Figure F-7 Temperature Control Assembly with Fittings 81
Figure F-8 A1284DD2 Stirrer Hub Assembly 82
Figure F-9 Stirrer Motor Assembly 83
Table of Contents6200
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Preface
Preface
Scope
This manual contains instructions for installing and
operating the Parr 6200 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
Related Instructions
Additional instructions concerning the installation
and operation of various component parts and peripheral items used with the 6200 Calorimeter have
been included and made a part of these instructions.
No.Description
201MLimited Warranty
418M1108P Oxygen Combustion Vessel
207MAnalytical Methods for Oxygen Bombs
230MSafety in the Operation of Laboratory
and Pressure Vessels
483MIntroduction to Bomb Calorimetry
Additional instructions for the printer, cooler, and
water handling systems are found in the respective
package and should be made a part of this book.
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.
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.
Note: The unit of heat used in this manual is
the International Table calorie, which is equal
to 4.1868 absolute joules.
Purpose
Heats of combustion, as determined in an oxygen
bomb calorimeter such as the 6200 Isoperibol
Calorimeter, are measured by a substitution procedure in which the heat obtained from the sample is
compared with the heat obtained from a standardizing material. In this test, a representative sample
is burned in a high-pressure oxygen atmosphere
within a metal pressure vessel or “bomb”. The
energy released by the combustion is absorbed
within the calorimeter and the resulting temperature
change is recorded.
Customer Service
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
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.
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
combustible materials; fire or explosion may
result. This device contains components which
may ignite such material.
2. Refer servicing to qualified personnel.
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.
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.
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Preface
Frequency: Calorimeters can be operated from
either a 50 or 60 Hertz power supply without affecting their operation or calibration.
Current: The total current drawn should not exceed
the rating shown on the data plate on the calorimeter by more than 10 percent.
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 6200 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 Installation, Chapter 2. This simple, stepwise 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 6200
Calorimeter. A review of the menus will provide
a good idea of the capabilities and flexibility
designed into this instrument.
7. Review the Calculations, Appendix B. This pro-
vides information about calculations performed
by the 6200 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
6200 Calorimeters will have an energy equivalent 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 Interfaces, Appendix
D, for the correct installation of any peripherals
connected to the 6200 Calorimeter.
10. After successful standardization, the 6200 Calorimeter should be ready for testing samples.
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Concept of Operation
Overview
• The 6200 Calorimeter has been designed to
provide the user with:
Concept of Operation
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.
1
• A traditional design calorimeter with removable
oxygen bomb and bucket.
• A moderately priced calorimeter which uses real
time temperature measurements to determine
heat leaks using a controlled calorimeter jacket.
• A high precision calorimeter capable of
exceeding the repeatability and reproducibility
requirements of all international standard test
methods.
• 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 communication capabilities.
• A calorimeter that is cost effective and which can
incorporate a user’s current bombs, buckets, and
accessories.
Removable Bomb
The Model 6200 Calorimeter utilizes the Parr 1108P
Oxygen Combustion Vessel. More than 20,000 of
these reliable 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 8,000
calories per charge.
The Model 6200 can also be equipped with a variety
of special purpose oxygen combustion vessels 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 Vessels can be fitted along with its unique
bucket to test samples ranging from 25 to 200 mg.
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.
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 final 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 cut the time required for a test by one-half
without significantly affecting the precision of the
calorimeter.
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Concept of Operation
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.
• Confirm equilibrium conditions.
• Fire the bomb.
• Confirm that ignition has occurred.
• Determine and apply all necessary heat leak
corrections.
• 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 preprogrammed to:
• Collect and store all required test data.
• Apply all required corrections for combustion
characteristics.
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.
• 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 6200 Calorimeter is equipped with one USB
connection for direct communication with its printer
and other peripherals. It is also equipped with an
Ethernet network connection for connections to
laboratory computers.
• Compute and report the heat of combustion for
the sample.
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Installation
Note: Some of the following manual sections contain information in the form of
warnings, cautions and notes that require
special attention. Read and follow these
instructions carefully to avoid personal injury
and damage to the instrument. Only qualified personnel should conduct the installation tasks described in this portion of the
manual.
Environmental Conditions
The 6200 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 8 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. The supply voltage must be within ±
10% of marked nominal voltage on the apparatus.
The supply voltage receptacle must have an earth
ground connection.
Required Consumables, Utilities and Power
Requirements
The 6200 Calorimeter System requires availability of
Oxygen, 99.5% purity, 2500 psig maximum.
The power requirements for the subassemblies of
the 6200 Calorimeter are:
The water reservoir of the calorimeter must be filled
with approximately 1.4 liters of water (distilled or
de-ionized preferred). This must be done prior to
turning on the heater and the pump. The reservoir is
filled through the tank fill elbow on the back of the
calorimeter. The tank is full once water stands in the
horizontal run of the filling elbow.
Power Connection
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 300 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. Go to the Calorimeter Operation page and
turn the heater and pump on. This begins circulating
and heating the calorimeter jacket water. Add water
to the filling elbow at the rear of the instrument as
required in order to keep it full.
Jacket Cooling Water Connection
It becomes necessary to use the jacket cooling water
connection only if the calorimeter operating room
temperature exceeds 24 °C (75 °F).
When required, an external water source is used to
cool the jacket of the 6200 Calorimeter. This is done
in either of the following ways:
1. Tap water is used for cooling and then run to a
drain.
2. Cooling water is re-circulated to the calorimeter
from a Parr 6510 Water Handling System.
2
Printer
100 to 240 VAC, 0.35 Amps 50/60 Hz
Printer Supplies
334C Printer Paper
335C Printer Ribbon
The water that provides the cooling goes through a
heat exchanger and does not mix with the water in
the jacket and its reservoir. There is a very low cooling load and tap water up to a temperature of 27 °C
should be adequate.
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2
Installation
Tap Water Cooling
Connect the tap water supply to the cold water inlet
on the back of the calorimeter using either 1/4”
copper or nylon tubing (HJ0025TB035). A 196VB
metering valve is provided with the calorimeter.
This valve should be installed in this inlet line near
the calorimeter. This valve is used to adjust the flow
of water to the heat exchanger to compensate for
differences in tap water temperatures and water line
pressures. Once the calorimeter is operating at equilibrium, check the jacket temperature that is displayed
on the operating page. If this temperature is cycling
significantly, close down on the metering valve to
reduce the flow of cooling water. If the jacket rises
above its 30 °C set point, open this valve to increase
the cooling. A ow rate of 100 ml/ minute is generally
all that is required.
Connect the cooling water outlet on the back
of the calorimeter to a drain using either nylon
(HJ0025TB035) or copper 1/4” tubing. A shut off
valve in tap water supply line is also a good idea
if the calorimeter will not be used for an extended
period.
Cooling with the Water Handling System
If the calorimeter is to be operated with a Parr Water
Handling System, connect the pump output to the
cooling water inlet and connect the cooling water
outlet to the return connection on the water handling
system. With this installation it is neither necessary
nor desirable to install the 196VB metering valve in
the inlet line. It is a good idea to keep all water line
runs as short as practical to avoid unwanted temperature changes in the water between the source and the
calorimeter.
Oxygen Filling Connection
The 6200 Calorimeter is equipped with an automatic
bomb oxygen filling 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 fitting 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 outlet fitting 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 filling 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 flowing 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.
If a balance is to be attached to the calorimeter it
will be necessary to use a USB hub so that multiple
devices can be connected. Any standard USB hub can
be used.
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 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 two 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. All 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
and bucket combination. The calorimeter is ready for
testing samples after an energy equivalent value has
been obtained.
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6200
Installation
2
Swagelok Tube Fittings
When Swagelok Tube Fittings are used, the instructions for installation are:
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,
tighten the Swagelok nut 3/4 turns from nger-
tight.
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.
Figure 2-1
Swagelok Tube Fittings
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
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 finger 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.
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2
Installation
Figure 2-2
6200 Calorimeter Back Panel
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6200
Line 3
Figure 2-3
Closed Loop Configuration with 6510
O2 Regulator
Line 2
6510 Water
Handling
System
Installation
2
Line 3
Line 1
~27 °C
Figure 2-4
Open Loop Configuration with Tap Water
O2 Regulator
Tap Water
· <27 °C
Line 2
Line 1
Drain
Line 1 & 2 – Maximum length of 10 feet, 1/4” OD, Polyurethane (Part Number HJ0025TB035)
Line 3 – Maximum length of 25 feet, 1/8” OD, Nylon (Part Number HX0012TB024)
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2
Installation
Figure 2-5
Open Loop Configuration with 1552
O2 Regulator
Tap Water
· >27 °C
Line 3
Line 2
Line 1
~27 °C
Line 1 & 2 – Maximum length of 10 feet, 1/4” OD, Polyurethane (Part Number HJ0025TB035)
Line 3 – Maximum length of 25 feet, 1/8” OD, Nylon (Part Number HX0012TB024)
Water
Cooler
Drain
1552
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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.
Instrument Description
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.
4. Data Displays. Most of these keys display values
that have been calculated by the calorimeter
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: Keys with a “double box” in the upper
left hand corner lead to sub-menus.
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 on the
screen toggles the choice to the other option.
The current setting is displayed in the lower
right corner of the key.
2. Option Selection. These data fields contain a list
of options. Touching the key on the screen steps
the user through the available choices. The
current setting is displayed in the lower right
corner of the key.
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
thermochemical corrections and to initiate
report on the display, printer or attached
computer.
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.
3. Value Entry Fields. These data fields are used to
enter data into the calorimeter. Touching the key
on the screen brings up a sub menu with a key
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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Notes
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6200
chaPter 4
Program Installation & Control
Software Installation
Program Installation & Control
Revising Default Settings
The default parameters of the 6200 Calorimeter can
be changed to guarantee that the 6200 Calorimeter,
when cold restarted, will always be in the desired
configuration before beginning a series of tests.
4
The program in the 6200 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.
Default Settings
Users who wish to permanently revise their default
settings may do so using the following procedure:
• Establish the operating parameters to be stored
as the user default settings.
• Go to the Program Info and Control Menu, User/
Factory Settings, User Setup ID, and enter the
desired User Setup ID.
• Select Save User Default Settings
To re-load the user default settings, go to the Pro-
gram Info and Control Page, User/Factory Settings,
Re-load User Default Settings, and YES.
Units are pre-programmed with default settings. See
pages 17 and 18 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
Information and Control Menu, then to User/Factory
Settings, and then touch Reload Factory Default
Settings and YES.
Non-volatile memory is provided to retain any and
all operator initiated program changes; even if
power is interrupted or the unit is turned off. If the
unit experiences an intentional or unintentional
“Cold Restart”, the controller will return to its default
settings.
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4
Program Installation & Control
6200 Factory Default Settings
Calorimeter Operations
Operating ModeDetermination
Bomb Installed/EE1/2400.0
Heater and PumpOFF
Operating Controls
Method of OperationDynamic
Reporting UnitsBTU/lb
Use Spiking CorrectionOFF
“OTHER” Multiplier4.1868
Calibrate Touchscreen
LCD Backlight Timeout(s)
LCD Backlight Intensity70%
Print Error MessagesON
LanguageEnglish
1200 S
Table 4-1
Calibration Data & Controls
Calibration Run Limit
EE Max Std Deviation0.0
Heat of Combustion of Standard 6318.4
Bomb Service Interval500
Control Chart Parameters
Charted ValueHOC Standard
Process Sigma0.1
Temp Rise High Warning3.3
Temp Rise Low Warning2.0
Use Bomb1
10
Bomb 1 Through 4
EE Value2400.0
Protected EE ValueOFF
Spike Controls
Use SpikingOFF
Heat of Combustion of Spike6318.4
Use Fixed SpikeOFF
Weight of Fixed Spike0.0
Prompt for Spike before WeightOFF
Program Information and Control
Date & Time Settings
Volume Level Adjust85%
Software and Hardware Info
Settings ProtectOFF
User/Factory Settings
Feature Key
Bomb Type Select
User Function Setup
Cold Restart
User/Factory Settings
User Setup ID62-1108
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Thermochemical Corrections Standardization
Fixed Fuse CorrectionON 50
Acid CorrectionFixed HNO3 10.0
Fixed Sulfur CorrectionON 0.0
Determination
Fixed Fuse CorrectionON 50
Acid CorrectionFixed HNO3 10.0
Fixed Sulfur CorrectionOFF 0.0
Net Heat/Dry Factors Net Heat & Dry Disable
Fixed Hydrogen
Fixed OxygenON 0.0
Fixed NitrogenON 0.0
Calculate Net Heat of CombustionOFF
Fixed Moisture as Determined OFF 0.0
Fixed Moisture as Received OFF 0.0
Dry CalculationOFF
OFF 0.0
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Table 4-1 (Continued)
6200 Factory Default Settings
Calculation Factors
Nitric Acid Factor1.58
Acid Multiplier0.0709
Sulfur Value is PercentON
Sulfur Multiplier0.6238
Fuse Multiplier1. 0
Use Offset Correction (ISO)OFF
Offset Value0.0
Data Entry Controls
Prompt for Bomb IDON
Weight Entry ModesTouch Screen
Acid Entry ModeTouch Screen
Net Heat Entry ModesTouch Screen
Auto Sample ID ControlsON
Sample Weight Warning above2.0
Spike Weight Entry ModeTouch Screen
Sulfur Entry ModeTouch Screen
Moisture Entry ModeTouch Screen
Auto Preweigh ControlsON
Auto Sample ID Controls
Automatic Sample IDON
Automatic Sample ID Increment1
Automatic Sample ID Number1
Auto Preweigh Controls
Automatic Preweigh IDON
Automatic Preweigh ID Increment 1
Automatic Preweigh ID Number1
Program Installation & Control
Communication Controls
Printer TypeParr 1758
Balance Port
Network Interface
Printer DestinationLocal (USB)
Bar Code Port
Network Data Devices
Balance Port Communications
Balance Type
Balance Port Device
Customize Balance Settings
Balance Port Settings
Number of Data Bits8
ParityNone
Number of Stop Bits1
HandshakingNone
Baud Rate9600
Data Characters from Balance8
Data Precision4
Transfer Timeout (seconds)10
Balance Handler Strings
Data Logger
Data LoggerOFF
Data Log Interval12s
Data Log Destination Log File and Printer
Select Data Log Items
Data Log FormatText Format
Generic
4
Reporting Controls
Report Width40
Automatic ReportingON
Auto Report DestinationPrinter
Individual Printed ReportsOFF
Edit Final ReportsOFF
Recalculate Final ReportsOFF
Use New EE Values in Recalculation OFF
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Notes
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Page 23
6200
Operating Instructions
chaPter 5
Operating Instructions
Operating the Calorimeter
All operations required to standardize the 6200
Calorimeter, or test an unknown sample, should
proceed step-wise in the following manner:
5
Operating the 1108P Oxygen Combustion Vessel
Detailed instructions for preparing the sample and
charging the 1108P Oxygen Combustion Vessels 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
filling 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
flow 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 filling pressures can be used, but
the bomb must never be filled to more than 600
psig (40 atm).
1. Turn on the calorimeter and activate the pump
and heater using Calorimeter Operations. Allow
at least 20 minutes for the calorimeter to warm
up and the jacket temperature to stabilize. Once
the jacket temperature comes within 0.5 °C of 30
°C and stays there for approximately 15 minutes, the calorimeter is ready to begin testing.
The Start key will be available at this time. 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 the sample weighing the material to 0.1
mg and charge the oxygen bomb as described in
the section entitled Operating the Filling Con-nection. Using an additional bomb and bucket
can increase the throughput of the 6200 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 approximately 3 to 5 °C below the
jacket 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.
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Page 24
5
Operating Instructions
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 fill the bucket. Instructions
for this automatic system are given in Operating
Instruction No. 454M.
4. Set the bucket in the calorimeter. Attach the
lifting handle (421A) to the two holes in the
side of the screw cap and partially lower the
bomb into 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.
Note: If bubbles continue to rise from the
bomb after the air in the screw cap has
escaped the test must be stopped and the
bomb not fired until the leak has been corrected.
5. Close the calorimeter cover. This lowers the
stirrer and thermistor probe into the bucket.
Make sure that the bucket thermistor does
not touch the bucket or 1108P when the lid is
lowered.
6. Select determination or standardization as
appropriate on the Calorimeter Operation menu
by toggling the OPERATING MODE key. After
pressing the STA RT 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.
the status bar. Just before it fires 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.
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 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.
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
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Parr Instrument Company
12. At the end of the testing period, turn OFF the
calorimeter at the power switch.
Page 25
6200
Operating Instructions
5
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 2811 Parr 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 in giving controlled 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 content 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 6200 Calorimeter has been designed to operate
with an oxygen filling pressure of 30 atm. Significant changes from this value are not recommended.
Combustion Capsules
Non-volatile samples to be tested in Parr oxygen
bombs 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 alloyed 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 capsule is required. When
superior corrosion resistance is needed, the platinum rhodium 43A5 capsule is required.
The stainless steel capsules will acquire a dull gray
finish after repeated use in an oxygen bomb due to
the formation of a hard, protective oxide film. 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.
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.
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 by Parr 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 deposits. Heating in a muffle 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.
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5
Operating Instructions
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.
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.
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 is available constructed of an alloy selected to specifically resist the
corrosive effects of samples with high chlorine or
chloride.
While no material will offer complete corrosion
resistance to these samples, the 1108PCL offers
significantly enhanced corrosion resistance for this
service.
Explosives and High Energy Fuels
The 1108P and 1108PCL used in the 6200 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
stainless steel 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.
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 determination. 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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Page 27
6200
Operating Instructions
5
Figure 5-7
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
5-7).
• 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.
• 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.
Poor Combustion
Because of the difference in combustion characteristics of the many different materials which
may be burned in an oxygen bomb, it is difficult 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.
• The combustion must produce sufficient turbulence 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.
• 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.
Volatile samples are defined as one with an initial
boiling point below 180 °C 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.
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Notes
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Page 29
6200
chaPter 6
Corrections & Final Reports
Corrections & Final Reports
If fixed 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.
6
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 Installation and Control, 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
If values for these corrections are not available, the
operator can use the SKIP key to bypass any of the
corrections. The report will remain at preliminary
status until an entry is made for fuse, acid and
sulfur.
Fixed Corrections
In many cases, fixed 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 fixed corrections are found in
Appendix B, Thermochemical Calculations.
Any value set-up as a fixed correction will be automatically applied and the controller will not prompt
the user for this value.
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.
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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Page 31
6200
Reporting Instructions
chaPter 7
Reporting Instructions
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.
7
Report Option Section
The 6200 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.
Reports can also be downloaded to a PC via the
Ethernet port or copied using an SD memory card.
Report Generation
There are two kinds of calorimeter reports: Preliminary and Final.
Preliminary Reports are generated at the conclusion
of a test. They will not contain the 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 fixed corrections are used for all of the thermochemical corrections a preliminary report will not be
generated.
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.
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.
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.
Select From List: This key displays the stored
results specified with the following two keys:
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.)
To bring the selected report or series of reports
to the display, press the DISPLAY key. To send the
reports to the printer press the PRINT key.
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.
Net Heat of Combustion
To have the Net Heat of Combustion print as part
of preliminary and nal reports, go to the Net Heat/
Dry Factors on the Thermochemical Corrections
Page and turn ON Calculate Net Heat of Combustion. During the reporting process, the controller will
prompt for the hydrogen (H) value.
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Notes
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Page 33
6200
chaPter 8
File Management
The 6200 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.
File Management
Clearing Memory
The FILE MANAGEMENT key on the main menu leads
to the file management sub-menu. The RUNDATA 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.
• Once a file is deleted there is no way to recover
the data.
Removable SD Memory
The controller of the 6200 Calorimeter can accept
SD memory cards. These cards can be used to:
• Copy test file data for transfer to a computer.
8
• 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 slots on the back
of the control section of the calorimeter. Keys are
provided on the FILE MANAGEMENT sub-menu to
initiate each of the above actions with the exception
of restoring or updating the controller’s operating
system.
Note: The calorimeter cannot read SDHC
cards. This limits the capacity of the SD
card to 2 GB or less.
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Notes
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Page 35
6200
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 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.
Jacket Temperature Troubleshooting
The jacket temperature is monitored with the use
of a thermistor installed in the temperature control
assembly. This assembly is heated by a heater
cartridge, A1459DD. In the Diagnostics Menu, select
Instrument Monitor. If the heater PID is ON and reading 100%, yet the jacket is at ambient temperature,
check the following possible causes.
If the heater PID is OFF, the heater and pump must
be turned on in the Calorimeter Operation screen to
perform the troubleshooting steps.
Maintenance & Troubleshooting
If the voltage is not present, then examine the 2040E
thermostat reset button. If the reset button extrudes
this means that the temperature in the temperature
control assembly has exceeded 75 ºC. Confirm
that water is flowing through the system, turn off
the power and then reset the switch by depressing
the button. If the thermostat continues to trip even
though water is flowing through the system, refer to
the error code “There Is A Problem With The Jacket
Thermistor” for further troubleshooting.
If there is no voltage present, and the reset button on
the thermostat is not tripped, refer to the error code
“There Is A Problem With The Jacket Thermistor” for
further troubleshooting. There may also be a problem with the calorimeter controller, A1279DD2, and
Parr Customer Service should be contacted.
Fuses
The replacement of protective fuses for the 6200
Calorimeter should be performed by qualified personnel.
All fuses except Parr part # 139E23 are located on
the A2140E I/O board located inside the instrument.
Please contact Parr Customer Service for instructions
on accessing the I/O board.
Note: Check the labels on the instrument for
correct fuse rating.
Part No.DescriptionTypeRatings
139E23Lines Protective
Fuses
1641E2Heater Fuse (F2)Fast-Acting2.5 Amps,
1641EPump Fuse (F1)Fast-Acting1 Amp,
Fast-Acting15 Amps,
250Vac
250Vac
250VAC
9
Caution!
Turn off the power to the calorimeter prior
to attempting to reset the thermostat. The
temperature control assembly can become
very hot. Use caution when servicing this
area of the calorimeter.
If line voltage (115V or 230V) is present across the
heater cartridge connection, check the resistance
across the heater cartridge. Approximately 70 ohms
will be seen with a 115V calorimeter. Approximately
140 ohms will be seen with a 230V calorimeter. If the
resistance is not correct the heater may have failed.
6200 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.
Start Button Dim:
The Start button will be dim (not lit) when the calorimeter is not ready to begin a test. When the heater
and pump are first turned on the jacket temperature
will be less than 30 °C. Once the jacket temperature
reaches 30 °C ± .5 °C it will be another 15 minutes
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9
Maintenance & Troubleshooting
before the Start button lights up. This is to make
sure that all of the jacket water is stable at the correct
temperature.
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 first
minute of the post-period.
The heater loop break limit has been detected. The heater
will now be shutdown.
This error means that the calorimeter is trying to heat
the water in the unit for an extended period of time.
When the heater and pump are initially turned on the
heater will be at 100% power until the jacket temperature approaches 29.5 °C. Once it gets close the power
being applied to the heater will be cut back to avoid
overshooting the target of 30 °C.
The calorimeter will turn off the heater and pump if
the heater is at 100% power for more than 10 minutes. If the jacket water is approximately 21 ºC or less
when the heater and pump is first turned on it is not
unusual to get this error. In this case clear the error
and restart the heater and pump. If the error occurs
again then there could be a problem.
• Check the 2040E Thermostat reset
• Check the water level in the calorimeter
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
• Bucket temperature outside the acceptable range
(3-5 °C below the jacket setpoint)
• Jacket requires water
The Current Run Has Aborted Due To Timeout.
The calorimeter has failed to establish an acceptable
final temperature within the time allowed. Possible
causes for this error are listed below:
There Is A Problem With The Bucket Thermistor.
Possible electrical open.
• Check connection to board
• Check quick disconnect between cables
• Replace probe
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.
• 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 I/O board calibration
information from the I/O board. If the I/O 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 fired. 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 Chapter 8, File Management.
Bomb EE Standard Deviation Warning.
The relative standard deviation for the calibration
runs in memory for the indicated bomb exceeds the
preset limit.
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.
• Poor jacket water circulation due to a kinked hose
or insufficient water in the tank
• A bomb leak
• Poor bucket stirring
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aPPendix a
Menu Operating Instructions
Menu Operating Instructions
Heater and Pump: The heater and pump must only
be turned on after the calorimeter water tank is filled
with water.
A
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 6200 Calorimeter.
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.
Note: The heater and pump must be turned
ON to bring jacket to the correct starting temperature before testing can commence.
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 filling
system used to fill the bomb. Pressing this same key
while the bomb is filling will abort the process.
Temperature Graph: Press this key to view the
Temperature vs. Time Plot Screen.
Temperature vs. Time Plot Screen
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.
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.
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.
Bucket Min Value: Press this key to access its
numeric dialog box to set a minimum bucket
value.
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Time Maximum: Press this key to access its
numeric dialog box to set the greatest amount
of time for the run.
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Menu Operating Instructions
A
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.
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.
Reporting Units: Toggles between BTU/lb, cal/g,
J/kg. Other, and MJ/kg. A user selected set of report-
ing units may be programmed by selecting “Other”.
Spiking Correction: 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 Controls
Other Multiplier: This button allows the user to
enter a final multiplier that is used when the reporting 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.
LCD Backlight Intensity: This key accesses a
sub-menu with a slide control which adjusts the
backlight intensity 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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A
Menu Operating Instructions
Program Information and Control Menu
Date & Time Settings: Access the sub-menu on
which Date & Time are set.
Date & Time Settings
Software and Hardware Info: This screen displays
important information such as the main software
version, I/O board hardware information, CPU type,
I/O rmware 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
Date: Displays current date and accesses the
sub-menu on which the date is set (YY/MM/DD)
format.
Time: Display current time and accesses the
sub-menu on which time is set in (HH:MM)
format.
Time zone: Allows the user to select the local
time zone. Pressing the button will toggle
through the time zones.
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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.
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.
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Menu Operating Instructions
A
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.
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.
User Function Setup: This key leads to sub menus
that support the conguration 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 Data and Controls Menu
EE Max Std 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 0.17 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. This interval may
be more frequent depending upon the nature of the
sample.
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.
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.
Control Chart Parameters
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Menu Operating Instructions
Charted Value: Toggles the charted value between 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 6200 is a .1 Process Sigma calorimeter.
Temp. Rise High Warning: Sets the high warn-
ing limit on the bucket temperature rise. A
temperature rise higher than this value will
generate a warning message.
Temp. Rise Low Warning: Sets the low warning limit on the bucket temperature rise. A
temperature rise lower than this value will
generate a warning message.
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 throughput. The respective EE values for
each bomb can be stored in memory.
Note: For rapid turn around between tests,
the 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.
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 serviced.
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 if the user does not wish to have the
calorimeter automatically update its own EE
value.
40
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.)
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6200
Menu Operating Instructions
A
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 dot.
Thermochemical Calculations Menu
Standardization Correction
Fixed Fuse Correction: Displays both the ON/OFF of
the fixed 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 fixed fuse
value is 50 calories for the 1108P style bomb.
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.
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.
Options for the Acid Correction:
»Fixed HNO
»Calculated HNO
»Entered Total
»Entered HNO
»Fixed Total
These options are discussed further in Appendix B Calculations.
Fixed Sulfur Correction: Displays both the ON/OFF
of the fixed 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 fixed sulfur value of zero should be
used.
3
3
3
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A
Menu Operating Instructions
Determination Correction
Fixed Fuse Correction: Displays both the ON/OFF
of the fixed 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.
Fixed 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.
Options for the Acid Correction:
»Fixed HNO
»Calculated HNO
»Entered Total
»Entered HNO
»Fixed Total
These options are discussed further in Appendix B Calculations.
Fixed Sulfur Correction: Displays both the ON/OFF
of the fixed 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.
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3
Calculation Factors
Nitric Acid Factor: The default is 1.58 calories
per 1000 calories of released energy.
Acid Multiplier: The multiplier is the normality of
the sodium carbonate used to titrate for the acid
correction. The default value of 0.0709 allows
for direct entry of the acid correction in calories.
If the bomb rinsings are titrated in order to
determine the acid correction, this multiplier is
the concentration of the base (equivalents/L) or
normality used for titration. In this case, the acid
correction is entered as milliliters of base used
to titrate the bomb rinsings.
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.
Calculation Factors: Accesses sub-menu, Calculation Factors which sets a number of options for the
way the thermochemical corrections are applied.
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Parr Instrument Company
Fuse Multiplier: The fuse corrections represent
the number of calories liberated by the burning thread used to ignite the sample. If another
measurement is used, the correction factor must
be entered here.
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Menu Operating Instructions
A
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, set to ON and enter the
appropriate value as the offset value.
Offset Value: Entry for the value when use offset
correction is turned ON.
Net Heat/Dry Heat Factors
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.
Fixed Hydrogen: ON/OFF and value entry.
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: ON/OFF and
value entry.
Fixed Moisture as Received: ON/OFF and
value entry.
Dry Calculation: ON/OFF. Turn on to have the
calorimeter calculate the result on a dry basis.
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.
Automatic Sample ID Controls: Accesses sub-menu
for controlling the automatic assignment of sample
identification numbers.
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Menu Operating Instructions
Automatic Sample ID Controls
Automatic Sample ID: When set to ON it 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.
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.
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.
Preweigh Sample ID Controls
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.
Auto Sample ID Increment: Establishes the
increment between sample numbers.
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.
Automatic Preweigh ID: ON/OFF toggle for this
feature.
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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Menu Operating Instructions
A
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.
Communication Controls Menu
Communication Controls: Accesses sub-menus
which set the communications protocols for the
printer and balances.
Printer Type: Toggles between a Parr 1758 and a
generic printer. When set for the 1758 Printer, all of
the features of this printer, such as bold printing,
will be activated.
Balance Port: Accesses sub-menu, Balance Port
Communications.
Automatic Report Destination: Directs the reports
to the printer port or the display.
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.
Balance Type: This key 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.
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Menu Operating Instructions
Balance Port Communications
Customize Balance Settings: Accesses submenu that 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 the
settings of an attached balance for proper communication.
»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
handshaking. Choose from Xon/Xoff,
RTS/CTS and None.
»Data Characters from Balance: This
setting 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.
»Data Precision: This key allows the user
to establish the number of digits to the
right of the decimal point that are passed
from the balance handler.
»Transfer Timeout (seconds): This value
determines how long the interface will
wait before giving up on a weight transfer. The value is entered in seconds.
»Balance Handler Strings: This key leads
to a submenu that allows the balance
template to be customized for unique balances or needs.
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.
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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Menu Operating Instructions
A
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 provides access to
a function that will format the user installed SD
card in a manner that is compatible with the CPU
Boot loader. Formatting the card this way is recommended prior to installing any program update files
on the SD card.
Copy Run Data to SD Card: This key copies all test
data to a SD memory 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.
Copy User Settings to SD Card: This key copies all
previously saved user setups to the 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.
Note: The calorimeter cannot read SDHC
cards. This limits the capacity of the SD
card to 2 GB or less.
Note: See the Report Generating section in
Chapter 7.
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A
Menu Operating Instructions
Diagnostics Menu
Allows the user to test many of the components and
subsystems of the calorimeter. These capabilities
must be used in conjunction with the Maintenance
Instructions to obtain the maximum benefits from
these capabilities.
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.
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.
View System Log: This key is used to display
the contents 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.
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6200
aPPendix B
Calculations
Calculating the Heat of Combustion
The 6200 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
Calculations
Energy Equivalent.
The energy equivalent (represented by W in the
formula, or abbreviated as EE) is determined by
standardizing the calorimeter as described in Ap-pendix 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.
B
Where:
H
=Gross heat of combustion.
c
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 6200 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.
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.
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.
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B
Calculations
Users may find it convenient to enter a fixed 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 fixed fuse correction of 50 calories
is applied to all tests. Total errors of more than 5
calories will seldom occur when using a fixed fuse
correction and the fuse wire supplied by Parr.
When using the 1108P Oxygen Combustion Vessel,
there are two components to the fuse correction:
• The heat introduced by heating the wire used to
ignite the cotton thread.
• The heat of combustion of the cotton thread
used to ignite the sample.
The semi-permanent heating wire is heated by dissipating an electrical charge from a capacitor. Since
this charge is controlled by the size of the capacitor
and the charging voltage, and because the capacitor
is fully discharged for each test, the energy released
can be calculated. In the 6200 Calorimeter this is a
fixed correction of 10 calories per test.
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,
including the assumption of a fixed nitric acid correction.
The 6200 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.
Cotton has a heat of combustion of 4000 calories
per gram. The actual thread being used should be
weighed to see how much is being burned. Ten centimeters of a fine thread will weigh approximately
0.003 grams which would release 12 calories as it
burns. Heavier threads weigh up to 0.010 grams per
10 centimeters and increase this correction to 40 calories per test. The finer the thread, the smaller errors
will be if the thread is not exactly ten centimeters in
length. Polyester thread is not recommended for use
in the bomb because it has a tendency to melt and
fall away from the heating wire before it ignites.
Using the fine thread mentioned above, the fuse
correction for the calorimeter would be the 10
calories from electrical heating plus 12 calories from
the burning thread for a total of 22 calories per test.
The thread supplied by Parr has a mass of approximately 1 milligram per centimeter. This results in a
total fuse correction of 50 calories.
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
6200 Calorimeter uses the most recent, published values for all thermochemical data.
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6200
Calculations
B
Thermochemical Calculation Details
Traditionally, standard solutions and procedures
have been established to simplify the calculations
related to the thermochemical corrections. The 6200
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.
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).
Acid Correction:
In the 6200 there are a number of settings for the
acid correction.
e1 is the nitric acid portion of the correction.
Fixed HNO3: The Acid Correction is a fixed value set
by the operator.
The calculation is:
e1 = (nitric acid value)(acid multiplier)(heat of
formation of nitric acid)
For an 1108P style bomb, the default nitric acid value
is 10 and acid multiplier is .0709. The heat of forma-
tion of nitric acid is 14.1 calories/milliequivalent so
the calculation is:
e1 = (10)(.0709)(14.1) or e1 = 9.9969 (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 nitric acid is 14.1 calories/
milliequivalent.
• 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).
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 fixed value set by the operator.
The calculation is:
e1 = [((total acid)(acid multiplier)) – (% sulfur)
(sample mass)(sulfur multiplier)](heat of
formation of nitric acid)
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B
Calculations
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:
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 filling 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.
Users may find it convenient to enter a fixed
value for the acid correction and avoid the need
to determine this correction for each test. Use of a
fixed value for the acid correction is highly recommended. 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 fixed nitric acid value. For
most work, it is recommended to set “Acid Value is
Nitric Acid Only”, in Calculation Factors to ON. Total
errors of more than 3 calories will seldom occur
when using fixed 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 fixed value of 0.0 to all standardization tests.
Benzoic acid contains no sulfur.
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 calorimetric procedures. However, the sum of e1 and e2,
above, is equal to the sum of the ASTM treatment of
e1 and e2.
Table B-1
Settings for ISO & BSI Methods
PageLineSetting Value
Thermochemical
Corrections
Calculations
Factors
Acid Correction (STD)Entered
HNO
Fixed Sulfur STDOff7
Acid Correction (DET)Entered
HNO
Fixed Sulfur DETOff7
Acid Multiplier0.154
Sulfur Value is Percent Off
Sulfur Multiplier0.1
Use Offset CorrectionOn
Offset Value-43.5
13
3
13
3
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Calculations
B
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.
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 6200 Controller for
dealing with these different procedures.
The analysis of bomb washings in these methods
call for a titration, first 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 fixed acid and sulfur, which are used
in preliminary reports, will reflect a sulfur correction
of 0, and a nitric acid correction of 10 calories.
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B
Calculations
Spiking Samples
It is sometimes necessary to add a spiking material
to samples which are very small, have a low heat of
combustion, or have a high moisture content to add
sufficient heat to drive the combustion to completion. Benzoic acid is an excellent material for spiking
for all of the same reasons it is a good standard
material. White oil is also an excellent material,
particularly for liquid samples. The 6200 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)
Ms=Mass of spiking material
This factor is added to the calculations when Spike
Controls, Use Spiking is set to ON. Heat of Combustion of Spike is entered as calories per gram. The
controller will prompt the user to enter the weight
of spiking material. Fixed spikes can be used when,
Use Fixed Spike is set to ON and entering the mass
of the spike on - Weight of Fixed Spike.
WT - e1 - e2 - e3 - (Hcs)(Ms)
m
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 airdried 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 calculations. If the percentage of hydrogen H, in the sample
is known, the net heat of combustion, H
pound can be calculated as follows:
Btu per
net
H
To calculate H
D5865.
=
net
(Liquid fuels, ASTM D240)
1.8Hc - 91.23H
for solid fuels please refer to ASTM
net
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6200
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
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.
C
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.
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 Parr 2811
Pellet Press.
Automatic Statistical Calculations
The 6200 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 6200 Calorimeter automatically determines and
uses (by default) 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 alues. 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 choose 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 Protect EE Value.
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C
Standardization
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 0.10%.
Control limits based on 99% confidence (3 sigma) values.
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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6200
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 0.10%.
Control limits based on 99% confidence (3 sigma) values.
The 6200 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 6200 Calorimeter are
set up for use with the Parr 1758 Printer.
Balance and Port Input Driver Specifications
The 6200 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.
FieldLength
ID2
space1
data9
space1
g1
CR1
LF1
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
FieldLength
polarity1
space1
data8
space1
stability2
CR1
LF1
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 contain either a “+” or a
space. Leading zeros in the data field are blanked,
except for the one to the left of the decimal point.
The stability field 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.
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D
Communications Interfaces
Generic Interface
FieldLength
data9
CR1
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.
Table D-1
6200 Data File Naming Convention
Test data files are named with the following convention.
Test TypeFilename
Preliminary Standardization
Final Standardization<ID>.std.finl.csv
Preliminary Determination<ID>.det.plim.csv
Final Determination<ID>.det.finl.csv
Pre-weigh<ID>.---.pwgh.csv
<ID>.std.plim.csv
Table D-2
6200 Calorimeter Run Data Template
FieldDescription
SampleIDchar[16]
TimestampMM/DD/YY HH:mm:ss
Mode0 = determination, 1 = standardization
Method0 = equilibrium, 1 = dynamic
State0 = preweigh, 1 = preliminary, 2 = final
Units0 = 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]
BombEEbomb energy equivalent
SampleWtsample weight
SpikeWtspike weight
Fusefuse value
FuseFinalfuse value is final
Acidacid value
AcidFinalacid value is final
Sulfursulfur value
SulfurFinalsulfur value is final
Hydrogenhydrogen value (net calc option)
HydrogenFinalhydrogen value is final (net calc op-
tion)
MADmoisture as determined value (dry
calc option)
MAD Finalmoisture as determined is final
JacketTempjacket temperature
InitTempinitial temperature
DeltaTtemperature rise
HOCgross heat of combustion
NetHOCdry net HOC (net calc options enabled)
DryHOCdry gross HOC (if dry calc option
enabled)
DryNetHOCdry net HOC (if both dry and net calc
options enabled)
Oxygenoxygen value (net calc option)
Oxygen Finaloxygen value is final
Nitrogennitrogen value (net calc option)
Nitrogen Finalnitrogen value is final
MARmoisture as received (dry calc option)
MAR Finalmoisture as received value is final
Dry Net HOC_ARDry net HOC as received value (if both
dry and net calc option enabled)
Bomb Namebomb name assigned to bomb ID
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Communications Interfaces
D
Ethernet 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 Configuration Protocol) server provides this address shortly after the
calorimeter is turned on or a static IP address can be
assigned. 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.
An FTP enabled web browser can be used to access
stored test data. The URL is of the following form.
In this case, 192.168.0.125 is the IP address of the
calorimeter.
www.parrinst.com
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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 defined in IETF RFC1001
and RFC1002.
The Samba server feature option in the Parr 6200
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 calorimeter or
To access the test data open the run data folder. To access the log file open the log data folder.
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://10.1.5.10
Where 10.1.5.10 is the IP address of the calorimeter. The following screenshot illustrates the calorimeter home page.
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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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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 Services
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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aPPendix e
Technical Service
Should you need assistance in the operation or service of your instrument, please contact the Technical
Service Department.
Technical Service
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.
Any correspondence must include the following
basic information:
The model and serial # of the instrument.
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.
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.
244VBUnion Bulkhead, 1/8 Tube
A476A3Slip Connector w / 1/8 NPT
438VBElbow, 45 °, 1/8 NPT x 1/8 Tube
HX0012TB024High Pressure Tube, 1/8, Nylon
180VBMale Elbow 1/8 T x 1/8 NPTM
527VBRestrictor 0.012 – 1/8 NPT
A1278DDOxygen Solenoid Assembly
697HC2Filter Sintered Bronze
243VB2Male Connector, 1/8 T x 1/8 NPT
394HCJEO-Ring EP 3/8 ID X 1/16 CS