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NO. 586M
Parr Instrument Company
6300
Oxygen Bomb Calorimeter
Operating Instruction Manual
For models produced after October 2010
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6300
TABLE OF CONTENTS
PREFACE — 7
Scope — 7
Explanation of Symbols — 8
Safety Information — 8
Intended Usage — 8
Cleaning & Maintenance — 8
General Specifications — 9
Environmental Conditions — 9
Getting Started — 9
CHAPTER 1
ONCEPT OF OPERATION — 11
C
A Highly Automated Procedure — 11
New Convenience and New Technology — 11
Isoperibol Operation — 11
Dynamic Operation — 11
Full Microprocessor Based Process Control — 12
Full Microprocessor Based Data Acquisition and
Handling — 12
Flexible Programming — 12
CHAPTER 2
NSTALLATION — 13
I
Required Consumables, Utilities and Power
Requirements — 13
Installing the Calorimeter — 13
6300 Calorimeter External Plumbing — 17
Combustion Aids — 35
Oxygen Charging Pressure — 35
Combustion Capsules — 35
Foodstuffs and Cellulosic Materials — 36
Coarse Samples — 36
Corrosive Samples — 36
Explosives and High Energy Fuels — 36
Volatile Sample Holders — 36
Poor Combustion — 37
CHAPTER 6
ORRECTIONS & FINAL REPORTS — 39
C
Entering Corrections and Obtaining the Final Report — 39
Manual Entry — 39
Fixed Corrections — 39
CHAPTER 7
EPORTING INSTRUCTIONS — 41
R
Report Option Section — 41
Report Generation — 41
Net Heat of Combustion — 42
CHAPTER 8
ILE MANAGEMENT — 43
F
Clearing Memory — 43
Removable SD Memory — 43
CHAPTER 3
NSTRUMENT DESCRIPTION — 21
I
Types of Controls — 21
Menu Keys — 21
Control Keys — 21
CHAPTER 4
ROGRAM INSTALLATION & CONTROL — 23
P
Software Installation — 23
Default Settings — 23
Revising Default Settings — 23
CHAPTER 5
PERATING INSTRUCTIONS — 27
O
To Begin a Test — 27
Operating the Oxygen Bomb — 27
Allowable Sample Size — 29
Attaching the Cotton Thread — 29
Closing the Bomb — 31
Fill Cycle — 31
Pre-Period — 31
Bomb Firing — 31
Post-Period — 33
Cool/Rinse — 33
Drain — 33
Samples — 35
CHAPTER 9
AINTENANCE & TROUBLESHOOTING — 45
M
Routine Maintenance — 45
6300 Maintenance Checklist — 47
Inspection of Critical Sealing Surfaces — 48
Bomb Exhaust Troubleshooting — 48
Jacket Fill and Cooling Problems — 50
Bomb Removal and Replacement — 51
6300 Calorimeter Error List — 51
APPENDIX A
ENU OPERATING INSTRUCTIONS — 53
M
Main Menu — 53
Calorimeter Operation Menu — 53
Temperature vs. Time Plot — 54
Temperature Plot Setup Menu — 54
Operating Controls Menu — 55
Program Information and Control Menu — 57
Calibration and Data Controls Menu — 58
Thermochemical Calculations Menu — 60
Calculation Factors Menu — 62
Net Heat/Dry Heat Factors — 63
Data Entry Controls Menu — 63
Reporting Controls Menu — 65
Communication Controls Menu — 66
File Management — 67
Run Data File Manager — 68
Diagnostics Menu — 68
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TABLE OF CONTENTS
APPENDIX B
ALCULATIONS — 71
C
Calculating the Heat of Combustion — 71
General Calculations — 71
Thermochemical Corrections — 71
Fuse Correction — 73
Acid and Sulfur Corrections — 73
ASTM Treatment for Acid and Sulfur — 74
ISO Calculations — 75
Spiking Samples — 75
Conversion to Net Heat of Combustion — 75
APPENDIX C
TANDARDIZATION — 77
S
Standardizing the Calorimeter — 77
Standard Materials — 77
Automatic Statistical Calculations — 77
APPENDIX D
OMMUNICATIONS INTERFACES — 81
C
USB Port — 81
Balance and Port Input Driver Specifications — 81
Mettler 011/012 Balance Interface — 81
Sartorius Balance Interface — 81
Generic Interface — 82
Ethernet Interface — 83
Samba Server Feature (Optional) — 84
Bar Code Port — 92
Network Data Services — 92
APPENDIX E
ECHNICAL SERVICE — 93
T
Return for Repair — 93
APPENDIX F
ARTS LISTS & DRAWINGS — 95
P
Principal Assemblies in Calorimeter — 95
A1250DD2 Controller Assembly — 96
A1251DD Oxygen Solenoid Assembly — 96
A1252DD Water Solenoid Assembly — 96
A1257DD Water Regulator Assembly — 97
A1258DD Temperature Control Assembly — 97
A1260DD Water Level Assembly — 97
A1264DD Air Can Assembly — 98
A1267DD Accessory/Installation Kit — 99
A1265DD Bucket and Stirrer Tube Assembly — 99
6300 Stirrer Motor and Drive — 100
A1255DD Bucket Stirrer Assembly — 100
A1266DD Cover Assembly — 100
6309B Spare Parts Kit — 101
1136 and 1136CL Oxygen Bomb — 103
1138 and 1138CL Oxygen Bomb — 105
APPENDIX G
OMB RINSE CONTAINER ASSEMBLY — 127
B
Overview — 127
Concept of Operation — 127
Connection — 127
Operation — 127
TABLES
Table B-1
Settings for ISO & BSI Methods — 74
Table C-1
Calorimeter Control Limit Values in J/g When
Benzoic Acid is Used as a Test Sample — 78
Table C-2
Calorimeter Control Limit Values in cal/g When
Benzoic Acid is Used as a Test Sample — 79
Table C-3
Calorimeter Control Limit Values in BTU/lb When
Benzoic Acid is Used as a Test Sample — 80
Table D-1
6300 Data File Naming Convention — 82
Table D-2
6300 Calorimeter Run Data Template — 82
FIGURES
Figure 2-1
Swagelok Tube Fittings — 15
Figure 2-2
6300 Calorimeter Back Panel — 16
Figure 2-3
Closed Loop Configuration with 6520A — 17
Figure 2-4
Closed Loop Configuration with 1564 — 17
Figure 2-5
Open Loop Configuration with 1552 — 18
Figure 2-6
Open Loop Configuration — 18
Figure 4-1
6300 Factory Default Settings — 24
Figure 5-1
Fill Flow Diagram — 28
Figure 5-2
Cotton Thread Assembly — 29
Figure 5-3
Pre-period/Post-period — 30
Figure 5-4
Rinse & Cool Flow Diagram — 32
Figure 5-5
Drain Flow Diagram — 34
Figure 5-6
Combustion Capsule with Adhesive Tape Seal — 37
Figure F-1
Parts Diagram for the 1136 and 1136CL Oxygen
Bombs — 102
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FIGURES (CONTINUED)
Figure F-2
Parts Diagram for the 1138 and 1138CL Oxygen
Bombs — 104
Figure F-3
6300 Oxygen Bomb Calorimeter Cutaway Right —
106
Figure F-4
6300 Oxygen Bomb Calorimeter Cutaway Left —
107
Figure F-5
6300 Oxygen Bomb Calorimeter Cover Open — 108
Figure F-6
A1250DD2 Control Schematic — 109
Figure F-7
A1251DD Oxygen Solenoid Assembly — 110
Figure F-8
A1200DD Internal Plumbing Diagram — 111
Figure F-9
A1252DD Water Solenoid Assembly — 112
Figure F-10
A1416DD Bomb Wash Pump Assembly and Fittings
— 113
Figure F-11
A1254DD Circulatory Pump Assembly — 114
Figure F-12
A1255DD Bucket Stirrer Assembly — 115
Figure F-13
A1256DD Water Assembly Tank — 116
Figure F-14
A1257DD Water Regulator Assembly — 117
Figure F-15
A1258DD Temperature Control Assembly — 118
Figure F-16
Cover Contact Pin Assembly — 119
Figure F-17
Stirrer Motor and Mount — 120
Figure F-18
A1260DD Water Level Control Assembly — 121
Figure F-19
A1265DD Bucket Assembly — 122
Figure F-20
6300 Air Can Assembly — 123
Figure F-21
A1450DD Bomb Head Assembly (1) — 124
Figure F-22
A1450DD Bomb Head Assembly (2) — 125
Figure G-1
Vessel Rinse Container — 128
TABLE OF CONTENTS
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PREFACE
PREFACE
SCOPE
This manual contains instructions for installing and
operating the Parr 6300 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.
No. Description
201M
207M
230M
483M
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
Table (IT) calorie, which is equal to 4.1868 absolute
joules.
Limited Warranty
Analytical Methods for Oxygen Bombs
Safety in the Operation of Laboratory and
Pressure Vessels
Introduction to Bomb Calorimetry
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.
Additional instructions concerning the installation and
operation of various component parts and peripheral
items used with the 6300 Calorimeter have been
included and made a part of these instructions.
Customer Service:
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
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PREFACE
EXPLANATION OF SYMBOLS
I On Position
O 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. 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:
Use a properly grounded electrical outlet of correct 1.
voltage and current handling capability.
Ensure that the equipment is connected to electrical 2.
service according to local national electrical codes.
Failure to properly connect may create a fire or
shock hazard.
For continued protection against possible hazard, 3.
replace fuses with same type and rating of fuse.
Disconnect from the power supply before 4.
maintenance or servicing.
To avoid personal injury:
Do not use in the presence of flammable or 1.
combustible materials; fire or explosion may result.
This device contains components which may ignite
such material.
Refer servicing to qualified personnel.2.
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.
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PREFACE
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 (over voltage) 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.
GETTING STARTED
These steps are offered to help the user become familiar
with, install, operate and develop the full capabilities of
the Parr 6300 Calorimeter.
parts of the calorimeter and make it easier to
understand the operating instructions which follow.
Turn the power switch ON (located on the back). 3.
Turn to the Instrument Description, Chapter 3, to
review the touch screen controls.
Review the 4. 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.
Review the 5. 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.
Turn to the 6. Menu Operating Instructions, Appendix
A, to review the menu functions used to modify
the program contained in the 6300 Calorimeter. A
review of the menus will provide a good idea of
the capabilities and flexibility designed into this
instrument.
Review the 7. Calculations, Appendix B. This provides
information about calculations performed by the
6300 Calorimeter.
Review 8. 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 6300 Calorimeters will
have an energy equivalent of approximately 940
calories per ºC with an 1138 oxygen bomb (800
calories per ºC with an 1136 oxygen bomb.) The
runs for standardization and determinations are
identical, except for the setting of the instrument to
the standardization or determination mode.
Review the 1. Concept of Operations, Chapter 1, to get
an understanding of the overall capabilities of the
calorimeter and microprocessor control.
Unpack and install the calorimeter in accordance 2.
with Installation, Chapter 2. This simple, step-wise
procedure will acquaint the user with the various
Review the 9. Communication Interfacing, Appendix
D, for the correct installation of any peripherals
connected to the 6300 Calorimeter.
After successful standardization, the 6300 10.
Calorimeter should be ready for testing samples.
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CHAPTER 1
CONCEPT OF OPERATION
A HIGHLY AUTOMATED PROCEDURE
Parr proudly introduces a new Oxygen Bomb
Calorimeter, No. 6300, in which new technology is
combined with time-proven calorimetric techniques to
produce a completely automatic system for measuring
the heat of combustion of solid and liquid fuels,
combustible wastes, foods, feeds and other oxygen
combustible materials. This new approach to bomb
calorimetry results in a remarkable simplification
of the steps required for a calorimetric test without
compromising the need for complete combustion, rapid
heat flow and precise thermometry which are essential
in a combustion calorimeter.
CONCEPT OF OPERATION
These new mechanical features support an established
technology in which water is circulated around the
bomb to bring all inner parts of the calorimeter to a
uniform temperature rapidly, while true isoperibol
operating conditions are maintained by an outer water
jacket. Microprocessor based, real time heat leak
corrections are applied to implement the isoperibol
jacketing method and to support the Parr rapid dynamic
method for predicting the final temperature rise. Precise
temperature measurements are made with thermistor
thermometry providing 0.0001ºC resolution over the
operating range of the calorimeter.
In addition to handling all test sequence operations, the
microprocessor makes all calculations and reports and
stores all results, as provided in earlier Parr isoperibol
and adiabatic calorimeters. A bright, backlit liquid
crystal display, prompts the operator through all setup
and operating steps with on-screen menus which make
user training quite simple.
1
In the 6300 Oxygen Bomb Calorimeter most of the
manual operations in conventional bomb calorimetry
have been eliminated by a new technology centered
around a semi-automatic bucket handling mechanism
and an automatic bomb filling, venting and rinsing
design. To perform a test the user simply loads a sample
into a holder, attaches a short auxiliary fuse, places
the head into the cylinder, seals with a 1/16 of a turn,
closes the cover and presses the START key to begin the
procedure.
NEW CONVENIENCE AND NEW TECHNOLOGY
The 6300 Calorimeter represents a blending of some
new unique design features with some long proven Parr
calorimetric technology to dramatically simplify the
user’s tasks during a calorimetric determination.
In this new design the bomb cylinder and bucket are
mounted in the calorimeter. The bomb is completely
surrounded by a bucket chamber, sealed co-axially
with the bomb head. After the bomb and bucket are
closed and sealed, the bomb is filled with oxygen, the
bucket chamber is filled with water, initial equilibrium
is established, the bomb is fired and the temperature
rise is monitored and recorded - all under automatic
microprocessor control. Then, at the completion of a
test, automatic control releases the residual pressure
in the bomb, rinses the bomb, cools the system and
empties the bucket.
ISOPERIBOL OPERATION
In Isoperibol operation, the calorimeter jacket is held
at a constant temperature while heat from the burning
sample causes the bomb and bucket temperature to
rise. The small heat flow between the bucket and
its surroundings during a test is monitored by a
microprocessor in the calorimeter, which continuously
determines the effect of any heat leak and applies
the necessary correction automatically. This system
differs from adiabatic operation in which the jacket
temperature must be adjusted continuously to match
the bucket temperature in an attempt to maintain a zero
temperature differential with no heat leaks between the
bucket and its surroundings. Calorimetrists have long
recognized the advantages of simplification and better
precision obtainable with a well designed and executed
Isoperibol system as opposed to the rapidly changing
jacket temperature required in an adiabatic calorimeter.
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
C
ONTROL
The microprocessor controller in this calorimeter has
been pre programmed to automatically prompt the user
for all required data and control input and to:
•
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.•
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 pre
programmed to:
The 6300 Calorimeter is equipped with a USB
connection plus an Ethernet port for direct
communication with attached peripherals and a
computer or network.
Collect and store all required test data.•
Apply all required corrections for combustion •
characteristics.
Compute and report the heat of combustion for the •
sample.
FLEXIBLE PROGRAMMING
The fifth generation software built into this calorimeter
and accessed through the screen menus permit the user
to customize the operation of the calorimeter to meet a
wide variety of operating conditions including:
A large selection of printing options.
•
Choice of accessories and peripheral equipment.•
Multiple options in regard to handling •
thermochemical corrections.
Choice of ASTM or ISO correction procedures.
•
A variety of memory management and reporting •
procedures.
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INSTALLATION
2
CHAPTER 2
INSTALLATION
REQUIRED CONSUMABLES, UTILITIES AND
P
OWER REQUIREMENTS
The 6300 Calorimeter System requires availability of
Oxygen, 99.5% purity, with appropriate connection,
2500 psig, maximum.
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.
Approximately 4 liters of tap water, with a total
hardness of 85 ppm or less, are required for filling the
calorimeter jacket reservoir. This water is provided via
the tap water connection at the rear of the calorimeter.
The inlet pressure should be in the range of 20 to 60
psig. The required flow rate is on the order of 0.5 liters/
minute. This connection also supplies cooling water
for the calorimeter. As a result, the temperature of the
water should not exceed 25 °C. The speed at which
the calorimeter will recycle between tests is a function
of the temperature of the incoming tap water. (The
performance will slow noticeably above 20 °C and will
become sluggish above 25 °C). Water consumption
is dependent on the incoming water temperature and
shouldn’t normally exceed 1.5 liters per test.
An open water drain connection is required.
INSTALLING THE CALORIMETER
Each Parr 6300 Calorimeter was completely assembled
and thoroughly tested prior to shipment. The following
stepwise procedure will guide the user through the
installation process.
Unpack the calorimeter and carefully check the
•
individual parts against the packing list. If shipping
damage is discovered, save the packing cartons
and report it immediately to the delivering carrier.
The calorimeter needs to be located near a water
drain. A cold-water tap water supply, oxygen
and an electrical outlet are also required. Set the
calorimeter on a sturdy, level, bench or table, free
from drafts, vibration and sources of radiant heat.
Make the calorimeter drain connection using the
•
provided 7/8” Tygon tubing (assembly A1336DD).
The calorimeter must be located so that the drain
tubing is always lower than the drain port at the rear
of the calorimeter. Failure to meet this requirement
will cause water to back up inside the calorimeter.
Make the tap water connection at the rear
•
of the calorimeter using 1/4” Nylon tubing
(HJ0025TB035). The inlet pressure should not
exceed 60 psig. Refer to figure 2-1 and 2-2. The inlet
connection incorporates a water filter, 1245DD,
just behind the inlet connection. When making
the water connection, a back-up wrench should
be placed on the water filter to insure a secure
connection and to prevent over tightening the filter.
NOTE:
During extended periods of inactivity (overnight or longer), shut off the tap water supply
to the calorimeter.
The power requirements for the subassemblies of the
6300 Calorimeter are:
Calorimeter
•
5A @ 120VAC
3A @ 230VAC
Printer
•
(100 to 240 VAC, 50/60 Hz) 0.35 A
Printer Supplies•
334C Printer Paper
335C Printer Ribbon
Make the connection to the rinse water source using
•
3/8” Tygon tubing (JT0038TB062A). A barbed
fitting is provided at the rear of the calorimeter
for this connection. A 10 liter carboy (231C2) is
provided as a distilled water rinse reservoir. Place a
149C in-line water filter at the end of the water line
that is inserted into the carboy.
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INSTALLATION
INSTALLING THE CALORIMETER (CONTINUED)
Make the connections to the oxygen supply at •
this time. Refer to figure 2-2 and 2-3. 1/8” O.D.
nylon pressure hose (HX0012TB024) is used to
connect the oxygen supply. The inlet connection
incorporates a flow restrictor just behind the inlet
connection. When making the oxygen connection,
a back-up wrench should be placed on the restrictor
to insure a secure connection and to prevent over
tightening the flow restrictor. The delivery pressure
for oxygen should be set at 450 psig. To install the
regulator, unscrew the protecting cap from the 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 tank outlet and
draw up the union nut tightly, keeping the gages
tilted slightly back from an upright position. Open
the tank valve and check for leaks. The bomb must
never be filled to more than 600 psig (40 atm).
Note:
The cause of any leaks must be corrected before
proceeding.
printer and the connections at the rear of the
calorimeter. Install the printer ribbon and printer
paper at this time. Apply power to the calorimeter
and turn on the printer.
SWAGELOK TUBE FITTINGS
When Swagelok Tube Fittings are used, the instructions
for installation are:
Simply insert the tubing into the Swagelok Tube 1.
Note:
During extended periods of inactivity (overnight or
longer), close the tank valve to prevent depleting the tank
in the event of a leak. When changing tanks, close the
tank valve prior to re-moving the regulator. Do not use oil
or combustible lubricants in connection with any part of
the oxygen filling system. Keep all threads, fittings and
gaskets clean and in good condition.
The exhaust and vent connections at the rear of the
•
calorimeter, are made with the dual tube A1006DD
assembly. The end of the assembly with the bomb
exhaust diffuser should be placed into the 10 liter
carboy (231C2). The carboy should be placed at
or below the level of the calorimeter to facilitate
complete draining of these lines.
Note:
This step is optional for use with A1050DD. See Appendix
G for A1050DD Bomb Rinse Container Installation and
Use.
Connect the printer USB cable between the 1758
•
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Fitting. Make sure that the tubing rests firmly on
the shoulder of the fitting and that the nut is fingertight.
Before tightening the Swagelok nut, scribe the nut at 2.
the 6 o’clock position.
While holding the fitting body steady with a back-3.
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.
For 3/16” and 4mm or smaller tube fittings, tighten 4.
the Swagelok nut 3/4 turns from finger-tight.
Figure 2-1
Swagelok Tube Fittings
INSTALLATION
Insert the tubing with pre-swaged ferrules into the 1.
fitting body until the front ferrule seats.
Tighten the nut by hand. Rotate the nut to the 2.
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.
2
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.
RETIGHTENING SWAGELOK TUBE FITTINGS
Swagelok tubing connections can be disconnected
and retightened many times. The same reliable leakproof seal can be obtained every time the connection is
remade using the simple two-step procedure.
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INSTALLATION
Figure 2-2
6300 Calorimeter Back Panel
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6300 CALORIMETER EXTERNAL PLUMBING
Figure 2-3
Closed Loop Confi guration with 6520A
O2 Regulator
DI Water
~Room Temp
5-10 °C
INSTALLATION
2
6520A
Water Recircualtion
System
Figure 2-4
Closed Loop Confi guration with 1564
O2 Regulator
DI Water
~Room Temp
5-10 °C
Rinse Collection
1552
Water
Cooler
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)
1564
Water
Recircualtion
System
Rinse Collection
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2
INSTALLATION
6300 CALORIMETER EXTERNAL PLUMBING (CONTINUED)
Figure 2-5
Open Loop Confi guration with 1552
O2 Regulator
Tap Water
· <25 °C
· <85 ppm
· <60 psig
1552
Water
Cooler
DI Water
~Room Temp
Drain
Figure 2-6
Open Loop Confi guration
O2 Regulator
Tap Water
· <25 °C
· <85 ppm
· <60 psig
5-10 °C
Rinse Collection
DI Water
~Room Temp
Rinse Collection
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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INSTALLATION
2
INSTALLING THE CALORIMETER (CONTINUED)
After the calorimeter displays the main menu, press •
the Calorimeter Operation button. This screen
should indicate that the jacket is filling with water.
The initial fill can take as long as 8 to 10 minutes
to complete. If the jacket filling process times out,
simply acknowledge the timeout message to resume
the jacket filling process. After the jacket is filled
press the Heater and Pump button in order to toggle
the heater and pump on.
Wait for the calorimeter jacket temperature to
•
stabilize within a half a degree of 30 °C. (When
the pump and heater are turned on after being off
for an extended period of time, it may take longer
than 10 minutes for the calorimeter warm up. This
may cause an error. Simply restart the heater and
pump.) While waiting for the jacket temperature to
stabilize, raise the calorimeter lid and remove the
bomb head by twisting 1/16 turn counterclockwise
and pulling straight up. Examine the bomb release
pin at the bottom of the combustion cylinder. If it
has become dislodged during shipping, position it
correctly using the long forceps supplied in the calorimeter accessory kit. Refer to figure F-19.
Lock the head in the bomb cylinder (see section
•
5-7), close the lid and while applying a slight
downward pressure. Press the CALORIMETER
OPERATION key on the main menu followed by
the Pretesting Cycle button to initiate a pre-test
cycle. (This button will not be available until the
jacket temperature has been stable for 15 minutes.)
During the initial portion of this cycle, check to
see that the oxygen supply pressure is set to 450
psig. Adjust as required. The calorimeter should
complete the pre-test cycle with no errors.
ENTER to store the default sample mass of 1 gram.
This test should go through Fill, Pre-period, Postperiod and Cool/Rinse Cycles without error. The
calorimeter is now ready to be standardized.
•
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 the standardization mode on
the Calorimeter Operation Page, by pressing the
Operating Mode button. If two bomb heads 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 by pressing the Bomb Installed/
EE key. Both bomb heads 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 calorimeter one degree.
Repeated standardization with any given bomb
head should yield an energy equivalent value with
a range of up to 4 calories per degree, centered on
the mean value for all tests using that bomb head.
The calorimeter is ready for testing samples after a
suitably constant energy equivalent value has been
obtained.
Assemble the bomb head stand (A38A), located in
•
the accessory kit. Remove the head from the calorimeter and place it on the stand. Place a 1 gram
pellet of benzoic acid in a combustion capsule
and place this unweighed sample on the capsule
holder of the bomb head. Attach 10 cm of fuse
thread as shown in figure 5-3. Install the bomb
head in the calorimeter and close the cover. Apply
a slight downward pressure on the cover and press
the START key to begin the test sequence. Press
the ENTER key to accept the displayed sample ID
number. At the sample weight prompt press 1 then
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INSTALLATION
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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.
Note:
Keys with a double box in the upper left hand corner lead
to sub-menus.
INSTRUMENT DESCRIPTION
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.
Data Displays.4. 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 submenu. 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.
CONTROL KEYS
3
MENU KEYS
The controls that change the data field information in
the menus will be one of the following:
Toggles.1. 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.
Option Selection.2. 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.
Value Entry Fields.3. 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.
Escape.1. This key is used to go up one level in the
menu structure.
Main Menu. 2. This key is used to return to the main
menu touch screen from anywhere in the menu
structure.
Start.3. This key is used to start a calorimeter test.
Report.4. 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
Help. 5. This key is used to access help screens related
to the menu currently displayed on the touch screen.
Abort.6. This key appears in the Start key location
while a test or pretest is running. Pressing this key
will abort the test or pretest in progress.
7. This key appears in the Escape key location
when the main menu is displayed. This key is used
to shut down the calorimeter program before turn-
ing off the power.
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INSTRUMENT DESCRIPTION
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PROGRAM INSTALLATION & CONTROL
4
CHAPTER 4
PROGRAM INSTALLATION &
CONTROL
SOFTWARE INSTALLATION
The program in the 6300 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.
REVISING DEFAULT SETTINGS
The default parameters of the 6300 Calorimeter can
be changed to guarantee that the 6300 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.
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
Units are pre programmed with DEFAULT
SETTINGS. See pages 24 and 25 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
Figure 4-1
6300 Factory Default Settings
Calorimeter Operations
Operating Mode Determination
Bomb Installed/EE 1/940.0
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 Backlight Intensity 70%
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
User Function Setup
Cold Restart
User/Factory Settings
User Setup ID 63-1138
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Compare settings with Factory Defaults
Calibration Data & Controls
Calibration Run Limit 10
EE Max Std Deviation 0.0
Heat of Combustion of Standard 6318.4
Bomb Service Interval 500
Use Bomb 1
Control Chart Parameters
Charted Value HOC Standard
Process Sigma 0.1
Temp Rise High Warning 8.5
Temp Rise Low Warning 5.1
Bomb Rinse Tank Control
Report Rinse Tank Empty ON
Rinse Tank Capacity 150
# Rinses Left 150
Reset Rinse Tank Counter
Rinse Time 25
Rinse Flush Time 20
Clear Time 100
# of Rinse Cycles 3
Program Information and Control
Date & Time Settings
Volume Level Adjust 85%
Software and Hardware Info
Settings Protect OFF
User/Factory Settings
Feature Key
Bomb Type Select
Bomb 1 Through 4
EE Value 800.0
Protected EE Value OFF
Thermochemical Corrections Standardization
Fixed Fuse ON 50.0
Acid Correction Fixed HNO
Fixed Sulfur ON 0.0
Determination
Fixed Fuse ON 50.0
Acid Correction Fixed HNO
Fixed Sulfur OFF 0.0
Net Heat/Dry Factors
Calculation Factors
Nitric Acid Factor 1.58
8.0
3
8.0
3
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PROGRAM INSTALLATION & CONTROL
Factory Default Settings
Continued
4
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
Net Heat/Dry Factors
Fixed Hydrogen OFF 0.0
Fixed Oxygen ON 0.0
Fixed Nitrogen ON 0.0
Calculate Net Heat of Combustion OFF
Fixed Moisture as Determined OFF 0.0
Fixed Moisture as Received OFF 0.0
Dry Calculation OFF
Data Entry Controls
Prompt for Bomb ID ON
Weight Entry Mode Touch Screen
Acid Entry Mode Touch Screen
Net Heat Entry Modes Touch Screen
Auto Sample ID Controls ON
Sample Weight Warning above 2.0
Spike Weight Entry Mode Touch Screen
Sulfur Entry Mode Touch Screen
Moisture Entry Modes Touch Screen
Auto Preweigh Controls ON
Auto Sample ID Controls
Automatic Sample ID ON
Automatic Sample ID Increment 1
Automatic Sample ID Number 1
Auto Preweigh Controls
Automatic Preweigh ID ON
Automatic Preweigh ID Increment 1
Automatic Preweigh ID Number 1
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
Report Schedule End of Postperiod
Communication Controls
Printer Type Parr 1758
Balance Port
Network Interface
Printer Destination Local USB
Bar Code Port
Network Data Devices
Balance Port Communications
Balance Type Generic
Balance Port Device
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 Destination Log File and
Printer
Select Data Log Items
Data Log Format Text Format
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PROGRAM INSTALLATION & CONTROL
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OPERATING INSTRUCTIONS
5
CHAPTER 5
OPERATING INSTRUCTIONS
TO BEGIN A TEST
Weigh the sample to 0.1 mg. 1.
Gently tap the capsules that contain powdered 2.
samples to compact the material. (Pellets are easier
to handle than loose samples and they burn slower
in the bomb, thereby reducing the chances for incomplete combustion.)
Carefully place the capsule into the capsule holder.3.
Attach 10 cm of ignition thread (see Figure 5-2).4.
Install bomb head in calorimeter.5.
Close calorimeter cover making certain the latch is 6.
engaged
Select determination or standardization as appro-7.
priate on Calorimeter Operations Page, Operating
Mode.
Press START to begin the test. Calorimeter will 8.
prompt operator for Cal ID number, Sample ID
numbers and weights in accordance with operating
modes set into the instrument.
OPERATING THE OXYGEN BOMB
Combustion with oxygen in a sealed bomb is a very
effective and reliable method for releasing all heat
energy obtainable from a sample, and for preparing
hydrocarbon compounds and carbonaceous materials
for analysis.
Note:
The following precautions must always be observed when
using this equipment:
Do not overcharge the bomb with sample or with a 1.
sample which might react with explosive violence.
Do not overcharge the bomb with oxygen. The 2.
initial charging pressure should not exceed 40 atm
(600 psig).
Do not fire the bomb if there is any indication that 3.
it is leaking.
Stand away from the calorimeter during firing and 4.
for at least 20 seconds after firing.
Keep the bomb in good condition at all times. Any 5.
parts that show signs of weakness or deterioration
must be replaced promptly.
Read the maintenance and safety instructions before 6.
starting to use the bomb, and urge all operating
personnel to read these instructions often.
Note:
Tape should always be stored in a sealed container to
minimize changes in its moisture and solvent content.
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5
OPERATING INSTRUCTIONS
Figure 5-1
Fill Flow Diagram
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OPERATING INSTRUCTIONS
5
ALLOWABLE SAMPLE SIZE
To stay within safe limits, the bomb should never be
charged with a sample which will release more than
8000 calories when burned in oxygen.
The initial oxygen pressure is set at 30 atmospheres (450
psig). This generally limits the mass of the combustible
charge (sample plus benzoic acid, gelatin, firing oil or
any combustion aid) to not more than 1.1 grams.
When starting tests with new or unfamiliar materials, it
is always best to use samples of less than .7 gram with
the possibility of increasing the amount if preliminary
tests indicate no abnormal behavior and sample will not
exceed the 8000 calorie limit.
To avoid damage to the bomb and calorimeter, and possible injury to the operator, it should be a standing rule
in each laboratory that the bomb must never be charged
with more than 1.5 grams of combustible material.
Figure 5-2
Cotton Thread Assembly
Samples containing sulfur should contain no more than
50 mg of sulfur and have a calorific value of at least
9000 BTU/lb.
Samples containing chlorine should be spiked to insure
that sample contains no more than 100 mg of chlorine
and liberates at least 5000 calories.
ATTACHING THE COTTON THREAD
Remove any moisture from the heating wire prior to attaching the cotton thread.
A cotton thread (845DD) is used as an auxiliary fuse to
ignite the sample (See Figure 5-2).
Four inches of thread is recommended for this auxiliary
thread which is looped over the heating wire, doubled
on itself, twisted to form a single strand and fed into the
sample cup to lay on the sample.
When contact is made through the heating wire, the
thread will ignite, drop into the sample cup and ignite
the sample.
One spool of thread, part number 845DD, is 563 yards.
Part number 845DD2 contains approximately 1000
pieces of thread pre-cut to 4 inches.
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5
OPERATING INSTRUCTIONS
WARNING - DO NOT OVERFILL THE BOMB
The safety relief valve on the regulator should protect the system from an over fi ll. If for any reason, the
bomb should accidentally be charged to more than 600 psig (40 atm), do not fi re the bomb. The dangerous pressures which might develop under such conditions could damage the bomb and injure the operator.
If there is any reason to believe that the bomb has been over-fi lled, stop the fi lling operation immediately,
exhaust the bomb and open it to check for any loss of sample before repeating the fi lling procedure.
Figure 5-3
Pre-period/Post-period
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OPERATING INSTRUCTIONS
5
CLOSING THE BOMB
Care must be taken not to disturb the sample when
moving the bomb head from the support stand to the
bomb cylinder in the calorimeter. Check the sealing
ring to be sure that it is in good condition and moisten
it with a bit of water so that it will slide freely into the
cylinder.
Notice that the bomb head grounding lug extends
beyond the outside diameter of the bomb head. A slot
for this lug is cut into the top of the calorimeter bucket
which holds the bomb cylinder. Position this lug approximately 20 degrees to the operators right and slide
the head into the cylinder and push it down as far as it
will go. Now rotate the bomb head 20 degrees to the left
until the lug contacts the left edge of the cut out and is
pointed to the front of the calorimeter.
FILL CYCLE
at the top of the bomb closes and isolates the bomb
from the oxygen filling line.
The controller monitors the operating temperature 3.
until it confirms that the initial equilibrium has been
established.
BOMB FIRING
Once the initial equilibrium is confirmed, the controller
initiates the firing sequence.
There are no changes to the circulation pattern, as
shown in Figure 5-3, from the pre-period through the
bomb firing and post-period.
A warning of five short beeps is sounded indicating 1.
the bomb is about to be fired.
Current is passed through the electrical leads to 2.
ignite the ignition thread.
Once the calorimeter is started and the cover is closed,
the fill sequence begins (see Figure 5-1).
The calorimeter checks the bomb ignition circuitry 1.
for continuity.
The water fill solenoid opens and water is pumped 2.
from the closed water supply tank into and through
the bucket that surrounds the bomb. Overflow from
the bucket is returned to the closed water tank.
Because the jacket and bucket are both filled with
water from the closed water tank, initial equilibrium
will be reached quickly.
The oxygen fill solenoid is opened and oxygen is 3.
added slowly to the bomb to bring its pressure to
approximately 30 atm.
PRE-PERIOD
At the completion of the fill sequence, the pre-period
begins (see Figure 5-3).
The controller monitors the temperature in the 3.
bucket to establish that a temperature rise actually
occurs. If no temperature rise occurs, the misfire
message is displayed on the controller and the abort
sequence is initiated.
The water fill solenoid valve closes and isolates the 1.
water in the bucket from the rest of the system.
Water within this bucket is circulated by the stirrer.
Water continues to circulate from the closed water
system through the jacket surrounding the bucket.
The oxygen filling valve closes and the pressure in 2.
the filling line is vented. The automatic check valve
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5
OPERATING INSTRUCTIONS
Figure 5-4
Rinse & Cool Flow Diagram
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OPERATING INSTRUCTIONS
5
POST-PERIOD
After fi ring is confi rmed, the post-period begins (see
Figure 5-3).
The controller monitors the temperature rise and 1.
determines the final temperature rise by either the
dynamic or equilibrium criteria as established by the
user.
Once the final temperature rise is determined, it is 2.
recorded with the test results.
COOL/RINSE
At the completion of the post-period, the rinse and
cool sequence begins (see Figure 5-4).
Tap water is circulated through the bucket to cool 1.
the bomb to the starting temperature.
DRAIN
At the completion of the bomb rinse sequence, the
drain sequence begins (see Figure 5-5).
The water in the bucket is drained out of the bucket 1.
and routed to the drain connection.
Once the bucket is drained, the calorimeter may be 2.
opened to remove the bomb head and load the next
sample.
The test result will be printed or displayed in ac-3.
cordance with the setting of the Report Schedule on
the Reporting Controls Submenu.
The release valve in the bottom of the bomb is 2.
opened and the residual pressure is released through
the bomb exhaust line.
Once the excess oxygen is vented, the bomb wash 3.
water from the carboy of the rinse water tank is
admitted through the bomb wash solenoid valve and
the check valve at the top of the bomb. The bomb
wash water is released to the wash bottle.
Several rinse patterns may be confi gured by the user
to meet various operational and analytical requirements.
The bomb is fi lled one more time with oxygen to help
fl ush the water residue from the interior of the bomb.
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5
OPERATING INSTRUCTIONS
Figure 5-5
Drain Flow Diagram
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OPERATING INSTRUCTIONS
5
SAMPLES
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 to 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.
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 6300 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 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 43A3KQ
Fused Quartz is required. When superior corrosion
resistance is needed, the Platinum Rhodium 43A5 Capsule or 43A3KQ Fused Quartz is required.
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.
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 powdered 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.
Also, when benzoic acid is combusted for standardization runs or for combustion aid purposes, it should be
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.
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 500ºC
for 24 hours to develop this protective coating uniformly
on all surfaces. This treatment should be repeated after
a capsule has been polished with an abrasive to remove
any ash or other surface 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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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 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.
1136 Oxygen Combustion Bomb
The 1136 bomb has been used extensively in our model
1281 calorimeter for the past ten years. It will safely
burn samples liberating up to a maximum 8000 calories
per charge using oxygen charging pressures up to 40
atm.
The 1136 bomb, like the 1138 bomb, is made of alloy 20
and is also available in Hastelloy G30
1136CL. These bombs are 340 mL in volume and are
rated to a maximum working pressure of 2000 psi. Like
the 1138, the bombs are hydrostatically tested to 3000
psi and the sample range is ~1g or 5000 – 8000 calories.
TM
as part number
EXPLOSIVES AND HIGH ENERGY FUELS
Materials which release large volumes of gas which detonate with explosive force or burn with unusually high
energy levels, should not be tested in this calorimeter.
Rather, they should be tested in a model 6100 or 6200
Calorimeter which can be equipped with an 1104 High
Pressure Oxygen Bomb designed specifically for these
types of samples.
CORROSIVE SAMPLES
1138 Oxygen Combustion Bomb
The 1138 bomb is made from alloy 20; a special niobium stabilized stainless steel selected for its resistance
to the mixed nitric and sulfuric acids produced during
the combustion process.
The 1138CL is made from the halogen resistant Hastelloy G30™. Hastelloy G30™ is an alloy rich in cobalt
and molybdenum and is able to resist the corrosive
effects of free chlorine and halogen acids produced
when burning samples with significant chlorine content. While no alloy will completely resist the corrosive
atmospheres produced when burning samples containing halogen compounds; users who intend to test these
materials are urged to select the 1138CL Bomb.
These bombs are 250 mL in volume and are rated to a
maximum working pressure of 2000 psi. The bombs
are hydrostatically tested to 3000 psi and the sample
range is ~1g or 5000 – 8000 calories.
VOLATILE SAMPLE HOLDERS
Volatile samples can be handled in a Parr 43A6 Platinum Capsule with a spun rim, or in a Parr 43AS Alloy Capsule which has a sturdy wall with a flat top
rim. These holders can be sealed with a disc of plastic
adhesive tape prepared by stretching tape across the top
of the cup and trimming the excess with a sharp knife.
The seal obtained after pressing this disc firmly against
the rim of the cup with a flat blade will be adequate for
most volatile samples. The tape used for this purpose
should be free of chlorine and as low in sulfur as possible. Borden Mystic Tape, No. M-169-C or 3M Transparent Tape, No. 610, are recommended for this purpose. The 3M Transparent Tape can be ordered through
Parr, Part No. 517A.
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.
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OPERATING INSTRUCTIONS
5
Note:
Tape should always be stored in a sealed container to
minimize changes in its moisture and solvent content
Figure 5-6
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 pres-
•
sure.
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 igni-
•
tion 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 180ºC 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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CHAPTER 6
CORRECTIONS & FINAL REPORTS
If the Spiking Correction is used, a spiking correction
must be entered before obtaining a Final Report.
6
CORRECTIONS & FINAL
REPORTS
ENTERING CORRECTIONS AND OBTAINING THE
FINAL REPORT
Final reports for each test can be obtained whenever the
operator is prepared to enter any required corrections
for fuse, acid and sulfur.
When entering corrections, the user can choose either
of two methods. These are:
Manual Entry
•
Fixed Corrections•
Refer to the Reporting Instructions, Chapter 7, for the
steps necessary to initiate a report from the controller.
MANUAL ENTRY
After the last entry has been made, the calorimeter will
automatically produce a Final Report.
If values for these corrections are not available, the
operator can use the SKIP key to bypass any of the
corrections; however, a Final Report will not be printed
until an entry is made for fuse, acid and sulfur.
FIXED CORRECTIONS
In many cases, 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.
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.
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CORRECTIONS & FINAL REPORTS
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CHAPTER 7
REPORTING INSTRUCTIONS
REPORTING INSTRUCTIONS
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.
7
REPORT OPTION SECTION
The 6300 Calorimeter can transmit its stored test data
in either of two ways. The REPORT DESTINATION
key on the Reporting Controls Page toggles the report
destination between the display and an optional printer
connected to the USB port of the calorimeter. This
page also selects the type of reports that are generated
automatically by the calorimeter.
REPORT GENERATION
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.)
Run Data Status
This key enables the operator to display only
preliminary reports, only final reports, both preliminary
and final reports, only pre weighed samples reports or
all stored reports.
Prompt For Final Values
When turned on, the controller will prompt the
operator to enter any missing corrections for fuse, sulfur
and acid in any selected preliminary reports. When
turned off preliminary reports will be displayed as
entered.
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.
Thermochemical corrections are entered by using the
following steps to select and edit preliminary reports.
The displayed files can be sorted by sample ID number,
by type, by status or by date of test by simply touching
the appropriate column.
Individual files can be chosen by highlighting them
using the up and down arrow keys to move the cursor.
Press the SELECT key to actually enter the selection.
Once selected the highlight will turn from dark blue to
light blue. A series of tests can be selected by scrolling
through the list and selecting individual files.
The double up and down keys will jump the cursor to
the top or bottom of the current display.
If a range of tests is to be selected, select the first test in
the series, scroll the selection bar to the last test in the
series and press EXTEND SEL to select the series.
The DESEL ALL key is used to cancel the current
selection of files.
To bring the selected report or series of reports to the
display, press the DISPLAY key. To send the reports to
the printer press the PRINT key.
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REPORTING INSTRUCTIONS
REPORT GENERATION (CONTINUED)
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 final reports, go to the
Thermochemical Corrections Page, Net Heat/
Dry Factors, 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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FILE MANAGEMENT
8
CHAPTER 8
FILE MANAGEMENT
The 6300 Calorimeter will hold data for 1000 tests in its
memory. These tests may be pre weights, preliminary or
final reports for either standardization or determination
runs. Once the memory of the controller is filled, the
controller will not start a new analysis until the user
clears some of the memory.
CLEARING MEMORY
The FILE MANAGEMENT key on the main menu
leads to the file management sub-menu. The RUN
DATA FILE MANAGER key leads to a listing of the
files.
Single files can be deleted by highlighting the file
•
and pressing the DELETE key. The controller will
then ask the user to confirm that this file is to be
deleted.
A series of files can be deleted by selecting the first
•
file in the series and then the last file in the series
using the EXTEND SEL key and then pressing the
DELETE key.
REMOVABLE SD MEMORY
The controller of the 6300 calorimeter can accept SD
memory cards. These cards can be used to:
• Copy test file data for transfer to a computer.
• Copy user settings for back up.
• Reload user settings to the controller to restore or
update the controller’s operating system.
SD memory cards are inserted into the slots on the
back of the control section of the calorimeter. Keys
are provided on the FILE MANAGEMENT submenu to initiate each of the above three actions with
the exception of restoring or updating the controllers
operating system.
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FILE MANAGEMENT
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MAINTENANCE & TROUBLESHOOTING
CHAPTER 9
M
AINTENANCE &
T
ROUBLESHOOTING
ROUTINE MAINTENANCE
Note:
See the corresponding water system manuals for information on the maintenance of those systems.
To service or remove the bomb cylinder from the bucket
assembly, remove the 941DD Wedge with needle nose
pliers. Remove the 668DD Check Valve from the bomb
cylinder. Remove the two SA1632RD18 Machine
Screws (see Figure F-20). Then remove the 942DD
Bushings and the 1081DD Quad-ring.
9
Daily Maintenance
Clean the 1444DDJB O-ring that seals the bomb head
and cylinder by wiping with a tissue. Wet this sealing
area with water prior to starting a series of tests. Clean
corresponding sealing area in cylinder in a similar
fashion. Both surfaces must be free of any accumulated
foreign matter, such as unburned sample material or
combustion by-products. Wet the hole in the center of
the head which contains the check valve.
With a tissue, clean the head where the large bucket
quad-ring contacts the head perimeter. Wet this sealing
area with water prior to starting a series of tests.
Remove, inspect and clean the cylinder check valve
(668DD) and corresponding sealing area in the bomb
cylinder. In extreme cases, i.e. a spilled sample, use soap
and water to clean the area.
Carefully lift the bucket and bomb assembly out of the
air chamber and position horizontally on the calorimeter to remove the 925DD Oxygen Bomb Retainer Nut
(see Figure F-19). Now the cylinder can be removed
from the bucket assembly. Note the position of the
locating pin.
To replace, follow these steps in reverse.
Fuses
The replacement of protective fuses for the 6300
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.
Contact Parr Customer Service for instructions on how
to access the fuses.
Note:
Check the labels on the instrument for correct fuse rating.
Parr
Part #
139E23 Lines Protective
1641E2 Heater Fuse (F2) Fast-Acting 2.5 Amps,
1641E Pump Fuse (F1) Fast-Acting 1 Amp,
997E5 Bomb Rinse (F5) Slo-Blo 5 Amps,
Description Type Ratings
Fast-Acting 15 Amps,
Fuses
250Vac
250VAC
250VAC
250VAC
50 to 100 Tests
Replace the heating wire, with 2.5” of 840DD2 360
degrees clockwise around screws. Clean 986DD
Electrode Contact Pins with mild abrasive, such as a
pencil eraser, clean bomb head electrode points in a
similar fashion, tighten screws holding heating wire in
place.
Quarterly
Change water in the Water Tank and replace the
1245DD and 149C water filters.
500 Tests
Under normal usage Parr oxygen bombs will give long
service if handled with reasonable care. However, the
user must remember that these bombs are continually
subjected to high temperatures and pressures which
apply heavy stresses to the sealing mechanism. The
mechanical condition of the bomb must therefore be
watched carefully and any parts that show signs of
weakness or deterioration should be replaced before
they fail.
Parr recommends that the following parts on the
oxygen bomb be changed every 500 tests or six months
whichever comes first: 840DD2, 1374HCJV (2),
394HC, 821DD (2), 1071DD, 1444DDJB, 659DD,
519AJV, 694DD. When reassembling the bomb head,
take care not to roll the 694DD O-ring as this will cause
an oxygen leak. Samples that contain chlorine or are
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MAINTENANCE & TROUBLESHOOTING
500 Tests (Continued)
abrasive may require this maintenance to be performed
on a more frequent interval such as every 250 tests. The
882DD and 969DD O-rings should also be replaced and
is positioned between the bucket and the air-can of the
calorimeter. For your convenience, these parts may be
purchased as kit number 6038, Firing Maintenance Kit.
See Figures F-1 and F-2 for O-ring locations.
Lubricate the 659DDJU and 357HCJB O-rings in the
bomb release cylinder with 811DD lubricant. See
Figures F-20 for O-ring locations. Clean the ignition
contacts.
The 1140DD Seal/Release mechanism should be
serviced with the same frequency as the bomb head.
This includes the replacement and lubrication of the
659DDJU, 1138DD, 969DD, 1143DD and 357HCJB
O-rings with 811DD lubricant. Tools required are:
screwdriver, snap ring pliers and needle nose pliers.
Turn off the gas supply to the calorimeter. Go to 1.
the Diagnostics Screen and turn on the bomb seal
command. Raise the lid and turn ON the O
Command. These steps are necessary to release the
gas pressure in the seal/release mechanism before
disassembling.
Turn off the calorimeter, once the oxygen has 2.
depressurized.
Insert the bomb head into the cylinder and lock into 3.
place.
Disengage the screws, SA1632RD018 that hold the 4.
bucket in the air can. Remove the 941DD plastic
wedge that secures the front of the air can assembly.
Lift the bomb and bucket as a unit from the calo-5.
rimeter air can chamber and disconnect the bucket
thermistor probe. Set this unit aside.
Remove the vessel spacer, 964DD and the associ-6.
ated O-ring, 969DD.
Remove the cylinder spacer, 1141DD, which sits on 7.
top of the snap ring, 1137DD.
Remove the snap ring that retains the cylinder insert 8.
in the release mechanism at the bottom of the air
can.
Withdraw both the insert and the release pin as a 9.
unit using needle nose pliers.
Remove any scoring on the release pin, above the 10.
smaller O-rings, 659DDJU in present with crocus
cloth. Replace the O-rings on the 966DD2 release
pin as well as the 1138DD O-ring that seals the
cylinder insert. Lubricate 659DDJU and 357HCJB
O-rings with 811DD lubricant.
Fill
2
Reverse the above procedure to reinstall the cylin-11.
der insert/pin as well as the bomb bucket assembly.
Make sure that the large side hole in the 1139DD
insert is oriented toward the left side of the instrument. The insert is keyed to the cylinder and can
not be fully inserted unless it is properly oriented.
5000 Tests
To deal with the realities of today’s test loads and cycle
times, the ASTM Committee recommends in method
E144 - 94(2006)e1 that “all seals and other parts that
are recommended by the manufacturer be replaced or
renewed after each 5000th firing or a more frequent
interval if the seals or other parts show evidence of
deterioration”. Oxygen bombs returned to Parr for
service will be tested in accordance with ASTM E144
- 94(2006)e1. A test certificate is provided with each
repair.
This service includes:
Disassembly, cleaning and inspection of all parts
•
Re-polishing of the inner surfaces of the bomb•
Re-assembly with new insulators, and seals, sealing •
rings, and valve seats
Proof testing
•
Hydrostatic testing•
The hydrostatic and proof testing of the oxygen bomb
should be performed after every 5000 firings or if:
The bomb has been fired with an excessive charge.
•
The ignition of any of the internal components has •
occurred.
There have been any changes in the threads on the •
bomb cylinder.
The bomb has been machined by any source other •
than Parr Instrument Company.
After repeated use with samples high in chlorine (over
1%), the inner surfaces of the bomb will become etched
to the point where appreciable amounts of metal salts
will be introduced during each combustion. Any bomb
which is being used for chlorine determination should
be polished at more frequent intervals to prevent the
development of deep pits. If the interior of the bomb
should become etched or severely pitted, the resistance
of the metal to further attack can be improved by
restoring the surface to its original polished condition.
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6300 MAINTENANCE CHECKLIST
Date Date Date Date
Change water
Replace 149C
Clean grill on heat
sink.(6520A)
Date Date Date Date
Replace 8400DD2
Heating Wire
Clean 986DD Electrode Contact Pins
MAINTENANCE & TROUBLESHOOTING
Quarterly Maintenance
50 to 100 Test Maintenance
9
Replace the following:
Date Date Date Date
Head:
1374HCJV (2) O-rings
394HC O-ring
694DD O-ring
519AJV O-ring
659DD O-ring
1444DDJB O-ring
Cylinder:
1071DD Quad ring
821DD O-ring
882DD O-ring
Bucket and Bomb Seal/Exhaust area:
659DD O-ring
1143DD O-ring
1138DD O-ring
659DDJU (2) O-rings
357HCJB O-ring
500 Test Maintenance
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MAINTENANCE & TROUBLESHOOTING
INSPECTION OF CRITICAL SEALING SURFACES
The sealing grooves and related surfaces for most of
the Parr bombs are machined to tolerances as small as
+/- 0.001” (0.03mm). As a result, any imperfection
in a sealing surface resulting from either normal use
or carelessness in handling the bomb can cause the
bomb to leak. If the damage or accumulated wear is
much less than 0.001” (0.03mm), then careful polishing
will restore the bomb sealing to an as new condition.
Imperfections that penetrate the sealing surface more
than one or two thousandths of an inch (0.03-0.06mm)
may render the seal surface unserviceable.
Any surface that comes in contact with an elastomer
seal should be carefully examined for imperfections
that would compromise its ability to seal. A freshly
sharpened pencil can be used to probe the metal sealing
surfaces for significant imperfection. If the pencil
point hangs up in the imperfection, further attention
is warranted. An attempt should be made to polish
(remove) any significant imperfections. This operation
generally requires the use of a lathe in order to
guarantee that the sealing surface to be repaired remains
concentric with the mating surface. Knowledge of the
dimensional tolerances and the ability to accurately
measure or gauge the affected area is required in order
to insure that too much polishing (metal removal)
has not taken place. We recommend that bombs with
significant imperfection of this nature be serviced at
Parr.
CAUTION!
Avoid prying elastomer seals (O-rings and
quad-rings) from seal grooves with metallic
tools.
The use of dental picks and other metallic tools to pry
the seals from their grooves is strongly discouraged.
These hard steel tools, if misused, can leave permanent
tool marks on the sealing surface, which are difficult
or impossible to remove. These blemishes are hidden
by the seal during normal use and as a result, are not
readily apparent as the cause of a leaking bomb.
Larger size seals (0.8” or 20 mm O.D.) typically used
to seal the bomb head can be extracted from its groove
using either of the following two methods:
Grasp the outer circumference of the seal with the 1.
thumb and forefinger and slide them together while
applying sufficient pressure on the seal to cause it to
pucker out of the groove. With the other hand, grab
the exposed, pinched section and pull the seal from
the groove.
Use a non-metallic object, such as the rounded 2.
corner of a plastic credit card, to simply pry the seal
from its groove.
Smaller diameter seals usually require a different
approach. A portion of the seal should be carefully
pulled, not pried, from the groove with a small pair of
pliers or a hemostat. The exposed portion of the seal
can then be cut, or pulled further to remove the seal.
The pliers or hemostat should never contact the sealing
surface, only the seal.
BOMB EXHAUST TROUBLESHOOTING
The bomb exhaust and sealing is controlled by movement of the 966DD2 piston inside of the 1140DD
bomb seal/release cylinder. This assembly is mounted
on the bottom of the calorimeter air can. The piston is
driven to the up position (exhaust) by applying oxygen
at 30 atm to the 1/8 male connector (344VB). The
piston is driven down (bomb seal) by applying pressure
to the 376VB elbow. The application of the oxygen
pressure is controlled by the A1251DD three station
solenoid valves. There is a flow restrictor, part 527VB,
on the inlet side of this solenoid which limits the maximum flow rate of oxygen and in turn creates a gradual
increase in pressure at the 1140DD bomb seal/release
cylinder when the solenoid is turned on. Failure of the
bomb to exhaust in a timely fashion can have more than
one cause. Certain causes can be eliminated systematically by checking the bomb exhaust diffuser, at the end
of the bomb exhaust line, for any restrictions in the six
small cross drilled holes. This fitting should be removed
from the tubing, inspected thoroughly and cleaned as
required.
Service the O-rings on the 966DD2 Piston
This process is described in the 500 test maintenance
section.
Confirm function of the 966DD2 piston
In order to reduce the amount of time it takes to duplicate and troubleshoot this type of situation, the I/O
diagnostics can be used to pressurize and exhaust the
bomb without having to run lengthy combustion or pretests.
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MAINTENANCE & TROUBLESHOOTING
9
WARNING:
This screen allows unconditional and arbitrary output control for testing purposes. Be
aware that all user and instrument protection is disconnected while on this screen.
This is very important and you should take
proper pre-caution.
Make sure the 668DD check valve is installed at the 1.
bottom of the cylinder.
Lock the head into the cylinder and close the calo-2.
rimeter lid.
Confirm the Exhaust is off.3.
Turn Bomb Seal on then off to retract the 966DD2 4.
piston.
Turn on O2 Fill to begin filling the bomb. The 5.
bomb will be completely filled in one minute, at
which time O2 Fill should be turned off. This seats
the check valve in the head which in turn seals the
contents of the bomb.
The calorimeter lid can be unlocked at this time.6.
Activating the Exhaust should initiate a bomb 7.
exhaust within two seconds. If it takes much longer
than two seconds before the bomb begins to vent,
then at least one of the two following conditions
outlined below exist.
If the bomb exhaust is initiated in a timely manner 8.
but fails to complete in 10 seconds, a blockage or
restriction in the bomb exhaust circuit is indicated.
This must be investigated and corrected.
If the bomb fails to exhaust, the 899DD Head Handle
and SN1632HX 8/32 Hex Nut can slowly be removed
to release the pressure in the bomb. See Figure 13-1.
If the piston moves properly with no applied bomb pressure, but still fails to initiate an exhaust of a pressurized
bomb in a timely fashion, at least one of the following
conditions exist:
The 527VB restrictor is partially blocked.1.
The exhaust line is blocked.2.
There is a gas leak between the outlet of the sole-3.
noid and the 1140DD cylinder. This also includes
the 357HCJB O-ring seal on the piston inside of the
cylinder.
The second condition can be eliminated by replacing
the tubing and clearing all connections.
The third condition can be eliminated by following the
procedure outlined in the section servicing the O-rings
on the 966DD2 piston and carefully inspecting the 1/8
nylon pressure hose and associated compression fittings
for leaks while this circuit is maintained at operating
pressure, using the calorimeter I/O diagnostics. A minute leak will result in a significant reduction in upward
thrust.
Confirm Correct Operation of the A1251DD Solenoid Valve
If the piston does not move, it is worthwhile at this
point to confirm that both sections of the A1251DD are
working properly (Figure F-7). For the location of the
A1251DD assembly (Figure F-4).
Disconnect the 1/8 nylon pressure hose at the elbow
connection nearest the back panel by using a 7/16
wrench. Apply power to the unit and re-enter the I/O
diagnostics. Turn the exhaust output on. The solenoid
should click and oxygen should flow from the elbow
connection on the A1251DD. Turn the exhaust output
off and re-connect the nylon pressure hose. Disconnect
the 1/8 nylon pressure hose at the middle connection.
Activating the bomb seal output should produce a click
from the solenoid and a flow of oxygen at the elbow.
Turn off the bomb seal output and reconnect the nylon
pressure hose. If neither solenoid produces a flow
of gas when activated and the O2 FILL key does not
produce a flow of gas, then, in all likelihood, the 527VB
flow restrictor is plugged and should be replaced. If
only one of the solenoids sources gas when activated,
then the problem must be further diagnosed as either
being electrical (I/O board, solenoid coil or external
wiring) vs. mechanical (in the valve) and dealt with in
an appropriate manner.
If either solenoid sources gas when it is off (i.e. leaks)
then replacement of the entire A1251DD solenoid assembly is indicated. For reference purposes, the normal
upward thrust generated by the 966DD2 piston is 50
pounds. The downward thrust is 20 pounds. Far less
than 20 pounds are required to move the piston in either
direction when the bomb is not pressurized.
The first condition can be eliminated by cleaning or
replacing the 527VB restrictor.
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JACKET FILL AND COOLING PROBLEMS
Jacket Fill Error – A problem has been detected while
attempting to fill the bomb jacket; please correct the
problem and press ‘OK’ to continue…
Error – Could not cool the bomb successfully; check
water supply and drain.
Jacket Fill Error: When the water level in the jacket
drops a level switch closes. This tells the CPU board
(through the I/O board) that more water is needed in
the jacket. If the jacket is still low after 10 minutes this
error will be generated. Pressing ‘OK’ will restart the
jacket fill process. To troubleshoot this error start with
step 3 below.
Cooling Error: At the end of the test cool water is
pumped into the bucket to bring down the temperature
of the cylinder quickly. If it takes too long to cool then
this error is generated.
There are several things to check for this cooling error.
The drain tubing should go straight to the water handling system or sink. The drain works by gravity. If
water backs up in the drain it can cause cooling problems.
The cooling water could be too warm. The cooling
water should be between 10 and 25 °C. The higher the
temperature the longer it can potentially take to cool the
bomb. The following steps assume that there is a water
handling system present.
Look at the display and note the temperature. The 1.
temperature should not read higher than 25 °C.
Take the top off the water handling system and 2.
look inside. There are two tubes. The shorter tube
should have water coming out of it in a good stream
into the top of the reservoir. If it doesn’t then the
recirculation pump in the water handling system is
bad (A308HWEE). The other tube should go to the
bottom of the reservoir.
Turn off the water handling system.3.
Remove the tube from the water input at the back of 4.
the 6300.
Get a bucket or point the hose into a sink or some-5.
thing.
Turn on the water handling system. Water should 6.
be pumped out very quickly (faster than 2 liters/
min). If water does not come out or is not very fast
then the A1418DD output pump on the water handling system is bad. Turn off the water handling
system.
Remove the 1245DD water filter. This is the fitting 7.
that attaches to the tubing that you took off in step
4. See the A1257DD Water Regulator Assembly
figure in Appendix F of the manual for a picture.
Attach the tube from the water handling system to 8.
1245DD water filter.
Turn on the water handling system. Water should 9.
be pumped out at the same rate that you saw in step
6. If the water flow is less than the 1245DD needs
to be cleaned or replaced.
Turn off the water handling system and re-attach 10.
the water filter and tube to the back of the 6300.
Refill the water handling system if it needs it. Turn
the water handling system back on.
Remove the lower cover of the 6300. This will give 11.
a view of all the solenoids and much of the tubing.
Find the A1275DD Cold Water Solenoid assembly. 12.
It is located on the bottom left of the calorimeter as
you face the front. Coming out of the front of this
solenoid is a right angle hose barb and a hose. Follow the hose to the other end (another right angle
hose barb that goes into the jacket reservoir) and
disconnect the tubing there.
Get a beaker capable of measuring 600 ml.13.
Go to the Diagnostics Menu and then to the I/O 14.
Diagnostics Menu.
Put the head into the calorimeter and lock it in 15.
place.
Turn on the H2O Fill solenoid. After a few sec-16.
onds (10 seconds or so) water should start to flow
through the disconnected tube.
Time the water flow into the beaker. The water 17.
should flow at a rate of 400 – 600 ml/min. If the
flow is less than 400 ml/min the water regulator
needs to be adjusted. Loosen the 1343DD retaining nut on the 1244DD regulator (note that this is
black plastic on black plastic and may be hard to
see initially). Turn the black plastic slotted screw
clockwise (to the right) to increase the water flow.
Adjust the water flow for approximately 500 ml/
min. Tighten the 1343DD retaining nut (this helps
keep the setting from shifting over time).
Reattach the hose to the hose barb going into the 18.
jacket reservoir.
Reinstall the cover.19.
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MAINTENANCE & TROUBLESHOOTING
9
BOMB REMOVAL AND REPLACEMENT
To service or remove the bomb cylinder from the bucket
assembly, remove the 941DD Wedge with needle nose
pliers. Remove the 668DD Check Valve from the bomb
cylinder. Remove the two SA1631RD018 Machine
Screws (see Figure F-20). Then remove the 942DD
Bushings and the 1081DD Quad-ring.
Carefully lift the bucket and bomb assembly out of
the air chamber and position horizontally on the
calorimeter to remove the 925DD Oxygen Bomb
Retainer Nut (see Figure F-19). Now the cylinder can
be removed from the bucket assembly. Note the position
of the locating pin.
To replace, follow these steps in reverse.
6300 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 and Pretest buttons dim.
The Start and Pretest buttons will be dim (not lit) when
the calorimeter is not ready to begin a test or pretest.
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 10
minutes before the Start and Pretest buttons light 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 and the test run is aborted.
If the cotton thread is gone when the bomb head is
extracted, the thread simply failed to ignite the sample.
In most cases, the sample can be re-run with a new
thread.
If the thread is present, make sure it is dry. If the
thread is dry, it is best to check and/or change the
metal heating wire. If it is wet, replace it and re-run the
sample if no sample has adhered to the wet thread.
The Lid has Failed to Lock or is not Closed Properly.
This error will be reported when the controller fails to
detect continuity through the bomb ignition circuit.
The most probable cause will be either a poor electrical
connection between the bomb’s internal electrodes and
the fuse wire, carbon build up on the electrodes or a fuse
wire that has burned out.
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.
The calorimeter suspects that there is a short and shuts
the system down in order to “save” itself. This is a fairly
normal occurrence if the lab temperature is very cool
at night. It is acceptable practice to ignore the warning
and re-start the unit. However, if this error occurs
more than three times in a row, then it may be a true
thermistor problem and the user should contact Parr
Technical Service.
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:
907DD failing (check valve head)
•
Poor jacket water circulation due to a kinked hose •
or insufficient water in the tank.
A bomb leak.
•
Poor bucket stirring.•
Leaking bucket water solenoid.•
Metal to metal contact between the bucket and the •
jacket.
• Lid not tight may be high in back.
Could Not Cool the Bomb Successfully.
The calorimeter has failed to establish the desired cool
down temperature within the time allowed. See Jacket
Fill and Cooling Problems section on page 47.
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:
Poor jacket water circulation due to a kinked hose
•
or insufficient water in the tank.
A bomb leak.
•
Poor bucket stirring.•
Leaking bucket water solenoid.•
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9
MAINTENANCE & TROUBLESHOOTING
Rinse Tank Level May Be Low.
The controller decrements the rinse tank counter each
time the bomb is rinsed. This message will be issued
when the counter is at or below zero when the bomb
rinse sequence is executed. This message is a reminder
that the rinse tank needs refilling, followed by a manual
resetting of the bomb rinse counter.
There Is A Problem With The Bucket Thermistor.
Possible electrical open. (1416E left side of bucket at
bottom):
Check connection to board.
•
Check quick disconnect.•
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.
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 noncurrent tests.
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.
Jacket Fill Error.
A timer is started whenever the jacket water tank needs
to be filled or topped off. If the jacket fill time exceeds
ten minutes, this error or warning will be issued and
the jacket fill process is halted. If the heater and pump
are on, they are turned off. Pressing the OK key on
the warning/error prompt box will restart the jacket
filling process. The heater and pump can’t be started
until the jacket water tank is completely filled. Repeated
or persistent errors or warnings are an indication of a
problem. See Jacket Fill and Cooling Problems section
on page 47.
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 counter on Calibration
Data and Control page for appropriate bomb number.
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APPENDIX A
MENU OPERATING INSTRUCTIONS
Help:
Press the HELP key on any screen to display the explanation text for that screen.
A
MENU OPERATING
INSTRUCTIONS
The settings and controls are organized into nine main
sections or pages which comprise the Main Menu.
This appendix describes all pages of the menu-based
operating system of the 6300 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.
MAIN MENU
Abort:
This key appears in the START key location while a test
or pretest is running. Pressing this key will abort the test
or pretest in progress.
:
This key appears in the Escape key location when the
main menu is displayed. This key is used to shut down
the calorimeter program before turning off the power.
CALORIMETER OPERATION MENU
The calorimeter will normally be operated from the
Calorimeter Operating Page, although tests can always
be started from any menu page.
Escape Key:
Selecting the ESCAPE key on any menu will return you
to the menu one level up.
Main Menu Key:
Selecting the MAIN MENU key on any menu will return you to the screen pictured on the right of this page.
Start Key:
Press the START key to begin any Determination or
Standardization run.
Report:
Press the REPORT key to begin the reporting process.
Operating Mode:
Sets the operating mode by toggling between Standardization (for instrument calibration) and Determination
(for test runs).
Temperature Graph:
Press this key to display a real-time plot of the bucket
and/or jacket temperature on the Temperature vs. Time
Plot screen.
Bomb/EE:
Used to identify the bomb presently installed in the
Calorimeter and its EE value.
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A
MENU OPERATING INSTRUCTIONS
CALORIMETER OPERATION MENU
(C
ONTINUED)
Start Preweigh:
This key is used to start the sample pre-weigh 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.
Heater and Pump:
The heater and pump must only be turned on after the
calorimeter water tank is filled with water.
Note:
The heater and pump must be turned ON to bring the
jacket to the correct starting temperature before testing can
commence.
Start Pretest:
This key is used to initiate a pretest cycle. A pretest
will cycle the calorimeter through the fill and cool/
rinse process. This function is used to pre-condition the
calorimeter.
TEMPERATURE PLOT SETUP MENU
Enable Bucket:
Toggles ON/OFF.
Bucket Autoscale:
Toggles ON/OFF.
TEMPERATURE VS. TIME PLOT
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.
Enable Jacket:
Toggles ON/OFF.
Jacket Autoscale:
Toggles ON/OFF.
Time Mode:
Toggles between Autoscale, Window, and Range.
Bucket Plot Symbol:
Toggles between:
No Point
•
Small Dot•
Round•
Square•
Up Triangle•
Down Triangle•
Diamond•
Bucket Min Value:
Press this key to access its numeric dialog box to set a
minimum bucket value.
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MENU OPERATING INSTRUCTIONS
A
Jacket Plot Symbol:
Toggles between: (same as Bucket Plot Color, p. 54).
Jacket Min Value:
Press this key to access its numeric dialog box to set a
minimum jacket value.
Time Window:
Sets the time scale for the X-axis.
Time Units:
Toggles between minutes and seconds.
Bucket Plot Color:
Toggles between:
Red
•
Green•
Yellow•
Blue•
Magenta•
Cyan•
White•
Black•
Bucket Max Value:
Press this key to access its numeric dialog box to set a
maximum bucket value.
OPERATING CONTROLS MENU
Method of Operation:
Offers an operating mode of either dynamic or equilibrium. In most cases, the dynamic mode with its curve
matching capability will save approximately 3-4 minutes
per test and will produce the same operating precision
as the slower equilibrium mode.
Reporting Units:
Offers a choice of Btu/lb, cal/g, J/kg, or MJ/kg for the
reporting units. A user selected set of reporting units
may be chosen by selecting “other”.
Jacket Plot Color:
Toggles between: (same as Bucket Plot Color, p. 54).
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 display.
Time Maximum:
Press this key to access its numeric dialog box to set the
greatest amount of time for the display.
Spiking Correction:
Accesses the Spike Controls sub-menu:
“Spiking” is the addition of material, such as benzoic
acid or mineral oil, to samples which are difficult to
burn in order to drive the combustion to completion.
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A
MENU OPERATING INSTRUCTIONS
OPERATING CONTROLS MENU (CONTINUED)
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 com-
bustion 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 sub-menu keyboard.
Note:
The precision of tests with fixed spikes can be no better
than the accuracy of the spike weight.
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.
Bomb Rinse Tank Controls:
Accesses sub-menu - Bomb Rinse Tank Control. Wash
water for the bomb is drawn from the Bomb Rinse
Tank. Users who wish to collect the bomb washings for
acid titrations or further analysis will want to fill it with
distilled or other suitable water.
Report Rinse Tank Empty.• When turned on the
calorimeter will notify the user when it believes
the rinse tank is empty based upon capacity of
tank and number of tests.
Rinse Tank Capacity.• Sets the number of tests
available from a full container. If the rinse timing controls have been changed, then the value
must be changed proportionally.
# Rinses Left.• This value provides an estimate of
how many rinses are left in the tank. This number is simply a counter not an actual measurement of the volume in the tank.
Reset Rinse Tank Counter.• Resets the counter
when the rinse tank has been refilled. This
counter must be reset after the rinse tank is
refilled.
Rinse Time.• This value establishes the time that
the rinse water solenoid is turned ON for each
rinse cycle. When the rinse water solenoid
is ON, distilled water from the rinse tank is
pumped, under pressure, into the bomb cylinder. This rinses the cylinder walls and the
bomb head. These rinsings are then pooled and
collected at the exhaust port of the calorimeter.
The factory default value is 2.5s. This value,
along with the # of rinse cycles, determines the
total volume of recovered rinse. These default
values will yield a total of 50 ml (approx.) of
bomb washings.
56
Rinse Flush Time.• This value is used to establish
a time between rinse cycles. During this time
the rinse solenoid is turned OFF. This off time
permits the rinse water to drain out before the
next rinse cycle begins. The factory default
value is 2s.
Clear Time.• This time value is used to establish a
post-rinse oxygen filling time for the bomb. This
step is used to clear the lines and valves of any
residual rinse water prior to the next test. The
factory default value is 10s.
# of Rinse Cycles.• This value establishes the
number of distinct rinse cycles used to rinse
the bomb. The factory default value is 3 rinse
cycles.
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MENU OPERATING INSTRUCTIONS
A
“Other” Multiplier:
Press this key to display the Other Multiplier dialog
box, where the user can enter a final multiplier to be
used when the reporting units are set to “Other”.
Calibrate Touchscreen:
This key prompts the user to touch the screen at predefined points in order to facilitate touch screen calibration. It is important that a touch screen stylus, rather
than a finger, be used in order to realize an accurate
calibration.
LCD Backlight Timeout:
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 brightness on the LCD display for optimum
viewing.
Date & Time:
Accesses a sub-menu to set the current date and time.
Date.• Displays current date and accesses submenu on which date is set in (YY/MM/DD)
format.
Time.• Displays current time and accesses submenu on which time is set in (HH:MM) format.
Time Zone.• Displays the selected time zone in
relation to Greenwich Mean Time. Pressing this
key will step through the time zones and automatically adjust the time setting.
Volume Level Adjust:
Opens a window with a slide adjustment to set the
volume of the key cliks and alarms of the calorimeter.
Default is 85%.
Print Error Messages:
When turned ON, all error messages will be printed on
the printer as well as displayed on the screen. When
turned OFF, messages will only display on the screen.
Language:
Steps the Calorimeter through the installed operating
languages.
PROGRAM INFORMATION AND CONTROL
MENU
Software and Hardware Info:
This screen displays important information such
as the main software version, I/O board hardware
information, CPU type, I/O firmware revision, and
Controller IP address.
Settings Protect:
Provides protection for the program options and settings on the menus. If this is turned ON, the user will
be warned that enumeration keys are locked when a
key is pressed. Enumeration 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 touchscreen.
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A
MENU OPERATING INSTRUCTIONS
PROGRAM INFORMATION AND CONTROL
M
ENU (CONTINUED)
User/Factory Settings:
This key leads to a sub-menu 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.
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. (Note that the calorimeter
will not let you exit this function without re-booting the
system).
User Function Setup:
This key leads to sub-menus that support the configuration of five factory/user definable function keys. The
function keys are accessible from the Diagnostics page.
Cold Restart:
This is essentially the same as cycling power on the
unit. All valid test data will be retained during this cold
restart procedure.
CALIBRATION AND DATA CONTROLS MENU
User Setup ID.• Used to enter a unique identifier
for recalling user settings.
•
Reload Factory Default Settings.• Used to erase all
of the settings and restore the factory default
settings.
Reload User Default Settings.• Used to restore the
last saved user’s setup should the program in the
instrument be corrupted for any reason.
Save User Default Settings.• Used to record the set-
up to the memory once the user has configured
the instrument to their operating requirements.
Compare Settings With Factory Defaults.• This but-
ton 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, remote operation of the calorimeter, or
Samba Server.
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 viewing or printing. Only runs that are at final
status will be used in this calculation.
EE Max Std Deviation:
Displays the maximum relative standard deviation in
percent that will be permitted for any EE value calcu-
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MENU OPERATING INSTRUCTIONS
A
lated 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. 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 sub-menu on which this limit is set. Parr recommends 500 firings for this service interval. (Parts may
need to be replaced on a more frequent basis 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.
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:
Leads to sub-menu, Bomb 1. Displays standardization
information for bomb and bucket combinations. While
only one bomb and bucket is installed in the calorimeter
at a time, a spare may be used for servicing and for
more rapid turn-around. The respective EE values for
each bomb can be stored in memory.
Note:
For rapid turn around between tests, the user may wish to
use an extra head. Each head should be assigned a bomb
ID. On the Data Entry Controls Menu, set the Prompt for
Bomb ID to “ON”.
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 classifi cation of the instrument.
The higher the process sigma the higher the
limits for acceptable values for precision
control.
The 6300 is a .1 Process Sigma calorimeter.
Temp. Rise High Warning: • Sets a limit for the temperature rise during a test. If the temperature
rise exceeds the limit the user will be warned.
Temp. Rise Low Warning:• Sets a lower limit warning for the temperature rise during a test. If the
temperature rise is lower than this setting the
user will be warned.
The following four values are displayed for the Bomb #
shown in the title on top of the screen.
Bomb EE Value.• Displays the calculated EE
value.
# Runs, EE Val.• Displays how many runs have
been used to determine the EE value.
Rel. Std. Dev.• Displays the relative standard de-
viation for the series of tests used to determine
the current EE value in percent of the EE value.
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MENU OPERATING INSTRUCTIONS
CALIBRATION DATA AND CONTROLS MENU
(C
ONTINUED)
Bomb Fire Count.• Displays the current bomb fir-
ing 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 (on the Calibration Data and Controls
screen), the user will be informed that the bomb
is ready for service.
Name.
Enables the operator to assign a unique alpha-numeric
label for the bomb ID. The ID can be up to 8 characters.
Protect EE Value:
Toggles between OFF and ON. When set to OFF, the
6300 automatically updates the EE value as new tests
are run. When set to ON, it keeps the EE value protected, whether it has been revised manually via the
Manual EE Entry key or calculated by the instrument.
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.
Update Statistics:
If the Protect EE Value is set to OFF, pressing this
key will cause the EE Value for this Calorimeter to
be updated using all standardization runs currently in
memory to the limit established in the Calibration Data
and Controls menu. If the Protect EE value is set to
ON, this key is not functional.
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:
This key 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 key 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
Each data point represents a Standardization run used
in the calculation of the EE Value for the Bomb ID
being displayed. The left side of the graph contains the
oldest runs and the right represents the most recent. To
view the run data used for a particular data point, click
on the data point with a stylus and the run data for that
point is displayed.
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.
THERMOCHEMICAL CALCULATIONS MENU
The Thermochemical Corrections Menu permits three
types of fixed corrections for standardization (instrument calibration) runs, and the same three types for
determination (test) runs. Pressing the LEFT side of
each key toggles the correction ON or OFF. Press the
RIGHT side of each key to access the specific numeric
dialog box where that fixed value can be set. Each
value entered for these fixed corrections is used in all
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preliminary reports.
When any fixed correction is set to ON, the specified
value will be used in the final reports, and the 6300
will not prompt for actual corrections to be entered.
(If all corrections are fixed, only a final report will be
generated.)
When any fixed correction is set to OFF, during the
data entry reporting steps the user will be prompted to
enter an appropriate desired value which will be used in
the final report.
MENU OPERATING INSTRUCTIONS
Options for the Acid Correction:
Fixed HNO
Calculated HNO
Entered Total
Entered HNO
Fixed Total
These options are discussed further in Appendix B Calculations.
3
3
3
A
Standardization Corrections
Fixed Fuse Correction:
Press this key on the LEFT side to toggle ON or OFF
the fixed fuse correction for standardization runs. Press
it on the RIGHT side to access the Fixed Fuse numeric
dialog box on which the value can be set. An appropriate fixed fuse value is 50 calories.
Acid Correction:
Displays both the ON/OFF of the fixed acid
corrections for standardization runs and the value of the
correction. This key toggles the options for treatment of
the acid correction and accesses a sub-menu on which
the value is set. An appropriate fixed HNO
calories when one-gram benzoic acid pellets are used to
calibrate the instrument.
value is 8
3
Fixed Sulfur Correction:
Press this key on the LEFT side to toggle ON or OFF
the fixed sulfur correction for standardization runs.
Press it on the RIGHT side to access the Fixed Sulfur numeric dialog box on which the value can be set.
When benzoic acid is used as the calibrant, a fixed
sulfur value of 0 should be used.
Determination Corrections
Fixed Fuse Correction:
Press this key on the LEFT side to toggle ON or OFF
the fixed fuse correction for determination runs. Press
it on the RIGHT side to access the Fixed Fuse numeric
dialog box on which the value can be set. An appropriate fixed fuse value is 50 calories.
Acid Correction:
Displays both the ON/OFF of the fixed acid
corrections for standardization runs and the value of the
correction. This key toggles the options for treatment of
the acid correction and accesses a sub-menu on which
the value is set. An appropriate fixed HNO
calories when one-gram benzoic acid pellets are used to
calibrate the instrument.
Options for the Acid Correction:
Fixed HNO
Calculated HNO
Entered Total
Entered HNO
Fixed Total
3
3
3
value is 8
3
These options are discussed further in Appendix B Calculations.
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MENU OPERATING INSTRUCTIONS
THERMOCHEMICAL CALCULATIONS MENU
(C
ONTINUED)
Fixed Sulfur Correction:
Press this key on the LEFT side to toggle ON or OFF
the fixed sulfur correction for determination runs. Press
it on the RIGHT side to access the Fixed Sulfur numeric dialog box on which the value can be 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, only final reports
will be generated. If any correction value is entered and
the toggle is set to OFF, then the preliminary report will
use the displayed fixed value, but the final report will use
the value entered when prompted during the reporting
process.
Calculation Factors:
Accesses the Calculation Factors sub-menu, which
provides for setting a number of options for the way the
thermochemical corrections are applied.
Net Heat/Dry Factors:
Accesses the Net Heat/Dry Factors sub-menu, which
provides for setting the net heat of combustion and Dry
Factors Thermochemical Corrections.
Nitric Acid Factor:
Ratio of the nitric acid correction when the released
energy corresponds to 6318 calories. The default is 1.58
calories per 1000 calories of released energy.
Acid Multiplier:
This multiplier is the normality of the sodium carbonate
used during the acid correction titration. The default
value of 0.0709 allows for direct entry of the acid correction in calories. If the bomb rinses are titrated in
order to determine the acid correction, press this key to
display the Acid Multiplier numeric dialog box, where
you can change the multiplier to represent the concentration of the base (equivalents/L) or normality used
for titration. If this is the case, the acid correction is
entered as milliliters of base used to titrate the bomb
rinses.
Sulfur Value is Percent:
When set to ON, the sulfur value is being entered as
weight percent sulfur. If another system is to be used,
this must be turned OFF and the sulfur multiplier set
accordingly.
Sulfur Multiplier:
Values entered by the user to be used for the sulfur
correction are multiplied by this value to get the product into units of milliequivalents. The default number
(0.6238) requires that the sulfur value be entered in
weight percent.
CALCULATION FACTORS MENU
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Fuse Multiplier:
The fuse corrections represent the number of calories
liberated by the burning fuse wire used to ignite the
sample. If another measurement is used, the correction
factor must be entered here. Press this key to access
the Fuse Multiplier numeric dialog box and enter this
multiplier value.
Use Offset Correction (ISO):
The thermochemical calculations used for treatment of
nitric acid and sulfuric acid corrections in the ISO and
B. S. methods require an offset correction to compensate for the back titration that is made. To use these
calculations, toggle this to ON and enter the appropriate
value as the offset value.
Offset Value:
The value used when Offset Correction is turned ON.
Press this key to access the Offset Value numeric dialog
box and change its value.
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MENU OPERATING INSTRUCTIONS
A
NET HEAT/DRY HEAT FACTORS
Fixed Hydrogen:
Press the LEFT side to toggle this setting On/Off.
Press the RIGHT side to display the Fixed Hydrogen
numeric dialog box and change its value.
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.
DATA ENTRY CONTROLS MENU
Prompt for Bomb ID:
Toggles ON or OFF. 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, balance (USB) port or through the network.
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.
Fixed Moisture as Determined:
Press the LEFT side to toggle ON or OFF whether to
use the entered moisture correction. Press the RIGHT
side to access the Fixed Moisture as Determined numeric dialog box and set the value. Units are weight %.
Fixed Moisture as Received:
Press the LEFT side to toggle ON or OFF whether to
use the entered moisture correction. Press the RIGHT
side to access the Fixed Moisture as Received numeric
dialog box and set the value. Units are weight %.
Dry Calculation:
Toggles the dry calculation ON or OFF.
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MENU OPERATING INSTRUCTIONS
DATA ENTRY CONTROLS MENU (CONTINUED)
Hydrogen Entry Mode:
This key steps through the options for entering hydrogen content for calculating the net heat of combustion
either manually through the touch screen or automatically through the balance (USB) port.
Oxygen Entry Mode:
This key steps through the options for entering oxygen
content for calculating the net heat of combustion either
manually through the touch screen or automatically
through the balance (USB) port.
Nitrogen Entry Mode:
This key steps through the options for entering nitrogen
content for calculating the net heat of combustion either
manually through the touch screen or automatically
through the balance (USB) port.
Auto Sample ID Controls:
Accesses sub-menu for controlling the automatic assignment of sample identification numbers.
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. Used when the Automatic Sample ID is
set to ON. Press this key to access a sub-menu
for entering a numeric increment.
Auto Sample ID Increment.• Establishes the incre-
ment between sample numbers; used when the
Automatic Sample ID is set to ON. Press this
key to access a sub-menu for entering a numeric
increment.
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, balance (USB) port or network.
Automatic Sample ID.• When set to ON the unit
will automatically assign sample identification
numbers in accordance with parameters set by
the other three keys on this menu. When set to
OFF, the user manually enters each sample ID
when prompted to do so.
Auto Sample ID Prefix.• An entry here will be used
as a prefix for all sample IDs, if the Automatic
Sample ID is set to ON. Press this key to access
a sub-menu for entering an alphanumeric prefix.
Sulfur Entry Mode:
This key steps through the options for entering the sulfur correction value either manually through the touch
screen or automatically through the balance (USB) port.
Moisture as Determined Entry Mode:
This key steps through the options for entering the
moisture as determined correction value either manually or through the touch screen or automatically through
the balance (USB) port.
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MENU OPERATING INSTRUCTIONS
A
Moisture as Received Entry Mode:
This key steps through the options for entering the
moisture as received correction value either manually or
through the touch screen or automatically through the
balance (USB) port.
REPORTING CONTROLS MENU
Report Width:
Toggle this key to set the column width of the printer
to either 40 or 80 columns. Select 40 when the 1758
Printer is used.
Auto Preweigh ID Controls:
Accesses sub-menu, used to automatically assign
Sample ID numbers when a series of samples are pre
weighed ahead of the time they are actually tested.
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 IDs.
Next Automatic Preweigh ID Number.• Shows the
next Sample ID 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.
Automatic Reporting:
Toggles the automatic reporting ON/OFF. When ON,
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 OFF, reports will only be generated by selecting
the REPORT key.
Automatic Report Destination:
Toggles to direct the reports to the Printer or the screen
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 of finalized
reports from the report menu.
Recalculate Final Reports:
When set to ON, causes a recalculation of stored final
reports using calibration data and menu settings currently in the Calorimeter.
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MENU OPERATING INSTRUCTIONS
REPORTING CONTROLS MENU (CONTINUED)
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.
Report Schedule:
Toggles between End of Post Period and end of Cool/
Rinse. This setting determines when the report will be
printed or displayed.
COMMUNICATION CONTROLS MENU
Balance Port:
Accesses sub-menu, Balance Port Communications.
Balance Type. Toggles through the available bal-•
ance 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.
Accesses sub-menus which set the communications
protocols for the printer and balances.
Printer Port Type:
Toggles between Parr 1758 and Generic.
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Customize Balance Setting.• Sets the communication parameters for the balance. Standard
options for data bits, parity, stop bits, handshaking, baud rate and balance type are provided to
match any devices that might be connected to
these ports.
Number of Data Bits. Standard options for
»
data bits. Toggles between 7 and 8.
Parity. Standard options for parity. Choose
»
from None, Odd or Even.
Number of Stop Bits. Standard options for
»
stop bits. Toggles between 1 and 2.
Handshaking. Standard options for hand-
»
shaking. Choose from Xon/Xoff, RTS/CTS
and None
Baud Rate. Standard options for baud rate.
»
Choose from 19.2K , 9600, 4800, 2400,
1800, 1200, 600, 300, 150, 134.5, 110, and
75.
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.
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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 balance template to be
customized for unique balances or needs.
Log Balance to Display.• Directs 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.• 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.
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 allows the user to format an installed SD card
in a manner that is compatible with the calorimeter.
Note:
Formatting will erase all files on the card!
Copy Run Data to SD Card:
This key copies all test data to an SD card inserted into
the rear of the calorimeter controller. This feature is
used as a means of either archiving data or transferring
it to a PC.
Note:
Subsequent use of the same SD card will overwrite the
data currently on the card.
Copy User Settings to SD Card:
This key copies all previously saved user setups to SD.
Copy User Settings From SD Card:
This key copies all user setups previously saved to SD
back to the calorimeter controller memory. This feature
can be used to configure multiple calorimeters in an
identical manner.
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MENU OPERATING INSTRUCTIONS
RUN DATA FILE MANAGER
The white upper portion of the Run Data File Manager
screen presents all tests in memory in a scrollable window. Test attributes include filename (sample ID), test
type, status, and date. Touching anywhere in the column related to a given test attribute will sort the file list
by that attribute. Successive touches will toggle between
an ascending and descending sort.
Select:
This key is used to begin the file selection process.
The up/down (single arrow) and page up/page down
(double arrow) keys are used to scroll up and down the
file list. Pressing the select key when a file is highlighted
blue will highlight the file with a cyan color. This indicates that it is selected. Multiple files throughout the list
can be selected in this fashion.
Extend Sel:
This key selects all files between the last file selected
and the file that is highlighted in blue.
Desel All:
This key deselects all files previously selected.
DIAGNOSTICS MENU
Provides the user with the means to test many of the
components and subsystems of the calorimeter. These
capabilities should be used in conjunction with this
instruction manual in order to obtain the maximum
benefits from these capabilities.
Pretesting Cycle:
This key initiates a pretest to run the calorimeter
through the fill and cool/rinse cycles. This function is
used to pre-condition the calorimeter if it has been sitting idle for an extended period of time (greater than 15
minutes).
Test Ignition Circuit:
Activates the ignition circuit. A volt meter can be
placed across the firing connections to ensure that the
actual firing charge is reaching these contacts.
Data Logger:
Displays ON/OFF status and accesses the Data Logger
Controls Menu for setting the specific logging controls.
Rename:
This key allows the user to rename the blue highlighted
filename.
Delete:
This key deletes all selected files.
Convert Type:
This key allows one or more selected tests to be converted from determinations to standardizations and vice
versa.
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Data Logger.• This key toggles the data logging
function ON/OFF.
Data Log Interval.• This key displays the inter-
val of which the selected data is logged. The
interval in seconds is defined in the Select Data
Items sub-menu (normally 12 seconds). This
roughly matches the update interval for the
bucket temperature.
Data Log Destination.• Options are logfile, printer
or both. When the logfile option is selected, the
logfile is located at /flash/log/datalog.csv. The
maximum allowed size for this file is roughly
one megabyte. If the file reaches this size, logging is halted.
MENU OPERATING INSTRUCTIONS
keys for fifteen items that can be individually
selected for logging. By default, both the bucket
and jacket temperatures are logged. All records
are date and time stamped. Helpful items to log
are:
D0 - Corrected calorimeter drift rate»
Tsum - Accumulated temperature rise»
T1 - Extrapolated temperature rise»
C0 - Temperature conversion counter»
Data Log Format.• Toggles between Text Format
and Data Format (csv). Data is either logged
with the supporting tag information (text) or in
a comma separated variable (csv) data format
as selected by the user. The text setting is useful
if the data log destination is a printer. The data
(csv) format is especially useful if the data is
ultimately transferred to another computer for
post processing, graphing, etc. The log file can
be transferred to another computer via FTP.
Delete Data Log File.• When this key is pressed the
contents of the data log file are deleted.
View System Log:
This key accesses its sub-menu which displays the contents of /flash/log/messages. This file is used primarily
to log application program debug messages. Press the
PRINT key to print these messages.
User Defined Functions:
This key leads to a sub-menu that offers five special
purpose user/factory definable function keys.
A
Select Data Log Items.• Press this key to access
the Data Log Items sub-menu, which provides
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MENU OPERATING INSTRUCTIONS
DIAGNOSTICS MENU (CONTINUED)
Combine Det. Reports.• Pressing this key com-
bines all determination reports into a single file
named /tmp/bigdetfile.txt.
Combine Std. Reports.• Pressing this key com-
bines all determination reports into a single file
named /tmp/bigstdfile.txt.
Rinse Bomb:
This key initiates a bomb rinse. This function can be
used to clean out the cylinder in the event a sample is
spilled inside the cylinder.
Instrument Monitor:
This key accesses its sub-menu screen which provides a
summary of most of the important instrument parameters. This screen is used to detail the course of a test
or to observe the heating/cooling performance of the
calorimeter.
View System Info:
Press this key to display a screen with current operating
system information/statistics such as:
Processes and their associated PIDs
•
Memory•
Mass Storage•
Network•
Press the PRINT key to print this information.
I/O Diagnostics:
Press this key to display the I/O Diagnostics sub-menu,
which allows the user to manipulate digital outputs for
troubleshooting. The I/O Diagnostics screen is used
to display the digital outputs at a basic level for troubleshooting. Both the bucket and jacket temperatures are
also displayed on this screen. Any output can be
selected using the left and right arrow keys. The selected output is turned ON (1) or OFF (0) using the 1 and 0
keys. Prior to entering the Diagnostics Menu, the controller stores the present state of the outputs. This state
is restored when you exit this screen. Digital outputs
cannot be manipulated while a test is in progress.
View Instrument Log:
Press this key to display a screen with contents of the
/tmp/instlog file. It contains a sequential log of the
instrument’s processing. Press the PRINT key to print
this log.
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APPENDIX B
CALCULATIONS
CALCULATING THE HEAT OF COMBUSTION
The 6300 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:
Hc =
Where:
H
c
T = Observed temperature rise.
W = Energy equivalent of the
e
1
e
2
e
3
m = Mass of the sample.
These calculations are made in calories, grams, and
degrees Celsius and then converted to other units if
required.
WT-e
= Gross heat of combustion.
calorimeter being used.
= Heat produced by burning the
nitrogen portion of the air trapped
in the bomb to form nitric acid.
= The heat produced by the
formation of sulfuric acid from the
reaction of sulfur dioxide, water
and oxygen.
= Heat produced by the heating wire
and cotton thread.
- e2 - e
1
m
3
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 Appendix
C - Standardization. It is an expression of the amount
of energy required to raise the temperature of the
calorimeter one degree. It is commonly expressed in
calories per degree Celsius. Since it is directly related to
the mass of the calorimeter, it will change whenever any
of the components of the calorimeter (i.e. the bomb,
bucket or amount of water) is changed.
THERMOCHEMICAL CORRECTIONS
Nitric Acid Correction.
In the high pressure oxygen environment within the
oxygen bomb, nitrogen that was present as part of the
air trapped in the bomb is burned to nitric oxide which
combines with water vapor to form nitric acid. All of
this heat is artificial since it is not a result of the sample
burning. The nitric acid correction removes this excess
heat from the calculation.
Sulfur Correction.
In the oxygen rich atmosphere within the bomb, sulfur
in the sample is oxidized to sulfur trioxide which
combines with water vapor to form sulfuric acid. This
liberates additional heat over the normal combustion
process which converts sulfur to sulfur dioxide. The
sulfur correction removes this excess heat from the
calculation.
Fuse Correction.
The fuse correction in the 6300 Calorimeter is
significantly different than the correction used in earlier
model Parr calorimeters where the correction was made
to compensate for the amount of fuse wire burned
in the test. There are two components to the fuse
correction in the 6300 Calorimeter:
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.
B
Temperature Rise.
The 6300 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).
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
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B
CALCULATIONS
THERMOCHEMICAL CORRECTIONS
(C
ONTINUED)
be calculated. In the 6300 Calorimeter this is a fixed
correction of 10 calories per test.
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.
ASTM AND ISO METHODS DIFFER
the user prefers. Care must be used to ensure the proper
corrections are applied, and the calculations made are
consistent with the procedure used.
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 HNO
correction of 8 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.
. A
3
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 6300 Calorimeter can be set up to apply the acid
correction by either the ASTM or ISO convention, as
Please note that the values entered into the test report
appear as entered in the report. Values for e
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 e
ASTM treatment of e1 and e2.
Note:
Please review the following section on Acid and Sulfur
Corrections. Different standard test methods use different
values for the heat of formation of sulfuric acid.
These differences are generally insignificant. The 6300
Calorimeter uses the most recent, published values for all
thermochemical data.
Thermochemical Calculation Details
Traditionally, standard solutions and procedures have
been established to simplify the calculations related to
and e2, above, is equal to the sum of the
1
, e2 and
1
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CALCULATIONS
B
the thermochemical corrections. The 6300 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.
FUSE CORRECTION
The fuse correction applied by the calorimeter is
calculated as:
e
= (fuse value) (fuse multiplier from
3
“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.
calculation factors page)
= (entered value)(fuse multiplier from
thermochemicals page)
sample (weight %).
Molecular weight of sulfur
• is 32.06.
Equivalent weight of sulfur in H
•
half of the molecular weight).
• is 14.1 calories/
Heat of formation of nitric acid
milliequivalent.
• (from SO
Heat of formation of sulfuric acid
36.1 calories/milliequivalent.
• is the mass of sample burned in the
Sample mass
bomb (grams).
• is multiplied by the product of the
Sulfur multiplier
user entered sulfur value and the sample mass to
arrive at the number of milliequivalents of sulfuric
acid in the bomb washings.
Sulfur Correction:
e2 = (percent sulfur)(sample mass)(sulfur multiplier)
(heat of formation of H2SO4).
Acid Correction:
In the 6300 there are a number of settings for the acid
correction.
is 16.03 (one
2SO4
) is
2
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 ignition
thread supplied by Parr.
ACID AND SULFUR CORRECTIONS
Total acid• is the amount of base required to titrate
the bomb washings (milliliters).
• is that portion of the total acid in the
Nitric acid
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
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 1138 bomb the default nitric acid value is 8 and
acid multiplier is .0709. The heat of formation of nitric
acid is 14.1 calories/milliequivalent so the calculation
is:
e1 = (8)(.0709)(14.1) or e1 = 7.9975 calories (rounds to 8)
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.
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CALCULATIONS
ACID AND SULFUR CORRECTIONS
(C
ONTINUED)
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)
Using the default acid and sulfur multipliers as well
as a heat of formation of nitric acid of 14.1 cal/
milliequivalent a 1 gram sample with 25 ml of washings
and 2 % sulfur would result in the following calculation:
e1 = [((25)(.0709)) – (2)(1)(.6238)] 14.1
e1 = [(1.7725) – (1.2476)] 14.1
e1 = [.5249] 14.1
e1 = 7.40109 calories
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)
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Parr Instrument Company
Example: For a test run with energy equivalent of
927.4022 and a corrected temperature rise of 6.892
would result:
e1 = (1.58/1000)(927.4022)(6.892)
e1 = 10.0988 calories
The calculated nitric acid method can be applied
to samples containing up to 2% nitrogen without
introducing a significant error in the resulting heat of
combustion value.
Table B-1
Settings for ISO & BSI Methods
Page Line Setting Value
Thermochemical
Corrections
Calculations
Factors
Acid Correction
(STD)
Fixed Sulfur STD Off 7
Acid Correction
(DET)
Fixed Sulfur DET Off 7
Acid Multiplier 0.154
Sulfur Value is
Percent
Sulfur Multiplier 0.1
Use Offset
Correction
Offset Value -43.5
Offset Value -43.5
Entered
HNO
Entered
HNO
Off
On
13
3
13
3
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 (e
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
(e
). Therefore the additional correction which must be
1
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 e
percentage point of sulfur per gram of sample.
formula, as 13.7 calories (44.0/32.06) for each
2
). This is adjusted by a
1
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CALCULATIONS
B
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 6300 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:
Hc =
Where:
Hcs = Heat of combustion of the spiking
M
s
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-e
= Mass of spiking material
- e2 - e3 - (Hcs)(Ms)
1
m
material (cal/g)
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.
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.
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 6300 Calorimeter can automatically
compensate for the addition of spiking materials to
these samples. The calculations are modified in these
cases as follows:
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
per pound can be calculated as follows:
H
net
To calculate H
D5865.
1.8Hc - 91.23H
=
(Liquid fuels, ASTM D240)
for solid fuels please refer to ASTM
net
net
Btu
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STANDARDIZATION
C
APPENDIX C
STANDARDIZATION
STANDARDIZING THE CALORIMETER
The Energy Equivalent Factor.
The term “standardization”, as used here, denotes the
operation of the calorimeter on a standard sample from
which the energy equivalent or effective heat capacity of
the system can be determined. The energy equivalent,
W or EE of the calorimeter is the energy required to
raise the temperature one degree, usually expressed as
calories per degree Celsius. Standardization tests should
be repeated after changing any parts of the calorimeter,
and occasionally as a check on both the calorimeter and
operating technique.
Standardization Procedure.
The procedure for a standardization test is exactly
the same as for testing a fuel sample. Use a pellet of
calorific grade benzoic acid weighing not less than 0.9
nor more than 1.1 grams. The corrected temperature
rise, T, is determined from the observed test data and
the bomb washings are titrated to determine the nitric
acid correction. The energy equivalent is computed by
substituting the following equation:
STANDARD MATERIALS
A bottle of 100 one-gram benzoic acid pellets (Part
No. 3415) is furnished with each calorimeter for
standardizing purposes. The Parr benzoic acid has
been calibrated against NIST benzoic acid. Additional
benzoic acid pellets can be obtained from Parr.
For very high precision measurements, a primary
standard benzoic acid powder can be purchased from
the National Institute of Standards & Technology,
Washington, D.C.
It is not common to have sulfur in standard materials,
or to use spikes in standardizations, but the capabilities
have been included in this calorimeter.
Users should take great care to ensure that the
conditions during standardization runs and
determinations are as identical as possible.
Caution:
Benzoic acid must always be compressed into
a pellet before it is burned in an oxygen bomb
to avoid possible damage from rapid combustion of the
loose powder. This is best accomplished by using a Parr
2811 Pellet Press.
AUTOMATIC STATISTICAL CALCULATIONS
W =
Where:
W = Energy equivalent of the
H = Heat of combustion of the
m = Mass of the standard benzoic acid
T = Temperature rise in °C.
e
1
e
2
e
3
Hm + e
calorimeter in calories per °C.
standard benzoic acid sample in
calories per gram.
sample in grams.
= Correction for heat of formation of
nitric acid in calories.
= Correction for sulfur which is
usually 0.
= Correction for heating wire and
combustion of cotton thread.
+ e2 + e
1
T
3
The 6300 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
6300 Calorimeter automatically determines and uses up
to ten tests in its memory and will update the EE Value
as additional standardizations are run. Only Final Tests
will be used in determining and updating EE values.
These values, the number of tests, and the relative
standard deviation for the tests used in determining the
EE value are stored in the Calibration Data Page under
the EE Value for each bomb.
The user can chose to turn off the automatic averaging
and updating procedure and protect the EE Values by
turning ON the protection feature for the appropriate
bomb on the Calibration Data and Control Page using
Protected EE Value.
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STANDARDIZATION
AUTOMATIC STATISTICAL CALCULATIONS
(C
ONTINUED)
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.
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.
Values are in J/g.
NUMBER OF
OBSERVATIONS
IN A GROUP
1 79.4
2 97.5 0.261% 56.1
3 115.3 0.228% 45.8
4 124.3 0.209% 39.7
5 130.1 0.196% 35.5
6 134.3 0.187% 32.4
7 137.6 0.181% 30.0
8 140.4 0.175% 28.1
9 142.7 0.171% 26.5
10 144.7 0.167% 25.1
11 146.4 0.164% 23.9
12 147.9 0.161% 22.9
13 149.4 0.159% 22.0
14 150.7 0.156% 21.2
15 151.8 0.154% 20.5
16 153.0 0.153% 19.8
17 154.0 0.151% 19.2
18 154.9 0.150% 18.7
19 155.8 0.148% 18.2
20 156.7 0.147% 17.7
21 157.4 0.146% 17.3
22 158.2 0.145% 16.9
23 158.9 0.144% 16.5
24 159.5 0.143% 16.2
25 160.2 0.142% 15.9
UCL FOR THE RANGE
(HIGH – LOW)
WITHIN THE GROUP
UCL FOR THE
RSD WITHIN
THE GROUP
The user can elect to have any number of stored
standardization runs used in determining the EE 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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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.
Values are in cal/g.
STANDARDIZATION
C
NUMBER OF
OBSERVATIONS
IN A GROUP
1 19.0
2 23.3 0.261% 13.4
3 27.5 0.228% 10.9
4 29.7 0.209% 9.5
5 31.1 0.196% 8.5
6 32.1 0.187% 7.7
7 32.9 0.181% 7.2
8 33.5 0.175% 6.7
9 34.1 0.171% 6.3
10 34.6 0.167% 6.0
11 35.0 0.164% 5.7
12 35.3 0.161% 5.5
13 35.7 0.159% 5.3
14 36.0 0.156% 5.1
15 36.3 0.154% 4.9
16 36.5 0.153% 4.7
17 36.8 0.151% 4.6
18 37.0 0.150% 4.5
19 37.2 0.148% 4.3
20 37.4 0.147% 4.2
21 37.6 0.146% 4.1
22 37.8 0.145% 4.0
23 37.9 0.144% 4.0
24 38.1 0.143% 3.9
25 38.3 0.142% 3.8
UCL FOR THE RANGE
(HIGH – LOW)
WITHIN THE GROUP
UCL FOR THE
RSD WITHIN
THE GROUP
MAXIMUM PERMISSIBLE DEVIATION
OF THE GROUP MEAN FROM THE
ACCEPTED VALUE OR GRAND MEAN
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STANDARDIZATION
Table C-3
Calorimeter Control Limit Values in BTU/lb When Benzoic Acid is Used as a Test Sample
Accepted heat of combustion taken as 11373 BTU/lb.
Instrument precision 0.10%.
Control limits based on 99% confidence (3 sigma) values.
Values are in BTU/lb.
NUMBER OF
OBSERVATIONS
IN A GROUP
1 34.1
2 41.9 0.261% 24.1
3 49.6 0.228% 19.7
4 53.4 0.209% 17.1
5 55.9 0.196% 15.3
6 57.8 0.187% 13.9
7 59.2 0.181% 12.9
8 60.4 0.175% 12.1
9 61.3 0.171% 11.4
10 62.2 0.167% 10.8
11 62.9 0.164% 10.3
12 63.6 0.161% 9.8
13 64.2 0.159% 9.5
14 64.8 0.156% 9.1
15 65.3 0.154% 8.8
16 65.8 0.153% 8.5
17 66.2 0.151% 8.3
18 66.6 0.150% 8.0
19 67.0 0.148% 7.8
20 67.4 0.147% 7.6
21 67.7 0.146% 7.4
22 68.0 0.145% 7.3
23 68.3 0.144% 7.1
24 68.6 0.143% 7.0
25 68.9 0.142% 6.8
UCL FOR THE RANGE
(HIGH – LOW)
WITHIN THE GROUP
UCL FOR THE
RSD WITHIN
THE GROUP
MAXIMUM PERMISSIBLE DEVIATION
OF THE GROUP MEAN FROM THE
ACCEPTED VALUE OR GRAND MEAN
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COMMUNICATIONS INTERFACES
D
APPENDIX D
COMMUNICATIONS
INTERFACES
USB PORT
USB Connection
The 6300 Calorimeter is equipped with a USB port for
connection to either a 40 or 80 column printer and/or a
computer.
The default parameters for the 6300 Calorimeter are set
up for use with the Parr 1758 Printer.
BALANCE AND PORT INPUT DRIVER
S
PECIFICATIONS
The 6300 Calorimeter supports input from multiple
balance types. Additionally, a generic input driver is
provided for communications with balances that do
not conform to the supported protocols. A new feature
supported by all balance input drivers is the ability to
change the expected number of characters in the data
field. The number of data characters indicated for each
of the drivers, below, are default values. This feature virtually eliminates the need for balance input drivers to be
re-written in the event the balance manufacturer elects
to alter the output string of a balance when new models
are introduced.
The format of an unknown balance can be determined
by logging the balance output to the printer attached to
the calorimeter. Those protocols which send a command string to the balance will do so while logging is
active. In order for the logging to produce meaningful
results, the cable connecting the balance to the balance
input port of the calorimeter must be correctly wired or
configured. In addition, the specifics of the data frame,
such as the baud rate, # of data bits, parity, # of stop
bits and handshaking (if used) must be the same for
both the balance and the calorimeter.
METTLER 011/012 BALANCE INTERFACE
Field Length
ID 2
space 1
data 9
space 1
g1
CR 1
LF 1
The ID field must contain “S_” to indicate a stable
mass. The data field contains the current mass, right
justified, with a decimal point. The balance should be
configured to send continuously.
SARTORIUS BALANCE INTERFACE
Field Length
polarity 1
space 1
data 8
space 1
stability 2
CR 1
LF 1
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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GENERIC INTERFACE
Field Length
data 9
CR 1
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
6300 Data File Naming Convention
Test data files are named with the following convention.
Test Type Filename
Preliminary
Standardization
Final Standardization <ID>.std.finl.csv
Preliminary
Determination
Final Determination <ID>.det.finl.csv
Pre-weigh <ID>.---.pwgh.csv
Table D-2
6300 Calorimeter Run Data Template
Field Description
SampleID char[16]
Timestamp MM/DD/YY HH:mm:ss
Mode 0 = determination, 1 = standardiza-
tion
Method 0 = equilibrium, 1 = dynamic
State 0 = preweigh, 1 = preliminary, 2 =
final
Units 0 = MJ/kg, 1 = Btu/lb, 2 = cal/g, 3
= J/kg, 4 = other
UnitMultIfOther
BombID [1,4]
BombEE bomb energy equivalent
SampleWt sample weight
SpikeWt spike weight
Fuse fuse value
unit multiplier in effect at time of
report
<ID>.std.plim.csv
<ID>.det.plim.csv
FuseFinal fuse value is final
Acid acid value
AcidFinal acid value is final
Sulfur sulfur value
SulfurFinal sulfur value is final
Hydrogen hydrogen value (net calc option)
HydrogenFinal hydrogen value is final (net calc op-
tion)
MAD moisture as determined value (dry
calc option)
MAD Final moisture as determined is final
JacketTemp jacket temperature
InitTemp initial temperature
DeltaT temperature rise
HOC gross heat of combustion
NetHOC dry net HOC (net calc options en-
abled)
DryHOC dry gross HOC (if dry calc option
enabled)
DryNetHOC dry net HOC (if both dry and net
calc options enabled)
Oxygen oxygen value (net calc option)
Oxygen Final oxygen value is final
Nitrogen nitrogen value (net calc option)
Nitrogen Final nitrogen value is final
MAR moisture as received (dry calc option)
MAR Final moisture as received value is final
Dry Net
HOC_AR
Bomb Name bomb name assigned to bomb ID
Dry net HOC as received value (if
both dry and net calc option enabled)
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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.
ftp://root:rootroot@192.168.0.125/../flash/data/
The datalog file can be accessed at:
ftp://root:rootroot@192.168.0.125/../flash/log/
datalog.csv
In this case, 192.168.0.125 is the IP address of the calorimeter.
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COMMUNICATIONS INTERFACES
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 Mircosoft’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 nonMicrosoft 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 6300 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 proximate interface
To access the test data open the run data folder. To access the log file open the log data folder.
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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TECHNICAL SERVICE
E
APPENDIX E
TECHNICAL SERVICE
Should you need assistance in the operation or service
of your instrument, please contact the Technical Service
Department.
Telephone: (309) 762-7716
Toll Free: 800-872-7720
Fax: (309) 762-9453
E-mail: parr@parrinst.com
Any correspondence must include the following basic
information:
The model and serial # of the instrument.1.
Software version(s) shown on the “Software and 2.
Hardware Information” page.
When calling by phone, it is helpful if the person is
close to the instrument in order to implement any
changes recommended by the Technical Service
Department.
RETURN FOR REPAIR
To return the instrument for repair, please call the
Technical Service Department for shipping instructions
and a RETURN AUTHORIZATION NUMBER. This
number must be clearly shown on the outside of the
shipping carton in order to expedite the repair process.
If you have not saved the original carton and traps,
please request an A1340DD packaging return kit.
We prefer the calorimeter to be shipped in our cartons
and traps to prevent shipping damage.
Ship repair to:
Parr Instrument Company
Attn: Service Department
RMA # XXXX
211- 53rd Street
Moline, Illinois 61265
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PARTS LISTS & DRAWINGS
APPENDIX F
PARTS LISTS & DRAWINGS
PRINCIPAL ASSEMBLIES IN CALORIMETER
Item Description
1136/1136CL O2 Combustion Vessel, 340 mL
1138/1138CL O2 Combustion Vessel, 250 mL
1795E Power Supply, 24V
1796E Power Supply, 5/12V
379VB2 Barbed Tee, 3/8T X 1/2T X 3/8T
412VB Union Fitting, drain
533VBAD Union Reducer, 3/8T – 1/4T
897E Capacitor, Ignition
909E Switch Power
911E Filter 10 amp, interference
A1050DD Rinse Container Assembly
A1250DD2 Controller Assembly
A1251DD Oxygen Solenoid Assembly
A1252DD Water Solenoid Assembly
A1416DD Wash Pump Assembly
A1254DDEB Pump Assembly Circulating 115V
A1254DDEE Pump Assembly Circulating 230V
A1255DD Propeller Assembly, stirrer
A1256DD Water Tank Assembly
A1257DD Water Regulator Assembly
A1260DD Water Level Assembly
A1264DD Air Can Assembly 6300
A1265DD Bucket and Stirrer Tube Assembly
A1275DDEB Cartridge, Heater Assembly, 120V
A1275DDEE Cartridge, Heater Assembly, 230V
A1274DD Wash Pump Divert Valve Assembly
139E23 Fuse Fast/ Act 15 Amp 250V
1641E Pump Fuse (F1), Fast-Act, 1 Amp, 250V
1641E2 Heater Fuse (F2), Fast-Act, 2.5 Amps, 250V
997E5 Bomb Rinse (F5), Slo-Blo, 5 Amps, 250V
F
WARNING:
For continued protection against possible hazard, replace fuses with
same type and rating of fuse.
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A1250DD2 CONTROLLER ASSEMBLY
Item Description
1926E Film Guard, LCD 1802E
A1821E Speaker Assembly with Cable
A1822E Power Cable Assembly
A1823E Touchscreen Cable Assembly, 12”
A2140E I/O Board
A2141E LCD Transition Board
A2154E CPU Board (GCM)
A2163E LCD Cable
A2164E Backlight Control Cable
A2166E I/O to CPU USB Cable
A2167E USB Peripheral Cable
1477DD Display Kyrocera/Hantronix Gasket
2147E LCD
1472DD LCD Encasement - Kyrocera
A1251DD OXYGEN SOLENOID ASSEMBLY
Item Description
180VB Elbow, Male, 1/8T X 1/8 NPTM
243VB2 Connector, Male, 1/8T X 1/8 NPTM
527VB Restrictor, .012” SS 1/8 NPTM-F
79HW2BB Plug, 1/8” NPT
A1272DD Oxygen Solenoid Assembly w/o Fittings
A1252DD WATER SOLENOID ASSEMBLY
Item Description
179VB Tee, Street, 1/8 NPT
247HWHJ Hose, Barb, Elbow, Nylon, 1/4T x 1/8M
321VB Water Solenoid Valve, 1/4T x NPTM
60HWHJ Hose, Barb, Straight
79HW2BB Plug, 1/8 NPT
A1276DD Cold Water Solenoid Assembly, with Connector
A92HWAD Male Connector, 1/4 T – 1/8 NPT
283VB Adapter, Male 1/4 T- 1/8 NPT
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A1257DD WATER REGULATOR ASSEMBLY
Item Description
1211DD Bracket, Water Regulator
1244DD Regulator, Water, 6300
1245DD Filter, Water, 1/4 NPT
447VB Connector, Female, 1/4 T X 1/4 NPTF
60HW3HJ Hose Barb, Nylon
A1258DD TEMPERATURE CONTROL ASSEMBLY
Item Description
1249DD Manifold, Temperature Control
1417E Thermistor, Jacket
538VB Connector, Male, 1/8 NPTM-T-BT Nylon
248HWHJ Elbow, Hose Barb, 1/2 T x 1/2 M, Nylon
386VB Nipple, 1/2 NPT Nylon
413VB Cap, 1/2 NPT Nylon
405VB Nipple, 1/2 NPT Brass
A1275DDEB Cartridge, Heater Assembly 120V
A1275DDEE Cartridge, Heater Assembly 240V
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A1260DD WATER LEVEL ASSEMBLY
Item Description
1231DD Mount Level Sensor
1797E Switch, Water Level
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A1264DD AIR CAN ASSEMBLY
Item Description
328E Hole Plug, 3/8”
344VB Connector, Male 1/8T x 1/16NPTM
357HCJB O-ring, Buna-N, 1/4 ID
659DD O-ring, Buna-N .5/32” ID x 1/16 C ID
857DD O-ring, Buna-N 3/8 ID
882DD O-ring, Buna-N .487 ID
941DD Wedge Bucket
942DD Bushing, Bucket, Retaining
962DD Cap, Bomb Release Cylinder
963DD Retainer, Vessel;
964DD Spacer, Vessel
965DD Adapter, Air Can
966DD2 Shaft, Pin Release
967DD Seal, Air Can
969DD O-ring, Buna-N, ½” ID x 1/8 CS
970DD Retaining Ring SS
1037DD Baffle, Bucket, Brass
1137DD Snap Ring, 0.75”
1138DD O-ring, 1/2” I.D.
1139DD Insert, Cylinder
1140DD Cylinder, Bomb Release, 6300
1141DD Spacer
1143DD O-ring, Type 316, .614 ID x .07 CS
1235DD Gasket, Air Can
A1248DD2 Air Can Assembly,6300
A92HWAD Male Connector, 1/4T – 1/8NPT
1224DD2 Plate Hinge Support
1226DD Mount Cover Plate
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A1267DD ACCESSORY/INSTALLATION KIT
Item Description
231C2 Container, PP 10L Foldable
271C Cap w/ 7/16 Hole for Container
3415 Benzoic Acid Pellets 100 Gram Bottle O-ring,
356HCW Pliers for Snap Ring
43AS Capsule, SS
811DD Lube/Sealant
840DD2 Heating Wire
845DD2 Ignition Thread, 4”
876DD Cutter, Plastic Tubing
1005DD Forceps
1347DD Elbow
A1006DD Waste Tube Assembly
A1336DD Drain Tube Assembly
A38A Bomb Head Support Stand
A1271DD Bomb Wash Filter
TX03SK 1/32 Socket Screw Key
TX09SK 3/32 Socket Screw Key
TX12SK 1/8 Socket Screw Key
TX06SK 1/16 Socket Screw Key
TX14SK 9/64 Socket Screw Key
149C In-line Filter
1344DD LCD Stylus
1889E LCD Screen Protector
HJ0025TB035 Tubing, Nylon 1/4 OD X .35W
JT0038TB062A Tubing, Tygon 3/8 OD X 1/16W
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A1265DD BUCKET AND STIRRER TUBE ASSEMBLY
Item Description
944DD O-ring, Buna-N .237 ID
946DD Seal ¼ SS
1129DD Pin, Anti-rotating (A940DD)
1416E Thermistor, Bucket
1462E2 Thermistor Cable
A940DD Tube Assy, Bucket; Soldered
A1255DD Bucket Stirrer Assembly, 6300
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6300 STIRRER MOTOR AND DRIVE
A1255DD BUCKET STIRRER ASSEMBLY
Item Description
682DD Snap Ring, Internal .50
683DD Wave Spring, .50 OD
684DD Ball Bearing, .50 OD
690DD V-Seal, Nitrile
715HC O-ring NBR 1-1/4 ID
954DD Propeller
1029DD Baffle Assembly
1242DD2 Pulley, Timing (6300)
SA114ORD04 4-40 X 1/4 RHMS 18-8 SS
SN1140HLHJ Nut, 4-40 Hex Lock
A1266DD COVER ASSEMBLY
Item Description
Contact Pin Assembly
986DD Pin Contact
987DD Block Contact Pin
988DD Spring Compression
989DD Snap Ring External .219”
1021DD Bushing 0.125 ID
SN1332HX 6-32 Hex Nut 18-8 SS
A1400DD Plunger/Knob Assembly
1218DD Cover, Air
1229DD3 Plate
1237DD2 Friction Hinge
1396DD Latch Block
1324DD2 Post, Latch Locking
A1230DD2 Cover/Tubing Assembly
HA0012TB031 Tubing, PTFE
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