controls

Automatic Preweigh ID: ON/OFF toggle for
this feature.
Moisture as Determined Entry Mode: This key steps through the options for entering the moisture as determined correction value either manually or through the touch screen or auto­matically through the balance (USB) port.
Moisture as Received Entry Mode: This key steps through the options for entering the moisture as received correction value either manually or through the touch screen or auto­matically through the balance (USB) port.
Automatic Preweigh ID Prefix: An entry here
will be used as a prefix for all pre-weigh
sample identification numbers.
Next Automatic Preweigh ID Number: Shows
the next sample identification number which
will be assigned and is used to enter the begin­ning Sample ID of any series
Automatic Preweigh ID Increment: Establishes the increment between samples.
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Reporting Controls Menu

Report Width: The column width of the printer being used can be set to 40 or 80 columns. Select 40 when the 1758 Printer is used.
Automatic Reporting: Preliminary reports will be generated at the conclusion of the test and final reports will be generated as soon as all of the thermochemical corrections are available when this automatic reporting feature is turned ON. When this is turned OFF, reports will only be generated through the reporting controls.
Automatic Report Destination: Directs the reports to the printer or the display.

Communication Controls Menu

Communication Controls: Accesses sub-menus which set the communications protocols for the printer and balances.
Printer Type: Toggle between Parr 1758 and Generic.
Balance Port: Accesses sub-menu, Balance Port
Communications. Sets the communication param­eters for the USB port used for the balance port. Standard options for data bits, parity, stop bits, handshaking, baud rate and balance type are pro­vided to match any devices that might be connected to these ports.
Individual Printed Reports: When set to ON, will generate header information for each report printed. In the OFF position, only one header will be printed for a series of tests.
Edit Final Reports: When set to ON, enables the user to revise sample weight and thermochemical corrections.
Recalculate Final Reports: When set to ON, causes a recalculation of stored final reports using calibration data and menu settings currently in the calorimeter.
Use New EE Value in Recalculation: When set to ON, any recalculation made will use the most recent EE value in the calculations. In the OFF position, all calculations will be made using the EE value which was effective when the test was originally run.
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Balance Port Communications

Balance Type: Toggles through the available balance templates.
Balance Port Device: This key displays a screen which allows the user to specify the balance
port device. The default (dev/ttyUSB0) is the
designation for the first USB to serial converter cable assigned by the calorimeter upon power up.
Customize Balance Setting: Sets the com­munication parameters for the balance port. Standard options for data bits, parity, stop bits, handshaking, baud rate and balance type are provided to match any devices that might be connected to these ports.
» Data Characters from Balance. This set-
ting is only used when the generic balance format is selected. This value determines the number of numeric data characters (0-9 . + -) to accept. Any additional charac­ters after this value and before the string terminating <CR> are discarded.
Log Balance to Display: This button will direct the incoming data stream from the balance to a display buffer. This function can be used to determine the data format from an unknown balance type. The display buffer is 40 charac­ters in length. The balance must be forced to issue at least 40 characters before the contents of the buffer are displayed.
Balance Port Loopback Test: This key initiates a loopback test on the port. A special loopback plug is required in order to perform this test.
Network Interface: Accesses a submenu for enter­ing details needed to communicate over a network.
Options include using a DHCP server or static IP
address.
Printer Destination: Accesses a submenu for choos­ing whether to print to an attached printer or to a network printer. If a network printer is to be used the IP address of the printer will also be entered here.
Bar Code Port: Accesses a submenu to set up a Bar Code Scanner for use with the calorimeter.
» Number of Data Bits. Standard options for
data bits. Toggles between 7 and 8.
» Parity. Standard options for parity.
» Choose from None, Odd or Even.
» Number of Stop Bits. Standard options
for stop bits. Toggles between 1 and 2.
» Handshaking. Standard options for hand-
shaking. Choose from Xon/Xoff, RTS/CTS
and None.
» Baud Rate. Standard options for baud
rate. Choose from 19.2K , 9600, 4800, 2400, 1800, 1200, 600, 300, 150, 134.5, 110, and 75.
Network Data Devices: Accesses a submenu to input the IP addresses of networked devices such as
balances and proximate analyzers.
Further information on establishing communica­tions for the Printer, Balance, Network Interface, Bar Code and other Network Data Devices can be found in Appendix D, Communication Interfaces, of this manual.
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File Management

Run Data File Manager: This key activates the File Manager. The File Manager is used to delete or rename test report files. It is also used to convert file types.
Format the SD Card: This key allows the user to format an installed SD card in a manner that is compatible with the calorimeter.
Note: Formatting will erase all files on the card!

Diagnostics Menu

Provides the user with the means to test many of the components and subsystems of the calorimeter.
Test Ignition Circuit: The key activates the ignition circuit. A volt meter can be placed across the ignition leads to ensure that the actual firing charge is reach­ing these contacts.
Data Logger: This key displays and leads to sub­menus which control the data logging function of the calorimeter.
Copy Run Data to SD Card: This key copies all test data to an SD card inserted into the rear of the calo­rimeter controller. This feature is used as a means of either archiving data or transferring it to a PC.
Note: Subsequent use of the same SD card will overwrite the data currently on the card.
Copy User Settings to SD Card: This key copies all previously saved user setups to SD.
Copy User Settings From SD Card: This key copies all user setups previously saved to SD back to the calorimeter controller memory. This feature can be used to configure multiple calorimeters in an identi­cal manner.
View System Log: This key is used to display the con-
tents of /ash/log/messages. This le is used primarily
to log application program debug messages.
User Defined Functions: This key leads to a sub-
menu that offers ve special purpose user/factory
definable function keys.
Instrument Monitor: This screen provides a summary of important instrument parameters. The monitor is used to detail the course of a test or to observe the
heating/cooling performance of the calorimeter.
View System Info: This key accesses current program information and settings such as: Processes and their associated PIDs (proportional (P), the integral (I), and the derivative (D) controls), memory, mass storage, network.
View Instrument Log: This screen displays the
contents of tmp/instlog. This le, among other things,
is the logfile destination for the data logger.
I/O Diagnostics: This key accesses a sub-menu which allows the user to manipulate digital outputs for troubleshooting.
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Calculations

aPPendix B

Calculations

Calculating the Heat of Combustion

The 6100 Calorimeter will automatically make all of the calculations necessary to produce a gross heat of combustion for the sample. However, it is impor­tant that the user understand these calculations to ensure the instrument is set up so the calculations match the procedures and the units are consistent throughout the process.

General Calculations

The calculation for the gross heat of combustion is done by:
WT-e1 - e2 - e3
Hc =
m
Where:
Hc= Gross heat of combustion.
T = Observed temperature rise.
W = Energy equivalent of the
calorimeter being used.
e1 = Heat produced by burning the
nitrogen portion of the air trapped in the bomb to form nitric acid.
e2 = The heat produced by the
formation of sulfuric acid from the
reaction of sulfur dioxide, water and oxygen.
e3 = Heat produced by the heating
wire and cotton thread.
m = Mass of the sample.
These calculations are made in cal/g and degrees
Celsius and then converted to other units if required.
Temperature Rise
The 6100 Calorimeter produces a corrected tempera­ture rise reading automatically. Corrections for heat leaks during the test are applied. (For a complete discussion of this process see Introduction to Bomb Calorimetry, Manual No. 483M.)
Energy Equivalent
The energy equivalent (represented by W in the above formula, or abbreviated as EE) is determined by standardizing the calorimeter as described in
Appendix C - Standardization. It is an expression of
the amount of energy required to raise the tempera­ture of the calorimeter one degree. It is commonly
expressed in calories per degree Celsius. Since it
is directly related to the mass of the calorimeter, it will change whenever any of the components of the calorimeter (i.e. the bomb, bucket or amount of water) is changed.

Thermochemical Corrections

Nitric Acid Correction
In the high pressure oxygen environment within the oxygen bomb, nitrogen that was present as part of the air trapped in the bomb is burned to nitric oxide
which combines with water vapor to form nitric acid. All of this heat is artificial since it is not a result of the sample burning. The nitric acid correction
removes this excess heat from the calculation.
Sulfur Correction
In the oxygen rich atmosphere within the bomb, sulfur in the sample is oxidized to sulfur trioxide
which combines with water vapor to form sulfuric acid. This liberates additional heat over the normal combustion process which converts sulfur to sulfur
dioxide. The sulfur correction removes this excess
heat from the calculation.
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ASTM and ISO Methods Differ

Current ASTM, ISO, and British Standard Methods differ on their treatment of the nitric and sulfuric acid thermochemical corrections. ASTM Methods call for titrating the bomb washings to determine the total acid present. This is assumed to be all nitric acid with a heat of combustion of -14.1 Kcal per mole. The amount of sulfur is then determined and converted to equivalents of sulfuric acid. The differ­ence between the heat of formation of sulfuric acid (-72.2 Kcal per mole or -36.1 calories per milliequiva­lent) and nitric acid is then subtracted as the sulfur correction.
Most other test methods treat nitric and sulfuric acid corrections as entirely separate values instead of combined values. This eliminates the requirement for a total acid determination and permits the nitric acid correction to be handled in a variety of ways, includ-
ing the assumption of a xed nitric acid correction.
The 6100 Calorimeter can be set up to apply the acid correction by either the ASTM or ISO convention, as the user prefers. Care must be used to ensure the proper corrections are applied, and the calculations made are consistent with the procedure used.
Please note that the values entered into the test report appear as entered in the report. Values for e1, e2 and e3 are calculated and used as energy correc­tions in accordance with the formulas and settings given above. The formulas used above to arrive at e1 or e2 are not the same as the formulas used for e1 and e2 which appear in most ASTM bomb calori-
metric procedures. However, the sum of e1 and e2,
above, is equal to the sum of the ASTM treatment of e1 and e2.
Note: Please review the following section on Acid and Sulfur Corrections. Different stan­dard test methods use different values for the heat of formation of sulfuric acid. These differences are generally insignificant. The 6100 Calorimeter uses the most recent, pub­lished values for all thermochemical data.
Thermochemical Calculation Details
Traditionally, standard solutions and procedures have been established to simplify the calculations related to the thermochemical corrections. The 6100 Calorimeter has been programmed to permit the user to use standard solutions and units which are most convenient, since the microprocessor can easily apply any conversion factors required.
Users may nd it convenient to enter a xed value
for the acid correction and avoid the need to de-
termine this correction for each test. Use of a xed
value for the acid correction is highly recommend-
ed. Fixed acid corrections can be entered when Acid
Correction - Thermochemical Corrections is set to
Fixed HNO3. A correction of 10 calories is a good number for the xed nitric acid value. Total errors of
more than 3 calories will seldom occur when using
xed nitric acid corrections.
Fixed sulfur corrections can be entered if a series of samples contain a constant amount of sulfur. Fixed sulfur corrections can be entered when Fixed Sulfur
- Thermochemical Corrections, is set to ON and then
enter percent sulfur as indicated on this line. Any errors will be proportional to the difference between the actual and assumed value for sulfur.
For ordinary work where benzoic acid is used, for standardizing the calorimeter, the Fixed Sulfur Cor­rection, for Standardizations should be ON applying
a xed value of 0.0 to all standardization tests.
Benzoic acid contains no sulfur.

Fuse Correction

The fuse correction applied by the calorimeter is calculated as:
e3 = (fuse value)(fuse multiplier from
calculation factors page)
“Fuse Value” is the number entered by the user and
the value which appears in the test report.
Note: Calculation Factors - Fuse Multiplier is normally set to 1.0 so the entered value is in calories
Users may nd it convenient to enter a xed value
for the fuse correction and avoid the need to deter­mine this correction for each test.
Fixed fuse corrections can be entered when Ther­mochemical Corrections, is set to ON. By default a
xed fuse correction of 50 calories is applied to all
tests. Total errors of more than 5 calories will seldom
occur when using a xed fuse correction and the
cotton thread supplied by Parr.
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B
Calculations

Acid and Sulfur Corrections

Total acid is the amount of base required to titrate the bomb washings (milliliters).
Nitric acid is that portion of the total acid in the bomb washings that result when the nitrogen in the air that is trapped in the bomb is burned at high pressure. Since this nitric acid does not result from the sample, and the combustion con­ditions are reasonably constant from test to test, the amount of nitric acid formed is also constant.
Acid multiplier is multiplied by the user entered acid value to arrive at the number of milliequiva­lents of acid. This value is normally the concen­tration (normality) of the base in equivalents per liter (N).
Percent sulfur is the concentration of sulfur in the sample (weight %).
Molecular weight of sulfur is 32.06.
Equivalent weight of sulfur in H2SO4 is 16.03
(one half of the molecular weight).
Heat of formation of nitric acid is 14.1 calories/
milliequivalent.
Fixed HNO3: The Acid Correction is a xed value set
by the operator.
The calculation is:
e1 = (nitric acid value)(acid multiplier)(heat of formation of nitric acid)
For an 1108P vessel the default nitric acid value is 10 and acid multiplier is .0709. The heat of formation
of nitric acid is 14.1 calories/milliequivalent so the
calculation is:
e1 = (10)(.0709)(14.1) or e1 = 9.9969 calories (rounds to 10)
When the Acid Correction is set to Fixed HNO3 the
value is considered a final value and the operator is not prompted for an acid value when reporting the results.
Entered HNO3: The Acid Correction is entered by the operator when reporting the results.
The calculation is the same as Fixed HNO3 above.
The value listed on the Acid Correction button is used for preliminary calculations. When finalizing the report the operator will be prompted for the acid value.
Heat of formation of sulfuric acid (from SO2) is
36.1 calories/milliequivalent.
Sample mass is the mass of sample burned in
the bomb (grams).
Sulfur multiplier is multiplied by the product of the user entered sulfur value and the sample mass to arrive at the number of milliequivalents of sulfuric acid in the bomb washings.
Sulfur Correction
e2 = (percent sulfur)(sample mass)(sulfur multiplier)
(heat of formation of H2SO4).
Acid Correction
In the 6100 there are a number of settings for the acid correction.
e1 is the nitric acid portion of the correction.
Fixed Total: The Acid Correction represents the total base required to titrate the bomb washings (in mil­liliters). This includes both nitric and sulfuric acid.
The correction is a xed value set by the operator.
The calculation is:
e1 = [((total acid)(acid multiplier)) – (% sulfur)
(sample mass)(sulfur multiplier)](heat of forma­tion of nitric acid)
Using the default acid and sulfur multipliers as well as a heat of formation of nitric acid of 14.1 cal/milliequiv­alent a 1 gram sample with 25 ml of washings and 2
% sulfur would result in the following calculation:
e1 = [((25)(.0709)) – (2)(1)(.6238)] 14.1 e1 = [(1.7725) – (1.2476)] 14.1 e1 = [.5249] 14.1 e1 = 7.40 calories
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When the Acid Correction is set to Fixed Total the
value is considered a final value and the operator is not prompted for an acid value when reporting the results.
Entered Total: The Acid Correction represents the total base required to titrate the bomb washings (in milliliters). This includes both nitric and sulfuric acid. The correction is entered by the operator when reporting the results.
The calculation is the same as the Fixed Total above.
The value listed on the Acid Correction button is used for preliminary calculations. When finalizing the report the operator will be prompted for the acid value.
Calculated HNO3: In ASTM D5865 there are provi­sions for calculating the nitric acid contribution.
For test samples that contain no nitrogen, the quantity of nitric acid formed during the combustion process is a function of the volume of the bomb, the
oxygen lling pressure, and the quantity of energy
released.
For the calculated nitric acid method:
e1 = (nitric acid factor/1000)(Energy Equivalent)
(corrected temperature rise)
Example: For a test run with energy equivalent of
2425.07 and a corrected temperature rise of 2.6348
would result:
e1 = (1.58/1000)(2425.07)(2.6348)
e1 = 10.10 calories
The calculated nitric acid method can be applied
to samples containing up to 2% nitrogen without
introducing a significant error in the resulting heat of combustion value.
Table B-1

Settings for ISO & BSI Methods

Page Line Setting Value
Thermochemical
Corrections
Calculations
Factors
Acid Correction
(STD)
Fixed Sulfur STD Off 7
Acid Correction
(DET)
Fixed Sulfur DET Off 7
Acid Multiplier 0.154
Sulfur Value is
Percent
Sulfur Multiplier 0.1
Use Offset Correction
Offset Value -43.5
Offset Value -43.5
Entered
HNO
3
Entered
HNO
3
Off
On
13
13

ASTM Treatment for Acid and Sulfur

In the ASTM treatment, the correction for acid formation assumes that all the acid titrated is nitric acid. Obviously, if sulfur is present in the sample, which in turn produces sulfuric acid, part of the correction for the sulfuric acid formed is already included in the ASTM nitric acid correction (e1). This is adjusted by a separate computation based upon the sulfur content of the sample. An additional cor­rection of 1.37 kcal must be applied for each gram
of sulfur converted to sulfuric from sulfur dioxide.
This is based upon the heat of formation of sulfuric
acid, from sulfur dioxide, under bomb conditions,
which is -72.2 kcal per mole or -36.1 calories per milliequivalent. But remember, a correction of 14.1 calories per milliequivalent of sulfuric acid is already included in the ASTM nitric acid correction (e1). Therefore the additional correction which must be applied for sulfur will be the difference between 36.1 and 14.1 or 22.0 calories per milliequivalent (44.0
Kcal per mole). For convenience, this is expressed, in the ASTM e2 formula, as 13.7 calories (44.0/32.06)
for each percentage point of sulfur per gram of sample.
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B
Calculations

ISO Calculations

Both the ISO 1928 and BSI 1016: Part 5 methods for testing the calorific value of coal and coke, deal with acid and sulfur corrections in a manner which is somewhat different than ASTM procedures. Provision has been made in the 6100 Controller for dealing with these different procedures.
The analysis of bomb washings in these methods
call for a titration, rst using 0.1N barium hydroxide
(V2) followed by filtering, and a second titration
using 0.1N HCL(V1) after 20 mL of a 0.1N sodium
carbonate has been added to the filtrate. Table B-1 gives the settings which allows the results of the two titrations, V1 and V2, to be entered into the controller directly for the calculation of the total acid correction. V1 should be entered at the prompt for acid and V2 is entered at the prompt for sulfur.
The settings in Table B-1 assume that the same procedure is carried out for both standardization and determination.
The offset value is the product of -1, the Heat of For­mation of Nitric Acid, the acid multiplier, and the 20 mL of 0.1 N sodium carbonate used in the analysis.
The formula used to get the total correction in calories is as follows:
V1(Acid Multiplier)(Heat of Formation of Nitric Acid)
V2(Sulfur Multiplier)(Heat of Formation of Sulfuric Acid)+offset value.
The values for xed acid and sulfur, which are used
in preliminary reports, will reflect a sulfur correction of 0, and a nitric acid correction of 10 calories.

Spiking Samples

There are times when a sample will not completely burn. This can be due to a number of things includ­ing low heat of combustion and high water content. In cases such as these a material is added to the sample in order to help it completely combust. This is known as a combustion aid or spike.
The 6100 Calorimeter can automatically compensate for the addition of spiking materials to these sam­ples. The calculations are modified in these cases as follows:
Hc =
Where: Hcs = The spiking material (cal/g) M
s
This factor is added to the calculations when Spike Controls, Use Spiking is set to ON.
There are generally two substances that Parr recom­mends using as a spike, benzoic acid and mineral (white) oil.
Benzoic acid is good as a spike for the same reasons that it is good as a standard. It is homogeneous and has an established heat of combustion.
Mineral oil is good for several reasons. It is inex­pensive, it has a high heat of combustion, and it is a liquid. As a liquid it can permeate the sample and help it to burn.
To use spiking go to the Main Menu and then to Operating Controls. Press Spiking Correction to get to the Spike Controls sub-menu. Once on the Spike Controls sub-menu change Use Spiking to ON. The heat of combustion of the spike must be entered
in cal/g. The default value of 6318.4 is the value for
benzoic acid.
If mineral oil is to be used for your spike then the heat of combustion of the mineral oil must be determined. Run 10 tests of the mineral oil in deter-
mination mode with the reporting units set to cal/g. The sample size should be approximately .6 grams.
Average the 10 results to get the heat of combustion of the mineral oil.
Note: When using a spike it is very impor­tant to be aware of the total energy being re­leased by the sample and the spike. Do NOT exceed 8000 calories total energy released.
WT-e1 - e2 - e3 - (Hcs)(Ms)
m
= Mass of spiking material
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When using a spike the total weight of the spike and
sample combined should not exceed 1.2 gram.
Example 1:
A customer is testing glucose (approximate heat of combustion 3800 cal/g) and is having a hard time
getting complete combustion. They decide to use benzoic acid for a spike. Benzoic acid has a heat of
combustion of 6318 cal/g. The customer would use
.7 g of the benzoic acid (4423 calories released) and .3 g of the glucose (1140 calories released) for a total of 5563 calories released in burning the sample.
Example 2: The same customer decides to use mineral oil as their spike. They run 10 tests of the mineral oil in determination mode and determine that the mineral
oil has an average HoC of 11000 cal/g. They input this value for the Heat of Combustion of Spike on
the Spiking Controls sub-menu. The customer would use .5 g of the mineral oil (5500 calories released) and .4 g of the glucose (1520 calories released) for a total of 7020 calories released in burning the sample.
In both cases the calorimeter would automatically remove the heat of combustion of the spike from the test results.
To prepare samples containing a spike follow the following steps:
1. Tare (zero out) the weight of a sample cup on the balance.
2. Add either the sample or the spike material (not both) to the sample cup.

Conversion to Other Moisture Bases

The calculations described above give the calorific
value of the sample with moisture as it existed when the sample was weighed. For example, if an air-
dried coal sample was tested, the results will be in terms of heat units per weight of air-dry sample. This can be converted to a moisture free or other basis by determining the moisture content of the air-dry sample and using conversion formulae published in ASTM Method D3180 and in other references on fuel technology.

Conversion to Net Heat of Combustion

The calorific value obtained in a bomb calorimeter test represents the gross heat of combustion for the sample. This is the heat produced when the sample burns, plus the heat given up when the newly formed water vapor condenses and cools to the temperature of the bomb. In nearly all industrial operations, this water vapor escapes as steam in the flue gases and the latent heat of vaporization, which it contains, is not available for useful work. The net heat of combustion obtained by subtract­ing the latent heat from the gross calorific value is therefore an important figure in power plant calcula-
tions. If the percentage of hydrogen H, in the sample is known, the net heat of combustion, H
pound can be calculated as follows:
H
To calculate H
D5865.
= 1.8Hc - 91.23H
net
(Liquid fuels, ASTM D240)
for solid fuels please refer to ASTM
net
Btu per
net
3. Record the weight when it is stable.
4. Tare the sample cup with the material in it.
5. Add the sample or spike material (whichever was NOT added in step 2) to the sample cup.
6. Record the weight.
7. Prepare the bomb with the sample normally.
8. Start the test. The calorimeter will ask for Bomb ID, Sample ID, Sample Weight, and Spike Weight. Input the appropriate values.
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C
Standardization

aPPendix c

Standardization

Standardizing the Calorimeter

The Energy Equivalent Factor
The term “standardization”, as used here, denotes
the operation of the calorimeter on a standard sample from which the energy equivalent or effec­tive heat capacity of the system can be determined. The energy equivalent, W or EE of the calorimeter is the energy required to raise the temperature one
degree, usually expressed as calories per degree
Celsius. Standardization tests should be repeated after changing any parts of the calorimeter, and occasionally as a check on both the calorimeter and operating technique.
Standardization Procedure
The procedure for a standardization test is exactly
the same as for testing a fuel sample. Use a pellet of calorific grade benzoic acid weighing not less than 0.9 nor more than 1.1 grams. The corrected temperature rise, T, is determined from the observed test data and the bomb washings are titrated to determine the nitric acid correction. The energy equivalent is computed by substituting the follow­ing equation:
Hm + e1 + e2 + e3
W =
T
Where: W = Energy equivalent of the calo-
rimeter in calories per °C.
H = Heat of combustion of the
standard benzoic acid sample in
calories per gram. m = Mass of the sample.
T = Temperature rise in °C. e1 = Correction for heat of formation
of nitric acid in calories. e2 = Correction for sulfur which is
usually 0. e3 = Correction for heating wire and
combustion of cotton thread or
fuse wire as appropriate.
Note: The 6100 performs all the necessary calculations once all of the corrections are entered.

Standard Materials

A bottle of 100 one-gram benzoic acid pellets (Part No. 3415) is furnished with each calorimeter for standardizing purposes. The Parr benzoic acid has been calibrated against NIST benzoic acid. Addition­al benzoic acid pellets can be obtained from Parr. For very high precision measurements, a primary standard benzoic acid powder can be purchased from the National Institute of Standards & Technol­ogy, Washington, D.C.
It is not common to have sulfur in standard mate­rials, or to use spikes in standardizations, but the capabilities have been included in this calorimeter.
Users should take great care to ensure that the con­ditions during standardization runs and determina­tions are as identical as possible.
Caution! Benzoic acid must always be compressed into a pellet before it is burned in an oxygen bomb to avoid possible damage from rapid combustion of the loose powder. This is best accomplished by using a 2811 Pellet Press.

Automatic Statistical Calculations

The 6100 Calorimeter includes a provision for calculating and using a mean energy equivalent for each of up to 4 separate bomb and bucket combina­tions. ASTM procedures recommend that the energy equivalent be determined by averaging ten tests. The 6100 Calorimeter automatically determines and uses up to ten tests in its memory and will update the EE Value as additional standardizations are run. Only Final Tests will be used in determining and updating EE values. These values, the number of tests, and the relative standard deviation for the tests used in determining the EE value are stored in the Calibration Data Page under the EE Value for each bomb.
The user can chose to turn off the automatic aver­aging and updating procedure and protect the EE Values by turning ON the protection feature for the appropriate bomb on the Calibration Data and Control Page using Protected EE Value.
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C
Any outliers or other tests which should not be included in the average EE Value must be deleted from the memory using the memory management procedures (see Chapter 8). A list of all tests associ­ated with any Cal ID can be printed from the Calibra­tion Data Page using Print Standardization Runs.
The user can elect to have any number of stored standardization runs used in determining the EE
Table C-1

Calorimeter Control Limit Values in J/g When Benzoic Acid is Used as a Test Sample

Accepted heat of combustion taken as 26454 J/g. Instrument precision 0.20%. Control limits based on 99% condence (3 sigma) values. Values are in J/g.
NUMBER OF
OBSERVATIONS
IN A GROUP
1 158.7 2 195.1 0.521% 112.2 3 230.5 0.455% 91.6 4 248.6 0.418% 79.4 5 260.2 0.393% 71.0 6 268.7 0.375% 64.8 7 275.3 0.361% 60.0 8 280.8 0.350% 56.1
9 285.4 0.341% 52.9 10 289.4 0.334% 50.2 11 292.8 0.327% 47.9 12 295.9 0.322% 45.8 13 298.7 0.317% 44.0 14 301.4 0.313% 42.4 15 303.7 0.309% 41.0 16 305.9 0.305% 39.7 17 307.9 0.302% 38.5 18 309.9 0.299% 37.4 19 311.5 0.297% 36.4 20 313.3 0.294% 35.5 21 314.8 0.292% 34.6 22 316.3 0.290% 33.8 23 317.8 0.288% 33.1 24 319.1 0.286% 32.4 25 320.4 0.284% 31.7
UCL FOR THE RANGE
(HIGH – LOW) WITHIN
THE GROUP
UCL FOR THE
RSD WITHIN THE
GROUP
value by entering this number on Calibration Data & Controls Page - Calibration Run Limit.
EE Max Std Deviation on this same page establishes the maximum allowable standard deviation for the
EE Value before an error condition is reported. The default value is zero which turns off this limit. But the user should enter a value appropriate for the test being made.
MAXIMUM PERMISSIBLE DEVIATION
OF THE GROUP MEAN FROM THE
ACCEPTED VALUE OR GRAND MEAN
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Standardization
Table C-2

Calorimeter Control Limit Values in cal/g When Benzoic Acid is Used as a Test Sample

Accepted heat of combustion taken as 6318 cal/g. Instrument precision 0.20%. Control limits based on 99% condence (3 sigma) values. Values are in cal/g.
NUMBER OF
OBSERVATIONS
IN A GROUP
1 37.9
2 46.6 0.521% 26.8
3 55.1 0.455% 21.9
4 59.4 0.418% 19.0
5 62.1 0.393% 1 7. 0
6 64.2 0.375% 15.5
7 65.7 0.361% 14.3
8 67.1 0.350% 13.4
9 68.2 0.341% 12.6 10 69.1 0.334% 12.0 11 69.9 0.327% 11. 4 12 70.7 0.322% 10.9 13 71.3 0.317% 10.5 14 72.0 0.313% 10.1 15 72.5 0.309% 9.8 16 73.1 0.305% 9.5 17 73.5 0.302% 9.2 18 74.0 0.299% 8.9 19 74.4 0.297% 8.7 20 74.8 0.294% 8.5 21 75.2 0.292% 8.3 22 75.6 0.290% 8.1 23 75.9 0.288% 7. 9 24 76.2 0.286% 7. 7 25 76.5 0.284% 7. 6
UCL FOR THE RANGE
(HIGH – LOW) WITHIN
THE GROUP
UCL FOR THE
RSD WITHIN THE
GROUP
MAXIMUM PERMISSIBLE DEVIATION
OF THE GROUP MEAN FROM THE
ACCEPTED VALUE OR GRAND MEAN
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Table C-3

Calorimeter Control Limit Values in BTU/lb When Benzoic Acid is Used as a Test Sample

Accepted heat of combustion taken as 11373 BTU/lb. Instrument precision 0.20%. Control limits based on 99% condence (3 sigma) values. Values are in BTU/lb.
Standardization
C
NUMBER OF
OBSERVATIONS
IN A GROUP
1 68.2
2 83.9 0.521% 48.3
3 99.1 0.455% 39.4
4 106.9 0.418% 34.1
5 111. 9 0.393% 30.5
6 115.5 0.375% 27.9
7 118.3 0.361% 25.8
8 120.7 0.350% 24.1
9 122.7 0.341% 22.7 10 124.4 0.334% 21.6 11 125.9 0.327% 20.6 12 127.2 0.322% 19.7 13 128.4 0.317% 18.9 14 129.6 0.313% 18.2 15 130.6 0.309% 1 7. 6 16 131.5 0.305% 1 7. 1 17 132.4 0.302% 16.6 18 133.2 0.299% 16.1 19 133.9 0.297% 15.7 20 134.7 0.294% 15.3 21 135.3 0.292% 14.9 22 136.0 0.290% 14.5 23 136.6 0.288% 14.2 24 137.2 0.286% 13.9 25 137.7 0.284% 13.6
UCL FOR THE RANGE
(HIGH – LOW) WITHIN
THE GROUP
UCL FOR THE
RSD WITHIN THE
GROUP
MAXIMUM PERMISSIBLE DEVIATION
OF THE GROUP MEAN FROM THE
ACCEPTED VALUE OR GRAND MEAN
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D
Communications Interfaces

aPPendix d

Communications Interfaces

USB Port for Connection

The 6100 Calorimeter is also equipped with a USB port for connection to either a 40 or 80 column
printer and/or a computer.
The default parameters for the 6100 Calorimeter are set up for use with the Parr 1758 Printer.

Mettler 011/012 Balance Interface

The ID field must contain
“S_” to indicate a stable
mass. The data field contains the current mass, right justified, with a decimal point. The balance should be configured to send continuously.

Sartorius Balance Interface

Field Length
ID 2 space 1 data 9 space 1 g 1 CR 1 LF 1
Balance and Port Input Driver Specifications
The 6100 Calorimeter supports input from multiple balance types. Additionally, a generic input driver is provided for communications with balances that do not conform to the supported protocols. A new feature supported by all balance input drivers is the
ability to change the expected number of characters
in the data field. The number of data characters indicated for each of the drivers, below, are default values. This feature virtually eliminates the need for balance input drivers to be re-written in the event the balance manufacturer elects to alter the output string of a balance when new models are intro­duced.
The format of an unknown balance can be deter­mined by logging the balance output to the printer attached to the calorimeter. Those protocols which send a command string to the balance will do so while logging is active. In order for the logging to produce meaningful results, the cable connecting the balance to the balance input port of the calo­rimeter must be correctly wired or configured. In addition, the specifics of the data frame, such as the baud rate, # of data bits, parity, # of stop bits and handshaking (if used) must be the same for both the balance and the calorimeter.
The polarity field must con-
tain either a “+” or a space.
Leading zeros in the data
eld are blanked, except
for the one to the left of the decimal point. The stability
eld must contain “g_” for
the calorimeter to accept a mass. The balance should be configured to transmit data upon receipt of the following command string:
[ESC] P [CR] [LF]
Note: The automatic data output option should not be used.
The calorimeter will send this command string once every few seconds after the ENTER key has been pressed during a mass entry sequence. The ENTER key should only be pressed when the mass
reading is stable. However, unstable readings
will be rejected and a warning will be issued. Acknowledging the warning by pressing the CLEAR
ENTRY key will re-issue the command string to the
balance on a periodic basis.
Field Length
polarity 1 space 1 data 8 space 1 stability 2 CR 1 LF 1
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Communications Interfaces
D

Generic Interface

The data field should consist of 9 numeric characters (0 through 9, +, - and space) terminated with a carriage return (CR). Leading zeros may be blanked as spaces and are counted. Non-numeric characters are ignored and will reset the input buffer if the data field has not been filled. Any characters received after filling the data field and before the carriage return are ignored.
Field Length
data 9 CR 1
Table D-1

6100 Data File Naming Convention

Test data files are named with the following convention.
Test Type Filename
Preliminary Standardization <ID>.std.plim.csv Final Standardization <ID>.std.finl.csv Preliminary Determination <ID>.det.plim.csv Final Determination <ID>.det.finl.csv Pre-weigh <ID>.---.pwgh.csv
Table D-2

6100 Calorimeter Run Data Template

Field Description
SampleID char[16] Timestamp MM/DD/YY HH:mm:ss Mode 0 = determination, 1 = standardization Method 0 = equilibrium, 1 = dynamic State 0 = preweigh, 1 = preliminary, 2 = final Units 0 = MJ/kg, 1 = Btu/lb, 2 = cal/g,
3 = J/kg, 4 = other
UnitMultIfOther unit multiplier in effect at time of
report BombID [1,4] BombEE bomb energy equivalent SampleWt sample weight SpikeWt spike weight Fuse fuse value FuseFinal fuse value is final Acid acid value AcidFinal acid value is final Sulfur sulfur value SulfurFinal sulfur value is final
Hydrogen hydrogen value (net calc option) HydrogenFinal
MAD moisture as determined value (dry
MAD Final moisture as determined is final JacketTemp jacket temperature InitTemp initial temperature DeltaT temperature rise
HOC gross heat of combustion NetHOC dry net HOC (net calc options enabled) DryHOC dry gross HOC
DryNetHOC dry net HOC (if both dry and net calc
Oxygen oxygen value (net calc option) Oxygen Final oxygen value is nal
Nitrogen nitrogen value (net calc option) Nitrogen Final nitrogen value is final MAR moisture as received (dry calc option) MAR Final moisture as received value is final
Dry Net HOC_AR
Bomb Name bomb name assigned to bomb ID
hydrogen value is final (net calc option)
calc option)
(if dry calc option enabled)
options enabled)
Dry net HOC as received value (if both
dry and net calc option enabled)
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Communications Interfaces

Network Interface

Calorimeter test data can be transferred to an Eth­ernet network connected computer using the FTP File Transfer Protocol. First, you must know the IP address of the network-connected calorimeter. The network DHCP (Dynamic Host Conguration Proto­col) server provides this address shortly after the calorimeter is turned on. The address can be seen
on the “software and hardware info” page, under “program information and control”. See the example
screenshot.
Users who don’t have a network infrastructure can create a simple network by connecting a router with
DHCP server capability to the calorimeter using
an ordinary CAT 5 network cable. The calorimeter should be connected to LAN side of the router. The PC in turn is also connected to the LAN side of the router using a similar CAT 5 cable. A D-Link 614+ router is recommended for this purpose. For this router, operated without a WAN connection, the pri­mary DNS address of the router (WAN setup) must be set to the IP address of the router found on the LAN setup page. Other routers behave differently in the absence of a WAN connection. Providing an active upstream connection to the WAN port of most routers generally minimizes the use of any obscure setup configurations.
A static IP address can be assigned by turning off the DHCP (Automatic Setting) on the Network Com­munications Page.
An FTP enabled web browser can be used to access stored test data. The URL is of the following form.
ftp://root:rootroot@192.168.0.125/../ash/data/
The datalog file can be accessed at:
ftp://root:rootroot@192.168.0.125/../ash/log/datalog.
csv
In this case, 192.168.0.125 is the IP address of the calorimeter.
After any changes to the Network Configuration the calorimeter will prompt the user to restart the system.
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D

Samba Server Feature (Optional)

Samba was originally developed as an implementa­tion of the SMB (Server Message Block) protocol. The most common use of SMB is in Microsoft’s CIFS (Common Internet File System) implementation. As a result, Samba has become a de facto Microsoft network compatibility tool. In relation to CIFS, Samba allows non-Microsoft operating systems to enjoy effectively seamless server and client opera­tion in networks catering to the needs of Windows
computers. It is an “open” standard and dened in
IETF RFC1001 and RFC1002.
The Samba server feature option in the Parr 6100 Calorimeter offers seamless file services to Win­dows based clients. It allows the calorimeter to interact with a Microsoft Windows client as if it is a Windows file server. The Samba server feature can be used to facilitate data file transfer from a
To access the test data open the run data folder. To access the log file open the log data folder.
calorimeter or proximate interface to a PC running
the Windows operating system. This method of file transfer, for some users, may be less cumbersome and more intuitive than using a web browser as an FTP client program to retrieve or log files.
When purchasing this feature, the user must supply Parr with the MAC address of the calorimeter (found
in the Software & Hardware Info menu screen). This
allows Parr to activate the feature key. In order to enable the calorimeter to use the bar code feature, the feature key needs to be entered into the instru­ment. Select the Program Information and Control
key from the Main Menu. Next, select Feature Key
and enter the feature key purchased from Parr In­strument Company into the instrument by using the
touchpad. Pressing the key labeled “ABC” allows
the user to switch from upper case letters, to lower case letters, to numerals, and finally to symbols.
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The following screenshot illustrates the contents of the calorimeter data directory as presented by a web browser.
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The calorimeter offers a web server service. Test reports can be viewed with a web browser using a URL of the following form.
http://10.1.5.28
Where 10.1.5.28 is the IP address of the calorimeter. The following screenshot illustrates the calorimeter home page.
Communications Interfaces
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Clicking on the Config button will display the screen below. Changes made on this screen will change the settings in the calorimeter.
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Clicking on the Run Data button displays a list of reports currently in the instrument memory.
Clicking on a test under the select sample ID box will display the data for the selected sample ID.
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Clicking on the System Info button will display the screen below.
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Clicking on the LCD Snap Shot button will display the current menu screen displayed by the calorimeter. If the backlight is not on, this screen will display a blank blue square.
Note: This is a picture only. The calorimeter cannot be remotely operated from this screen. Remote operation requires the appropriate Feature Key.
Please contact Parr Instrument Company for more details about available Feature Keys.
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Clicking on the Documentation button will display the screen below. Clicking on any of the links will open the corresponding web page.
Note: Connection to the internet is required for these links.
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D

Bar Code Port

The use of barcodes in the laboratory has become
a highly accurate, rapid and inexpensive way to
identify samples. When purchasing this feature, the user must supply Parr with the MAC address of
the calorimeter (found in the Software & Hardware
Info menu screen). This allows Parr to activate the feature key.
In order to enable the calorimeter to use the bar code feature, the feature key needs to be entered into the instrument.
Select the “Program Information and Control” key from the Main Menu. Next, select “Feature Key”
and enter the feature key purchased from Parr Instrument Company into the instrument by using
the touch pad. Pressing the key labeled “ABC”
allows the user to switch from upper case letters, to lower case letters and finally to numerals.. A CD containing all the necessary documentation and setup information for using both the scanner and the printer is provided at the time of purchase. A PC based program used for printing bar coded labels is also provided on this CD.

Network Data Devices

These keys allow the user to specify the IP address­es of one or more Balance Interface devices on the network. Balance Interface devices are polled from
device 1 to 15 for sample and/or spike weights when
the weight entry mode is set to Network.
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E
Technical Service

aPPendix e

Technical Service

Contact Technical Service

Should you need assistance in the operation or service of your instrument, please contact the Technical Service Department.
Telephone: (309) 762-7716 Toll Free: 1-800-872-7720
Fax: (309) 762-9453
E-mail: parr@parrinst.com
Any correspondence must include the following basic information:
1. The model and serial # of the instrument.
2. Software version(s) shown on the “Software and
Hardware Information” page.
When calling by phone, it is helpful if the person is close to the instrument in order to implement any changes recommended by the Technical Service Department.

Return for Repair

To return the instrument for repair, please call the Technical Service Department for shipping
instructions and a RETURN AUTHORIZATION
NUMBER. This number must be clearly shown on the outside of the shipping carton in order to
expedite the repair process.
If you have not saved the original carton and traps, please request an A1341DD packaging return kit.
We prefer the calorimeter to be shipped in our cartons and traps to prevent shipping damage.
Ship repair to:
Parr Instrument Company Attn: Service Department RMA # XXXX 211- 53rd Street Moline, Illinois 61265
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E
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F
Parts Lists & Drawings

aPPendix f

Parts Lists & Drawings

Principal Assemblies in Calorimeter

Item Description
1108 Oxygen Combustion Vessel A391DD Oval Bucket A570DD Regulator Assembly, Oxygen A1279DD2 Controller Assembly A1268DD Stirrer Motor Assembly, 12V A1284DD2 Stirrer Hub Assembly A38A Head Support Stand
A297E Lead Wire A1278DD Oxygen Solenoid 1940E Power Supply 897E Capacitor, 40V, 81000 uF 1317DD Lid Seal 1417E2 Thermistor Bucket 538VB Male Connector 1/8 NPTM-T-BT
Nylon 549DD Gas Spring 139E23 Fuse, Fast-Acting 15 Amp 250 VAC
For continued protection against possible hazard, replace fuses with same type and rating of fuse.

Parts List for A1279DD2 Controller Assembly

Item Description
1926E Film Guard, LCD 1802E SA1332RD04 6-32 x 1/4 RHMS 18-8 SS SA1140RD08 4-40 x 1/2 RHMS 18-8 SS
A1821E Speaker Assembly with Cable
A1822E Power Cable Assembly A1823E Touchscreen Cable Assembly, 12” A2140E Board, I/O A2141E LCD Transition Board A2163E Cable, LCD A2164E Cable, Backlight Control A2166E Cable, I/O to CPU USB A2167E Cable, USB Peripheral Cable 1477DD Gasket, Display Kyrocer/Hantronix 2147E LCD 1472DD LCD Encasement - Kyrocera A2154E3 CPU Board 6100

Parts List for A1284DD2 Stirrer Hub Assembly

Item Description
1282DD Hub, Stirrer 1283DD2 Shaft, Stirrer 1242DD3 Pulley, Timing 682DD Snap Ring, Internal .50 683DD Wave Spring, .50 OD 684DD Ball Bearing A540DD Stirrer Assembly
1288DD Coupler, Stirrer Shaft 1242DD3F Set Screw, Pulley
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Parts Lists & Drawings
F

Parts List for Oxygen Filling System

Item Description
244VB Union Bulkhead, 1/8 Tube A476A3 Slip Connector w/ 1/8 NPT 438VB Elbow, 45 °, 1/8 NPT x 1/8 Tube
HX0012TB024 High Pressure Tube, 1/8, Nylon
180VB Male Elbow 1/8 T x 1/8 NPTM 527VB Restrictor 0.012 – 1/8 NPT A1278DD Oxygen Solenoid Assembly 697HC2 Filter Sintered Bronze 243VB2 Male Connector, 1/8 T x 1/8 NPT
394HCJE O-ring EP 3/8 ID X 1/16 CS

6100 Stirrer Motor and Drive Parts List

Item Description
1285DD Mount, Motor, 6100 1241DD2 Belt Timing, 6100 1242DD3 Pulley Timing 6100
A1268DD Motor, Stirrer, 6100

Printer and Supplies

Item Description
1758 USB Printer 334C Printer Paper 335C Printer Ribbon

Spare and Installation Parts List

Item Description
20VB Valve Seat 230A O-ring, Bomb Head, 2-3/8 ID 238A O-ring, 3/16 ID
394HCJE O-ring, 3/8 ID
415A O-ring, 7/16 ID 3415 Benzoic Acid Pellets
(1.0 grams, 100 tablets) 421A Bomb Lifter 43AS Sample Capsule, SS 475A Service Clamp Head A38A Head Support and Stand A719E Cordset 115V A719EEE Cordset 230V 1344DD Stylus 1889E Film, Display protection TX03SKMM Metric Hex Wrench .89mm A570DD Oxygen Regulator 143AC Insulator, Delrin 388A Spacer 401A Sleeve Insulator 96AC Electrode Insulator 378A Packing Cap PA1332RD04 G-32 x 1/4 RHMS 840DD2 Heat Wire 845DD2 Ignition Thread A391DD Oval Bucket
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Parts Lists & Drawings
Figure F-1

6100 Compensated Jacket Calorimeter Cutaway Front

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Figure F-2

6100 Compensated Jacket Calorimeter Cutaway Rear

Parts Lists & Drawings
F
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F
A2141E
PARR INSTRUMENT CO.
APPROVED
BY
BY
SCALE
DWG NO.
DATE
DRAWN
DESCRIPTION
REVISIONS
FOR
DATE
CONTROLLER SCHEMATIC
02-26-10
NTS
6100/6200 CALORIMETER
MAW
SIZE
C
A1279DD2
UNMARKED RADII .03"
211 53rd STREET
MOLINE, ILLINOIS 61265
DO NOT SCALE DRAWING
TOLERANCES
IN INCHES
UNLESS OTHERWISE SPECIFIED
1/X .... ±1/64
.00 .... ±.010
.000 .... ±.003
ANGULAR ... ±1/2°
COMPANY.
DRAWN IN 3rd ANGLE PROJECTION
OR BETTER
64
MACHINED SURFACES:
PROPRIETARY
NEITHER THE DRAWING
NOR INFORMATION
CONTAINED HEREIN
MAY BE COPIED,
REPRODUCED, OR
OTHERWISE USED
WITHOUT WRITTEN
PERMISSION FROM
PARR INSTRUMENT
SHEET 1 OF *
02-26-10
MAW FOR HJA
Parts Lists & Drawings
A2165E
ON ENCASEMENT)
(SEE SHEET 2 FOR INSTALLATION
BOARD
LCD TRANSISTION
1472DD
LCD ENCASEMENT
J6
J9
A2164E BACKLIGHT CONTROL CABLE ASSY
DISPLAY CABLE
BOARD TO
TRANSITION
J2
Figure F-3

A1279DD2 Control Schematic

A2165E
REF
IN THIS VIEW
CONTACTS ARE
EXPOSED
A
J1
J10
J8
2147E
LCD DISPLAY
ASSEMBLY
CABLE
SPEAKER
A1821E
DETAIL "A"
J1
SCREEN CABLE ASSY
A1823E TOUCH
A2163E LCD CABLE ASSY
J5
J17
J19
J100
J4
J8
J1
USB PORT
BACK PANEL
CABLE ASSY
A2167E USB PERIPHERAL
J6
CONNECTS IN UPPER PORT
OF J4 OF CPU
J10 J9
A2154E
CPU BOARD
A1822E POWER CABLE ASSY
PIN #1
P8
IO BOARD
A2140E
CONNECTS IN LOWER PORT OF J4 ON CPU
(RED WIRE ON CABLE CONNECTS TO PIN #1)
A2166E IO TO CPU USB CABLE ASSY
PIN #1
P6
USB PORT
Electrostatic Discharge (ESD) hazards. Observe precautions for handling
electrostatic sensitive devices.
ATTENTION:
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Figure F-4

A1278DD Oxygen Solenoid Assembly

Parts Lists & Drawings
F
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Parts Lists & Drawings
Figure F-5

A1284DD2 Stirrer Hub Assembly

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Figure F-6

Stirrer Motor Assembly

Parts Lists & Drawings
F
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Notes
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584M R02 12/09/13
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