Parr Instrument 6100 User Manual
6100
Compensated Jacket Calorimeter
Operating Instruction Manual
For models produced after October 2010
584M
Table of Contents6100
Preface 3
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
Chapter 1 6
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
Chapter 2 8
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
www.parrinst.com
1
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
2
Parr Instrument Company
Appendix F 70
Parts Lists & Drawings 70
Principal Assemblies in Calorimeter 70
Parts List for A1279DD2 Controller Assembly 70
Parts List for A1284DD2 Stirrer Hub Assembly 70
Parts List for Oxygen Filling System 71
6100 Stirrer Motor and Drive Parts List 71
Printer and Supplies 71
Spare and Installation Parts List 71
6100
Preface
Figures
Swagelok Tube Fittings 10
6100 Compensated Jacket Calorimeter Back Panel 11
2811 Pellet Press 20
3601 Gelatin Capsules 21
43A6 Combustion Capsule with Adhesive Tape Seal 21
43AS Combustion Capsules 21
Combustion Capsule with Adhesive Tape Seal 22
6100 Compensated Jacket Calorimeter Cutaway Front 72
6100 Compensated Jacket Calorimeter Cutaway Rear 73
A1279DD2 Control Schematic 74
A1278DD Oxygen Solenoid Assembly 75
A1284DD2 Stirrer Hub Assembly 76
Stirrer Motor Assembly 77
Customer Service
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
Tables
Factory Default Settings 16
Settings for ISO & BSI Methods 49
Calorimeter Control Limit Values in J/g When Benzoic
Acid is Used as a Test Sample 53
Calorimeter Control Limit Values in cal/g When Benzoic
Acid is Used as a Test Sample 54
Calorimeter Control Limit Values in BTU/lb When Benzoic
Acid is Used as a Test Sample 55
6100 Data File Naming Convention 57
6100 Calorimeter Run Data Template 57
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
Preface
Scope
This manual contains instructions for installing and
operating the Parr 6100 Calorimeter. For ease of use,
the manual is divided into nine chapters.
Concept of Operation
Installation
Instrument Description
Program Installation & Control
Operating Instructions
Corrections & Final Reports
Reporting Instructions
File Management
Maintenance & Troubleshooting
Subsections of these chapters are identified in the
Table of Contents.
To assure successful installation and operation, the
user must study all instructions carefully before
starting to use the calorimeter to obtain an understanding of the capabilities of the equipment and the
safety precautions to be observed in the operation.
Related Instructions
Additional instructions concerning the installation
and operation of various component parts and peripheral items used with the 6100 Calorimeter have
been included and made a part of these instructions.
No. Description
201M Limited Warranty
483M Introduction to Bomb Calorimetry
418M 1108P Oxygen Combustion Vessel
207M Analytical Methods for Oxygen Bombs
Additional instructions for the printer are found in
the respective package and should be made a part
of this book.
Note: The unit of heat used in this manual is
the International Table calorie, which is equal
to 4.1868 absolute joules.
www.parrinst.com
3
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.
4
Parr Instrument Company
Current: The total current drawn should not exceed
the rating shown on the data plate on the calorimeter by more than 10 percent.
6100
Preface
Environmental Conditions
Operating: 15 ºC to 30 ºC; maximum relative humidity of 80% non-condensing. Installation Category II
(over voltage) in accordance with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25 ºC and 65 ºC; 10% to 85% relative
humidity.
Provisions for Lifting and Carrying
Before moving the instrument, disconnect all connections from the rear of the apparatus. Lift the
instrument by grabbing underneath each corner.
Cleaning & Maintenance
Periodic cleaning may be performed on the exterior
surfaces of the instrument with a lightly dampened
cloth containing mild soap solution. All power
should be disconnected when cleaning the instrument. There are no user serviceable parts inside the
product other than what is specifically called out
and discussed in this manual. Advanced troubleshooting instructions beyond the scope of this
manual can be obtained by calling Parr Instrument
Company in order to determine which part(s) may
be replaced or serviced.
Getting Started
These steps are offered to help the user become
familiar with, install, operate and develop the full
capabilities of the Parr 6100 Calorimeter.
1. Review the Concept of Operations, Chapter 1, to
get an understanding of the overall capabilities
of the calorimeter and microprocessor control.
2. Unpack and install the calorimeter in accordance
with the Installation Instructions, Chapter 2. This
simple, step-wise procedure will acquaint the
user with the various parts of the calorimeter
and make it easier to understand the operating
instructions which follow.
3. Turn the power switch ON (located on the back).
Turn to the Instrument Description, Chapter 3, to
review the touch screen controls.
4. Review the Program Installation and Control,
Chapter 4, to match the factory settings to the intended mode of operation. Any required changes
can be made to the program parameters located
in the Main Menu.
5. Review the Reporting Instructions, Chapter 7, to
become familiar with the manner in which calorimetry corrections are entered. Also discussed
are generating final reports, editing and clearing
memory.
6. Turn to the Menu Operating Instructions, Ap-
pendix A, to review the menu functions used
to modify the program contained in the 6100
Calorimeter. A review of the menus will provide
a good idea of the capabilities and exibility
designed into this instrument.
7. Review the Calculations, Appendix B. This pro-
vides information about calculations performed
by the 6100 Calorimeter.
8. Review Standardization, Appendix C. This will
serve two important functions. First, it provides
instructions on generating the energy equivalent
factor required to calculate the heat of combustion of unknown samples. Secondly, it will give
the user the opportunity to run tests on a material with a known heat of combustion to become
familiar with the instrument and confirm that the
instrument and operating procedures are producing results with acceptable precision. Most
6100 Calorimeters will have an energy equiva-
lent of approximately 2400 calories per ºC. The
runs for standardization and determinations are
identical, except for the setting of the instrument
to the standardization or determination mode.
9. Review the Communication Interfacing, Appendix D, for the correct installation of any peripherals connected to the 6100 Calorimeter.
10. After successful standardization, the 6100 Calorimeter should be ready for testing samples.
Note About Nomenclature:
Historically, burning a sample enclosed in a
high pressure oxygen environment is known
as Oxygen Bomb Calorimetry and the vessel
containing the sample is known as an Oxygen
Bomb. The terms bomb and vessel are used
interchangeably.
www.parrinst.com
5
1
Concept of Operation
chaPter 1
Concept of Operation
Overview
The 6100 Calorimeter has been designed to provide
the user with:
The Model 6100 can also be equipped with a vari-
ety of special purpose oxygen bombs for unusual
samples and/or applications. The 1104 High Strength
Oxygen Combustion Vessel is designed for testing
explosives and other potentially hazardous materials.
The 1109A Semimicro Oxygen Combustion Vessel can
be fitted along with its unique bucket to test samples
ranging from 25 to 200 mg.
• A traditional design calorimeter with removable
oxygen bomb and bucket.
• A moderately priced calorimeter which uses real
time temperature measurements to determine
heat leaks without using a controlled calorimeter
jacket.
• A full featured calorimeter that does not require
circulating water.
• A compact calorimeter requiring minimum
laboratory bench space.
• A modern intuitive graphical user interface for
ease of operation and training.
• A calorimeter with up to date digital hardware,
software and communications capabilities.
• A calorimeter that is cost effective and which can
incorporate a user’s current bombs, buckets, and
accessories.
Removable Bomb
The Model 6100 Calorimeter utilizes the Parr 1108P
Oxygen Combustion Vessel. More than 20,000 of the
1108 style oxygen combustion vessels have been
placed in service on a world wide basis. This bomb
features an automatic inlet check valve and an adjustable needle valve for controlled release of residual
gasses following combustion. They are intended for
samples ranging from 0.6 to 1.2 grams with a maximum energy release of 8000 calories per charge.
The 1108P Oxygen Combustion Vessel is made of
high-strength, high nickel stainless steel designed
to resist the corrosive acids produced in routine fuel
testing. An alternative 1108PCL vessel is available,
constructed of an alloy containing additional cobalt
and molybdenum to resist the corrosive conditions
produced when burning samples containing chlorinated compounds.
Removable Bucket
The A391DD removable bucket has been designed to
hold the bomb, stirrer and thermistor with a minimum volume of water and to provide an effective
circulating system which will bring the calorimeter to
rapid thermal equilibrium both before and after firing.
Compensated Jacket Operation
The 6100 Calorimeter is intended for the user who
wants a calorimeter with the convenient automatic
features provided in a modern isoperibol calorimeter,
but whose precision requirements can be met with a
static system. To meet these criteria, the temperature
controlled water jacket and its accessories have
been removed from the 6200 Isoperibol Calorimeter
and replaced with an insulating jacket around the
bucket chamber. This eliminates all water and water
connections, resulting in a significant saving in cost.
To obtain the best precision with an uncontrolled
jacket, the 6100 Calorimeter has temperature monitoring capability built into the jacket. This allows the
calorimeter to measure the actual jacket temperature
and apply the appropriate heat leak corrections in
real time. While, not equal to a controlled jacket, the
6100 method offers a significant improvement over
the traditional static jacket and makes it possible to
obtain reasonable precision without the long preand post-periods normally required for static jacket
calorimetry. It also makes it possible to use the Parr
Dynamic Method for rapid testing. As with all static
jacket calorimeters, best results are obtained when
the instrument is operated in a location where it is
not subject to air drafts and fluctuating temperatures. The preferred operating environment is in a
temperature controlled room (+/- 1 C). It is a well
accepted principle of reliable analysis that any instrument calibration be checked regularly. The optimum
frequency for checking the 6100 Calorimeter depends
largely on the temperature stability of the operating
environment. As general rule, the instrument calibration should be evaluated at least every tenth test. The
calorimeter controller software conveniently offers
both a graphical control chart approach in addition to
6
Parr Instrument Company
6100
Concept of Operation
1
an automatic rolling average calculation to support
calibration maintenance and verification. Following
the aforementioned guidelines and using reference
samples, such as benzoic acid, the process sigma
(precision classification) of the 6100 Calorimeter can
be taken as 0.1%.
Dynamic Operation
In its Dynamic Operating Mode, the calorimeter uses
a sophisticated curve matching technique to compare
the temperature rise with a known thermal curve to
extrapolate the nal temperature rise without actually waiting for it to develop. Repeated testing, and
over 20 years of routine use in fuel laboratories, has
demonstrated that this technique can significantly
cut the time required for a test by one-half without
significantly affecting the precision of the calorimeter.
Full Microprocessor Based Process Control
The microprocessor controller in this calorimeter has
been pre programmed to automatically prompt the
user for all required data and control input and to:
• Generate all temperature readings in the calorimeter.
• Monitor jacket as well as bucket temperature.
• Collect and store all required test data.
• Apply all required corrections for combustion
characteristics.
• Compute and report the heat of combustion for
the sample.
Flexible Programming
The fifth generation software built into this calorimeter and accessed through the screen menus permit
the user to customize the operation of the calorimeter
to meet a wide variety of operating conditions including:
• A large selection of printing options.
• Choice of accessories and Peripheral equipment.
• Multiple options in regard to handling
thermochemical corrections.
• Choice of ASTM or ISO Correction procedures.
• A variety of memory management and reporting
procedures.
• Complete freedom for reagent concentrations and
calculations.
• Confirm equilibrium conditions.
• Fire the bomb.
• Confirm that ignition has occurred.
• Determine and apply all necessary heat leak cor-
rections.
• Perform all curve matching and extrapolations
required for dynamic operation.
• Terminate the test when it is complete.
• Monitor the conditions within the calorimeter and
report to the user whenever a sensor or operating
condition is out of normal ranges.
Full Microprocessor Based Data Acquisition and Handling
In addition to its process control functions, the microprocessor in the calorimeter has been pre programmed to:
• Unlimited choice of reporting units.
• Automatic bomb usage monitoring and reporting.
• A choice of Equilibrium or Dynamic test methods.
• Automatic statistical treatment of calibration runs.
• Enhanced testing and trouble shooting procedure.
The 6100 Calorimeter is equipped with a universal
serial bus (USB) connection for communication with
a printer, balance, or other device. If more than one
device is to be used at the same time a USB hub will
need to be used. It is also equipped with an Ethernet
network connection for connections to laboratory
computers.
www.parrinst.com
7
2
Installation
chaPter 2
Installation
Environmental Conditions
The 6100 Calorimeter is completely assembled and
given a thorough test before it is shipped from the
factory. If the user follows these instructions, installation of the calorimeter should be completed with
little or no difficulty. If the factory settings are not
disturbed, only minor adjustments will be needed to
adapt the calorimeter to operating conditions in the
user’s laboratory.
This apparatus is to be used indoors. It requires at
least 4 square feet of workspace on a sturdy bench or
table in a well-ventilated area with convenient access
to an electric outlet, running water and a drain.
Required Consumables, Utilities and Power Requirements
The 6100 Calorimeter System requires availability of
Oxygen, 99.5% purity, 2500 psig maximum.
The power requirements for the subassemblies of the
6100 Calorimeter are:
Calorimeter
115VAC, 2.0 Amps. 50/60 Hz
230VAC, 2.0 Amps, 50/60 Hz
Printer
100 to 240 VAC, 0.35 Amps 50/60 Hz
Plug the power line into any grounded outlet providing proper voltage that matches the specification on
the nameplate of the calorimeter. The calorimeter will
draw approximately 100 watts of power. Grounding is
very important not only as a safety measure, but also
to ensure satisfactory controller performance. If there
is any question about the reliability of the ground
connection through the power cord, run a separate
earth ground wire to the controller chassis.
Turn the power switch to the on position. After a short
time, the Parr logo will appear on the LCD display
followed by a running description of the instrument
boot sequence. When the boot sequence is complete,
the calorimeter Main Menu is displayed.
Oxygen Filling Connection
The 6100 Calorimeter is equipped with an automatic
bomb oxygen lling system. This system consists of
an oxygen pressure regulator with a relief valve that
mounts on an oxygen tank and a controlled solenoid
inside the calorimeter. To install the regulator on the
oxygen supply tank, unscrew the protecting cap from
the oxygen tank and inspect the threads on the tank
outlet to be sure they are clean and in good condition. Place the ball end of the regulator in the outlet
and draw up the union nut tightly, keeping the gages
tilted slightly back from an upright position. Connect
the regulator to the oxygen inlet tting on the back of
the calorimeter case. This hose should be routed so
that it will not kink or come in contact with any hot
surface. Connect the high-pressure nylon hose with
the push on connector to the oxygen bomb outlet
connection on the back of the calorimeter.
All connections should be checked for leaks. Any
leaks detected must be corrected before proceeding.
Instructions for operating the filling connection are in
the Operating Instructions chapter. Adjust the pressure regulator to deliver 450 psi of O2. Assemble the
oxygen bomb without a charge and attach the lling
hose to the bomb inlet valve. Press the O2 Fill key
on the Calorimeter Operation page and observe the
delivery pressure on the 0 – 600 psi gage while the
oxygen is owing into the bomb. Adjust the regulator, if needed, to bring the pressure to 450 psi. If there
is any doubt about the setting, release the gas from
the bomb and run a second check.
Printer and Balance Connections
Connect the printer to the calorimeter at this time.
The Parr 1758 Printer is configured and furnished with
a cord to connect directly to the USB port on the back
of the calorimeter.
The balance port connection, if needed, should be
made at this time. If both a printer and a balance will
be used then a USB hub will need to be installed.
Contact Parr to determine the correct cable to connect
the balance to the calorimeter.
Standardizing the Calorimeter
The calorimeter must be accurately standardized
prior to actually performing calorimetric tests on
sample materials. Review Appendix C - Standardization, in order to become familiar with the general
8
Parr Instrument Company
6100
Installation
2
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
www.parrinst.com
9
2
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.
10
Parr Instrument Company
6100
Notes
2
www.parrinst.com
11
3
Instrument Description
chaPter 3
Instrument Description
Types of Controls
All calorimeter configurations and operations are handled by a menu-driven system operated
from the bright touch screen display. The settings and controls are organized into nine main
sections or pages which comprise the MAIN MENU.
12
Note: Keys with a “double box” in the upper left hand corner lead to sub-menus.
Parr Instrument Company
6100
Menu Keys
The controls that change the data field information in the menus will be one of the following:
1. Toggles: These data elds contain ON/OFF or YES/NO choices. Simply touching the key
2. Option Selection: These data fields contain a list of options. Touching the key on the
3. Value Entry Fields: These data fields are used to enter data into the calorimeter. Touching
4. Data Displays: Most of these keys display values that have been calculated by the calorim-
Instrument Description
on the screen toggles the choice to the other option. The current setting is displayed in the
lower right corner of the key.
screen steps the user through the available choices. The current setting is displayed in the
lower right corner of the key.
the key on the screen brings up a sub menu with a key pad or similar screen for entering
the required value. Some keys lead to multiple choices. Always clear the current value before entering a new value. Once entered the screen will revert to the previous menu and
the new value will be displayed in the lower right corner of the key.
eter and are informational only. Certain ones can be overridden by the user entering a desired value through a sub-menu. The value is displayed in the lower right corner of the key.
3
Note: Some keys will respond with an opportunity for the user to confirm the specified action to minimize accidental disruptions to the program and/or stored data.
Control Keys
There are five control keys which always appear in the right column of the primary displays.
These keys are unavailable when they are gray instead of white.
1. Escape: This key is used to go up one level in the menu structure.
2. Main Menu: This key is used to return to the main menu touch screen from anywhere in
the menu structure.
3. Start: This key is used to start a calorimeter test.
4. Report: This key is used to access the test results stored in the calorimeter, to enter ther-
mochemical corrections and to initiate a report on the display or printer.
5. Help: This key is used to access help screens related to the menu currently displayed on
the touch screen.
6. Abort: This key appears in the start key location while the test is running. Pressing this
key will abort the test in progress.
7. This key appears on the main menu only and is used to prepare the calorimeter for
turning off the power.
www.parrinst.com
13
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.
14
Parr Instrument Company
6100
Notes
4
www.parrinst.com
15
4
Program Installation & Control
Table 4-1
Factory Default Settings
Calorimeter Operations
Operating Mode Determination
Bomb Installed/EE 1/2400.0
Operating Controls
Method of Operation Dynamic
Reporting Units BTU/lb
Use Spiking Correction OFF
“OTHER” Multiplier 4.1868
Calibrate Touchscreen
LCD Backlight Timeout(s)
LCD Backlight Intensity 70%
Print Error Messages ON
Language English
1200 s
Spike Controls
Use Spiking OFF
Heat of Combustion of Spike 6318.4
Use Fixed Spike OFF
Weight of Fixed Spike 0.0
Prompt for Spike before Weight OFF
Program Information and Controls
Date & Time Settings
Software and Hardware Info
Settings Protect OFF
User/Factory Settings
Feature Key
Bomb Type Select
User Function Setup
Cold Restart
User/Factory Settings
User Setup ID 61-1108
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Calibration Data & Controls
Calibration Run Limit
EE Max Std Deviation 0.0
Heat of Combustion of Standard 6318.4
Bomb Service Interval 500
Control Chart Parameters
Use Bomb 1
10
Bomb 1 Through 4
EE Value 2400.0
Protected EE Value OFF
Thermochemical Corrections Standardization
Fixed Fuse Correction ON 50
Acid Correction Fixed HNO3 10.0
Fixed Sulfur Correction ON 0.0
Heat of Formation Sulfuric Acid
Heat of Formation Nitric Acid 14.1
36.1
Determination
Fixed Fuse Correction ON 50
Acid Correction Fixed HNO3 10.0
Fixed Sulfur Correction OFF 0.0
Calculation Factors
Nitric Acid Factor 1.58
Acid Multiplier 0.0709
Sulfur Value is Percent ON
Sulfur Multiplier 0.6238
Fuse Multiplier 1.0
Use Offset Correction (ISO) OFF
Offset Value 0.0
16
Parr Instrument Company
6100
Program Installation & Control
4
Net Heat/Dry Factors
Fixed Hydrogen OFF 0.0
Fixed Oxygen ON 0.0
Fixed Nitrogen ON 0.0
Calculate Net Heat of Combustion OFF
Fixed Moisture as Determined OFF 0.0
Fixed Moisture as Received OFF 0.0
Dry Calculation OFF
Data Entry Controls
Prompt for Bomb ID ON
Weight Entry Mode Touch Screen
Acid Entry Mode Touch Screen
Net Heat Entry Values Touch Screen
Auto Sample ID Controls ON
Sample Weight Warning above 2.0
Spike Weight Entry Mode Touch Screen
Sulfur Entry Mode Touch Screen
Moisture Entry Modes Touch Screen
Auto Preweigh Controls ON
Auto Sample ID Controls
Automatic Sample ID ON
Automatic Sample ID Increment 1
Automatic Sample ID Number 1
Auto Preweigh Controls
Automatic Preweigh ID ON
Automatic Preweigh ID Increment 1
Automatic Preweigh ID Number 1
Communication Controls
Printer Type Parr 1758
Balance Port
Network Interface
Printer Destination Local (USB)
Bar Code Port
Network Data Devices
Balance Port Communications
Balance Type Generic
Balance Port Device /dev/ttyUSB0
Customize Balance Settings
Balance Port Settings
Number of Data Bits 8
Parity None
Number of Stop Bits 1
Handshaking None
Baud Rate 9600
Data Characters from Balance 8
Data Precision 4
Transfer Timeout (seconds) 10
Balance Handler Strings
Data Logger
Data Logger OFF
Data Log Interval 10s
Data Log Destination Log File and Printer
Select Data Log Items
Data Log Format Text Format
Reporting Controls
Report Width 40
Automatic Reporting ON
Auto Report Destination Printer
Individual Printed Reports OFF
Edit Final Reports OFF
Recalculate Final Reports OFF
Use New EE Values in Recalculation OFF
www.parrinst.com
17
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.
18
Parr Instrument Company
6100
Operating Instructions
5
4. Set the bucket in the calorimeter. Attach the
lifting handle to the two holes in the side of the
screw cap and partially lower the bomb in the
water. Handle the bomb carefully during this operation so that the sample will not be disturbed.
Push the two ignition lead wires into the terminal sockets on the bomb head. Orient the wires
away from the stirrer shaft so they do not become tangled in the stirring mechanism. Lower
the bomb completely into water with its feet
spanning the circular boss in the bottom of the
bucket. Remove the lifting handle and shake any
drops of water back into the bucket and check for
gas bubbles.
5. Close the calorimeter cover. This lowers the stirrer and thermistor probe into the bucket.
6. Select determination or standardization as appropriate on the Calorimeter Operation page,
by toggling the operating mode key. Press the
START key. The calorimeter will now prompt the
operator for Bomb ID number, sample ID number, sample weight and spike weight in accordance with the instructions set into the Operating Controls page.
7. The calorimeter will now take over and conduct
the test. During the time it is establishing the
initial equilibrium, it will display PREPERIOD on
the status bar. Just before it res the bomb, it
will sound a series of short beeps to warn the
user to move away from the calorimeter. Once
the bomb has been fired, the status bar will display POSTPERIOD. The calorimeter will check to
make certain that a temperature rise occurs and
will then look for the final equilibrium conditions
to be met. If it fails to meet either the initial or
final equilibrium conditions, or if it fails to detect
a temperature rise within the allotted time, the
calorimeter will terminate the test and advise the
user of the error.
one minute to avoid entrainment losses. After
all pressure has been released, unscrew the cap;
lift the head out of the cylinder and examine the
interior of the bomb for soot or other evidence
of incomplete combustion. If such evidence is
found, the test will have to be discarded. Otherwise, wash all interior surfaces of the bomb,
including the head, with a jet of distilled water
and collect the washings in a beaker.
10. Titrate the bomb washings with a standard
sodium carbonate solution using methyl orange,
red or purple indicator. A 0.0709N sodium carbonate solution is recommended for this titration to simplify the calculation. This is prepared
by dissolving 3.76 grams of Na2CO3 in the water
and diluting to one liter. NaOH or KOH solutions
of the same normality may be used.
11. Analyze the bomb washings to determine the
sulfur content of the sample if it exceeds 0.1%.
Methods for determining sulfur are discussed in
Operating Instructions No. 207M.
12. At the end of the testing period, go to the main
menu and press the key. Press YES to con-
firm System Shutdown. Turn off the calorimeter
at the power switch when prompted by the
display.
8. At the conclusion of the test, the calorimeter will
signal the user.
9. Open the cover and remove the bomb and
bucket. Remove the bomb from the bucket and
open the knurled valve knob on the bomb head
to release the residual gas pressure before attempting to remove the cap. This release should
proceed slowly over a period of not less than
www.parrinst.com
19
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. Signicant 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
shallow capsules measuring approximately 1” diameter and 7/16” deep. These are available in stainless
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.
20
Parr Instrument Company
6100
Operating Instructions
5
Figure 5-2
3601 Gelatin Capsules
Capsules should be monitored for wear. Do not use
the capsule if the wall or base thickness is less than
0.025”.
New capsules are heated in a muffle furnace at 500 ºC
for 24 hours to develop this protective coating
uniformly on all surfaces. This treatment should be
repeated after a capsule has been polished with an
abrasive to remove any ash or other surface depos-
its. Heating in a mufe 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.
www.parrinst.com
21
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.
22
Parr Instrument Company
• Set the cup in the capsule holder and arrange
the auxiliary fuse so that it touches the center of
the tape disc.
• Just before starting the test, prick the disc with
a sharp needle to make a small opening which
is needed to prevent collapse of the disc when
pressure is applied.
• Fill the bomb with the usual oxygen charging
pressure.
• The calorimeter will fire the bomb and complete
the test in the usual manner.
6100
Operating Instructions
5
Volatile samples are defined as one with an initial
boiling point below 180 ºC per ASTM D-2.
Low volatile samples with a high water content,
such as urine or blood, can be burned in an open
capsule by absorbing the liquid on filter paper pulp
or by adding a combustion aid, such as ethylene
glycol.
Poor Combustion
Because of the difference in combustion characteristics of the many different materials which
may be burned in an oxygen bomb, it is difcult 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.
www.parrinst.com
23
Loading...