1356Calorimeter Operating Instruction Manual

Transcription

Operating Instruction Manual
No. 369M
1356
Isoperibol Bomb Calorimeter
1356 Calorimeter Operating Instruction Manual
TABLE OF CONTENTS
Preface
Scope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . I
Getting Started. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . II
Concept of Operation (Chapter 1)
1-1
Isoperibol Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Dynamic Operation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1
Full Microprocessor Based Process Control . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Full Microprocessor Based Data Acquisition and Handling . . . . . . . . . . . . . 1-2
Flexible Programming . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-2
Installing the Calorimeter (Chapter 2)
2-1
Unpack . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Install the Water Handling System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
Installing the Water Cooler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Install the Printer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
The Balance Port Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Smart Link Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Installing the Oxygen Filling System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Standardization. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-7
Instrument Description (Chapter 3)
3-1
Main Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Page and Line No. Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Types of Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Keyboard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Program Installation & Control (Chapter 4)
Software Installation. . . . . . . . . . . . . . . . . . . .
Default Settings . . . . . . . . . . . . . . . . . . . . . . .
Revised Default Settings. . . . . . . . . . . . . . . . .
Fig. 4-1 Factory Default Settings . . . . . . . . . .
Operating Instructions (Chapter 5)
Operating the 1108 Oxygen Bomb . .
Operating the Filling Connection . . .
Operating the Calorimeter . . . . . . . .
Operating Suggestions . . . . . . . . . . .
Combustion Aids . . . . . . . . . . . . . . .
Combustion Capsules. . . . . . . . . . . .
Coarse Samples . . . . . . . . . . . . . . . .
Explosives and High Energy Fuels . .
Volatile Samples . . . . . . . . . . . . . . . .
Poor Combustion . . . . . . . . . . . . . . .
Oxygen Charging Pressure. . . . . . . .
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4-1
. 4-1
. 4-1
. 4-1
. 4-2
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5-1
. 5-1
. 5-1
. 5-2
. 5-4
. 5-5
. 5-5
. 5-6
. 5-6
. 5-6
. 5-8
. 5-8
i-i
TABLE OF CONTENTS
Corrections & Final Reports (Chapter 6)
6-1
Entering Corrections and Obtaining the Final Report . . . . . . . . . . . . . . . . . . 6-1
Manual Entry. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1
Fixed Corrections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Automatic Data Transfers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Reporting Instructions (Chapter 7)
Report Option Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Report Destination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Report Generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
7-1
. 7-1
. 7-1
. 7-2
Memory Management (Chapter 8)
8-1
Clearing Memory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Editing Memory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-1
Maintenance and Trouble Shooting (Chapter 9)
9-1
Oxygen Bomb . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Installing Support Rod Mounting Plates . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-2
1356 Calorimeter Controller and Keyboard Display Removal . . . . . . . . . . . . 9-3
Keyboard/Display Removal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Removing the Entire Controller from the Calorimeter. . . . . . . . . . . . . . . . . . 9-3
1356 Series Calorimeter Firmware Update Procedure. . . . . . . . . . . . . . . . . . 9-4
Acquire the Program Update . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Connect the Calorimeter Controller to the PC . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Update the Calorimeter Controller Program . . . . . . . . . . . . . . . . . . . . . . . . . 9-4
Troubleshooting the 1356 Calorimeter Controller . . . . . . . . . . . . . . . . . . . . . 9-5
Fuses . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-5
Keyboard Inoperative . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Temperature Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-8
Bomb Firing Problems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-9
Low Oxygen Pressure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-9
Bucket Thermistor Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-10
Instructions for Adjusting Cover. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-10
How to Check the Motor. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11
Motor Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11
EE Standard Deviation Exceeds Limit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11
Preperiod or Postperiod Time Limit Violation . . . . . . . . . . . . . . . . . . . . . . . 9-11
1356 Calorimeter Error List. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-12
i-ii
TABLE OF CONTENTS
Appendix A - Menu Operating Instructions
A-1
Calorimeter Operation Page 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
Operating Controls Page 2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2
Program Information and Control Page 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . A-4
Calibration Data and Controls Page 4 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-5
Thermochemical Calculations Page 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-7
Data Entry Controls Page 6 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-9
Reporting Controls Page 7 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-11
Communication Controls Page 8 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-13
Diagnostics Page 9 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-16
Appendix B - Calculations
B-1
Calculating the Heat of Combustion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
General Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
Thermochemical Corrections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-1
ASTM and ISO Methods Differ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-2
Fuse Correction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-3
ACID and SULFUR Corrections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-3
ASTM Treatment for Acid and Sulfur . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5
ISO Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-5
Calculate HNO3 from the Energy Release . . . . . . . . . . . . . . . . . . . . . . . . . . . B-6
Correction Equation Set 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7
Spiking Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-8
Conversion to Other Moisture Bases . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-8
Conversion to Net Heat of Combustion (Need New) . . . . . . . . . . . . . . . . . . B-8
Magnitude of Errors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-9
Precision Statements and the Confidence Factor . . . . . . . . . . . . . . . . . . . . . B-9
Calorimeter Control Limits when Benzoic Acid is Used as a Test Sample . . . . B-10
Appendix C- Standardization
C-1
Standardizing the Calorimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Standard Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-1
Automatic Statistical Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C-2
i-iii
TABLE OF CONTENTS
Appendix D - Communication Interfaces
D-1
Required Software Versions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-1
Required Hardware . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2
Smart Link Configurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2
Smart Link Configuration Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-2
Smart Link Configuration Cabling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3
RS232C Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-4
Terminal Port Connections. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-4
Balance Input Driver Specifications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-4
Mettler 011/012 Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-5
Sartorius Balance Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-5
Ohaus Balance Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-6
Generic Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-6
Computer Interface Description for the 1266/1356 Calorimeters . . . . . . . . . D-6
Appendix E - Technical Service
E-1
Appendix F - 1356 Calorimeter Parts List
F-1
Replacement Parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-1
Hinge Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-2
5 Year Recomended Spare Parts . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . F-3
Recommended Spare Parts Per 5000 Tests . . . . . . . . . . . . . . . . . . . . . . . . . . F-4
Appendix G - 1356 Drawings
i-iv
G-1
TABLE OF CONTENTS
Figures
Fig. 2-1
Fig. 2-2
Fig. 2-3
Fig. 2-4
Fig. 2-5
Fig. 2-6
Fig. 2-7
Fig. 2-8
Fig. 2-9
Fig. 3-1
Fig. 4-1
Fig. 5-7
Fig. 9-1
Tables
Table
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1552 Water Cooler Electrical Circuits . . . . . . . . . . . . . . . . . . . . . . . . 2-2
1552 Water Cooler Front View. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
1552 Water Cooler Top View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Swagelok 1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Swagelok 2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Swagelok 3. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
1356 Calorimeter External Plumbing. . . . . . . . . . . . . . . . . . . . . . . . . 2-4
1356 Calorimeter Electrical Hookup . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
1356 Calorimeter Back View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
1356 Calorimeter Keyboard . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Factory Default Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Combustion Capsule with Adhesive Tape Seal. . . . . . . . . . . . . . . . . 5-7
1108 Oxygen Bomb Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
4-1 Calorimeter Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
9-2 1266 / 1356 Calorimeter Controller Fuses. . . . . . . . . . . . . . . . . . . . 9-5
9-3 Power Connections - Voltage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
9-4 Power Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
9-5 Power Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
B-1 Settings for ISO and BSI Methods . . . . . . . . . . . . . . . . . . . . . . . . . B-4
B-2 Entered and Reported Acid Value is Taken as Nitric Acid Only. . . B-6
B-3 Entered and Reported Acid Value is Considered Total Acid . . . . . B-6
B-4 Calculate HNO3 if Fixed and Acid is HNO3 Only . . . . . . . . . . . . . . B-6
B-5 Calculate HNO3 if Fixed and Acid is Total Acid . . . . . . . . . . . . . . . B-6
B-6 Calorimeter Control Limits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-10
B-7 Calorimeter Control Limits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-11
D-1 Software Required . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3
D-2 Smart Link Cables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3
D-3 Calorimeter Test Report Field Definitions . . . . . . . . . . . . . . . . . . . D-7
D-4 Test Information Field #1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-8
D-5 Test Information Field #2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-8
D-6 1356 Terminal Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-9
D-7 1356 Balance Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-9
D-8 1356 Printer Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-9
i-v
PREFACE
Scope
This manual contains instructions
for installing and operating the Parr
1356 Calorimeter. For ease of use, the
manual is divided into ten chapters.
Concept of Operation
Installation
Instrument Description
Program Installation and Control
Operating Instructions
Corrections & Final Reports
Reporting Instructions
Memory Management
Maintenance Instructions
Appendices
Subsections of these chapters are
identified in the Table of Contents.
To assure successful installation
and operation, the user must study all
instructions carefully before starting to
use the calorimeter to obtain an
understanding of the capabilities of the
equipment and the safety precautions
to be observed in the operation.
Customer Service:
Questions concerning
the installation or
operation of this
instrument can be
answered by the
Parr Customer Service
Department:
309-762-7716
800-872-7720
Fax: 309-762-9453
www.parrinst.com
[email protected]
I
Additional instructions concerning
the installation and operation of
various component parts and
peripheral items used with the 1356
Calorimeter have been included and
made a part of these instructions.
No.
Description
201M Limited Warranty
202M Introduction to Bomb
Calorimetry
205M 1108 Oxygen Combustion
Bomb
207M Analytical Methods for
Oxygen Bombs
245M 1552 Water Cooler
246M 1563 Water Handling System
Additional instructions for the
printer are found in the respective
package and should be made a part
of this book.
264M Dot Matrix Printer DP8340
Series Users Manual
These steps are offered to help
the user become familiar with, install,
operate and develop the full
capabilities of the Parr 1356
Calorimeter.
1. Review the Concept of Operations,
Chapter 1, to get an understanding
of the overall capabilities of the
calorimeter and microprocessor
control.
2. Unpack and install the
calorimeter in accordance with the
Installation Instructions, Chapter 2.
This simple, step-wise procedure
will acquaint the user with the
various parts of the calorimeter
and make it easier to understand
the operating instructions which
follow.
3. Turn to the Instrument Description,
Chapter 3, to review the keyboard
controls.
4. Review the Program Installation
and Control, Chapter 4, to match
the factory settings to the intended
mode of operation. Any required
changes can be made to the
program parameters located in
the Main Menu.
5. Review the Reporting Instructions,
Chapter 7, to become familiar with
the manner in which calorimetry
corrections are entered. Also
discussed are generating final
reports, editing and clearing
memory.
6. Turn to the Menu Operating
Instructions, Appendix A, to review
the menu functions used to modify
the program contained in the 1356
Calorimeter. A review of the
7.
8.
9.
10.
menus will provide a good idea
of the capabilities and flexibility
designed into this instrument.
Review the Calculations, Appendix
B. This provides information about
calculations performed by the 1356
Calorimeter.
Review Standardization,
Appendix C. This will serve two
important functions. First, it
provides instructions on
generating the energy equivalent
factor required to calculate the
heat of combustion (HOC) 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
1356 Calorimeters with 1108
Oxygen Combustion Bombs and
2000 grams of water will have an
energy equivalent of
approximately 2400 +/-15
calories per °C. The steps for
standardization and
determinations are identical,
except for the setting of the
instrument to the standardization
or determination mode.
Review the Communication
Interfacing, Appendix D, for the
correct installation of any Smart
Link peripherals to the 1356
Calorimeter.
After successful standardization,
the 1356 Calorimeter should be
ready for testing samples.
Getting
Started
II
CONCEPT OF OPERATION
1
he Parr 1356 Oxygen Combustion
Bomb Calorimeter has been
designed to provide rapid and reliable
heat of combustion values for solid
and liquid fuels. This instrument
combines fourth generation
microprocessor hardware and software
with the calorimeter designs, technical
T
knowledge and customer support
developed by Parr in the century that
calorimetry has been a principal thrust
of our company. This chapter explains
the important design and operating
concepts incorporated into the 1356
Calorimeter.
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 15 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.
1-1
1
Determine and apply all necessary
heat leak corrections.
G. Perform all curve matching and
extrapolations required for
dynamic operation.
H. Terminate the test when it is
complete.
I. Monitor the conditions within the
calorimeter and report to the user
whenever a sensor or operating
condition is out of normal ranges.
Full
Microprocessor
Based
Process
Control
The microprocessor controller
in this calorimeter has been
preprogrammed to automatically
prompt the user for all required data
and control input and to:
A. Generate all temperature readings
in the calorimeter.
B. Monitor jacket as well as bucket
temperature.
C. Confirm equilibrium conditions.
D. Fire the bomb.
E. Confirm that ignition has occurred.
F.
In addition to its process control
functions, the microprocessor in
the calorimeter has been
preprogrammed to:
A. Collect and store all required test data.
B. Apply all required corrections for
combustion characteristics.
C. Compute and report the heat of
combustion for the sample.
Full Microprocessor
Based Data
Acquisition
and Handling
The fourth 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. A large selection of printing
options.
B. Choice of accessories and
peripheral equipment.
C. Multiple options in regard to
handling thermochemical
corrections.
D. Choice of ASTM or ISO correction
procedures.
E. A variety of memory management
and reporting procedures.
F. Complete freedom for reagent
concentrations and calculations.
G. Unlimited choice of reporting units.
H. Automatic bomb usage monitoring
and reporting.
I. A choice of Equilibrium or
Dynamic test methods.
J. Automatic statistical treatment of
calibration runs.
K. Enhanced testing and trouble
shooting procedure
Flexible
Programming
The 1356 Calorimeter is equipped
with three RS232C connections for
direct communication with its printer,
an attached balance and a computer.
It is also equipped with the Parr
Smart Link network connection for
networking with other calorimeters,
fuel testing instruments, balances
and computers.
1-2
INSTALLATION
2
he 1356 Calorimeter is completely
assembled and given a thorough
test before it is shipped from the
factory. If the user follows these
instructions, installation of the
calorimeter should be completed
T
with little or no difficulty. If the factory
settings are not disturbed, only minor
adjustments will be needed to adapt
the calorimeter to operating conditions
in the user’s laboratory.
Unpack
1. Unpack the calorimeter carefully.
If shipping damage is discovered,
report it immediately to the
delivering carrier. The calorimeter
and all of its component parts are
packed in one carton. The unit has
had all internal connections made,
and other than a connection to
oxygen supply, no additional
assembly should be required. Set
the calorimeter on a sturdy bench
or table in a location that is
reasonably free from drafts and
protected from sources of radiant
heat; preferably in an airconditioned room. There should
be convenient access to an
appropriately grounded
electrical outlet.
2. Raise the cover of the calorimeter
and swing it vertically to the back.
Remove the calorimeter bucket
and discard the packing material.
Check the calorimeter bucket and
note the three dimples in the
bottom which rest on supporting
pins when the bucket is placed in
the jacket. The single dimple must
always be placed to the back of the
jacket. There will also be two
ignition wires extending into the
oval chamber through the opening
in the left side of the jacket.
Installing
the Water
Handling
System
3. If operation of the calorimeter will
be done in conjunction with a 1563
Water Handling System, make the
water connections at this time.
Connect the line supplying water
from the filling system to the
connection at the lower left hand
corner at the water jacket (rear
view). The metering valve at this
connection should be fully open
2-1
when used with a 1563 Water
Handling System. Adjustment of
the systems temperature to
between 30° and 32 °C will
provide water at the correct
temperature for the 1356
Calorimeter. Step 4 may be
skipped if the water connection
has been made to the 1563
Water Handling System.
2
4. The 1552 Water Cooler is intended
to provide a uniform water supply
in the temperature range from
7° to 10 °C for maintaining the
desired bucket temperature for
each run. The amount of cold
water needed for the water
handling system is determined
by the thermostat in the water
handling system.
If a water cooler will be used,
make the connections at this time.
Refer to Fig. 2-4. Install the 1552
Water Cooler so that heat from the
compressor will not be directed
toward the calorimeter. In any
installation, the cooler should be
placed at or below the working
surface of the calorimeter. Allow a
minimum clearance of 6 inches in
front of the unit, 3 inches in the
rear and at least 1 inch on the
sides for air circulation. Install the
two 232VB Union Male Elbows on
the water inlet and outlet
connections (see Fig. 2-3).
Connections between the
calorimeter and the cooler should
be make with the furnished 1/4”
tubing. A temperature adjustment
screw is located in an opening on
the front of the cooler. Set this
adjustment screw at the coldest
setting (fully clockwise – see
Fig. 2-2).
Installing the
Water Cooler
Note:
Do not plug in water cooler at this
time.
Figure 2-1 1552 Water Cooler Electrical Circuits
2-2
2
Installation
Continued
Figure 2-4 Swagelok 1
12
Figure 2-3 1552 Water Cooler Top View
1
2
11
3
10
9
4
8
5
7
6
12
1
2
11
10
3
9
4
8
Figure 2-2 1552 Water Cooler Front View
5
7
6
Note:
2-3
When Swagelok Tube Fittings are
used, the instructions for installation
are:
1. Simply insert the tubing into the
Swagelok Tube Fitting. Make sure
that the tubing rests firmly on the
shoulder of the fitting and the nut
is tight.
2. Before tightening the Swagelok
nut, scribe the nut at the 6:00 clock
position.
3. While holding the fitting body with
a back-up wrench, tighten the nut
1-1/4 turns. Watch the scribe mark,
make one complete revolution and
continue to the 9:00 clock position.
4. For 3/16” and 4mm or smaller tube
fittings, tighten the Swagelok nut
3/4 turn from finger tight.
2
Fig. 2-7 1356 Calorimeter External Plumbing
Fig 2-8 1356 Calorimeter Electrical Hookup
2-4
2
Install the
Printer
5. Connect the printer to the
calorimeter at this time. The Parr
1755 Printer is configured and
furnished with a cord to connect
directly to the RS232C port of the
calorimeter.
6. Plug the power line into any
grounded outlet providing proper
voltage which matches the
specification on the nameplate of
the calorimeter. The calorimeter
will draw approximately 300
watts of power. Grounding is
very important not only as a safety
measure, but also to ensure
satisfactory controller
performance. If there is any
question about the reliability of
the ground connection through
the power cord, run a separate
earth ground wire to the
controller chassis.
The Balance
Port
Connection
7. The balance port connection, if
used, should be made at this time.
Refer to figure 2-8 for the correct
cable to connect the balance to the
calorimeter.
Smart Link
Connection
8. Connection to the Parr Smart Link
Network, if needed, can be made
at this time. A detailed discussion
of the Parr Smart Link can be
found in Appendix D Communication Interfaces. The
termination Settings are done in
software, See Menu page 8.1 line
5. If one Smart Link cable is
plugged into the rear of the
calorimeter (end of Smart Link
Installing
the Oxygen
Filling System
11. The 1356 Calorimeter is equipped
with an automatic bomb oxygen
filling system. Thus system consists
of an oxygen pressure regulator
with a relief valve that mounts on
an oxygen tank. A control and
measurement system is mounted in
the calorimeter case. The
connection tubing to connect the
regulator to the solenoid assembly
and the solenoid assembly to the
bomb itself are included.
2-5
position), no change is required
as the default value is ON. If two
cables are used (middle of the
Smart Link), then the setting must
be set to OFF.
9. Connect the printer power cable
and the printer communications
cable between the 1755 printer and
the connection at the rear of the
calorimeter.
To install the regulator, unscrew
the protecting cap from the oxygen
tank and inspect the threads on the
tank outlet to be sure they are
clean and in good condition. Place
the ball end of the regulator in the
outlet and draw up the union nut
tightly, keeping the gages tilted
slightly back from an upright
position. Connect the regulator to
the inlet fitting on the back of the
calorimeter case. Flexible high
2
Controller
Solenoid
Valve Assy.
Fig. 2-9 1356 Calorimeter Back View
pressure, 1/8” diameter nylon
tubing is provided.
Attach the bomb filling hose
(1/8” tubing) to the tubing
connector nearest the back of the
calorimeter case. These hoses
should be routed so that they will
not kink or come in contact with
any hot surface. All connections
should be checked for leaks. Any
leaks detected must be stopped
before proceeding. Instructions for
operating the filling connection
are in the Operating Instructions
chapter. The pressure regulator
was set at the factory to deliver
oxygen at 450 psig, the
recommended charging pressure,
and should be checked before
starting to use the system by
observing the pressure attained
during an actual filling operation.
To do this, assemble the oxygen
bomb without a charge and attach
2-6
2
Installing
the Oxygen
Filling System
Continued
the filling hose to the bomb inlet
valve. Then push the 02 button on
the calorimeter control panel and
observe the delivery pressure as
shown on the 0-600 psi gage while
oxygen is flowing into the bomb.
Adjust the regulator, if needed, to
bring the pressure to 450 psig. If
there is any doubt about the
setting, release the gas from the
bomb and run a second check.
During extended periods of
inactivity (overnight or longer),
close the tank valve to prevent
leakage. When changing oxygen
tanks, close the tank valve and
depress relief valve to exhaust
the system. Do not use oil or
Standardization 12. 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, Item
1, Operating Mode. The YES/NO
keys are used to select the desired
operating mode. If two bomb head
and buckets are being used with
the calorimeter to maximize
sample throughput, the
calorimeter can be configured to
prompt for a Bomb ID at the start
2-7
combustible lubricants on this
filling system or on any devices
handling oxygen under pressure.
Keep all threads, fittings, and
gaskets clean and in good
condition.
The recommended 450 psig
filling pressure is slightly higher
than the 30 atm prescribed in Parr
bomb and calorimeter instruction
manuals. This difference is
insignificant. Higher or lower
settings can be used, but the bomb
must never be filled to more than
600 psig (40 atm). If pressures
below 28 atm are used, the low
pressure warning will always
occur.
of each test. The Bomb ID can also
be selected on the Calorimeter
Operations Page, Line 2, using the
YES/NO keys. Both bomb and
bucket combinations will need to
be standardized separately. The
end result of a standardization test
is an energy equivalent value, or
the amount of energy required to
raise the temperature of the
calorimeter one degree. Repeated
standardization with any given
bomb head should yield an energy
equivalent value with a range of 3
to 4 calories per degree, centered
around the mean value for all tests
using that bomb bucket
combination. The calorimeter is
ready for testing samples after a
suitably constant energy
equivalent value has been
obtained
3
INSTRUMENT DESCRIPTION
ll calorimeter configurations and
operations are handled by a menudriven system operated from the
easy-to-use keyboard with a large,
bright display. The settings and
controls are organized into nine
main sections or pages. This is
the MAIN MENU.
Main Menu
1 Calorimeter Operation
2 Operating Controls
3 Program Information and
Control
4 Calibration Data and Control
5 Thermochemical Calculations
6 Data Entry Controls
7 Reporting Control
8 Communication Control
9 Diagnostics
A
Any page number or line number
on a page can be selected by:
Cursor Control - The up and
down arrow keys can be used to move
the reverse video to the desired
page/line number. Once the desired
page/line number is highlighted, press
the ENTER key.
Types of Controls The controls that
change the data field information in
the menus will be one of the following:
1.
2.
Toggles. These data fields
contain ON/OFF or YES/NO
choices. The right and left arrow
keys are used to change the
setting to the desired choice.
Once the desired setting is
displayed, press the ENTER key
to record the change.
Option Selection. These data
fields contain a list of options. The
right and left arrow keys are used
to step through the options. Once
the desired option is displayed,
Note:
When the cursor highlights the line
number and title, as opposed to the
data field, a page or sub-menu can be
accessed by pressing the ENTER key.
(See Command Codes in this chapter.)
Page and
Line Number
Selection
Number Control - Page/Line
numbers can also be selected by
simply pressing the desired page/line
number on the keyboard.
3.
4.
press the ENTER key to record
the change.
Value Entry Fields. These data
fields are used to enter data into
the calorimeter. Most data fields
will accept any value entered by
the user through the keyboard.
Certain data fields may only
accept certain values from a table
built into the menu similar to the
option selection described above.
Once the correct value is displayed in the field, press the
ENTER key to record the value.
Data Displays. Most of these
data fields display values that
have been calculated by the
Types of
Controls
3-1
3
Types of Controls
Continued
calorimeter and are informational
only. Certain display values can be
overridden by the user entering a
desired value through the
keyboard.
Command Codes. Line
numbers that access sub-menus
or statements initiating an action
(the controller will ask, “Do you
wish to continue (Yes or No)?” to
prevent accidental disruptions to
5.
Keyboard
Before using the 1356 Calorimeter,
the operator should understand the
various keys on the keyboard (see
Figure 3-1). The brief descriptions
the program and/or stored data).
Note:
To return to previous pages from
a sub-menu, press ESCAPE. To
return to the Main Menu, press
SHIFT, ESCAPE. Remember, no
value or setting chosen is stored
in the program until the ENTER
key is pressed.
given here will identify these keys and
their functions. Instructions in later
chapters provide detailed operating
instructions.
Fig. 3-1 1356 Calorimeter Keyboard
NO
3-2
YES
CLEAR
MEM.
7
8
9
PRINT
SCREEN
4
5
6
HELP
1
2
3
START
F1
F2
SKIP
.
0
E
ENTER
F3
O2
FILL
SHIFT
RESET
REPORT
CLEAR
ENTRY
ESCAPE
3
Key
Description
▲
the oxygen filling system
used to fill the bombs. The
reset key can be used to
abort the filling procedure.
Moves the cursor UP on any
of the menu pages.
▲
NO
▲
YES
▼
START
Changes menu functions
that are either an ON/OFF or
YES/NO toggle to OFF, NO,
or to select an option from
the list provided.
Changes menu functions
that are either an ON/OFF or
YES/NO toggle to ON, YES,
or to select an option from
the list provided.
PRINTSCREEN Prints information
(except graphics) which is
currently shown on the
instrument display to the
printer.
HELP
This key is used to start a
test. After pressing, the
controller will prompt the
user to enter all preliminary
data required for the test.
Used to access a set of help
menus that are available to
assist the user in setting up
and/or operating this
calorimeter.
SHIFT
This key is used to change
the function of a key in much
the same way that the shift
key operates on a typewriter.
For example, the numeric
keys (1-9) can be used with
the SHIFT key to provide
access up to nine
programmed functions.
0-9 & (.)
The DECIMAL and 0-9 keys
are used for all manual data
entries. The decimal key can
also be used for other
functions described later
in this manual.
E—
This key is used to enter a
negative number when
Used to enter sample IDs
and weights when a series of
samples will be weighed
before they are tested. This
preweighing sequence will
prompt the user for sample
IDs and weights.
F2
not used
F3
This key is used to initiate
edit capabilities for sample
weight, bomb ID, spike
weight, fuse, acid, and sulfur
or hydrogen values.
02 Fill
CLEAR MEM. Clears tests from the
memory. When it is pressed,
the controller will prompt for
the beginning and ending
Sample IDs to be deleted
from memory.
Moves the cursor DOWN on
any of the menu pages.
F1
This key is used to activate
Keyboard
Continued
3-3
3
Keyboard
Continued
CLEAR ENTRY Erases incorrect
values and error messages
from the display. If the user
is not satisfied with the value
shown on the display, press
the CLEAR ENTRY key and
re-enter the value.
ENTER
3-4
sent to the display, to the
attached printer, or over
the Smart Link to another
controller. Before any
preliminary reports can be
made final, the controller
will prompt the user to
provide any missing data;
such as fuse, acid and/or
sulfur corrections.
required. It is entered before
the digits and also used to
indicate that the numbers
are being entered in
scientific notation.
The ENTER key is used in
two ways: 1.To access
sub-menus. 2.To store data
field information into the
controller.
If there is a sub-menu, the
line will be highlighted when
the cursor is on that line.
Press the ENTER key to
access the sub-menu.
If there is no sub-menu,
the data field will be
highlighted. If new data
field information is selected
or entered through the
keyboard by the user, the
ENTER key must be pressed
to store the information. (See
Types of Controls in this
chapter for a complete
description.)
RESET
Aborts a test or to escape
from a special sub-routine.
(i.e. reporting or memory
management.)
REPORT
Initiates the reporting
process. Reports can be
SKIP
Allows the user to omit the
entry of data requested by
the calorimeter, to pass over
a prompted request for
information already held in
memory, and to select a data
field when a double column
appears (see Page 5 Thermochemical
Corrections, Lines 1-6).
ESCAPE
Used to go up one level in
the menu structure. For
example, pressing ESCAPE
one time will shift the menu
from sub-menu Page 5.6 to
5. Pressing ESCAPE a
second time will return to
the main menu. Press the
SHIFT, ESCAPE key to return
directly to the main menu
from a sub-menu.
4
PROGRAM INSTALLATION & CONTROL
The program in the 1356
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.
Units are preprogrammed with
DEFAULT SETTINGS. See Figure 4-1
on the next page 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 Page
3, Line 7 - Re-load Factory Default
Settings, press ENTER and YES.
Battery backed-up 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.
The default parameters of the
1356 Calorimeter can be changed to
guarantee that the 1356 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 Page 3, Line 9 - Save User
Default Settings, and press the ENTER
key.
Press YES, the controller will
prompt the user for a “User Rev.”. This
can be any number that is helpful in
identifying the user’s setup. Enter
number and press the ENTER key.
To re-load the user default setting,
go to Page 3, Line 8 - Re-load User
Default Settings, press the ENTER key
and YES.
Software
Installation
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
Revised
Default
Settings
4-1
4
Fig.4.1
Factory Default
Settings
Main Menu
1 Calorimeter Operation
2 Operating Controls
3 Program Info & Control
4 Calibration Data & Control
5 Thermochemical Corrections
6 Data Entry Controls
7 Reporting Controls
8 Diagnostics
Page 2.3
Spike Controls
1 Use Spiking
2 Heat of Comb of Spike
3 Use Fixed Spike
4 Weight of Fixed Spike
5 Ask for Spike before
Weight
Page 1
Calorimeter Operations
1 Operating Mode
2 Bomb Installed/EE
3 Heater and Pump
Sample ID
Sample Weight
Spike Weight
Jacket Temperature
Bucket Temperature
Page 3
Program Info & Controls
1 Software Versions
2 Hardware Versions
3 Date (YYYYMMDD)
4 Time (HHMMSS)
1532
5 User Setup ID
?????
6 Password Protection
OFF
7 Reload Factory Settings
8 Reload User Settings
9 Save User Settings
0 Cold Restart
Page 2
Operating Controls
1 Method of Operation
2 Reporting Units
3 Use Spiking Correct.
4 “OTHER” Multiplier
5 LCD Controls
6 LCD Light Timeout(s)
7 Print Error Messages
8 Display Stored Samples
9 Language
4-2
CAL 1
Detr.
1/2400.0
OFF
0
0.0000
0.0000
30.0000
29.0000
Dynamic
Btu/lb.
OFF
1.0
600
ON
English
OFF
6318.0
OFF
0.0
OFF
Page 4
Calibration Data & Controls
1 Use Bomb
1
2 Bomb type in use
1108
3 Jacket Temp–SP
35
4 Calibration run limit
10
5 EE max STD deviation
0.15
6 Bomb calibration sub menu
7 HOC of standard
6318.0
8 Bomb service interval
500
4
Page 5
Thermochemical Corrections
Standardization 1 Fixed Fuse
ON 15.0
2 Fixed Acid
ON 10.0
3 Fixed Sulfur
ON 0.0
Page 4.6
Bomb Calibration
1 Bomb 1
2 Bomb 2
3 Bomb 3
4 Bomb 4
5 Bomb 5
6 Bomb 6
7 Bomb 7
8 Bomb 8
Page 4.6-1
Bomb 1
1 EE value
2 Protected EE value
3 Number of runs
4 Rel. Std. Dev
5 Bomb–firing count
6 Print standardization
7 Update statistics
Determination 4 Fixed Fuse
5 Fixed Acid
6 Fixed Sulfur
7 Calculation Factors
8 Calculate Net Heat
2400.0
OFF
0
0.0
0
Page 5.7
Calculation Factors
1 Acid is Nitric Acid Only
2 Acid Multiplier
3 Sulfur Value is Percent
4 Sulfur Multiplier
5 Fuse Multiplier
6 Use Correction (ISO)
7 Offset Value
8 Hydrogen Multiplier
9 Calc. HNO3
0 HNO3/Energy
ON 15.0
ON 10.0
OFF 0.0
OFF
ON
0.0709
ON
0.6238
1.0
OFF
0.0
50.68
OFF
1.58
4-3
4
Fig.4.1
Factory Default
Settings
Continued
Discussion for menu page 5.7;
Items 9 and 0 (calculated HNO3)
The nitric acid formed in the bomb
during the combustion process is
derived from the nitrogen in the air
that occupies the bomb prior to
pressurizing it with oxygen. The
quantity of nitric acid formed is a
function of the interior volume of the
bomb, the oxygen filling pressure and
the quantity of energy released in the
bomb during a test. For a given bomb
volume and filling pressure, the
relationship between the amount of
nitric acid formed and the energy
released is reasonably constant.
If the fixed acid flag for a given
test mode is ON and calculate HNO3
is selected (turned ON), then e1 is
calculated based on the amount of
energy released during the test. In this
case, the amount of nitric acid
calculated (in calories) is the product of
the calorimeter energy equivalent, the
temperature rise and the
“HNO3/Energy” factor divided by 1000.
This HNO3/Energy factor is 1.58 for a
Parr 1108 style bomb at 30 atmospheres filling pressure. If the “acid is
HNO3 only” flag is ON then the reported acid value is e1. If this flag is OFF,
then the reported acid value is e1+e2.
See the discussion in Appendix B
(Thermochemical Corrections) for a
more thorough discussion related to
how these corrections are calculated
and handled.
Page 6
Data Entry Controls
1 Weight Entry
2 Spike Entry
3 Acid Entry
4 Sulfur Entry
5 Hydrogen Entry
6 Prompt for Bomb ID
7 Use Long Sample IDs
8 AutoSampleID Controls
9 Auto Controls
0 Weight Warning above
Page 7
Reporting Controls
1 Printer Controls
2 Report Dest
3 Automatic Reporting
4 Individual Reports
5 Report Format
6 Overwrite Final Reports
7 Edit Final Reports
8 Recalc Final Reports
9 Use New EE Values
Page 6.9
Sample ID Controls
1 Automatic Preweigh ID
2 Preweigh ID Increment
3 Preweigh ID Number
4-4
Keyboard
Keyboard
Keyboard
Keyboard
Keyboard
ON
OFF
ON
ON
2.0
ON
1.0
1.0
Page 8
Communication Controls
1 Smart Link Controls
2 Printer Port (RS232C)
3 Balance Port (RS232C)
4 Terminal Port (RS232C)
Printer
ON
OFF
Text
OFF
OFF
OFF
OFF
4
Page 8.1
Smart Link Controls
1 Smart Link ID (0-15)
2 Baud Rate
3 Report Type
4 Timeout (x 0.01 s)
5 Smart Link Termination
6 Use a 4 digit year
Page 8.2
Printer Port
Communications
1 Data Bits
2 Parity
3 Stop Bits
4 Handshaking
5 Baud Rate
0
9600
Short Report
50
OFF
OFF
Page 8.4
Terminal Port Communications
1 Data Bits
8
2 Parity
None
3 Stop Bits
1
4 Handshaking
Xon/Xoff
5 Baud Rate
9600
6 Terminal Type
VT100
7 Remote Terminal
ON
8 Emulate 1745
ON
CAL I
8
None
1
Xon/Xoff
9600
Page 9
Diagnostics
1 Self-Test
2 I/O Diagnostics
3 Thermometry Diagnostics
4 Communication Diagnostics
5 Keyboard Diagnostics
6 User Defaults Up/Down Load
7 Data Logger Menu
8 Print Error List
Page 8.3
Balance Port Communications
1 Data Bits
7
2 Parity
Even
3 Stop Bits
1
4 Handshaking
None
5 Baud Rate
2400
6 Balance type
Mettler 011
7 Data Char
9
8 Log to Printer
Page 9.2
I/O Diagnostics
1 Activate Ignition Circuit
2 Test 02 Fill Function
3 I/O Driver Diagnostic
4-5
Fig.4.1
Factory Default
Settings
Continued
Page 9.2.3
Calorimeter 1 I/O Diagnostics
Ignition Fire = Off
Output = 0x0000
Input = 0x0cff
Bucket temperature
27.98814
Jacket temperature
29.86350
Heater Duty Cycle
0.00%
Calorimeter Status
Alternate Menu 1 (Access by Shift 1)
The alternate 1 (shift 1) screen
presents key calorimeter parameters
and updates them on a real time
basis. These items include the date,
time, calorimeter state (idle, pre
period or post period), bucket and
jacket temperatures, digital I/O
Page 9.7
Data Logger Controls
1 Data Logger
2 Interval In Seconds
3 Data Log Items
4 Computer Format
5 Destination
6 Process Log Dest
7 Process Log Items
8 Print Ram Buffer
9 Clear Ram Buffer
OFF
10
OFF
Printer
Printer
images and the heater duty cycle.
The remaining items on this page
are parameters directly related to
the course of the current calorimetric
test. These items are used by Parr
Instrument Company technicians to
evaluate calorimeter performance.
Some of these items are described
below.
Table 4-1 Calorimeter Status
Parameter
D0
Tsum
C0
T1
4-6
Description
Calorimeter drift rate (10s time base)
corrected for systematic heat leaks.
The accumulated temperature rise after the sample is
ignited. This value is the temperature rise for an
Equilibrium Method test.
This is a counter that is initialized to zero at the
start of a test and then incremented every 10s.
At firing, the counter is again reset to zero.
This value is the extrapolated portion of the temperature
rise for a Dynamic Method test.
4
Alternate Report
Destination Setup
These calorimeters are set up, by
default, to issue a printed report at the
conclusion of a test. Provision has
been made to have a duplicate report
issued at either the terminal or the
balance port. This feature is enabled
on menu page A2 (alternate 2). To
access this page, press the ENTER and
hold the SHIFT key and then 2. This
menu page has the following entries:
1 Alt. Report Destination Null Device
/ Terminal / Balance
2 Alternate Report Format Data /
Text
When the destination is set to the
null device, duplicate reports are not
issued. The format for the additional
report can include the text and
formatting of the original report (text
option) or just the unique data items
associated with the report (data). In the
later case, datum is delimited with a
comma and the report is terminated
with carriage return <CR> and line
feed <LF> characters.
Dry Calculation Setup
1 Dry Calculation
OFF
2 Fixed Moisture (%)
0.0
3 Moisture Entry Mode Keyboard
4 Moisture Multiplier
5.83
See Appendix B - Calculations for the
calculation that uses these parameters
when Dry Calculation is ON
4-7
OPERATING INSTRUCTIONS
5
Operating the
1108 Oxygen
Bomb
Detailed instructions for preparing
the sample and charging the 1108
Oxygen Bomb are given in Operating
Instructions No. 205M. Follow these
instructions carefully, giving particular
attention to the precautions to be
observed in charging and handling the
bomb.
Operating
the Filling
Connection
To fill the bomb, connect the hose
to the bomb inlet valve and push the
02 button on the calorimeter control
panel. The calorimeter will then fill the
bomb to the preset pressure and
release the residual pressure in the
connecting hose at the end of the
filling cycle. The main display will
read 02 FILL while the bomb is being
charged. It will take approximately 40
seconds to fill the bomb. (Pushing the
RESET key will stop the flow of oxygen
at any time.) Once the display returns
to its normal reading, the user can
disconnect the coupling and proceed
with the combustion test.
If the charging pressure fails to
reach approximately 28 atmospheres
during the filling cycle, an ERROR 78
message will be reported on the
display and/or printer. If this occurs,
check the system carefully for low tank
pressure, a closed tank valve or leaks
in the system.
The charging cycle can be started
at any time, but once it is started it
will lock out any other keyboard or
reporting activity until it is completed.
It will not interrupt a test in progress.
If the charging cycle should be
started inadvertently, it can be
stopped immediately by pushing
the RESET key.
During extended periods of
inactivity, overnight or longer, close
the tank valve to prevent leakage.
When changing oxygen tanks, close
the tank valve and push the 02 FILL
key to exhaust the system. Do not use
oil or combustible lubricants on this
filling system or on any devices
handling oxygen under pressure. Keep
all threads, fittings, and gaskets clean
and in good condition. Replace the two
394HCJE O-rings in the slip connector
if the connector fails to maintain a
tight seal on the bomb inlet valve.
The recommended 450 psig filling
pressure is slightly higher than the 30
atm prescribed in Parr bomb and
calorimeter instruction manuals. This
difference is insignificant. Higher or
lower settings can be used, but the
bomb must never be filled to more
than 600 psig (40 atm). If pressures
below 28 atm are used, the low
pressure warning will always occur.
5-1
5
All operations required to
standardize the 1356 Calorimeter, or
test an unknown sample, should
proceed step-wise in the following
manner:
1. Turn on the calorimeter. The bomb
parts should be wetted and then
dried in the manner used at the
conclusion of a test. This serves to
wet all sealing parts, as well as
leaving the bomb with the same
amount of residual water which
will exist in all subsequent testing.
2. Prepare the sample and charge the
oxygen bomb as described in
Operating Instructions No. 205M,
the Filling Connection Section.
The throughput of the 1356
Calorimeter can be increased by
using multiple bombs and water
buckets. With this arrangement,
the calorimeter can operate almost
continuously since the operator
will be able to empty a bomb and
recharge it while a run is in
progress. A bomb and bucket for
the next run will be ready to go
into the calorimeter as soon as it is
opened. Each bomb and bucket
combination will have to be
standardized separately and the
proper energy equivalent for each
set must be used when calculating
the heat of combustion.
3. Fill the calorimeter bucket by first
taring the dry bucket on a solution
or trip balance; then add 2000 (+/0.5) grams of water. Distilled water
is preferred, but demineralized or
tap water containing less than 250
ppm of dissolved solids is
satisfactory. The bucket water
temperature should be
approximately 1° to 2 °C below the
room temperature. It is not
necessary to use exactly 2000
grams, but the amount selected
must be duplicated within +/-0.5
gram for each run. Instead of
weighing the bucket, it can be
filled from an automatic pipet, or
from any other volumetric device
if the repeatability of the filling
system is within +/-0.5 ml.
To speed and simplify the
bucket filling process, and to
conserve water and energy, Parr
offers a closed-circuit Water
Handling System (No. 1563). This
provides a water supply, cooled to
the starting temperature and held
in an automatic pipet ready for
delivery in the exact amount
needed to fill the bucket. A 1552
Water Cooler is required when
using the 1563 Water Handling
System. Instructions for this
automatic system are given in
Operating Instruction No. 246M.
Operating the
Calorimeter
5-2
5
Operating the
Calorimeter
Continued
5-3
4. Set the bucket in the calorimeter.
Attach the lifting handle to the two
holes in the side of the screw cap
and partially lower the bomb in the
water. Handle the bomb carefully
during this operation so that the
sample will not be disturbed. Push
the two ignition lead wires into the
terminal sockets on the bomb
head. Orient the wires away from
the stirrer shaft so they do not
become tangled in the stirring
mechanism. Lower the bomb
completely into water with its feet
spanning the circular boss in the
bottom of the bucket. Remove the
lifting handle and shake any drops
of water back into the bucket and
check for gas bubbles.
5. Close the calorimeter cover. This
lowers the stirrer and thermistor
probe into the bucket.
6. Select determination or
standardization as appropriate on
Page 1, Calorimeter Operations,
Line 1, using the left arrow key to
toggle between the choices. Press
Start (Deter.) or Shift Start (STD) to
begin the test. The calorimeter will
now prompt the operator for Bomb
ID number, sample ID number,
sample weight and spike weight
in accordance with the instructions
set into the operating modes on
menu pages 2 and 6.
7. The calorimeter will now take over
and conduct the test. During the
time it is establishing the initial
equilibrium, it will display
PREPERIOD on the status bar.
Just before it fires the bomb, it will
sound a series of short beeps to
warn the user to move away from
the calorimeter.
Once the bomb has been
fired, the status bar will display
POSTPERIOD. The calorimeter will
check to make certain that a
temperature rise occurs and will
then look for the final equilibrium
conditions to be met. If it fails to
meet either the initial or final
equilibrium conditions, or if it fails
to detect a temperature rise within
the allotted time, the calorimeter
will terminate the test and advise
the user of the error.
8. At the conclusion of the test, the
calorimeter will signal the user.
9. Open the cover and remove the
bomb and bucket. Remove the
bomb from the bucket and open
the knurled valve knob on the
bomb head to release the residual
gas pressure before attempting to
remove the cap. This release
should proceed slowly over a
period of not less than one minute
to avoid entrainment losses. After
all pressure has been released,
unscrew the cap; lift the head out
of the cylinder and place it on the
support stand. Examine the
interior of the bomb for soot or
other evidence of incomplete
combustion. If such evidence is
found, the test will have to be
discarded.
10. Wash all interior surfaces of the
bomb with a jet of distilled water
and collect the washings in a
beaker.
5
11. Remove all unburned pieces of
fuse wire from the bomb
electrodes; straighten them and
measure their combined length in
centimeters. Subtract this length
from the initial length of 10
centimeters and multiply this
burned length by 2.3 calories per
cm (for Parr 45C10 Fuse Wire) to
obtain the fuse correction. The
scale on the fuse wire card can be
used to obtain this value directly.
12. Titrate the bomb washings with a
standard sodium carbonate
solution using methyl orange, red
or purple indicator. A 0.0709N
sodium carbonate solution is
recommended for this titration to
simplify the calculation. This is
prepared by dissolving 3.76 grams
of Na2CO3 in the water and
diluting to one liter. NaOH or KOH
solutions of the same normality
may be used.
13. Analyze the bomb washings to
determine the sulfur content of the
sample if it exceeds 0.1%.
Methods for determining sulfur
are discussed in Operating
Instructions No. 207M.
14. At the end of the testing period,
turn OFF the calorimeter at the
power switch.
Large particles may not burn
completely and small particles are
easily swept out of the capsule by
turbulent gases during rapid
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 combustion.
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.
Note:
Particle size is important because
it influences the reaction rate.
Compression into a pellet is
recommended because the pressure
developed during combustion can be
reduced as much as 40% when
compared to the combustion of the
material in the powder form. In
addition in giving controlled burn
rates, the pelletizing of samples keeps
the sample in the fuel capsule during
combustion.
Operating
Suggestions
5-4
5
Combustion
Aids
Combustion
Capsules
5-5
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:
Combustion aids add 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 in the form of a pellet to avoid
possible damage to the bomb which
might result from rapid combustion of
the loose powder.
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 is required, or where the
superior corrosion resistance of a
Pt-Rh, the 43A5 Capsule is required.
The stainless steel capsules will
acquire a dull gray finish after repeated
use in an oxygen bomb due to the
formation of a hard, protective oxide
film. This dull finish not only protects
the capsule, but it also promotes
combustion and makes it easier to
burn the last traces of the sample.
It is recommended, therefore, that
new capsules be heated in a muffle
furnace at 480 °C for four 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 a
nalytical balance.
Foodstuffs and Cellulosic Materials.
Fibrous and fluffy materials generally
require one of three modes of
controlling the burn rate. Fibrous
materials do not pelletize readily and
generally require either moisture
content of 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.
5
In most cases it may be necessary
to burn coarse samples without size
reduction since grinding or drying may
introduce unwanted changes. There is
no objection to this if the coarse
sample will ignite and burn
completely. Whole wheat grains and
coarse charcoal chunks are typical of
materials which will burn satisfactorily
without grinding and without additives
or a special procedure.
Corrosive Samples. The 1108
Oxygen Bomb is made of a corrosion
resistant alloy designed to withstand
the corrosive mixture of sulfuric and
nitric acids produced in normal fuel
testing operations. Samples containing
chlorine and particular samples
containing more than 20 mg of
chlorine or samples with high sulfur
contents will greatly accelerate
corrosion of the bomb. An alternate
1108CL Bomb is available constructed
of an alloy selected to specifically
resist the corrosive effects of samples
with high chlorine or chloride.
While no material will offer
complete corrosion resistance to these
samples, the 1108CL Bomb offers
significantly enhanced corrosion
resistance for this service.
Parr offers the 1104 High Pressure
Oxygen Bomb designed specifically for
testing materials which detonate with
explosive force, burn with unusually
high energy levels or release large
volumes of gas. This bomb is much
heavier in construction than the 1108
and should be used when testing these
types of materials. The program in the
calorimeter can be modified to
accommodate the slower heat transfer
later of the 1104 bomb with the
selections on Page 4, Line 2 of the
Main Menu
Volatile Sample 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, is 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. This can be done 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 Page 2.3 - Spike Controls, Line 2 Heat of Combustion of Spike.
Coarse
Samples
Explosives and
High Energy
Fuels
Volatile
Samples
5-6
5
Volatile
Samples
Continued
Fig 5-7 Combustion Capsule with Adhesive Tape Seal
Note:
Tape should always be stored in a
sealed container to minimize changes
in its moisture and solvent content.
Use the following procedure when
filling and handling any of these
tape-sealed sample holders:
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
5-7
the disc with a sharp needle to make a
small opening which is needed to
prevent collapse of the disc when
pressure is applied.
Fill the bomb with the usual
oxygen charging pressure.
The calorimeter will fire the bomb
and complete the test in the usual
manner.
Volatile samples are defined as
one with an initial boiling point below
180 °C per ASTM D-2.
Low volatile samples with a high
water content, such as urine or blood,
can be burned in an open capsule by
absorbing the liquid on filter paper
pulp or by adding a combustion aid,
such as ethylene glycol.
5
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
combustion for all samples.
The following fundamental
conditions should be considered
when burning samples:
Some part of the sample must be
heated to its ignition temperature to
start the combustion and, in burning, it
must liberate sufficient heat to support
its own combustion regardless of the
chilling effect of the adjacent metal
parts.
The combustion must produce
sufficient turbulence within the bomb
to bring oxygen into the fuel cup for
burning the last traces of the sample.
Loose or powdery condition of the
sample which will permit unburned
particles to be ejected during a violent
combustion.
The use of a sample that contains
coarse particles which may 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 noncombustible material in the sample.
If the moisture, ash and other non
combustible material in the sample
are approx. 20% or more of the charge,
it may be difficult to obtain complete
combustion. This condition can be
remedied by adding a small amount of
benzoic acid or other combustion aid.
The 1356 Calorimeter has been
designed to operate with an oxygen
filling pressure of 30 atm. Significant
changes from this value are not
recommended.
Poor
Combustion
Oxygen
Charging
Pressure
5-8
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 from three methods.
These are:
Manual Entry
Fixed Corrections
Automatic Data Transfer
Program and Installation chapter
(also see Figure 4-1 in this manual)
provide the default settings used
to setup the method preferred by
the user. Refer to the Reporting
Manual Entry
During the reporting process, the
controller will prompt the user to enter
the following values:
Fuse Correction
Key in the Fuse Correction and
press the ENTER key. The default
setting for this value is to be
entered in calories.
Acid Correction
Key in the Acid Correction and
entered in milliliters of standard
alkali required to titrate total acid
or calories.
Sulfur Correction
Key in the Sulfur Correction and
6-1
6
Instructions, Chapter 7, for the
steps necessary to initiate a report
from the controller.
Calculated Titer
A new ASTM alternative
is available.
The nitric acid correction can
be calculated based on the energy
release of the sample. A discussion
of this procedure is found in
Chapter Four for menu page 5.7
where correction is entered.
entered as percent sulfur in the
sample.If fixed values for fuse, acid
and sulfur are turned OFF on Menu
Page 5, Lines 1-6, then the user
must manually enter the values at
the prompt. If “Use Spiking
Correction” on Page 2, Line 3 is
turned ON, a spiking correction
must be entered before obtaining a
Final Report. After the last entry
has been made, the calorimeter
will automatically produce a Final
Report. If values for these corrections are not available, the operator can use the SKIP key to bypass
any of the corrections, however, a
Final Report will not be printed
until an entry is made for fuse,
acid and sulfur.
6
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.
Fixed
Corrections
Acid and/or sulfur corrections can
be automatically transferred into the
calorimeter from a Parr 1760 Sulfur
Analyzer. Sulfur corrections can also
be transferred from a Parr 1742 Sulfur
Interface.
Page 6 - Data Entry Controls, Lines
1-4 can be set for automatic transfer
from devices connected via the Smart
Link when default is set to automatic
entry.
The calorimeter will poll the
attached device when the user initiates
the reporting process. If a value is not
found, the user will have the option of
entering it manually.
Mention the difference for the new
bomb style.
Automatic
Data Transfers
6-2
REPORTING INSTRUCTIONS
7
Report Option
Selection
The 1356 Calorimeter can transmit
data four ways:
RS232C port to a 40 or 80 column
printer to provide a printed report.
Smart Link which formats and
prints the data on another calorimeter
with an attached printer.
Use Alternate Menu 2 to send a
duplicate report to the balance or the
terminal port
Use Alternate Menu 3 to send
duplicate reports directly to a PC
without an installed computer
interface.
After the cabling and
communication requirements are
completed in the Installation, Chapter
2, and the calorimeter must be
programmed to format and direct the
report. This option is on Page 7 Reporting Controls, Line 1 - Printer
Controls.
Report
Destination
Report(s) can be directed to a
printer, null device or display. This
selection is on Page 7 - Reporting
Controls, Line 2 - Report Destination.
The default is selected by pressing
the YES or NO key.
Printer Reports - Are printed on
the selected printer. The ID No. of the
report being printed will be briefly
displayed on the screen while printing.
Null Device Reports - If previously
completed tests require changes, the
null device default is used to recalculate
the test results without printing.
Displayed Reports - Are shown on
the calorimeter screen. The report is
viewed by pressing the DOWN arrow,
UP arrow or ESCAPE to clear.
Note:
The default setting sends the
calorimetric reports to the printer
until changed by the user.
7-1
7
Report
Generation
There are two kinds of calorimeter
reports; preliminary and final.
Preliminary reports are generated
at the conclusion of a test when one or
more of the calorimeter corrections
(fuse, acid, sulfur or spike) are not
fixed. If a preliminary report is
requested, the Sample ID will be
displayed and prompt the user for a
correction value for required fuse, acid,
sulfur or spike before providing the
report. If Smart Link Communication is
enabled for acid, sulfur or a fixed fuse
correction, this prompting for
information is eliminated. To provide a
report with the information “as is”,
press SHIFT and REPORT. Preliminary
reports will remain preliminary and the
energy equivalent or heat of
combustion value reports will reflect
the user’s setup on Page 5 Thermochemical Corrections.
Final reports contain all of the
final or fixed calorimetric corrections
needed to give an energy equivalent
or a heat of combustion value.
To start a report:
Press the REPORT key.
Calorimeter will prompt “From
ID>”. Enter beginning ID of the test(s)
to be reported and press the ENTER
key.
Calorimeter will prompt “To ID>”.
Enter final ID of the test(s) to be
reported and press the ENTER key.
The reporting process begins.
To stop printing:
Press RESET - The calorimeter will
reset and printing will stop after the
buffer is cleared.
Press SHIFT and RESET - Clears
buffer and stops printing immediately.
Net Heat of Combustion
To have the Net Heat of
Combustion print as part of
preliminary and final reports, go to
Page 5 - Thermochemical Corrections
and turn ON Line 8 - Calculate Net
Heat of Combustion. During the
reporting process, the controller will
prompt for the hydrogen (H) value.
This information will not transfer over
the Smart Link.
7-2
MEMORY MANAGEMENT
Clearing
Memory
Editing
Memory
8-1
8
he calorimeter will hold data for
tests within its memory. These
tests may be either preliminary, final,
determination, or calibration reports.
Once the memory of the controller is
filled, any attempt to start a new
analysis will cause the controller to
T
display “RUN, LIST, FULL”. The user
must then clear some of the memory
before proceeding or use the overwrite
capability on Page 7, Line 6. The
overwrite capability does not affect
or remove preliminary tests.
This capability allows the operator
to delete Sample ID numbers (and all
related data and results) for a single
report, sequence of reports or for all
reports.
deleted and press the ENTER key.
To clear some or all memory:
Press CLEAR MEM.
ID>”. Enter beginning ID of the Test(s)
to be deleted and press the ENTER key.
Enter final ID of the test(s) to be
Note:
A single test can be deleted by
entering the same Sample ID No. for
the “From ID>” and “To ID>”. To clear
all reports, enter 1 for the “From ID>”
and 999999 for the “To ID>”. This will
clear all tests including the calibration
tests. One way to avoid this is to give
the calibration tests a Sample ID
number in the range from 1 to 100.
Then clear the range 101 to 999999.
The user can add or change
previously gathered test information.
This feature is provided principally to
permit editing of sample weights or
other information to preliminary tests.
To revise the sample weights, spike
weights, Cal ID number, fuse, acid, and
sulfur or hydrogen values on final
reports:
Go to Page 7 - Reporting Controls,
Line 7 - Edit Final Reports and select
ON.
Go to Page 7 - Reporting Controls,
Line 2 - Report Destination and select
Display.
ID>”. Enter beginning ID of the Test(s)
to be edited and press the ENTER key.
Enter final ID of the test(s) to be edited
and press the ENTER key. (The
calorimeter will identify the report(s)
as either preliminary or final.)
Highlight the data field to be edited
by pressing the UP or DOWN arrow
key
Press the CLEAR key, enter the new
value on the keyboard and press
ENTER. The report will immediately
recalculate the heat of combustion
when a new value is entered.
To edit a report:
Press the F3 key.
Note:
This sequence can be canceled by
pressing the RESET key.
9
MAINTENANCE AND TROUBLE SHOOTING
Under normal usage the 1108 Parr
Oxygen Bomb will give long service if
handled with reasonable care.
However, the user must remember
these bombs are continually subjected
to high temperatures and pressures
that apply heavy stresses to the
sealing mechanism. The mechanical
condition of the bomb must therefore
be watched carefully and any parts
showing signs of weakness or
deterioration should be replaced
before they fail. It is recommended
the 1108 Oxygen Combustion Bomb
have O-rings and valve seats replaced
after 6 months, 500 firings or at more
frequent intervals if the bomb has
been subject to heavy usage or if it
shows any evidence of damage.
Detailed information can be found in
Bulletin 205M supplied as a part of this
manual. This 1108 Oxygen Combustion
Bomb is the only part of the
calorimeter system that requires
routine maintenance. All other
problems will require diagnosis and
parts replacement
Oxygen Bomb
Fig 9-1 1108 Oxygen Bomb Assembly
9-1
9
Installing
Support Rod
Mounting
Plates
9-2
Turn off the instrument, disconnect
the harness plug from the logic pack
and open the cover. Then loosen the
eight set screws that secure the lower
link assemblies (S shaped) to the
assembly shaft rod. Remove the flat
head machine screws from the lower
linkages used to connect to the cover
brackets. These flat head machine
screws and retaining washers have
been fastened with Loctite and may
require more than normal effort to
loosen them. Care must be exercised
in this step as the cover may slip down
and possibly bend the thermistor
probe.
Remove the round head machine
screw that secures the tube clips to the
lower linkages and carefully move the
cover to the closed position. Remove
the two flat head machine screws that
secure the upper linkage to the support
rod mounting plates.
From the rear of the calorimeter,
with a nut driver or socket wrench,
remove the six nuts that secure the
support rod mounting plate to the
calorimeter chassis. Remove the two
snap rings that secure the retaining pin
to the upper U bracket and gas spring,
and remove retaining pin. The lower
linkages that were previously loosened
via set screws can now be moved
toward the center on the shaft
assembly rod.
Lower the shaft assembly rod and
remove both support rods mounting
plates from the shaft assembly rod.
Position the new mounting plates,
A536DD3 and A535DD3 on the shaft
assembly rod.
Secure the mounting plates with
previously removed nuts, finger tight.
With previously removed flat heat
machine screws and retaining
washers, secure the upper linkage to
the support rod mounting plates. Use
the retaining pin to secure the gas
spring to the U bracket. Reattach the
snap rings on the retaining pin. Push
the lower linkages to the outer most
position on the shaft assembly rod.
Raise cover to open position. Attach
tube clips to the lower linkage
assembly with the nut and washer and
indicators for the various electrical
outputs of the controller. The neon
lamp associated with each between
the two linkage assemblies. Reattach
lower linkage arms to the cover
bracket with the flat head machine
screws and retaining washers.
Position lower linkage assemblies
to out most position against the
support rod mounting plate. Lower the
cover and align cover so that cover has
a uniform alignment with calorimeter
chassis, front, side and rear. No air gap
should exist between rear portion of
cover and the calorimeter chassis.
Now secure the nuts on the support
rod mounting plates, alternating
between left and right hand plates
until all six nuts have been tightened.
Raise the cover and recheck the
lower linkages to be sure they are at
outer most position adjacent to
respective mounting plates. Secure
the 8 set screws. Reattach cable
connector, lower cover and recheck
cover adjustment.
9
The 1356 Calorimeter Controller
can be physically separated into
halves. The upper portion consists of
the keyboard, LCD display and
associated driver board. This display
and keyboard assembly is attached to
the lower portion of the controller with
two cables. Six screws are used to
mate the upper portion of the
controller to the lower half.
1. Disconnect the power cord
from the rear of the controller.
2. Remove the six screws located
on the display bezel.
3. Remove the bezel.
4. Separate the keyboard and the
display assembly from the
lower portion of the controller
by lifting the upper assembly
from the lower edge.
5. Unplug the 2 cables attached to
the backside of the display
driver board (A1641E).
1. Disconnect the power cord and
any Smart Link and/or printer
cables from the rear of the
controller.
2. Disconnect the two orange plugs
from the side of the controller.
3. Disconnect the BNC connectors
attached to the ends of the bucket
and jacket thermistor probes.
4. Remove the six screws located on
the display bezel and remove the
bezel.
5. Push the rear of the controller near
the bottom of the case. This will
force the display panel up.
6. Grab hold of the front edge of the
controller which has been forced
7.
up in the preceding step, and
guide it out of the front of the
calorimeter case, tilting where
necessary to provide clearance
for the BNC jacks.
The controller may now be
separated, if desired, by following
the procedure given for the logic
pack removal.
If the controller is returned for
evaluation and/or repair, both the
upper and the lower portions must
be secured with screws.
Otherwise, they must be
separated to avoid damage in
transit.
1356
Calorimeter
Controller and
Keyboard
Display
Removal
Keyboard/
Display
Removal
Removing the
Entire
Controller
from the
Calorimeter
9-3
9
1356
Series
Calorimeter
Firmware
Update
Procedure
minimum system consisting of a
486/33 processor running the
Microsoft Windows 95 operating
system. Windows 98 and Windows
NT 4.0 are also supported.
Overview
This procedure describes the
firmware or program update procedure
for the 1266 and 1356 Calorimeters.
The program update is transferred
from a file located on a PC (via an
RS-232 serial or COM port) to the
non-volatile Flash ROM located on the
CPU board in the controller. A program
update utility program, provided by
Parr, is used to facilitate this file
transfer. The PC based, program
update utility will operate on a
Preliminary Steps
Before updating the calorimeter
controller firmware, you should make
careful note of any important
controller settings. The new controller
firmware will overwrite the existing
controller configuration.
Acquire the
Program
Update
The latest calorimeter firmware is
maintained at ftp://ftp.parrinst.com/outgoing. Go to the product specific
directory (1266 or 1356) and then to
the program_update sub-directory.
Transfer all the files in this directory to
a single directory (for example, Parr)
on your computer. To install the
firmware download utility on the PC,
run the setup program, setup.exe.
Connect the
Calorimeter
Controller to
the PC
Connect a cable, consisting of the
A1507E printer cable and the 1454E
adapter, between the terminal port at
the rear of the controller and an
unused RS-232 serial port (COM 1 or 2)
on the PC. The 1454E (RJ-45 to 9 pin D)
adapter is provided as an accessory
item with each calorimeter.
Update the
Calorimeter
Controller
Program
After the installation, execute the
download utility and click on
“Communications” on the menu bar to
select the PC COM port to be used.
Cycle power on the controller and
immediately click on the <- - -> button.
This should display the calorimeter
controller boot monitor menu in the
terminal window. Click on 1 to
download a new program. Click yes
when prompted. This will erase the
current program in the Flash ROM.
When the monitor program displays
“Send S-records now” click the <Send
S-records> button and select the file
do be used to update the controller.
This file will have a program extension
of “.fu”. You will have to navigate to
the directory (for example, Parr) where
this file is located or enter the full path.
This begins the actual firmware
download that may take up to 30
minutes to complete. When the
download is complete, a CRC (checksum) calculation will verify that the
program is correct. Cycle power on
the controller to start the new
program. Reconfigure the calorimeter
controller as requited to re-establish
any important operating parameters.
9-4
9
The 1356 calorimeter controller is
equipped with a generous set of error
messages to inform the user in the
event of a malfunction. Some of the
error messages refer to conditions that
may exist if certain inputs are not
sensed properly, such as the
temperature probes. Other error
conditions may result if certain outputs
are not activated at the proper time.
The rear panel of the 1356 Controller
has a series of five holes that serve as
test points and indicators for the
various electrical outputs of the
controller. The lamp associated with
each output will glow when the
respective output has been turned ON.
The lamp may glow dimly all the time
if the load has been removed or is
defective (open). The fuses for the
outputs are located underneath the
cover on the side of the controller.
Power should be removed from the
controller before removing the fuse
cover. Refer to the following table
for fuse assignments.
Troubleshooting
the 1356
Calorimeter
Controller
Fuses
Table 9-2 1266 / 1356 Calorimeter Controller Fuses
Location/Use
IO Board/O2 Solenoid
IO Board/Stirrer
IO Board/ Transformer primary
Power Supply/Ignition Circuit
Power Supply/All outputs except above
Fuse
F3
F4
F6
F1
F2
Rating1
1A fast acting
1A fast acting
1.6A slo-blo
1A fast acting
10A fast acting
Parr #
1641E
1641E
997E2
1641E
1641E4
Littlefuse #
217001
217001
21801.6
217001
217010
All fuses are 5 x 20 mm, glass type.
The output for O2 solenoid may
be forced on by shorting the pins
through the hole above the indicator
lamp. These pins may be shorted by
using a thin blade screwdriver. There
is no danger if the screwdriver touches
the case since only low voltages are
present at these pins. A blown fuse or
a problem with the solid state relay is
indicated if the output or indicator
lamp fails to come on when these pins
are shorted. If the indicator light comes
on when the pins are shorted and the
output O2 solenoid is not activated,
then the output needs servicing or
replacement. Refer to the following
tables for the pin outs of the three
Wago connectors used in conjunction
with the IO board.
9-5
9
Troubleshooting
the 1356
Calorimeter
Controller
Continued
Table 9-3 11 Position Connector Pinout Table
11 Position
Wago header pin #
1
2
3
4
5
6
7
8
9
10
11
Output
Stirrer motor hot (1356 only)
Stirrer motor neutral (1356 only)
Chassis Ground (not used)
Low voltage stirrer output (1356 only)
LV stirrer out return (1356 only)
Bomb ignition
Bomb ignition
Connected to 9
Connected to 8
O2 pressure switch (input)
O2 pressure switch (ground)
10 Position
Wago header pin #
4
5
8
Output
O2 solenoid hot
O2 solenoid neutral
Chassis Ground (pump)
12 Position Wago header
(inside controller) pin #
1
2
3
4
5
6
8
9
10
11
12
9-6
Connection
AC power to transformer line
AC power to transformer neutral
AC from switch neutral
AC from switch hot
Chassis ground
SSR #1 (line)
NC
Bomb ignition Cap Bomb ignition Cap +
SSR #3 (+5 VDC)
SSR #4 (open collector)
9
If a problem is suspected with the
controller on the basis of the above
test procedure, the entire controller
should be returned to Parr Instrument
Company for repair. Board level
schematics, parts and parts lists for
the controller circuit boards are
not available.
Power supply voltages
The nominal controller power
supply voltages are indicated in the
following figure.
1356 Electric Circuit Diagram
Voltage tolerances for regulated
outputs are 5%. Vbulk is not regulated
and is typically 13 VDC with a 120/240
VAC line voltage input. Power fail is
TTL high when the controller is operating properly. None of the operating
voltages are adjustable.
9-7
9
Keyboard
Inoperative
Temperature
Problems
A bad keyboard panel will result in
the calorimeter responding to only
some rows or columns of keys and
ignoring others. If the keyboard has
failed completely, the calorimeter will
not respond to any key presses. In
either case, the calorimeter will power
up or display the main menu. If the
calorimeter does not power up
normally, then there is another
problem and the lack of response to
key presses is probably a symptom of
this other problem and not the result
of a failed keyboard panel.
When any row or column of keys
fail on the keyboard panel of a 1356
Calorimeter, the panel is unrepairable
and must be replaced. A replacement
keyboard panel can be ordered from
Parr. The Parr part number is 1601E.
See Page 9-3 for replacement
instructions.
Temperature problems on the 1356
Calorimeter can range from incorrect
to erratic temperatures or “No
Temperature” error messages for
either the bucket or jacket or both.
pin 2 on the IO board. Pin 1 is the
upper most connection. If the cable is
properly connected at both ends and
the +/- 15 V supply voltages are
correct, then the problem lies with
the IO board.
Problems with either the
bucket or the jacket temperature,
but not both. Determine if the
problem is in the probe by temporarily
reversing the probe connections. If the
problem changes channels, then the
probe is faulty. The part number for
the probe is 893E. If the problem does
not change, then the problem lies with
the I/O board in the controller. Check
the thermistor cable inside the
controller that runs from the
thermistor probe sockets to the front
of the IO board. The red wire on the
bucket probe BNC connector is tied to
9-8
Problems with both the bucket
and jacket temperatures.
Check the resistance of each probe.
The resistance is nominally 2000
ohms. Replace probes as needed. If
the problem still exits, check the
thermistor cable inside the controller
which runs from the thermistor probe
sockets to the front of the IO board. If
the cable is properly connected at both
ends and the +/- 15 V supply voltages
are correct, then the problem lies with
the IO board.
9
Ignition problems on the 1356
Calorimeter can be generally attributed
to one of the following sources:
connector at the side of the
controller.
4. The IO board is bad.
1. Breakdown of insulator and
0ring on the insulated electrode
assembly in the 1108 Oxygen
Bomb. Any resistance reading
less than 100 ohm between the
insulated electrode and the bomb
head is an indication of insulation
breakdown.
2. One or both ignition lead wires
have broken internal wire strands.
Connecting the ohmmeter to the
ends of the wire and flexing the
wire may detect this. Any
fluctuations in the reading indicate
broken strands of wire. Readings
for bad ignition wires generally go
to infinity when the wire is flexed.
3. Failure of the terminations at the
controller. Insure that the wire
terminations for ignition wire are
properly inserted into the orange
The voltage output at the rear of
the controller is nominally 30 VDC
shortly after the controller beeps during the firing sequence. If no voltage is
measured at the controller at the end
of the firing cycle, then the problem
must be in the controller.
Attach a DC voltmeter to the large
(81000 MFD) capacitor in the controller
and activate the ignition circuit from
the diagnostics page. While the
controller displays “CHARGING”, the
voltage on the capacitor should ramp
up to 30 volts DC in one minute. If
little or no voltage is measured on the
capacitor during the charging period,
then the connections to capacitor are
bad or the I/O board is bad. If the
voltage ramps up to 30 volts during
the charging period, and the
connections are all good, then the
IO board is bad.
The pressure switch must see at
least 400 psi in the bomb charging line
at the end of the one minute filling
cycle otherwise a low oxygen fill error
message will be issued. The
recommended oxygen line pressure
to the calorimeter is 450 psig.
A common reason for this error
message is a plugged orifice at the
input of the oxygen solenoid block.
This generally occurs shortly after
changing the oxygen tank if the tank
connection is not clean. The problem
may be resolved by back flushing
the solenoid block.
If the oxygen pressure switch
connections are shorted out and the
controller indicates a closed
connection on the IO diagnostics page,
then the oxygen pressure switch has
failed. If the controller fails to indicate
a closed connection, then a failure of
the CPU board is likely.
Bomb Firing
Problems
Low Oxygen
Pressure
9-9
9
Bucket
Thermistor
Replacement
Instructions
for Adjusting
Cover
9-10
Open the calorimeter cover, and
remove the power cord from the rear
of the instrument. Use an Allen wrench
to remove the twelve button head
screws that secure the cover to the
bottom plate of the cover assembly.
The screws at the rear of the cover
must be removed with the cover in a
not fully pushed back position. Before
removing the last screw, grasp the
cover assembly so that it does not
drop and become damaged.
Remove the two cable clips that
secure the thermistor cable to the
hinge assembly. Also, remove the
cable ties that secure the cable to
the plastic water tubing and to the
mounting bracket. With the cover
closed, remove the nut and plastic
ferrule that secures the probe to the
cover water jacket assembly. Remove
the probe from cover through the
cover and jacket hinge openings.
Disconnect the BNC connector from
the microprocessor case.
Reversing the above procedure,
install the new thermistor probe
using the previously removed nut
and ferrule.
1. Turn off instrument and open
cover.
2. Loosen 8 set screws that secure
the lower link assemblies, S
shaped, to the assembly shaft rod.
3. Carefully move the cover to the
closed position.
4. From the rear of the calorimeter,
with a nut driver or socket wrench,
loosen the six kep nuts that secure
the support rod mounting plate to
the calorimeter chassis.
5. Align cover so that cover has
a uniform alignment with
calorimeter chassis, front, side
and rear. No air gap should exist
between rear portion of cover
and the calorimeter chassis.
6. Position lower linkage assemblies
to outer most position against the
support rod mounting plate.
7. Now secure the nuts on the
support rod mounting plates,
alternating between left and right
hand plates until all six nuts have
been tightened.
8. Raise the cover and recheck the
lower linkages to be sure they are
at outer most position adjacent to
respective mounting plates.
Secure the 8 set screws.
9. Lower cover and recheck cover
adjustment.
9
The stirrer motor does not work or
is intermittent, which is generally due
to weakened torque capability. With
cover open and stirrer operating, one
should be able to stop stirring with
force of two fingers and on release the
stirrer should start. If motor does not
restart, replace the motor.
How to Check
the Motor
Remove the stirrer assembly from
the motor coupler. From the bottom
side of the cover, remove the 12 button
head socket screws that secure the top
cover of the metal plate. Remove the
motor’s electrical leads from the termi-
nal strip and note the terminal
connection for each lead wire. Remove
the 2 round head screws that secure
the motor to the cover and transfer
the coupler to the new motor.
Motor
Replacement
This error is generally attributed to
a calibration test that caused the range
of calibration tests to be larger than 12
calories/C. The cause of this may be
due to the fact that:
1. The oxygen bomb has 500 firings
and requires the replacement of
O-rings and valve seat.
2. The operator may have used the
wrong bomb, that is each bomb is
required to have its own EE value.
3. An operator is different than the
person that established the
original EE value; it may be
necessary for each operator to
have his or her own EE value.
4. The EE value may be an outlier
and discarded after using a
statistical review procedure.
EE Standard
Deviation
Exeeds Limit
There are four or five possible
causes of preperiod or postperiod time
limit violation. The causes are listed in
order of probability.
3. Water in the bottom of test
chamber.
4. A hose to the cover is crimped
when closed so that no water flows
to the cover. Crimp in plastic hose
generally may occur when hose
strikes the cable harness at the side
of power supply, A600DDEA.
5. The bucket temperature is started
at temperatures which are more
than 5 °C below the jacket
temperature of 35 °C.
6. Bomb leak
7. Bent or loose probe
8. Jacket water level
Preperiod or
Postperiod
Time Limit
Violation
1. The stirrer motor does not work or
is intermittent, which is generally
due to weakened torque capability.
With cover open and stirrer
operating, one should be able to
stop stirring with force of two
fingers and on release the stirrer
should start.
2. The bucket tipped so as to touch
the wall of test chamber.
9-11
9
1356
Calorimeter
Error List
Error: 35
Calibration EEPROM Bad read.
Error: 36
Calibration EEPROM Bad write.
Error: 40
Cold Restart - The
instrument has just
completed a cold restart.
All memory and calibration data has been reset
to their default values.
This could have been
caused by initial startup,
disconnection of the CPU
board, or a failure of the
battery backup.
Error: 41
Low Battery Voltage - The
CPU battery backup
needs replacement.
Error: 56
User Defaults Bad Write,
See Error 59
Error: 57
User Defaults Bad
Checksum, See Error 59
Error: 58
User Defaults Out of
Sync, See Error 59
Error: 59
Bad Upload Checksum Errors 56-59 will result if
the user default setup
can’t be stored to nonvolatile memory, or has
become corrupted.
Error: 62
9-12
Bad State Value - This
error will result if a check
of the input and output
images results in an
ambiguous condition.
Error: 64
Error: 66
Open Fuse Connection The controller has detected an open firing circuit
prior to firing the bomb.
Check and/or replace the
bomb fuse wire
Misfire
Error: 68
Pre-period Time-out The calorimeter has failed
to establish an acceptable
initial temperature, prior
to firing the bomb, within
the time allowed.
Possible causes for this
error are listed below:
• A bomb leak.
• Poor bucket stirring.
• Metal to metal contact
between the bucket and
the jacket.
• Lid not tight may be
high in back.
Error: 70
Post-period Time-out The calorimeter has failed
to establish an acceptable
final temperature within
the time allowed.
Possible causes for this
error are listed below:
• A bomb leak.
• Poor bucket stirring.
Error: 72
Run Aborted - This
message is issued if the
operator presses the
RESET key while a test
run is in progress.
Error: 74
O2 Fill Aborted
9
Error: 76
Error: 98
O2 Bad Pressure Sensor The oxygen pressure
switch was found to be
closed prior to filling the
bomb. Replace the
pressure switch.
Error: 110 Bomb 2 EE Std. Dev.
Exceeds Limit, See
Error 109
Exceeds Limit, See
Error 109
CAL not ready
Error: 100 CAL not running
Exceeds Limit, See
Error 109
Error: 102 Run in Progress - An
attempt was made to
start a test run or perform
diagnostics while a test
run is in progress.
Exceeds Limit, See
Error 109
Error: 105 Moisture value not found
Exceeds Limit, See
Error 109
Error: 108 Bomb Firing Count
Exceeds Limit - 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 Menu
Page 4 for appropriate
bomb number.
Exceeds Limit - The
relative standard
deviation for the
calibration runs for the
indicated bomb exceeds
the preset limit.
Exceeds Limit, See
Error 109
Exceeds Limit, See
Error 109
Error: 117 Temperature Rise
Exceeds Limit - The
temperature rise of the
test exceeded the
warning limit. This
indicates that the
maximum loading limit
of 8000 calories has
been exceeded.
Error: 119 Heater and Pump are OFF An attempt was made to
start a test run without
the water circulating
pump and heater being
turned on.
9-13
9
1356
Calorimeter
Error List
Continued
Error: 121 Jacket Temperature out
of Tolerance - A test run
can’t be started unless
the jacket temperature is
within the range of 29.5
to 30.5C.
Error: 123 Jacket Temperature
Exceeds Limit - The
jacket temperature has
exceeded the high limit
value of 40C. This usually
indicates a problem
with the heater control
circuitry.
Error: 126 S-Record: Bad Record
Number - Will be issued if
information downloaded
to the memory of the
Controller CPU is
determined to be invalid
during the download
procedure.
Error: 127 S-Record: Bad Byte
Count, See Error: 126
Error: 128 S-Record: Bad Address,
See Error: 126
Error: 129 S-Record: Bad Data, See
Error: 126
Error: 130 S-Record: Bad Checksum,
See Error: 126
Error: 131 Bad Remote Data
Request, Error: 126
Error: 132 Weight Not Found
Error: 133 Spike Weight Not Found
Error: 134 Acid Value Not Found
9-14
Error: 135 Sulfur Value Not Found
Error: 136 Hydrogen Value Not
Found - The controller
has not found the desired
datum for the sample ID
entered. This error results
during a Smart-Link
transfer if the datum or ID
can’t be located on the
Smart-Link network.
Error: 137 Weight Already Entered
Error: 138 Spike Weight Already
Entered
Error: 139 Acid Value Already
Entered
Error: 140 Sulfur Value Already
Entered
Error: 141 Hydrogen Value Already
Entered - An attempt was
made to re-enter a value
which is already present
in the test report.
Error: 142 Balance - Data is Not
(0-9, +, -, e, E)
Error: 143 Balance - Data Does Not
Match Template
Error: 144 Balance - Data is Unstable
Error: 145 Balance - Weight is
Negative - These errors
will result during a
balance transfer if the
datum is not within the
expected range or can’t
be interpreted properly
9
Error: 146 Invalid Password - This
error will result if an
incorrect password is
given at a prompt for a
password. If the
password is forgotten,
the entire CPU program
will need to be reloaded.
Error: 170 Run List Full - This error
will be issued when the
memory set aside for test
runs is exhausted. The
operator must either clear
space in the memory or
enable automatic
overwriting of the
oldest FINAL report.
Error: 147 Invalid sub-menu pointer
Error: 148 Invalid function pointer
Error: 149 Password Protected This error will result if an
attempt is made to access
a menu that has been
password protected.
Error: 171 Duplicate Sample ID This error will be
generated if an attempt
is made to use an ID
number that already
exists in the memory
of the controller.
Error: 155 BG and FG Colors are the
same
Error: 172 Sample ID Not Found This error will be
generated during the
reporting or clearing of
memory if the requested
ID can’t be found.
Error: 168 Run List Erased - The
stored test data run list
has been deleted and
reinitialized. This error
will occur as a result a
loss of battery backup to
the CPU board.
Error: 173 Bad Bomb ID - This error
will be issued if a bomb
ID outside the range of
1-4 is given at the prompt
for a bomb ID.
Error: 150 Weight is Zero - A sample
mass of zero is not an
allowed value.
Error: 169 Run List Modified - On
power up, the CPU scans
the run list and validates
each run area. This error
will result if one or more
of these areas are found
to be corrupted. Corrupted
run areas are cleared.
Error: 174 Smart Link - Master
Arbitration Error Will
result if the controller
encounters an error
during a Smart Link
transaction. The specific
type of error may be
useful in determining the
exact nature of the fault.
9-15
9
1356
Calorimeter
Error List
Continued
Error: 175 Smart Link - Slave
Arbitration Error, See
Error: 174
Error: 176 Smart Link - Bad Packet
Checksum, See Error: 174
Error: 177 Smart Link - Unit Did Not
Respond, See Error: 174
Error: 178 Smart Link - Output
Buffer Overrun, See Error:
174
Error: 179 Smart Link - Slave
Release Time-out, See
Error: 174
Error: 180 Smart Link - Master
Release Time-out, See
Error: 174
Error: 181 Smart Link - No Data
Available, See Error: 174
Error: 182 Smart Link - No
Response, See Error: 174
Error: 188 Open Jacket Probe 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 probe
resistance is 1000 to 5000
ohms.
Error: 191 RTS/CTS Handshake
Error, See Error 194
Error: 192 Transmitter Error, See
Error 194
Error: 193 Receiver Error, See
Error 194
Error: 194 Corrupted Data - These
errors will result if the
controller detects an
error during a serial
communication
exchange.
Error: 183 Shorted Bucket Probe
Error: 184 Shorted Jacket Probe
Error: 187 Open Bucket Probe 893E left side of bucket at
bottom:
• Check Connection to
board.
• Check quick
disconnects.
• Replace probe.
9-16
Error: 197 Data Log Buffer Full - This
message is issued when
RAM allocated for
data/process logging is
exhausted. Any logging
in progress is halted.
Error: 206 Factory Defaults Bad
Checksum, See Error: 207
9
Error: 207 Factory Defaults Out of
Sync - One of these
errors will be generated
when an attempt is made
to reload the factory
defaults, and a check
indicates that the factory
defaults are not valid.
Error: 256 Boot Block Bad
Command
Error: 208 Edit Final NOT Enabled An attempt was made to
edit a final report.
Error: 263 Bad Factory Defaults
Revision
Error: 209 Divide by Zero Error The controller attempted
to do a mathematical
calculation with a divisor
of zero.
Error: 257 Boot Block Bad Erase
Error: 258 Boot Block Write Timeout
Error: 259 Boot Block Bad Write
Error: 264 Bad User Defaults
Revision
Error: 265 I/O: Output Complete
Timeout
Error: 266 System data write error
Error: 253 Boot Block Bad Block
Number
Error: 254 Boot Block Erase
Suspended
Error: 267 Low Water Level
Error: 271 Sample ID Currently Busy
Error: 255 Boot Block Bad Vpp
9-17
APPENDIX A
MENU OPERATING INSTRUCTIONS
hen the START key is pressed,
the calorimeter will prompt the
user for the Sample ID number. If the
automatic Sample ID is turned ON, the
next sample will be displayed and if it
is correct, press the ENTER key. If it is
not correct, press CLEAR ENTRY and
key in the correct identification number
followed by ENTER. The instrument
will then prompt for sample weight, if
set up for keyboard entry. Again, key in
W
the weight followed by ENTER. If the
weight is set up for automatic transfer,
the value will be displayed and entered
directly. Spiking, if activated, is entered
the same as the sample weights.
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 1356 Calorimeter.
The calorimeter will normally be
operated from Page 1, although tests
can be started from many Main Menu
pages. The number of free areas in the
memory and the number of rinses left
in the wash tank are always displayed
at the top of this page.
At the bottom of the page is a
“status bar”. This bar provides the
current status of the calorimeter and a
graphical representation of where the
instrument is in its operating cycle.
Line 1 Operating Mode - Sets the
operating mode by toggling
between standardization and
determination.
Line 2 Bomb Installed/EE - Used to
identify the bomb presently
installed in the calorimeter
and its EE value.
Calorimeter
Operation
Page 1
A-1
Operating
Controls
Page 2
Line 1 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.
Line 2 Reporting Units - Offers a
choice of Btu/lb., Cal/g, J/kg or
MJ/kg for the reporting units.
Line 3 Use Spiking Correction Accesses sub-menu, Page 2.3 Spiking Controls. Spiking is
the material addition, such as
benzoic acid or mineral oil, to
samples which are difficult to
burn in order to drive the
combustion to completion.
Line 4 Other Multiplier
Line 5 LCD Contrast - Controls
the liquid crystal display on
the calorimeter. The number
entered sets the backlighting
intensity in values between 1
and 100. Higher numbers
provide brighter backlighting.
Most users will want to set to
100 for maximum backlighting.
A-2
Line 6 LCD Backlight Time-out The unit is equipped with an
automatic circuit to shutoff the
backlight when it is not being
used. The LCD screen
backlight will shutoff if there
is no keyboard activity for the
number of seconds entered.
Pressing any key will
automatically turn the
backlighting ON. A setting of
0 will keep the backlight ON
at all times.
Line 7 Print Error Messages - When
turned ON, all error messages
will be printed on the printer
and displayed on the screen.
Line 8 Display Stored Samples Displays a listing of all
Sample ID’s stored in the
memory of the calorimeter.
Line 9 Language - Options are
English, German, French or
Czech.
Spike Controls Page 2.3
Line 1 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.
Line 2 Heat of Combustion of Spike The heat of combustion of
spike is entered here, Cal/g.
Line 3 Use Fixed Spike - When set to
ON, a constant amount of
spike is to be added to each
test.
Line 4 Weight of Fixed Spike - The
weight of the fixed spike is
entered here. Normally the
calorimeter will prompt the
user for the weight of the
sample and then the weight of
the spike.
Line 5 Prompt for Spike before
Weight - When set to ON, the
above sequence will be
reversed.
Note:
The precision of tests with
fixed spikes can be no better
than the repeatability
of the spike weight.
A-3
APPENDIX A
Program
Information
and Control
Page 3
Line 1 Software Version - Displays
the current version of
software installed in the
calorimeter.
Line 2 Factory Hardware Version Displays the current serial
number of hardware installed
in the calorimeter.
Line 3 Date and Time - Used to enter
the current date and time.
Line 4 User Setup ID - Displays the
last user entered ID number
for the setup stored in the
calorimeter.
Line 5 Password Protection Provides password protection
for the program options and
settings on the menus. If this
feature is turned ON, the user
will be prompted for a number, up to six digits long,
which will be the password for
all protected settings. Once
protected, any attempts to
change a setting will be met
with a prompt for the password. The program revision
will only be made after the
correct password has been
entered. If access is required
to sensitive areas protected by
password and the password is
not known, new E-proms will
be required.
Line 6 Re-load Factory Default
Settings - Used to erase all of
the settings and restore the
A-4
Line 7 Re-load User Default Settings Used to restore the user’s
setup should the program in
the instrument be corrupted
for any reason.
Line 8 Save User Settings to Memory Used to record the setup to
the memory once
the user has configured the
instrument to their operating
requirements.
Note:
Lines 6 through 9 make global
changes to the setup of the
calorimeter and, therefore,
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.
Line 9 Cold Restart - Returns the
instrument to its initial state. It
will re-load from the memory
the user’s setup if it was saved
using Line 8 - Save Users
Settings to memory, and all
valid test data will be retained
during this cold restart
procedure. Otherwise the
instrument will return to the
APPENDIX A
Line 1 Use Bomb - Used to enter the
bomb number of the bomb
currently installed in the
calorimeter. The left and right
arrow keys are used to toggle
through the bomb
identification numbers
available for each bomb.
Line 2 Bomb Type in Use - Used to
enter the type of bomb being
used in the calorimeter.
Different bombs have different
heat capacities. The left and
right arrow keys are used to
toggle through the bomb
types the software supports.
Line 3 Jacket Temperature Set Point Used to set the Temperature
of the calorimeter jacket in °C.
Line 4 Calibration Run Limit Establishes the maximum
number of runs that will be
included in determining the EE
value of a bomb and bucket
combination. Most test
methods suggest 10 tests.
Some ASTM test methods call
for more then ten calibration
tests. This limit can be
adjusted to cover this case.
If more than the set maximum
is present, the most recent
tests will be used; if less than
the limit is present, all available
tests will be used.
the calorimeter. If this value is
exceeded, the user will be
warned to take corrective
action before proceeding with
testing. This calorimeter is
capable of achieving a value
of .15 or better.
Calibration
Data and
Controls
Page 4
Line 6 Bomb 1 - Leads to sub-menu,
Page 4.7 - Bomb 1. Contains
the standardization information for bomb and bucket
combinations. For rapid turn
around between tests, users
may wish to use more than
bomb and bucket in the
calorimeter. Each
combination should be
assigned a bomb number
and an EE Value. Use Page 6,
Line 6 to have the calorimeter
prompt for the bomb
combination being used in the
test before the test is started.
Line 7 Heat of Combustion of
Standard - Contains the heat
of combustion in calories per
gram for the material used to
standardize the calorimeter.
For benzoic acid, this value is
6318 calories per gram.
Line 8 Bomb Service Interval Establishes the maximum
number of times a bomb may
be fired before it is flagged as
due for service.
Line 5 EE Max STD Deviation Establishes the maximum
relative standard deviation in
percent that will be permitted
for any EE value calculated by
A-5
APPENDIX A
Calibration
Data and
Controls
Page 4
Continued
Bomb 1Page 4.6.1
Line 1 EE Value - Contains the
calculated EE value for the
corresponding bomb.
Line 2 Protected EE Value - When set
to ON, protects the EE values
if the user does not wish
to have the calorimeter
automatically update its own
EE value. Enter into Line 1 the
determined EE value and it
will not change unless revised
through the keyboard.
Line 3 Number of Runs - Shows how
many runs have been used to
determine the EE value.
Line 4 Relative Standard Deviation Reports the relative standard
deviation for the series of
tests used to determine the
current EE value.
Line 5 Bomb Firing Count - Contains
the current bomb firing count
or the number of times the
bomb has been fired since it
was last serviced. When this
count matches the limit set on
Page 4 - Calibration Data &
Controls, Line 4 - Bomb
Service Interval, the user will
be informed that the bomb is
ready for service.
A-6
Line 6 Print Standardization Runs Will print all of the tests that
have been incorporated into
the calculated EE value. This
will be helpful in evaluating a
series of tests which fail to
produce a satisfactory EE
value and relative standard
deviation.
Line 7 Update Statistics - This code
will cause the EE Value for this
calorimeter ID to be updated
using all standardization runs
currently in memory. (5)
Bombs 2 through 8, Pages
4.6.2 through 4.6.8. Accesses
sub menus Page 4.6.2 through
4.6.8 for Bombs 2 through 8.
Provides the same controls as
Page 4.6.1 through 8
APPENDIX A
Note:
To access the numeric field
from the ON/OFF toggle
position, press the SKIP
key. The SKIP key will also
return you to the ON/OFF
choices.
Line 1 Fixed Fuse Correction
(Standardization) - Turns
ON/OFF the fixed fuse
corrections for standardization
runs. The actual fixed
correction for this value is
entered in the second
data field.
Line 2 Fixed Acid Correction
ON/OFF the fixed acid
correction for this value is
data field.
Line 3 Fixed Sulfur Correction
ON/OFF the fixed sulfur
correction for this value
is entered in the second
data field.
Line 4 Fixed Fuse Correction
(Determination) - Turns ON/OFF
the fixed fuse corrections for
determination runs. The actual
fixed correction for this value is
data field.
Line 5 Fixed Acid Correction
the fixed acid corrections for
fixed correction for this value
data field.
Thermochemical
Calculations
Page 5
Line 6 Fixed Sulfur Correction
the fixed sulfur corrections for
fixed correction for this value
data field.
Note:
When fixed corrections are
turned ON, the value in the
attached field will be used in
the final reports. The
calorimeter will not prompt
for actual corrections. If all
corrections are fixed, then
there is no preliminary If
values for these corrections are
entered into these lines, and
the toggle is set to OFF, then
the fixed value will be used in
the preliminary report, but not
in the final report.
Line 7 Calculation Factors - Accesses
sub-menu, Page 5.7 Calculation Factors which sets
a number of options for the
way the thermochemical
corrections are applied.
Line 8 Calculate Net Heat of
Combustion - Turns ON/OFF
the calculations for the net
heat of combustion for
materials with significant
hydrogen content. When set
to ON, the calorimeter will
prompt for hydrogen content
during the reporting data
entry steps.
A-7
APPENDIX A
Thermochemical
Calculations
Page 5
Continued
Calculation Factors Page 5.7
Line 1 Acid Value is Nitric Acid Only When set to ON, the acid value
is nitric acid only. When set to
OFF, it represents both nitric
and sulfuric acid.
Line 2 Acid Multiplier - The
multiplier is the normality of
the sodium carbonate used to
titrate for the acid correction.
Line 3 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 on Line
4 set accordingly.
Line 4 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 here requires that the
sulfur value be entered in
weight percent.
A-8
Line 5 Fuse Multiplier - The fuse
corrections represent the
number of calories liberated by
the ignition wire or burning
thread used to ignite the
sample. If another
measurement is used, the
correction factor must be
entered here.
Line 6 Use Offset Correction (ISO) The thermochemical
calculations used for treatment
of nitric acid and sulfuric acid
corrections in the ISO and B. S.
methods require an offset
correction to compensate for
the back titration that is made.
To use these calculations, set
to ON and enter the
appropriate value on Line 7.
Line 7 Offset Value - Entry for the
value when Line 6 above is
turned ON.
APPENDIX A
Line 1 Weight Entry Mode - This data
field contains options for
entering the sample weight
through the keyboard,
instruments connected via the
Smart Link port or through the
balance port connection.
Line 6
Prompt for Bomb ID - In the ON
position the controller will
prompt for a Bomb ID (1-8) when
a test is started. This identifies
the correct EE Value to use from
Page 4.6.1 through 4.6.8
Data Entry
Controls
Page 6
Line 7 Use Long Sample ID Numbers
Line 2 Spike Weight Entry Mode This data field contains
options for entering the spike
weight value through the
keyboard, instruments
connected via the Smart Link
port or through the balance
port connection.
Line 3 Acid Entry Mode - This
data field contains options for
entering the acid correction
value through the keyboard,
Line 4 Sulfur Entry Mode - This data
field contains options for
entering the sulfur correction
value through the keyboard,
Line 8 Automatic Sample ID Number Displays the next Sample ID
which will be assigned and is
used to enter the beginning
Sample ID of any series. The
user can always override the
automatic Sample ID by
entering the desired number
and press the ENTER key.
Line 9 Preweigh Menu - Accesses
sub-menu, Page 6.9 - Preweigh
Sample ID Controls used to
automatically assign Sample
ID numbers when a series of
samples are pre-weighed
ahead of the time they are
actually tested.
Line 0 Weight Warning Above - 2.0
Line 5 Hydrogen Entry Mode - This
data field contains options for
entering the hydrogen content
for calculating the net heat of
combustion. This can be done
only through the keyboard.
A-9
APPENDIX A
Data Entry
Controls
Page 6
Continued
Preweigh Sample ID Controls Page 6.9
Line 1 Automatic Preweigh ID ON/OFF toggle for this feature.
Line 2 Automatic Preweigh ID
Increment - Establishes the
increment between samples.
A-10
Line 3 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.
APPENDIX A
Line 1
Printer Controls - Accesses
sub-menu, Page 7.1 - Printer
Type which contains the printer
selection and controls.
Line 2
Report Destination - Directs the
reports to the Printer Port, the
Smart Link Port, Display or Null
Device.
Line 3
Automatic Reporting Preliminary reports will be
generated at the conclusion of
the test and final reports will be
generated as soon as all of the
thermochemical corrections are
available when this automatic
reporting feature is turned ON.
When this is turned OFF, reports
will only be generated through
the reporting controls.
Line 4
Line 5
Individual 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.
Report Format - Offers a choice
of text or data for the report format. The data format is intended
for rapid transmission to an
attached computer.
Line 6
Overwrite Final Reports Establishes what the calorimeter
will do when its memory is full
of tests. In the ON position it will
automatically erase the oldest
test and replace it with the new
one. In the OFF position it will
not proceed until the user has
cleared memory space using the
memory management system.
Line 7
Edit Final Reports - When set to
ON and F3 is pressed, enables
the user to revise sample weight
and thermochemical corrections.
Line 8
Recalculate Final Reports - When
set to ON, causes a recalculation
of stored final reports using
calibration data and menu
settings currently in the
calorimeter.
Line 9
Use New EE Value in
Recalculation - When set to ON,
the recalculation made on Line 8
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.
Reporting
Controls
Page 7
A-11
APPENDIX A
Reporting
Controls
Page 7
Continued
Printer Controls Page 7.1
Line 1
Line 2
A-12
Printer Type - Toggles between a
Parr 1756 and a generic printer.
When set for the 1756 Printer, all
of the features of this printer,
such as red/ black printing, will
be activated.
Printer Connection - Sets the
printer location. The printer can
be connected directly to the
printer port or to another device
connected via the Smart Link.
Line 3
Remote Printer Unit ID
(0-15) - If printer is attached to
another device on the Smart
Link, the address of the device
must be entered here.
Line 4
Report Width - The column
width of the printer being used
can be set to 20, 40 or 80.
APPENDIX A
Line 1 Smart Link Controls Accesses sub-menu, Page 8.1 Smart Link Controls which set
the unit ID, baud rate and
report type.
Line 2 Printer Port (RS232C) Accesses sub-menu, Page 8.2 Printer Port Communications.
Line 3 Balance Port (RS232C) Accesses sub-menu, Page 8.3
Line 4 Terminal Port (RS232C) Accesses sub-menu, Page 8.4 Terminal Port Communications.
Sets the communication
parameters for the RS232C
ports used for a terminal port.
Standard options for data bits,
parity, stop bits, handshaking,
baud rate, terminal type and
remote terminal are provided
to match any devices that
might be connected to
these ports.
Communication
Controls Page 8
A-13
APPENDIX A
Communication
Controls Page 8
Continued
Smart Link Controls Page 8.1
Smart-Link Termination for the
1266 and 1356 Calorimeters
Unlike older Parr Instrument Company
calorimeters incorporating a
Smart-Link port, the 1266 and 1356
Calorimeters do not have a termination
switch. Instead, the Smart-Link
termination is software controlled and
set from controller front panel. The
Smart-Link termination menu item
(ON/OFF) is located in the
Communication Controls – Smart-Link
menu. Additionally, the green LED on
the rear of the controller indicates the
current state of the Smart-Link
termination. When the LED is lit, the
port is terminated. The Smart-Link port
should ONLY be terminated when ONE
Smart-Link cable is connected to the
controller.
Line 1 Smart Link Unit ID (0-15) Sets the Smart Link address.
If only one calorimeter is
installed on the link, the
address is 0. If more than one
is installed refer to the Smart
Link instructions in
Appendix D.
Line 2 Smart Link Baud Rate - Sets
the baud rate. Smart Links
normally run at 9600 baud
unless unusual circumstances
dictate slower speeds.
Line 3 Smart Link Report Type Toggles between short report
and long report.
Line 4 Timeout (x0.01s) 50
Line 5 Smart Link Termination - Used
to identify instrument at the
end of a Smart Link Network
Line 6 Use four digit year Off
Printer Port Communications Page 8.2
Line 1 Number of Data Bits Standard options for data bits.
Toggles between 7 and 8.
Line 2 Parity - Standard options for
parity. Choose from None,
Odd, Even, Mark or Space.
Line 3 Number of Stop Bits Standard options for stop bits.
A-14
Line 4 Handshaking - Standard
options for handshaking.
Choose from Xon/Xoff,
RTS/CTS and None.
Line 5 Baud Rate - Standard options
for baud rate. Choose from
9600, 4800, 2400, 2000, 1800,
1200, 600, 300, 150, 134.5, 110,
75 and 19.2K.
APPENDIX A
Balance Port Communications Page 8.3
Balance Port Communications.
Sets the communication parameters
for the RS232C ports used for a
balance port. Standard options for data
bits, parity, stop bits, handshaking, and
baud rate and balance type are
provided to match any devices that
might be connected to these ports.
9600, 4800, 2400, 2000, 1800,
1200, 600, 300, 150, 134.5, 110,
75 and 19.2K.
RTS/CTS and None.
Line 6 Balance Type - Choose from
Mettler 011, Mettler 03,
Sartorious, Ohaus or Generic.
Terminal Port Communications Page 8.4
RTS/CTS and None.
19.2k, 9600, 4800, 2400, 2000,
1800, 1200, 600, 300, 150,
134.5, 110, and 75.
Line 6 Terminal Type - Standard
options for terminal. Choose
from ADM-31 or VT100.
Line 7 Remote Terminal - When set
to ON, a remote terminal can
be used for diagnostic
purposes.
A-15
APPENDIX A
Diagnostics
Page 9
Provides the user with the means to
test many of the components and
subsystems of the calorimeter.
These capabilities must be used in
conjunction with the Maintenance
Instructions, Chapter 9, to obtain the
maximum benefits from these
capabilities.
Line 1 Self-Test - Initiates a test
of first the ROM and then
the RAM section of the
calorimeter controller. A
message line at the bottom
of this test screen reports
whether each section passed
this test.
Line 2 I/O Diagnostics - Accesses
sub-menu, Page 9.2 - I/O
Diagnostics. Allows the user
to test the ignition circuit,
pump motor and the
input/output drivers in the
Calorimeter.
Line 3 Thermometry Diagnostics Accesses sub-menu, Page 9.3.
The user can use this page to
confirm that valid temperature
values are being generated
by the bucket and jacket
thermistor.
A-16
Line 4 Communication Diagnostics Primarily for factory
testing and will not be useful
to most users, unless special
diagnostic equipment is used.
Line 5 Keyboard Diagnostics Accesses sub-menu, Page 9.5 Keyboard Diagnostics.
Line 6 EEPROM Up/Down Load Primarily for factory testing
and will not be useful to most
users, unless special
diagnostic equipment is used.
Line 7 Data Logger Menu - Primarily
for factory testing and will not
be useful to most users,
unless special diagnostic
equipment is available.
Line 8 Print Error List - Provides a list
of all error messages.
APPENDIX A
I/O Diagnostics Page 9.2
Line 1 Activate Ignition Circuit Activates the ignition circuit.
A volt meter can be placed
across the firing connections
on the cover plate assembly
to ensure that the actual
firing charge is reaching
these contacts.
Line 2 Motor Diagnostics - Accesses
sub-menu, Page 9.2.2 Motor Diagnostics. Selects
the pump motor test routines
and will allow the user the
opportunity to test the motor
in all four of its operating
modes.
Line 3 I/O Driver Diagnostic - Leads
to sub-menu, Page 9.2.3 - I/O
Diagnostics. This is a very
valuable diagnostic tool which
lets the user step through all
of the inputs/outputs and
manually turn them ON/OFF
to confirm that they are
working properly or to locate
operating problems. At the
top of this page will be listed
the current I/O function to be
tested. The YES/NO keys are
used to turn this function ON
or OFF. The UP and DOWN
arrow keys are used to scroll
through the I/O functions to
be tested. Supplemental
diagnostic information is
shown on the lower section
of these screens. Use the
help screen to view the bit
definitions of the I/O
functions.
I/O Diagnostics Page 9.2
Displays a diagram of the controller
keyboard. When a key is pressed, its
corresponding block on the display will
turn dark to confirm that the key is
actually working. To return to Page 9,
the ESCAPE key must be pressed two
times (once to test and a second to
ESCAPE).
A-17
CALCULATIONS
APPENDIX B
Calculating
the Heat of
Combustion
The 1356 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:
Temperature Rise.
The 1356 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. 202M).
Hc= WT – e1 – e2 – e3
m
Where:
Hc = Gross heat of combustion.
T = Observed temperature rise.
W = Energy equivalent of the
calorimeter being used.
e1 = Heat produced by burning the
nitrogen portion of the air
trapped in the bomb to form
nitric acid.
e2 = The heat produced by the
formation of sulfuric acid from
the reaction of sulfur dioxide,
water and oxygen.
e3 = Heat produced by the burning
fuse.
m = Mass of the sample.
These calculations are made in
calories, grams, and degrees Celsius,
and then converted to other units if
required.
Thermochemical
Corrections
B-1
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
Energy Equivalent.
The energy equivalent (represented
by W in the above formula, or abbreviated as EE) is determined by standardizing the calorimeter as described in
Appendix C - Standardization. It is an
expression of the amount of energy
required to raise the temperature of
the calorimeter one degree. It is commonly expressed in calories per
degree Celsius. Since it is directly related to the mass of the calorimeter, it
will change whenever any of the components of the calorimeter (i.e. the
bomb, bucket or amount of water)
is changed.
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 and combines with
water vapor to form sulfuric acid.
This liberates additional heat over the
normal combustion process where
APPENDIX B
sulfur is converted to sulfur dioxide.
The sulfur correction removes this
excess heat from the calculation.
Fuse Correction the fuse correction
accounts for the heat introduced by the
burning of the fuse. The value is
normally determined from the fuse
wire card by using the burned pieces
to determine the length of the wire
burned. A fuse multiplier is provided
on page 5.7 Line 5 for users that want
to use other systems to enter this
correction.
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 1356 Calorimeter can be set up
to apply the acid correction by either
the ASTM or ISO convention, as the
user prefers. Care must be used to
ensure the proper corrections are
applied, and the calculations made are
consistent with the procedure used.
ASTM and ISO
Methods Difer
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 1356 Calorimeter uses the most
recent, published values for all
thermochemical data.
Thermochemical Calculation
Details
Traditionally, standard solutions
and procedures have been established
to simplify the calculations related to
the thermochemical corrections.
The 1356 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.
B-2
APPENDIX B
Fuse
Correction
The fuse correction applied by the
calorimeter is calculated as:
e3 = (fuse value)(fuse multiplier).
e3 = (entered value)(Page 5.7 Line 5,).
“Fuse Value” is the number entered
by the user and the value which
appears in the test report.
Note:
Page 5.7 - Calculation Factors, Line
5 - Fuse Multiplier is normally set to
1.0 so the entered value is in calories
(Press SKIP to add the fixed value).
ACID and
SULFUR
Correction
B-3
Total acid is the amount of base
required to titrate the bomb washings
(milliliters).
Nitric acid is that portion of the
total acid in the bomb washings that
result when the nitrogen in the air that
is trapped in the bomb is burned at
high pressure. Since this nitric acid
does not result from the sample, and
the combustion conditions are
reasonably constant from test to test,
the amount of nitric acid formed is
also constant.
Acid multiplier is multiplied by the
user entered acid value to arrive at the
number of milliequivalents of acid.
This value is normally the
concentration (normality) of the
base in equivalents per liter (N).
Percent sulfur is the concentration
of sulfur in the sample (weight %).
Molecular weight of sulfur is 32.06.
Equivalent weight of sulfur in
H2SO4 is 16.03 (one half of the
molecular weight).
Heat of formation of nitric acid is
14.1 calories/milliequivalent.
Heat of formation of sulfuric acid
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 Page 5 - Thermochemical
Corrections, Line 1 or 4 is set to ON. A
fixed fuse correction of 15 calories is a
good value to use for the fixed correction. Total errors of more than 5 calories will seldom occur when using a
fixed fuse correction.
(from SO2) is 36.1 calories/
milliequivalent.
Sample mass is the mass of
sample burned in the bomb (grams).
Sulfur multiplier is multiplied by
the product of the user entered sulfur
value and the sample mass to arrive at
the number of milliequivalents of
sulfuric acid in the bomb washings.
Example:
(Percent Sulfur) x (Sample Mass) x
10 = milligrams of sulfur (milligrams of
sulfur) / (equivalent wt. of S in H2SO4)
= milliequivalents of H2SO4 Sulfur
Multiplier is then 10 / equivalent wt. of
S in H2SO4 or 10/16.03 = 0.6238
e1 is the nitric acid portion of the
total acid correction.
e2 is the sulfuric acid portion of the
total acid correction.
e1 + e2 is the total bomb acid
correction.
Calculation for e1 when entered
acid value is total acid:
[((total acid) (acid mult))-(percent
sulfur) (sample mass) (sulfur mult) ]
(heat of formation of HNO3)
APPENDIX B
Total acid milliequivalence milliequivalence of H2SO4 =
milliequivalence of HNO3.
(milliequivalents of HNO3) (heat of
formation of HNO3) = heat (in calories)
due to HNO3 produced.
Calculation for e1 when entered
acid value is nitric acid only:
(nitric acid) (acid multiplier) (heat of
formation of HNO3).
Calculation of e2 when entered
sulfur value is % sulfur:
e2 = (percent sulfur) (sample mass)
(sulfur multiplier) (heat of formation of
H2SO4).
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 Page 5 - Thermochemical
Corrections, Line 2 or 5 is set to ON. A
correction of 10 calories is a good number for the fixed nitric acid value. For
most work, it is recommended to set
“Acid Value is Nitric Acid Only”, Page
5.7, Line 1 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 Page
5 - Thermochemical Corrections, Line 3
or 6 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, or standardizing the
calorimeter, the Fixed Sulfur
Correction, Page 5, Line 3 should be
ON applying a fixed value of 0.0 to all
standardization tests. Benzoic acid
contains no sulfur.
Please note that the values entered
into the test report appear as entered
in the report. Values for e1, e2 and e3
are calculated and used as energy
corrections in accordance with the
formulas and settings given above.
The formulas used above to arrive at
e1 or e2 are not the same as the
formulas used for e1 and e2 which
appear in most ASTM bomb
calorimetric procedures. However, the
sum of e1 and e2, above, is equal to
the sum of the ASTM treatment of e1
and e2.
Table B-1 Settings for ISO & BSI Methods
Page
5
5.7
Line
2
3
5
6
1
2
3
4
6
7
Setting
Off
Off
Off
Off
On
On
On
-
Value
13
7
13
7
0.154
0.1
-43.5
B-4
APPENDIX B
ASTM
Treatment for
Acid and Sulfur
In the ASTM treatment, the
correction for acid formation assumes
that all the acid titrated is nitric acid.
Obviously, if sulfur is present in the
sample, which in turn produces
sulfuric acid, part of the correction for
the sulfuric acid formed is already
included in the ASTM nitric acid
correction (e1). This is adjusted by a
separate computation based upon the
sulfur content of the sample. An
additional correction of 1.37 Kcal must
be applied for each gram of sulfur
converted to sulfuric from sulfur dioxide. This is based upon the heat of
formation of sulfuric acid, from sulfur
dioxide, under bomb conditions, which
is -72.2 Kcal per mole or -36.1 calories
per milliequivalent. But remember, a
correction of 14.1 calories per
milliequivalent of sulfuric acid is
already included in the ASTM nitric
acid correction (e1). Therefore the additional correction which must be
applied for sulfur will be the difference
between 36.1 and 14.1 or 22.0 calories
per milliequivalent (44.0 Kcal per
mole). For convenience, this is
expressed, in the ASTM e2 formula,
as 13.7 calories (44.0/32.06) for each
percentage point of sulfur per gram
of sample.
ISO
Calculations
Both the ISO 1928 and BSI 1016:
Part 5 methods for testing the calorific
value of coal and coke, deal with acid
and sulfur corrections in a manner
which is somewhat different than
ASTM procedures. Provision has been
made in the 1356 Controller for dealing
with these different procedures.
The analysis of bomb washings in
these methods call for a titration, first
using O.1N barium hydroxide (V2)
followed by filtering, and a second
titration using 0.1N HC1(V1) after 20 ml
of a 0.1N sodium carbonate has been
added to the filtrate. Table B-1 gives
the settings which allows the results of
the two titrations, V1 and V2, to be
entered into the controller directly for
the calculation of the total acid
correction. V1 should be entered at
the prompt for acid and V2 is entered
at the prompt for sulfur. The settings in
Table B-1 assume that the same
procedure is carried out for both
standardization and determination.
The offset value is the product of 1, the Heat of Formation of Nitric Acid,
the acid multiplier, and the 20 ml of 0.1
N sodium carbonate used in the
analysis.
The formula used to get the total
correction in calories is as follows:
V1(Acid Multiplier)(Heat of
Formation of Nitric Acid)V2(Sulfur
Multiplier)(Heat of Formation of
Sulfuric Acid)+offset value.
The values for fixed acid and sulfur,
which are used in preliminary reports,
will reflect a sulfur correction of 0, and
a nitric acid correction of 10 calories.
B-5
APPENDIX B
The following tables illustrate all
possible combinations for the four
flags related to the “acid” correction
value. For clarity, the calorimetry
corrections for e1-3 are provided for
all cases.
Calculate
HNO3 from
the Energy
Release
Table B-2 Entered and Reported Acid Value is Taken as Nitric Acid Only
FLAG
Calc. HNO3
Fixed Acid Std.
Fixed Acid Detr.
Acid is HNO3 Only
OFF
ON 1
ON 1
ON
OFF
ON 1
OFF 2
ON
OFF
OFF 2
ON 1
ON
OFF
OFF 2
OFF 2
ON
Use Correction Equations Set 1
Table B-3 Entered and Reported Acid Value is Considered Total Acid
FLAG
Calc. HNO3
Fixed Acid Std.
Fixed Acid Detr.
Acid is HNO3 Only
OFF
ON 1
ON 1
OFF
OFF
ON 1
OFF 2
OFF
OFF
OFF 2
ON 1
OFF
OFF
OFF 2
OFF 2
OFF
ON
OFF 2,7
ON 3,5
ON
ON
OFF 2,7
OFF 2,7
ON
ON
OFF 2,8
ON 3,6
OFF
ON
OFF 2,8
OFF 2,8
OFF
Use Correction Equations Set 2
Table B-4 Calculate HNO3 if Fixed and Acid is HNO3 Only
FLAG
Calc. HNO3
Fixed Acid Std.
Fixed Acid Detr.
Acid is HNO3 Only
ON 4,5
ON 3
ON 3
ON
ON
ON 3,5
OFF 2,7
ON
Table B-5 Calculate HNO3 if Fixed and Acid is Total Acid
FLAG
Calc. HNO3
Fixed Acid Std.
Fixed Acid Detr.
Acid is HNO3 Only
ON 4,6
ON 3
ON 3
OFF
ON
ON 3,6
OFF 2,8
OFF
B-6
APPENDIX B
Calculate
HNO3 from
the Energy
Release
Continued
1. Use the fixed acid value to
the right on menu page 5 in
preliminary reports and don’t
prompt for an acid value when
the test is reported in an attempt
at making it final.
2. Use the fixed acid value to
the right on menu page 5 in
preliminary reports and prompt
for an acid value when test is
reported again in an attempt
at making it final.
3. Calculate HNO3 from the energy
released and don’t prompt for an
acid value when the preliminary
test is reported in an attempt at
making it final. Use Correction
Equation Set 3.
4. Turning the calculate HNO3 flag
ON will force both fixed acid flags
ON and CALC will be displayed to
5.
6.
7.
8.
the right on menu page 5. The
user has the option of turning one
or the other (or both) fixed acid
flags OFF after the calculate HNO3
flag is turned ON.
Reported acid value is e1. If the
EE value or the temperature rise is
altered via the editing process, the
nitric acid value used in the
calculations and displayed on
the report changes.
Reported acid value is e1+e2.
If the EE value, sulfur or the sulfur
temperature rise changes via the
editing process, then the nitric acid
portion of the total acid correction
changes. As a result, the reported
acid value (e1+e2) must also
change.
Use Correction Equation Set 1
Use Correction Equation Set 2
Correction
Equation
Set 1
e1 = (nitric acid)(acid multiplier)(Hf of
HNO3)
e2 = (amount of sulfur)(sulfur
multiplier)(Hf of H2SO4) Amount
of sulfur is (%S * sample mass)
when sulfur value is entered as a
%, otherwise it is taken as the
entered value only.
e3 = (entered fuse value)(fuse
multiplier)
Correction
Equation
Set 2
e1 = (total acid)(acid multiplier) –
(amount of sulfur)(sulfur
multiplier)](Hf of HNO3)
multiplier)(Hf of H2SO4)
Amount of sulfur is
(%S * sample mass) when sulfur
value is entered as a %,
otherwise it is taken as the
entered value only.
multiplier)
Correction
Equation
Set 3
e1 = temperature rise * EE
*((HNO3/Energy)/1000)
multiplier)(Hf of H2SO4)
Amount of sulfur is (%S * sample
mass) when sulfur value is
entered as a %, otherwise it is
taken as the entered value only.
multiplier)
B-7
APPENDIX B
It is sometimes necessary to add a
spiking material to very small samples
or those that 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
solid0 samples. The 1356 Calorimeter
can automatically compensate for the
addition of spiking materials to these
samples. The calculations are
modified in these cases as follows:
Hc=
Where Hcs = Heat of combustion of
the spiking material
Ms = Mass of spiking material
This factor is added to the
calculations when Page 2.3 - Spike
Controls, Line 1 - Use Spiking is set to
ON. Line 2 - 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 Line 3 Use Fixed Spike is set to ON and
entering the mass of the spike on
Line 4 - Weight of Fixed Spike.
Spiking
Samples
WT – e1 – e2 – e3 – Hcs(Ms)
m
The calculations described above
give the calorific value of the sample
with moisture as it existed when the
sample was weighed. For example, if
an air-dried coal sample was tested,
the results will be in terms of heat
units per weight of air-dry sample.
This can be converted to a moisture
free or other basis by determining the
moisture content of the air-dry sample
and using conversion formulae
published in ASTM Method D3180 and
in other references on fuel technology.
Conversion
to Other
Moisture
Bases
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, Hnet Btu
per pound can be calculated as
follows:
Hnet=1.8Hc - 92.7H (Solid fuels,
ASTM D2015) Hnet=1.8Hc - 91.23H
(Liquid fuels, ASTM D240)
Conversion to
Net Heat of
Combustion
(Need New)
B-8
APPENDIX B
Magnitude
of Errors
The following examples illustrate
the magnitude of errors which may
result from faulty calorimeter
operations. They are based upon
an assumed test in which 1.000 gram
sample of benzoic acid produced a
2.8000 °C temperature rise in a
calorimeter having an energy
equivalent of 2400 calories per °C.
An error of 1 milliliter in making
the acid correction will change the
apparent energy detected by 1.0 cal.
An error of 1 centimeter in
measuring the amount of fuse wire
burned will change the apparent
energy detected by 2.3 cal.
An error of 1 gram in measuring
the 2 kilograms of water will change
the apparent energy detected by
2.08 cal.
An error of 1 milligram in weighing
the sample will change the apparent
energy detected by 6.7 cal.
If all of these errors were in the
same direction, the total error would
be 12.8 cal.
Precision
Statements
and the
Confidence
Factor
One of the most important factors
in a calorimeter’s performance is the
attainable precision using a standard
sample, such as benzoic acid. For
example, say that vendors X and Y
offer calorimeters. Vendor X’s
specifications state that its instrument
precision is 0.088% RSD (relative
standard deviation) and vendors Y’s
specification is 0.10%. Neither of the
data sheets for the instruments supplies a confidence level for the
specification, nor do they state
how the results are distributed.
When questioned closely, the
vendors will state that their
specifications are based on a normal
distribution and have the following
confidence levels:
In this example, the actual
precision of both instruments is
identical! Vendor X, choosing a confidence level of 95% is willing to risk 5%
of the test results being outside of the
2 sigma (95%) confidence limits.
Vendor Y, choosing a confidence level
of 99%, is only willing to risk 1% of the
test results exceeding the 3 sigma
(99%) confidence limits. Identical
instrument performance can yield
different specifications depending on
how aggressive the instrument
manufacturer chooses to be with
the specification.
Before comparing two different
instruments or test methods, it is
important to gain an understanding of
the philosophy with respect to the
confidence level. The confidence level
must be clarified when there is doubt
as to what it is. Parr Instrument
Company uses a very conservative
99% confidence level for its precision
specification as it relates to
combustion calorimeters.
Vendor
X
Y
B-9
Stated
Precision
0.088%
0.10%
Confidence
Level
95%
99%
APPENDIX B
A standard sample with a known
heat of combustion, such as benzoic
acid, can be used demonstrate that the
results produced by a calorimeter are
in statistical control. The following two
tables illustrate the upper control limit
(UCL) for the range (largest value
minus the smallest value) within an
arbitrary number of measurements.
The tables also provide this same type
of information in the form of a relative
standard deviation (RSD). Additionally,
the tables also provide the maximum
permissible deviation of the group
mean from the accepted heat of the
combustion value for benzoic acid. All
control limits are based on 99%
confidence (3 sigma) values. The
instrument precision is taken as 0.10%
RSD. This would be the expected value
if a large number (> 100) tests were
run. Most of the popular calorimeter
test methods covering isoperibol
combustion calorimetry assumes a
precision level (RSD) of 0.10%.
Calorimeter
Control Limits
when Benzoic
Acid is Used
as a Test
Sample
Table B-6 Calorimeter Control Limits
Number of
observations
in a group
UCL for the range
(high - low) within
the group (Btu/lb.)
UCL for the
relative standard
deviation within
the group (%)
Maximum
permissible
deviation of the
group mean from
the accepted value1
(Btu/lb.)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
41.9
49.6
53.4
55.9
57.8
59.2
60.4
61.3
62.2
62.9
63.6
64.2
64.8
65.3
0.261
0.228
0.209
0.196
0.187
0.181
0.175
0.171
0.167
0.164
0.161
0.159
0.156
0.154
34.1
24.1
19.7
17.1
15.3
13.9
12.9
12.1
11.4
10.8
10.3
9.8
9.5
9.1
8.8
1. Accepted value for the heat of combustion of benzoic acid taken is as 11373 Btu/lb.
B-10
APPENDIX B
Calorimeter
Control Limits
when Benzoic
Acid is Used
as a Test
Sample
Continued
Table B-7 Calorimeter Control Limits
Number of
observations
in a group
UCL for the range
(high - low) within
the group (J/g)
UCL for the
relative standard
deviation within
the group (%)
Maximum
permissible
deviation of the
group mean from
the accepted value1
(J/g)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
97.2
114.8
123.8
129.6
133.8
137.1
139.9
142.2
144.1
145.8
147.4
148.8
150.1
151.3
0.261
0.228
0.209
0.196
0.187
0.181
0.175
0.171
0.167
0.164
0.161
0.159
0.156
0.154
79.1
55.9
45.6
39.5
35.4
32.3
29.9
28.0
26.4
25.0
23.8
22.8
21.9
21.1
20.4
1. Accepted value for the heat of combustion of benzoic acid is taken as 26454 J/g.
It is prudent to run 1 standard
sample for every 20 analysis, as a
running check on the calorimeter
performance. This check procedure
does two things.
1. It provides documented records
that can be used to assure users
of the laboratory’s services that a
specified level of precision is
achieved in the routine
performance of its measurements.
2. It provides for early warning
to analysts when methods or
equipment begins to develop a
bias or show deterioration of
precision.
B-11
There are a wide variety of
scenarios for using or interpreting
the results obtained when standard
samples are analyzed. A few of these
are illustrated below.
If a single benzoic acid sample is
run as a determination, one would
expect that it would be within 79.1 J/g
or 34.1 Btu/lb. (3 sigma) of the accepted
value. If tests are run in duplicate, then
the mean value (average) of the two
results must be within 55.9 or 24.1
Btu/lb. of the accepted value.
Additionally, the range on the duplicate
tests shouldn’t exceed 97.2 J/g or 41.9
Btu/lb. If either of the first two criteria
are not met, then the calibration factor
APPENDIX B
or energy equivalent of the calorimeter
becomes suspect. If the third criteria
(range of duplicate tests) can’t be met,
then factors affecting the precision of
the instrument need to be investigated.
The tables tell us that a series of 5
tests run as calibrations should
produce an energy equivalent with a
relative standard deviation no greater
than 0.196%. A series of ten tests have
an UCL for the relative standard
deviation of 0.167%.
Both the number of tests in a
group and the UCL for the RSD
(EE Maximum Standard Deviation)
can be set on page 4 of the calorimeter
operating menus. This flexibility is
provided in order that a wide variety of
testing environments or objectives can
be easily accommodated.
B-12
STANDARDIZATION
Standardizing
the Calorimeter
Standard
Materials
C-1
APPENDIX C
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 1.25 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:
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
standardization, 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.
W=
Hm + e1 + e2 + e3
t
Where:
W = Energy equivalent of the
calorimeter in calories per degree
Celsius.
H = Heat of combustion of the
standard benzoic acid sample in
calories per gram.
m = Mass of the standard benzoic acid
sample in grams.
t = Temperature rise in °C.
e1 = Correction for heat of formation of
nitric acid in calories.
e2 = Correction for sulfur which is
usually 0.
e3 = Correction for heating wire and
combustion of cotton thread.
APPENDIX C
The 1356 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 1356 Calorimeter automatically
determines and uses up to 10 tests in
its memory and will update the EE
Value as additional standardization is
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 on Pages 4.4 through 4.7,
Line 1 - EE Value.
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 Pages 4.6.1 through
4.6.8, Line 2 - Protected EE Value.
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 Page 4.6.1
through 4.6.8, Line 6 - Print
Standardization Runs.
The user can elect to have any
number of stored standardization runs
used in determining the EE value by
entering this number on Page 4 Calibration Data & Controls, Line 4 Calibration Run Limit. Line 5 - 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 and the ASTM
limit is .15%, but the user should enter
a value appropriate for the test
being made.
Automatic
Statistical
Calculations
C-2
COMMUNICATION INTERFACES
Required
Software
Versions
D-1
APPENDIX D
he Parr Smart Link is designed to
facilitate the connection and control
of a network of equipment. Included
are: 1356 Calorimeter,1271 Calorimeter,
1281 Calorimeter, 1760 Sulfur Analyzer,
1720 or 1730 Calorimeter Controllers,
1741 Balance Interfaces and 1750
Proximate Analyzers with attached
analytical balances, 1745 Computer
Interface and/or the 1747 PC Smart Link
Board and associated computer, and
1742 Sulfur Interface for automatically
entering and storing sulfur values.
Successful installation of the Smart
Link network will depend upon all
elements of the communications
network (Smart Link) being preset,
properly configured and connected.
A step-by-step review of the Smart Link
communications network and the
configuration requirements for all
devices installed on the Link is
provided in this chapter (see Smart
Link Configuration Checklist) to ensure
that the system is properly addressed
before attempting to use it.
The Parr Smart Link is a
combination of the hardware
(circuit board, connectors and cables)
T
used to interconnect these devices and
the software (programs) required to
identify the devices on the network and
control the bi-directional transfer of
data between these devices. Inherent in
the programs which are an integral
part of the Smart Link are the protocols
for sending and receiving data,
avoiding interference when the
network is busy and ensuring the
security and validity of the data.
In addition to the intelligent
network control feature of the Smart
Link, there are two additional important
advantages offered by the
communications link when compared
with more conventional direct coupling
methods such as multiple RS232C
connectors. Since devices can be
connected in series (or daisy-chained)
there is no practical limit to the number
of devices that can be connected and
only a single connection port is
required for each device. The Smart
Link is also capable of communicating
with devices up to 1000 meters away
as opposed to the 50 foot restriction for
RS232C lines.
Before proceeding with the
installation of the 1356 Calorimeter on
the Parr Smart Link, the user must
ensure that all of his devices have the
versions of software capable of
communicating over the Smart Link
and have been configured for the
intended network (see Table D-1).
The version of software installed
in a Parr device can be determined by
performing the self-test procedure and
checking the printed or displayed
message. Users who do not have the
required software installed should
contact the Technical Service
Department at Parr Instrument
Company.
APPENDIX D
This 1356 Calorimeter is fully
equipped for operation on the Smart
Link. The 1760 Sulfur Analyzer, as well
as 1720 and 1730 Controllers must
have the optional 1722 Smart Link
board installed to communicate on the
Smart Link. The 1750 Proximate
Analyzer and the 1741, 1742, 1745 and
1747 Interfaces include all of the
required Smart Link hardware.
Required
Hardware
Each device on the Smart Link has
several parameters associated with it to
help: 1) identifies the instrument and,
2) control the flow of information to
and from instruments on the link.
Each category of device has its own
fixed identification which automatically
identifies it on the Smart Link.
Addresses of individual instruments
within a class, such as calorimeter
controllers, must be changed from the
default setting only if more than one
device in the same category is installed
on the link. The second device within
the category must have its address set
to one, and the third set to two, etc.
All devices on the Smart Link are
set, by default, to communicate at a
rate of 9600 baud. All devices on the
Smart Link must communicate at the
same transmission speed.
Smart Link
Configurations
1. Software versions verified for all
devices connected on the Smart
Link.
2. Any devices which are not the only
device within their category have
had their addresses changed to
1, 2 or higher as needed.
3. The two devices at the ends of
the Smart Link have termination
settings set to closed as viewed
from the rear of the calorimeter;
open is to the left and closed is to
the right.
4. All other devices, other than the
ones on the ends, have all
terminations set open.
5. All devices have been checked to
see that a transmission rate of 9600
baud has been set.
6. All devices on the Link have been
turned ON.
Smart Link
Configuration
Checklist
D-2
APPENDIX D
Smart Link
Configuration
Checklist
Continued
Smart Link
Configuration
Cabling
Table D-1 Software Required
Device
1356 Calorimeter
1281 Calorimeter
1271 Calorimeter
1261 Calorimeter
1720 Controller
1730 Controller
1741 Balance Interface
1745 Computer Interface
1747 PC Interface
1750 Proximate Analyzer
1760 Sulfur Analyzer
Software Version
66.0 or Higher
81.0 or Higher
71.0 or Higher
61.0 or Higher
20.4S or Higher
30.2S or Higher
41.3 or Higher
45.1S or Higher
1.0 or Higher
50.2 or Higher
60.1 or Higher
Smart Link devices, including the
1356 Controller, can be connected
using any of the cables listed in
Table D-2.
Table D-2 Smart Link Cables
Cable
A597E4
A597E
A597E2
A597E3
Cable Length
10 Feet
25 Feet
100 Feet
Custom to 1000
Feet Maximum
Smart Link cables can be linked as
extension cords. If a device is removed
from the link, the two cables should be
connected to each other to maintain
D-3
the continuity of the link. All devices
should be turned off before cables are
connected or disconnected.
APPENDIX D
The 1356 Calorimeter is also
equipped with an RS232C port for
connection to either a 40 or 80 column
printer and/or a computer (see Figure
2-8). Before making either of these
connections the data transmission rate
of the calorimeter and the printer or
computer must be matched. Generally
the baud rates on either device can be
changed to achieve this match. Printer
Port Communications for the 1356
Controller are on Page 8.2 -Printer Port
Communications, Lines 1-5.
The default parameters for the 1356
Calorimeter are set up for use with the
Parr 1755 Printer. Table D-7 identifies
and describes the pinout for the
RS232C port.
Parr offers the 1454E Connecting
Cable for connections from the
identified RS232C port to devices
located within five feet of the
calorimeter. Users may have longer
cables designed to match their devices
and installations using these
specifications. RS232C ports are not
designed for communicating over
distances greater than 50 feet.
All report transmissions to a
computer must be initiated at the
calorimeter controller.
Run area data consists of 22 fields
with commas separating each field.
Each calorimeter is furnished with
1454E Adapter for attaching 9 pin
female connector to computer with 8
pin opening. The RJ45 female and
RJ45 male connector may be obtained
from an electronic supply store.
The 1356 Calorimeter supports
input from the four balance types
indicated below. Additionally, a generic
input driver is provided for
communications with balances that do
not conform to the four supported
protocols. A new feature supported by
all five 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, 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.
RS232C
Connection
Terminal Port
Connections
Balance
Input Driver
Specifications
D-4
APPENDIX D
Mettler
011/012
Interface
Field
ID
space
data
space
g
CR
LF
Length
2
1
9
1
1
1
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.
Mettler 03 Balance Interface
Sartorious
Balance
Interface
Field
NULL
ignored
space
data
space
ignored
CR
LF
Length
1
6
1
9
1
3
1
1
Field
polarity
space
data
space
stability
CR
LF
Length
1
1
8
1
2
1
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:
D-5
[ESC] [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.
APPENDIX D
calorimeter to accept a mass. The
balance should be configured to send
its data upon receipt of the P9print
display data) command. The
calorimeter will send this command
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. The auto print feature is also
compatible with this calorimeter input
balance driver routine.
Ohaus
Balance
Interface
Generic
Interface
The data field should consist of 9
numeric characters (0 through 9, +, and space) terminated with a carriage
return (CR). Leading zeros may be
blanked as spaces and are counted.
Non-numeric characters are ignored
and will reset the input buffer if the
data field has not been filled. Any
characters received after filling the
data field and before the carriage
return are ignored.
Scope
This feature effectively adds the
appropriate functionality of the Parr
1745 Computer Interface to the
1266/1356 Calorimeters.
Communications with the host take
place via the terminal port.
All responses begin with six null characters and a STX character. This is
then followed by the data related to
the issued command. The response is
terminated with a <CR> <LF> and an
ETX character. Syntactically incorrect
commands are ignored.
Computer
Interface
Description
for the
1266/1356
Calorimeter
Supported Commands
All commands from the host start
with the letter “S” and end with a carriage return <CR>or a line feed <LF>.
SVER <CR>
This command returns the
calorimeter controller firmware
version.
Field
polarity
data
space
mode
stability
address
CR
LF
Length
1
7
1
5
1
2
1
1
The single character polarity field
should contain a space. The Data field
contains the current display mass,
right justified, with a decimal point.
The contents of the mode and address
field are ignored by the calorimeter.
The stability field must be blank for the
Field
data
CR
Length
9
1
D-6
APPENDIX D
Computer
Interface
Description
for the
1266/1356
Calorimeter
Continued
SSS20 <CR>
This command returns all of the
sample ID numbers currently stored in
the memory of the controller. Commas
delimit the ID values.
SRC[0],Sample ID <CR>
Same as above. Parenthetical text
is optional.
SR20,Sample ID <CR>
This command retrieves a
calorimeter test report for a single ID.
The report format is illustrated in Table
1. Commas delimit the field names.
Error Code
*2
Error Messages
*5
Meaning
Polled device failed
to respond
Specified sample ID
does not exist.
Table D-3 Calorimeter Test Report Field Definitions
Field
Test Information Field 1. See Table D-4
Test Information Field 2. See Table D-5
Date
Time
Calorimeter ID
Sample ID
Sample Mass
Initial Temperature
Final Temperature
Temperature Rise
Acid
Sulfur
Fuse
Energy Equivalent
Heat of Combustion
Spike Mass
Heat of Combustion
D-7
Value Type / Format
Hexadecimal (00 – FF)
Hexadecimal (00 – FF)
Integer MMDDYYYY or MMDDYY
Integer HHMMSS
Integer (0 – 15)
Integer for short form sample ID #’s.
Float for long format 8.3 type ID #s.
Float
Float
Blank field for isoperibol calorimeters
Float
Float
Float
Float
Float
Float
Float
Float
APPENDIX D
Table D-4. Test Information Field #1
Bit0
0
1
0
1
Bit1
0
0
1
1
Bit2
1
1
Standardization
Determination
Bit3
0
1
0
1
Bit4
0
0
1
1
Bit5
1
1
Equilibrium
Dynamic
Test Method
Adiabatic Reference
Adiabatic Rapid
Adiabatic Dynamic
Isoperibol
Test Type
Units
MJ/kg
BTU/lb.
cal/g
User Defined
Isoperibol Type
Bits 6 and 7 are not used.
Table D-5. Test Information Field #2
Bit
1
1
2
3
4
5
6
7
Description
1 if acid entered
1 if sulfur entered
1 if fuse entered
Not Used
1= Preliminary Report
0 = Final Report
0= Channel
1= Channel 2
1 if run area is busy
1 if run area is used
D-8
APPENDIX D
Table D-6 1356 Terminal Port
Direction
1356-Terminal
➝
➝
➝
➝
➝
➝
➝
1
2
3
4
5
6
7
8
Pin Description
Spare Output (Not Used)
Carrier Detect (DCD)
Frame Ground
Received Data
Transmitted Data
Data Set Ready (DSR)
Ready to Send (RTS)
Signal Ground
Clear to Send (CTS)**
Data Terminal Ready
➝
8 Pin
RJ-45 Pin #
➝
10 Pin
RJ-45 Pin #
1
2
3
4
5
6
7
8
9
10
➝
Computer
Interface
Description
for the
1266/1356
Calorimeter
Continued
➝
** Held at +12V(space or logic 0) while the 1356 is on.
Table D-7 1356 Balance Port
Direction
1356-Balance
➝
➝
➝
➝
➝
➝
➝
➝
➝
➝
1
2
3
4
5
6
7
8
Pin Description
Spare Output (Not Used)
Frame Ground
Transmitted Data
Received Data
Data Terminal Ready (DTR)
Signal Ground
Ready to Send (RTS)
➝
8 Pin
RJ-45 Pin #
➝
10 Pin
RJ-45 Pin #
1
2
3
4
5
6
7
8
9
10
** Held at +12V (space or logic 0) while the 1356 is on.
Table D-8 1356 Printer Port
1
2
3
4
5
6
7
8
Pin Description
Spare Output (not used)
Not Used
Frame Ground
Received Data
Transmitted Data
Signal Ground
Data Terminal Ready
** Held at +12V (space or logic 0) while the 1356 is on.
D-9
Direction
1356-Printer
➝
➝
➝
➝
➝
➝
➝
8 Pin
RJ-45 Pin #
➝
➝
➝
10 Pin
RJ-45 Pin #
1
2
3
4
5
6
7
8
9
10
➝
➝
APPENDIX E
hould you need assistance in
the operation or service of your
instrument, please contact the
Technical Service Department.
S
Telephone: (309)762-7716
Toll Free: 1-800-872-7720
Fax: (309)762-9453
When calling, please make note
of and have available the following:
1.
2.
3.
4.
5.
The serial # of the calorimeter
Date purchased.
Software Version (Page 3, Line 3).
User Setup ID (Page 3, Line 4).
Factory Default Version (Page 3,
Line 5).
6. The number and type of any Smart
Link peripherals and their software
revisions.
TECHNICAL SERVICE
It is also helpful if the person
calling is close to the 1356 Calorimeter
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 or it will be refused.
Ship repair to:
Parr Instrument Company
Attn: Service Department
211 53rd Street
Moline, Illinois 61265
E-1
1356 CALORIMETER PARTS LIST
Replacement
Parts
Item
A476A3
A391DD
393DD
531DD
549DD
558DD
581DD
A540DD
A570DD
A594DDEA
A594DDEF
A596DDEB
A596DDEE
A598DD
A599DD
421A
539DD
A297E
A719E
893E
394HCJE
697HC2
HX0012TB024
213VB
214VB
TX06SK
TX25SK
F-1
APPENDIX F
Description
Slip connector, 1/8 NPTF
Oval, bucket
Bucket support
Coupler, stirrer shaft
Gas Spring
Seal, cover
Ring, retainer
Stirrer assembly
Oxygen regulator assembly
Circuit board assembly
I/O Circuit board
Stirrer Motor 115/60
Stirrer Motor 230/50
Oxygen Solenoid assembly, 115V
Oxygen Solenoid assembly, 230V
Pressure switch assembly
Replacement tubing set
Vessel lifter
Top plate
Lead Wire
Cord set, 115V
Thermistor, 1/8 OD, 7.8” L
Cord set, 230V, CE plug
Keyboard display
O-ring
Gas filter
Tubing, oxygen
Compression nut, 1/8” OD
Ferrule set, 1/8” OD
1/16” Allen wrench
1/4” Allen wrench
APPENDIX F
Qty.
1
1
2
1
1
1
6
1
1
1
2
1
6
1
2
2
1
1
6
6
1
Part No.
A525DD
A526DD
527DD
A530DD2
A535DD3
A536DD3
536DD2
A545DD2
A546DD2
549DD
567DD
579DD
581DD
616DD
A618DD
619DD
621DD
622DD
632DD
SA1632FS08
SN3118HX
Description
Lower RH Link
Lower LH Link
Upper Link
Lift Shaft
RH Plate
LH Plate
Washer
RH Mounting
LH Mounting
Gas Spring
Spacer
Pin
Retaining Ring
Lower Trunnion
Strut Strap
Strut Strap
Upper Trunnion
Threaded Rod
Bushing Pivot
Screws
Jam Nut
Hinge
Assembly
F-2
APPENDIX F
5 Year
Recommended
Spare Parts
F-3
Qty.
1
1
1
1
1
1
1
1
1
6
6
6
1
Part No.
A591DD
A593DD
A594DD
A595DD
A596DD
A598DD
A633DD
893E
180HW
214VB
218VB
222VB
359VB
Description
Heater assembly
Pump/motor assembly
Stirrer motor assembly
Solenoid assembly, water
Solenoid assembly, oxygen
Pressure switch assembly
Pump/motor assembly
Thermistor
Solenoid, 1/8 NPTF
Ferrule set, brass; 1/8T
Filter, in-line; 1/8T
APPENDIX F
Qty.
3PKG (2)
3PKG(2)
1PKG(12)
3PKG(12)
1PKG(2)
1PKG(2)
1
3PKG(2)
1PKG(2)
1
5PKG(2)
5PKG(2)
5PKG(12)
3PKG(2)
1PKG(2)
7PKG(3)
1PKG(6)
6
1PKG(2)
1PKG(2)
1PKG(12)
1PKG(6)
1
Part No.
4A10
5A10
230A
238A
378A
388A
400A
401A
402A
403A
404A2
406A
415A
96AC
143AC
45C10
149C
263C
264C
A297E
7VBCM
20VB
3415
Description
Straight electrode w/sleeve
Loop electrode w/sleeve
O-ring, NBR, 2-3/8ID x 1/8CS
O-ring NBR, 3/16ID x 1/16CS
Packing cup
Spacer
Valve needle
Sleeve insulator
Electrode core
Check valve
Deflector nut
Lock nut, SS
O-ring 7/16 x 1/16CS, NBR
Electrode insulator
Insulator, delrin
Fuse wire, Ni alloy, 10cm
In-line filter
Printer paper, 40 column
Ribbon, replacement
Lead Wire
Monel Washer
Valve seat, Kel-F
Benzoic acid, bottle of 100
Recommended
Spare Parts
Per 5000 Tests
F-4
APPENDIX G
G-1
APPENDIX G
G-2
DRAWINGS
G-3
APPENDIX G
APPENDIX G
G-4
APPENDIX G
G-5
APPENDIX G
G-6
APPENDIX G
G-7
Parr Instrument Company
211 Fifty-Third Street
Moline, Illinois 61265 USA
309/762-7716 800/872-7720
Fax: 309/762-9453
Telex 270226
Printed in USA
03/99

1356Calorimeter Operating Instruction Manual

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