6200
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Operating Instruction Manual
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No. 442M
6200
Oxygen Bomb Calorimete
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6200Calorimeter O
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TABLE OF CONTENTS
Preface I
Scope............................................................................................................I
Explanation of Symbols.................................................................................II
Safety Information.........................................................................................II
Intended Usage.............................................................................................III
Cleaning & Maintenance...............................................................................III
General Specifications..................................................................................III
Environmental Conditions.............................................................................III
Provisions for Lifting and Carrying................................................................III
Getting Started..............................................................................................IV
Concept of Operation 1-1
Overview..................................................................................................... 1-1
Dynamic Operation ..................................................................................... 1-2
Full Microprocessor Based Process Control............................................... 1-2
Full Microprocessor Based Data Acquisition and Handling......................... 1-2
Flexible Programming ................................................................................. 1-2
Installation 2-1
Filling the Jacket Reservoir......................................................................... 2-1
Power Connection....................................................................................... 2-1
Jacket Cooling Water Connection............................................................... 2-1
Oxygen Filling Connection.......................................................................... 2-2
Printer and Balance Connections................................................................ 2-2
Swagelock Tube Fittings............................................................................. 2-3
Retightening Swagelock Tube Fittings........................................................ 2-3
6200 External Plumbing.............................................................................. 2-5
Standardizing the Calorimeter..................................................................... 2-7
Instrument Description 3-1
Types of Controls........................................................................................ 3-1
Menu Keys.................................................................................................. 3-1
Control Keys................................................................................................ 3-1
Program Installation & Control 4-1
Software Installation.................................................................................... 4-1
Default Settings........................................................................................... 4-1
Revising Default Settings............................................................................ 4-2
Factory Default Settings.............................................................................. 4-3
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Operating Instructions 5-1
Operating the 1108 Oxygen Bomb.............................................................. 5-1
Operating the Filling Connection................................................................. 5-1
Operating the Calorimeter........................................................................... 5-2
Samples and Sample Holders..................................................................... 5-5
Combustion Aids......................................................................................... 5-5
Oxygen Charging Pressure......................................................................... 5-5
Combustion Capsules................................................................................. 5-6
Foodstuffs and Cellulosic Materials ............................................................ 5-6
Coarse Samples.......................................................................................... 5-6
Corrosive Samples...................................................................................... 5-7
Explosives and High Energy Fuels ............................................................. 5-7
Volatile Sample Holders.............................................................................. 5-7
Poor Combustion ........................................................................................ 5-8
Corrections & Final Reports 6-1
Entering Corrections and Obtaining the Final Report ................................. 6-1
Manual Entry............................................................................................... 6-1
Fixed Corrections........................................................................................ 6-1
Reporting Instructions 7-1
Report Option Selection.............................................................................. 7-1
Report Generation....................................................................................... 7-1
File Management 8-1
Clearing Memory......................................................................................... 8-1
Removable Compact Flash Memory........................................................... 8-1
Maintenance & Troubleshooting 9-1
Oxygen Bomb ............................................................................................. 9-1
Jacket Temperature Troubleshooting ......................................................... 9-1
Fuses .......................................................................................................... 9-1
6200 Calorimeter Error List......................................................................... 9-2
Appendix A - Menu Operating Instructions A-1
Calorimeter Operation Menu....................................................................... A-1
Temperature vs. Time Plot Screen ............................................................. A-2
Temperature Plot Setup Menu.................................................................... A-2
Operating Controls Menu............................................................................ A-4
Program Information and Control Menu...................................................... A-5
Calibration and Data Controls Menu........................................................... A-6
Thermochemical Calculations Menu........................................................... A-8
Data Entry Controls Menu........................................................................... A-10
Reporting Controls Menu............................................................................ A-11
Communication Controls Menu.................................................................. A-12
File Management Menu ............................................................................. A-14
Diagnostics Menu....................................................................................... A-15
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TABLE OF CONTENTS
Appendix B – Calculations B-1
Calculating the Heat of Combustion............................................................ B-1
General Calculations................................................................................... B-1
Appendix C- Standardization C-1
Appendix D - Communication Interfaces D-1
Appendix E - Technical Service E-1
Appendix F – 6200 Calorimeter Parts & Diagrams F-1
Thermochemical Corrections...................................................................... B-2
ASTM and ISO Methods Differ.................................................................... B-3
Acid and Sulfur Corrections ........................................................................ B-4
ASTM Treatment for Acid and Sulfur .......................................................... B-6
ISO Calculations ......................................................................................... B-6
Spiking Samples ......................................................................................... B-7
Conversion to Other Moisture Bases .......................................................... B-7
Conversion to Net Heat of Combustion....................................................... B-7
Standardizing the Calorimeter..................................................................... C-1
Standard Materials...................................................................................... C-1
Automatic Statistical Calculations............................................................... C-2
Printer Port.................................................................................................. D-1
Balance Port................................................................................................ D-1
Mettler 011/012 Balance Interface.............................................................. D-1
Sartorius Balance Interface......................................................................... D-2
Generic Interface......................................................................................... D-3
Run Date Template..................................................................................... D-4
Ethernet Interface........................................................................................ D-5
Bar Code Port ............................................................................................. D-10
Network Data Devices................................................................................. D-10
Return for Repair......................................................................................... E-1
Principal Assemblies in Calorimeter............................................................ F-1
Parts List for A1279DD Controller Assembly .............................................. F-1
Parts List for Temperature Control Assembly ............................................. F-2
Parts List for A1284DD2 Stirrer Hub Assembly .......................................... F-2
Spare and Installation Parts List ................................................................. F-2
Parts List for Water Tank Assembly............................................................ F-3
Parts List for Cooling Water Supply............................................................ F-3
Parts List for Oxygen Filling System........................................................... F-3
Parts List for 6200 Stirrer Motor and Drive.................................................. F-3
F-1 6200 Oxygen Bomb Calorimeter Cutaway Front ............................. F-4
F-2 6200 Oxygen Bomb Calorimeter Cutaway Rear.............................. F-5
F-3 A1279DD Control Schematic........................................................... F-6
F-4 Oxygen Solenoid Assembly............................................................. F-7
F-5 Water Tank Assembly...................................................................... F-8
F-6 A1311DD Circulating Pump Assembly ............................................ F-9
F-7 Temperature Control Assembly.......................................................F-10
F-8 A1284DD2 Stirrer Hub Assembly ....................................................F-11
F-9 Stirrer Motor Assembly ....................................................................F-12
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Figures
2-1 6200 Calorimeter Back Panel ........................................................... 2-4
2-2 Closed Loop Configuration with 6510............................................... 2-5
2-3 Closed Loop Configuration with 1563............................................... 2-5
2-4 Open Loop Configuration with Tap Water......................................... 2-6
2-5 Open Loop Configuration with 1552 ................................................. 2-6
4-1 6200 Factory Default Settings........................................................... 4-3
5-7 Combustion Capsule with Adhesive Tape Seal............................... 5-7
F-1 6200 Oxygen Bomb Calorimeter Cutaway Front ............................. F-4
F-2 6200 Oxygen Bomb Calorimeter Cutaway Rear.............................. F-5
F-3 A1279DD Control Schematic........................................................... F-6
F-4 Oxygen Solenoid Assembly............................................................. F-7
F-5 Water Tank Assembly...................................................................... F-8
F-6 A1311DD Circulating Pump Assembly ............................................ F-9
F-7 Temperature Control Assembly.......................................................F-10
F-8 A1284DD2 Stirrer Hub Assembly ....................................................F-11
F-9 Stirrer Motor Assembly ....................................................................F-12
Tables
B-1 Settings for ISO & BSI Methods......................................................... B-5
C-1 Calorimeter Control Limits.................................................................. C-2
D-1 6200 Calorimeter Serial Ports Pin-Out............................................... D-3
D-2 Calorimeter Run Data Template......................................................... D-4
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6200Calorimeter O
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PREFACE
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
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.
Customer Service:
Questions concerning
the installation or
operation of this
instrument can be
answered by the
Parr Customer Service
Department:
309-762-7716
800-872-7720
Fax: 309-762-9453
www.parrinst.com
parr@parrinst.com
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
201M Limited Warranty
483M Introduction to Bomb
Calorimetry
205M 1108 Oxygen Combustion
Bomb
207M Analytical Methods for
Oxygen Bombs
230M Safety Precautions
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.
Note:
The unit of heat used in
this manual is the
international calorie,
which is equal to 4.1868
absolute joules
.
Scope
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PREFACE
Explanation of Symbols
6200Calorimeter O
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I
O
~
On position
Off position
Alternating Current (AC)
This CAUTION symbol may be present on
the Product Instrumentation and literature.
If present on the product, the user must
consult the appropriate part of the
accompanying product literature for more
information.
ATTENTION, Electrostatic Discharge
(ESD) hazards. Observe precautions for
handling electrostatic sensitive devices.
Protective Earth (PE) terminal. Provided
for connection of the protective 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. NOTE: This connection shall
be bonded to Protective earth at the
source of supply in accordance with
national and local electrical code
requirements.
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6200Calorimeter O
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PREFACE
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.
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.
General Specifications
Electrical Ratings
120VAC, 6.0 Amps. 50/60 Hz
240VAC, 3.0 Amps, 50/60 Hz
Before connecting the calorimeter to an
electrical outlet, the user must be certain
that the electrical outlet has an earth ground
connection and that the line, load and other
characteristics of the installation do not
exceed the following limits:
Voltage: Fluctuations in the line voltage
should not exceed 10% of the rated nominal
voltage shown on the data plate.
Frequency: Calorimeters can be operated
from either a 50 or 60 Hertz power supply
without affecting their operation or
calibration.
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: 15ºC to 30ºC; maximum relative
humidity of 80% non-condensing.
Installation Category II (overvoltage)
in accordance with IEC 664.
Pollution degree 2 in accordance
with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25ºC and 65ºC; 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.
III
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6200Calorimeter O
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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 the Installation
Instructions, Chapter 2. This simple,
step-wise procedure will acquaint the
user with the various parts of the
calorimeter and make it easier to
understand the operating instructions
which follow.
3. Turn the power switch ON (located on
the back). Turn to the Instrument
Description, Chapter 3, to review the
touch screen controls.
4. Review the Program Installation and
Control, Chapter 4, to match the factory
settings to the intended mode of
operation. Any required changes can be
made to the program parameters located
in the Main Menu.
5. Review the Reporting Instructions,
Chapter 7, to become familiar with the
manner in which calorimetry corrections
are entered. Also discussed are
generating final reports, editing and
clearing memory.
6. Turn to the Menu Operating Instructions,
Appendix 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 provides 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 Interfacing,
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.
IV
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1 CONCEPT OF OPERATION
The 6200 Calorimeter has been
designed to provide the user with:
• 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
communications 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 1108 oxygen bomb. More than 20,000
of these reliable oxygen combustion bombs
have been placed in service on a world wide
basis. This bomb features an automatic
inlet check valve and an adjustable
needle valve for controlled release
of residual gasses following
combustion. They are intended for
samples ranging from 0.6 to 1.2
grams with a maximum energy
release of 8000 calories per charge.
The 1108 oxygen bomb is made of highstrength, high nickel stainless steel
designed to resist the corrosive acids
produced in routine fuel testing. An
alternative 1108CL bomb is available,
constructed of an alloy containing additional
cobalt and molybdenum to resist the
corrosive conditions produced when burning
samples containing chlorinated compounds.
The Model 6200 can also be equipped
with a variety of special purpose oxygen
bombs for unusual samples and/or
applications. The 1104 high strength
oxygen bomb is designed for testing
explosives and other potentially hazardous
materials. The 1109/1109A semimicro
oxygen bombs 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.
Overview
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1
Dynamic
Operation
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.
Full Microprocessor
Based
Process
Control
A. Generate all temperature readings in
B. Monitor jacket as well as bucket
C. Confirm equilibrium conditions.
D. Fire the bomb.
E. Confirm that ignition has occurred.
Full Microprocessor
Based Data
Acquisition
and Handling
Flexible
ramming
Pro
user to customize the operation of the
calorimeter to meet a wide variety of operating
conditions including:
A. A large selection of printing options.
B. Choice of accessories and peripheral
C. Multiple options in regard to handling
D. Choice of ASTM or ISO correction
E. A variety of memory management and
F. Complete freedom for
In its Dynamic Operating Mode,
the calorimeter uses a sophisticated
The microprocessor controller in
this calorimeter has been
preprogrammed to automatically
prompt the user for all required data
and control input and to:
the calorimeter.
temperature.
In addition to its process
control functions, the
microprocessor in the
calorimeter has been
preprogrammed to:
The fifth generation software
built into this calorimeter and
accessed through the screen menus
permit the
equipment.
thermochemical corrections.
procedures.
reporting procedures.
reagent concentrations and
calculations.
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.
F. Determine and apply all necessary
heat leak corrections.
G. Perform all curve matching and
extrapolations required for dynamic
operation.
H. Terminate the test when it is
complete.
I. Monitor the conditions within the
calorimeter and report to the user
whenever a sensor or operating
condition is out of normal ranges.
A. Collect and store all required
test data.
B. Apply all required corrections for
combustion characteristics.
C. Compute and report the heat of
combustion for the sample.
G. Unlimited choice of reporting
units.
H. Automatic bomb usage
monitoring and reporting.
I. A choice of Equilibrium or
Dynamic test methods.
J. Automatic statistical treatment of
calibration runs.
K. Enhanced testing and trouble
shooting procedure.
The 6200 Calorimeter is equipped with
two RS232C connections for direct
communication with its printer and an
attached balance. It is also equipped with
an Ethernet network connection for
connections to laboratory computers.
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2 INSTALLATION
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.
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
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.
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 water handling system.
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.
This apparatus is to be used indoors. It
requires at least 4 square feet of workspace
on a sturdy bench or table in a well-ventilated
area with convenient access to an electric
outlet, running water and a drain. The supply
voltage must be within ± 10% of marked
nominal voltage on the apparatus. The supply
voltage receptacle must have an earth ground
connection.
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.
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.
Filling the
Reservoi
Connection
Tap Water Cooling
Connect the tap water supply
to the cold water inlet on the back
of the calorimeter using either ¼”
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 flow rate of 100 ml / minute is generally all
that is required.
Connection
13
Jacket
Powe
Jacket
Cooling
Wate
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Jacket
Cooling
Water
Connection
Continued
calorimeter will not be used for an extended
period.
Oxygen
Filling
Connection
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 back of the calorimeter.
Printer and
Balance
Connections
Connect the cooling water outlet
on the back of the calorimeter to a
drain using either nylon
(HJ0025TB035) or copper ¼” tubing.
A shut off valve in tap water supply
line is also a good idea if the
The 6200 Calorimeter is
equipped with an automatic bomb
oxygen filling system. This system
Connect the printer to the
calorimeter at this time. The Parr
1757 Printer is configured and
furnished with a cord to connect
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.
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 O
without a charge and attach the filling hose
to the bomb inlet valve. Press the O
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.
directly to the RS232C printer port on the
back of the calorimeter.
The balance port connection, if used,
should be made at this.
. Assemble the oxygen bomb
2
fill key
2
2-2
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2
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
fittings, tighten the Swagelok nut
3/4 turns from finger-tight.
Swagelok tubing connections can be
disconnected and retightened many times.
The same reliable leak-proof seal can be
obtained every time the connection is
remade using the simple two-step
procedure.
1. Insert the tubing with pre-swaged ferrules
into the fitting body until the front ferrule
seats.
2. Tighten the nut by hand. Rotate the nut to
the 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
6200Calorimeter O
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.
erating Instruction Manual
Retightening
Tube Fittings
Swagelok
Tube
Fittings
Swagelok
2-3
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6200 Calorimeter Back Panel
Figure 2-1
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Line 1 & 2 – Maximum length of 10 feet
-¼” OD, Polyurethane (Part Number HJ0025TB035)
Line 3 - Maximum length of 25 feet
1
-
/8” OD, Nylon (Part Number HX0012TB024)
Closed Loop Configurations
Figure 2-2
6200
Calorimete
Externa
Plumbin
Figure 2-3
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Open Loop Configurations
Figure 2-4
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Figure 2-5
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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 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.
Standardizing
the Calorimete
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3 INSTRUMENT DESCRIPTION
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.
Note:
Keys with a “double box” in the upper
left hand corner lead to sub-menus.
The controls that change the data field
information in the menus will be one of the
following:
1. Toggles. These data fields 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.
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 pad or similar screen for entering
the required value.
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.
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.
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.
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.
Menu Keys
Control Keys
Types of
Controls
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4 PROGRAM INSTALLATION & CONTROL
Software
Installation
Default
Settings
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.
Units are preprogrammed with
default settings. See pages 4-3 and
4-4 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.
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.
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
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.
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 Program Info and Control Page,
User/Factory Settings, Re-load User Default
Settings, and YES.
Revising
Default
Settings
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Factory Default
Settings
Calorimeter Operation
Operating Mode Determination
Bomb Installed/EE 1/2400.0
Heater and Pump OFF
Operating Controls
Method of Operation Dynamic
Reporting Units Btu/lb
Use Spiking Correction OFF
“OTHER” Multiplier 4.1868
Calibrate Touchscreen
LCD Backlight Timeout(s) 1200 S
LCD Contrast 30%
Print Error Messages ON
Language English
Spike Controls
Use Spiking OFF
Heat of Combustion of Spike 6318.4
Use Fixed Spike OFF
Weight of Fixed Spike 0.0
Prompt for Spike before Weight OFF
Program Info and Control
Date XX/XX/XXXX
Time XX:XX
Software and Hardware Info
Settings Protect OFF
User/Factory Settings
Feature Key
Bomb Type Select
User Function Setup
Cold Restart
User / Factory Settings
User Setup ID 00000001
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Figure 4- 1
6200 Factory Default Settings
Calibration Data & Control
Calibration Run Limit 10
EE Max Std Deviation 0.0
Heat of Combustion
of Standard 6318.4
Bomb Service Interval 500
Use Bomb 1
Bomb 1 Through 4
EE Value 2400.0
Protected EE Value OFF
Thermochemical Corrections
Standardization
Fixed Fuse Correction ON 15.0
Fixed Acid Correction ON 10.0
Fixed Sulfur Correction ON 0.0
Determination
Fixed Fuse Correction ON 15.0
Fixed Acid Correction ON 10.0
Fixed Sulfur Correction OFF 0.0
Calculate Net Heat of Combustion OFF
Calculation Factors
Acid Value is Nitric Acid Only ON
Acid Multiplier 0.0709
Sulfur Value is Percent ON
Sulfur Multiplier 0.6238
Fuse Multiplier 1.0
Use Offset Correction (ISO) OFF
Offset Value 0.0
Fixed Hydrogen OFF 0.0
Hydrogen Multiplier 50.68
Dry Calculation OFF
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Data Entry Controls
Prompt for Bomb ID ON
Weight Entry Mode Touch Screen
Acid Entry Mode Touch Screen
Hydrogen Entry Mode Touch Screen
Auto Sample ID Controls ON
Sample Weight Warning above 2.0
Spike Weight Entry Mode Touch Screen
Sulfur Entry Mode Touch Screen
Moisture Entry Mode Touch Screen
Auto Preweigh Controls ON
Auto Sample ID Controls
Automatic Sample ID ON
Automatic Sample ID Increment 1
Automatic Sample ID Number 1
Auto Preweigh Controls
Automatic Preweigh ID ON
Automatic Preweigh ID Increment 1
Automatic Preweigh ID Number 1
Reporting Controls
Report Width 40
Automatic Reporting ON
Auto Report Destination Printer
Individual Printed Reports OFF
Edit Final Reports OFF
Recalculate Final Reports OFF
Use New EE Values
in Recalculation OFF
Communication Controls
Printer Port (RS232)
Balance Port (RS232)
Network Interface
Printer Destination Local (RS232)
Bar Code Port (RS232)
Network Data Devices
Printer Port Communications
Number of Data Bits 8
Parity None
Number of Stop Bits 1
Handshaking Xon/Xoff
Baud Rate 9600
Printer Type Parr 1757
Balance Port Communications
Balance Type Custom
Customize Balance Settings
Balance Port Settings
Number of Data Bits 8
Parity None
Number of Stop Bits 1
Handshaking None
Baud Rate 9600
Data Characters from Balance 8
Data Precision 4
Transfer Timeout (seconds) 10
Balance Handler Strings
Data Logger
Data Logger OFF
Data Log Interval 12s
Data Log DestinationLog File and Printer
Select Data Log Items
Data Log Format Text Format
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5 OPERATING INSTRUCTIONS
Operating the
1108 Oxygen
Bomb
Operating
the Filling
Connection
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,
Detailed Instructions for
preparing the sample and charging
the 1108 Oxygen Bomb are given
in Operating Instructions No.
To fill the bomb, connect the
hose to the bomb inlet valve and
push the O2 button on the
205M. Follow these instructions carefully,
giving particular attention to the precautions
to be observed in charging and handling the
bomb.
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).
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All operations required to standardize
the 6200 Calorimeter, or test an unknown
sample, should proceed step-wise in the
following manner:
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 10 minutes, the
calorimeter is ready to begin testing.
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
Connection. 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.
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.
Operating the
Calorimete
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Operating the
Calorimeter
Continued
5. Close the calorimeter cover. This
6. Select determination or
7. The calorimeter will now take over
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 in the water. Handle the
bomb carefully during this operation
so that the sample will not be
disturbed. Push the two ignition lead
wires into the terminal sockets on
the bomb head. Orient the wires
away from the stirrer shaft so they
do not become tangled in the stirring
mechanism. Lower the bomb
completely into water with its feet
spanning the circular boss in the
bottom of the bucket. Remove the
lifting handle and shake any drops of
water back into the bucket and
check for gas bubbles.
lowers the stirrer and thermistor
probe into the bucket.
standardization as appropriate on
the Calorimeter Operation menu by
toggling the operating mode key.
After pressing the start key, the
calorimeter will now prompt the
operator for Bomb ID number,
sample ID number, sample weight
and spike weight in accordance with
the instructions set into the operating
controls page.
and conduct the test. During the
time it is establishing the initial
equilibrium, it will display
PREPERIOD on 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.
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10. Remove all unburned pieces of fuse
wire from the bomb electrodes;
straighten them and measure their
combined length in centimeters.
Subtract this length from the initial
length of 10 centimeters and multiply
this burned length by 2.3 calories
per cm (for Parr 45C10 Fuse Wire)
to obtain the fuse correction. The
scale on the fuse wire card can be
used to obtain this value directly.
11. 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.
12. Analyze the bomb washings to
determine the sulfur content of the
sample if it exceeds 0.1%.
for determining sulfur are discussed
in Operating Instructions No. 207M.
13. At the end of the testing period, turn
OFF the calorimeter at the power
switch.
Methods
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