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Transcript of Bomba Cal 1266
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8/12/2019 Bomba Cal 1266
1/113
1266Isoperibol Bomb Calorimeter
No. 367MOperating Instruction Manual
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8/12/2019 Bomba Cal 1266
2/113i-i
1266 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. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1Installing the Water Cooler . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Install the Printer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
The Balance Port Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Smart Link Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-5
Fill the Water Jacket . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 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 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1Types of Controls . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-1
Keyboard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Program Installation & Control (Chapter 4) 4-1
Software Installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Default Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Revised Default Settings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-1
Fig. 4-1 Factory Default Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Operating Instructions (Chapter 5) 5-1
Operating the 1108 Oxygen Bomb. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1Operating the Filling Connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-1
Operating the Calorimeter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-2
Operating Suggestions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-4
Combustion Aids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Combustion Capsules. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-5
Coarse Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Explosives and High Energy Fuels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Volatile Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-6
Poor Combustion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
Oxygen Charging Pressure. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5-8
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TABLE OF CONTENTS
Corrections & Final Reports (Chapter 6) 6-1
Entering Corrections and Obtaining the Final Report . . . . . . . . . . . . . . . . . . 6-1
Manual Entry. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-1Fixed Corrections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Automatic Data Transfers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6-2
Reporting Instructions (Chapter 7) 7-1
Report Option Selection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
Report Destination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
Report Generation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 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
1266 Calorimeter Controller and Keyboard Display Removal . . . . . . . . . . . . 9-3
Keyboard/Display Removal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-3
Removing the Entire Controller from the Calorimeter. . . . . . . . . . . . . . . . . . 9-3
1266/1356 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 . . . . . . . . . . . . . . . . . . . . . . . . . 9-4Troubleshooting the 1266 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
Cooling Coil Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-11
Pump Replacement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-12
EE Standard Deviation Exceeds Limit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-12
Preperiod or Postperiod Time Limit Violation . . . . . . . . . . . . . . . . . . . . . . . 9-12
Jacket Over Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-13
1266 Calorimeter Error List. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-13
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1266 Calorimeter Operating Instruction Manual
TABLE OF CONTENTS
Appendix A - Menu Operating Instructions A-1
Calorimeter Operation Page 1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
Operating Controls Page 2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-2Program 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-1Thermochemical 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
Correction Equation Set 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7
Correction Equation Set 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-7
Spiking Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-8Conversion 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
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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-3
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 - 1266 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 - 1266 Drawings G-1
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Figures
Fig. 2-1 1552 Water Cooler Electrical Circuits . . . . . . . . . . . . . . . . . . . . . . . . 2-2
Fig. 2-2 1552 Water Cooler Front View. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Fig. 2-3 1552 Water Cooler Top View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Fig. 2-4 Swagelok 1. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Fig. 2-5 Swagelok 2. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Fig. 2-6 Swagelok 3. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-3
Fig. 2-7 1266 Calorimeter External Plumbing. . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Fig. 2-8 1266 Calorimeter Electrical Hookup . . . . . . . . . . . . . . . . . . . . . . . . . 2-4
Fig. 2-9 1266 Calorimeter Back View . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-6
Fig. 3-1 1266 Calorimeter Keyboard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-2
Fig. 4-1 Factory Default Settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-2
Fig. 5-7 Combustion Capsule with Adhesive Tape Seal. . . . . . . . . . . . . . . . . 5-7
Fig. 9-1 1108 Oxygen Bomb Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-1
Tables
Table 4-1 Calorimeter Status . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4-6
Table 9-2 1266 / 1356 Calorimeter Controller Fuses. . . . . . . . . . . . . . . . . . . . 9-5
Table 9-3 Power Connections - Voltage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Table 9-4 Power Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Table 9-5 Power Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9-6
Table B-1 Settings for ISO and BSI Methods. . . . . . . . . . . . . . . . . . . . . . . . . B-4
Table B-2 Entered and Reported Acid Value is Taken as Nitric Acid Only. . . B-6
Table B-3 Entered and Reported Acid Value is Considered Total Acid . . . . . B-6
Table B-4 Calculate HNO3 if Fixed and Acid is HNO3 Only . . . . . . . . . . . . . . B-6
Table B-5 Calculate HNO3 if Fixed and Acid is Total Acid . . . . . . . . . . . . . . . B-6
Table B-6 Calorimeter Control Limits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-10
Table B-7 Calorimeter Control Limits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . B-11
Table D-1 Software Required . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3
Table D-2 Smart Link Cables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-3
Table D-3 Calorimeter Test Report Field Definitions . . . . . . . . . . . . . . . . . . . D-7
Table D-4 Test Information Field #1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-8
Table D-5 Test Information Field #2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-8
Table D-6 1266 Terminal Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-9
Table D-7 1266 Balance Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-9Table D-8 1266 Printer Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D-9
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1266 Calorimeter Operating Instruction Manual
TABLE OF CONTENTS
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This manual contains instructions
for installing and operating the Parr
1266 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.
Additional instructions concerning
the installation and operation of
various component parts and
peripheral items used with the 1266
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
1266 Calorimeter Operating Instruction Manual
I
P R E F A C E
Scope
Customer Service:
Questions concerningthe installation oroperation of thisinstrument can beanswered by theParr Customer Service
Department:309-762-7716800-872-7720Fax: [email protected]
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1266 Calorimeter Operating Instruction Manual
II
These steps are offered to help
the user become familiar with, install,
operate and develop the full
capabilities of the Parr 1266
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 finalreports, 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 1266
Calorimeter. A review of the
menus will provide a good idea
of the capabilities and flexibility
designed into this instrument.
7. Review the Calculations, Appendix
B. This provides information about
calculations performed by the 1266
Calorimeter.
8. Review Standardization,
Appendix C. This will serve two
important functions. First, it
provides instructions on
generating the energy equivalent
factor required to calculate the
heat of combustion (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
1266 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.
9. Review the CommunicationInterfacing, Appendix D, for the
correct installation of any Smart
Link peripherals to the 1266
Calorimeter.
10. After successful standardization,
the 1266 Calorimeter should be
ready for testing samples.
GettingStarted
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T
he Parr 1266 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
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 1266
Calorimeter.
1266 Calorimeter Operating Instruction Manual
1-1
CONCEPT OF OPERATION 1
IsoperibolOperation
DynamicOperation
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.
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.
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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. 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.
1266 Calorimeter Operating Instruction Manual
1
FullMicro-
processorBasedProcessControl
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.
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 thermochemicalcorrections.
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
The 1266 Calorimeter is equipped
with three RS232C connections fordirect 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.
Full Micro-processorBased DataAcquisitionand Handling
FlexibleProgramming
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T
he 1266 Calorimeter is completely
assembled and given a thorough
test before it is shipped from the
factory. If the user follows these
instructions, installation of the
calorimeter should be completed
with little or no difficulty. If the factory
settings are not disturbed, only minor
adjustments will be needed to adapt
the calorimeter to operating conditions
in the users laboratory.
1266 Calorimeter Operating Instruction Manual
2-1
INSTALLATION 2
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 connections to
cooling water and oxygen
supplies, 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 air-
conditioned room. There should
be convenient access to running
water, to a drain and appropriate
grounded electrical outlet. Running
water and a drain are not
required when the unit is used in
conjunction with a Parr 1563
Water Handling System.
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.
Installingthe WaterHandlingSystem
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 waterfrom 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
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 1266 Calorimeter. Step 4
may be skipped if the water
connection has been made to
the 1563 Water Handling System.
4. Connect a cold water line to theinlet valve in the lower left hand
corner of the water jacket on the
back of the calorimeter. This is the
water connection to the cooling
coil within the jacket. It will not fill
the jacket with water. The inlet
water connection is made with
1/4 copper tubing furnished for
this purpose. Keep all water lines
as short as possible to avoid
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unwanted temperature changes.
If the supply pressure exceeds 60
psig, it will be necessary to install
a reducing valve to keep the
pressure below the 60 psig
maximum. Ideally, the product
of the cooling water flow rate
in liters per minute, and the
difference between the jacket
set point and the inlet water
temperature in degrees C should
be 3.6 degree-liters per minute.
1266 Calorimeter Operating Instruction Manual
2
5. 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 and jacket
temperatures 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 made 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 clockwisesee Fig. 2-2).
Note:
Do not plug in water cooler at this
time.
Installing theWater Cooler
Figure 2-1 1552 Water Cooler Electrical Circuits
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1266 Calorimeter Operating Instruction Manual
2-3
2
InstallationContinued
Figure 2-3 1552 Water Cooler Top View
Figure 2-4 Swagelok 1
Figure 2-5 Swagelok 2
Figure 2-6 Swagelok 3
When Swagelok Tube Fittings areused, the instructions for installationare:
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.
Figure 2-2 1552 Water Cooler Front View
Note:
12 1
2
3
4
5
67
8
9
10
11
12 12
3
4
5
67
8
9
10
11
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6. Attach a drain line to the discharge
connection of the solenoid valve
attached to the back of the
calorimeter jacket. Flexible plastic
tubing is normally used for the
cooling water outlet or drain.
A small black collar is installed in
the outlet fitting on the
calorimeter. Insert the tubing into
the connector. To remove the
tubing, press in on the black collar
and pull out on the tube.
1266 Calorimeter Operating Instruction Manual
2
Fig. 2-7 1266 Calorimeter External Plumbing
Fig 2-8 1266 Calorimeter Electrical Hookup
Caution!
DO NOT TURN ON THECALORIMETER ATTHIS TIME. THECALORIMETER MUSTBE FILLED WITHWATER BEFORETURNING ON HEATERAND PUMP. THIS WILLPREVENT IMMEDIATEHEATER BURNOUT.
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2
1266 Calorimeter Operating Instruction Manual
2-5
Caution!
THE CALORIMETERMUST BE FILLEDWITH WATER BEFORETURNING ON HEATERAND PUMP. THIS WILLPREVENT IMMEDIATEHEATER BURNOUT.
Install thePrinter
7. 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.
8. 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 1000
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 BalancePortConnection
9. 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 LinkConnection
10. 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
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.
11. Connect the printer power cable
and the printer communications
cable between the 1755 printer and
the connection at the rear of the
calorimeter.
Fill theWater Jacket
12. The water jacket of the calorimeter
must be filled manually with
approximately 9 liters of water. Tofill the jacket, raise the cover and
remove the filling plug which is
the 1/2 diameter plug located on
top of the jacket between the
bucket chamber and the right-hand
cover hinge. Add water through
this opening until the water level
is just below the top plate of the
jacket.
13. Go to the Calorimeter Main Menu
and press 1, Calorimeter
Operation. Press the down arrowkey twice and press the YES key
to activate the calorimeter water
pump and heater. As water is
circulated to the cover of the
calorimeter, the water level will
fall. Top off the jacket until it
remains within approximately 1/8
below the top plate and replace
the filling plug. To turn off the
pump, push the F1 key again.
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1266 Calorimeter Operating Instruction Manual
2
Fig. 2-9 1266 Calorimeter Back View
SolenoidValve
High Temp.Cut Out
Heater
CoolingInlet Valve Pump Motor
Oxygento Bomb
OxygenInletSolenoid
Valve Assy.
Controller
14. The 1266 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.
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
Installing theOxygen FillingSystem
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1266 Calorimeter Operating Instruction Manual
2-7
2
15. 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 thestandardization 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
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 givenbomb 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.
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
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
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.
Standardization
Installing theOxygen Filling
SystemContinued
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A
ll calorimeter configurations and
operations are handled by a menu-
driven 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
1266 Calorimeter Operating Instruction Manual
INSTRUMENT DESCRIPTION3
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.
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.)
Number Control - Page/Line
numbers can also be selected by
simply pressing the desired page/line
number on the keyboard.
Page andLine NumberSelection
Types ofControls
Types of Controls The controls that
change the data field information in
the menus will be one of the following:
1. Toggles. These data fields
contain ON/OFF or YES/NO
choices. The right and left arrowkeys are used to change the
setting to the desired choice.
Once the desired setting is
displayed, press the ENTER key
to record the change.
2. 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,
press the ENTER key to record
the change.
3. 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 dis-
played in the field, press the
ENTER key to record the value.
4. Data Displays. Most of these
data fields display values that
have been calculated by the
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calorimeter and are informational
only. Certain display values can be
overridden by the user entering a
desired value through the
keyboard.
5. 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
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.
1266 Calorimeter Operating Instruction Manual
3-2
3
Types of ControlsContinued
Keyboard Before using the 1266 Calorimeter,the operator should understand the
various keys on the keyboard (see
Figure 3-1). The brief descriptions
given here will identify these keys and
their functions. Instructions in later
chapters provide detailed operating
instructions.
7 8 9
4 5 6
1 2 3
. 0 E
ESCAPEREPORTRESETSHIFT
SKIP
HELP
PRINTSCREEN
CLEARMEM.
CLEARENTRY
NO YES
F1 F2
F3FILL
O2
ENTER
START
Fig. 3-1 1266 Calorimeter Keyboard
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Key Description
Moves the cursor UP on anyof the menu pages.
NO 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.
YES 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.
Moves the cursor DOWN onany of the menu pages.
START 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.
F1 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 This key is used to activate
the oxygen filling system
used to fill the bombs. The
reset key can be used to
abort the filling procedure.
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.
PRINTSCREEN Prints information
(except graphics) which is
currently shown on the
instrument display to the
printer.
HELP 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 keysare 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
1266 Calorimeter Operating Instruction Manual
3
KeyboardContinued
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required. It is entered before
the digits and also used to
indicate that the numbers
are being entered in
scientific notation.
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 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
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.
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.
1266 Calorimeter Operating Instruction Manual
3-4
3
KeyboardContinued
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1266 Calorimeter Operating Instruction Manual
PROGRAM INSTALLATION & CONTROL4
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.
DefaultSettings
The default parameters of the
1266 Calorimeter can be changed to
guarantee that the 1266 Calorimeter,
when cold restarted, will always be in
the desired configuration before
beginning a series of tests.
Users who wish to permanentlyrevise 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 users setup. Enternumber 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.
RevisedDefaultSettings
SoftwareInstallation
The program in the 1266
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 users work.
Note:
Changes to the program
are made by use of the menu structure
described in Appendix A of this
manual. Any of these items can be
individually entered at any time to
revise the operating program.
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1266 Calorimeter Operating Instruction Manual
4-4
4
Fig.4.1Factory DefaultSettingsContinued
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 HNO3is 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 atmos-
pheres filling pressure. If the acid is
HNO3 only flag is ON then the report-
ed acid value is e1. If this flag is OFF,
then the reported acid value is e1+e
2.
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 Keyboard
2 Spike Entry Keyboard
3 Acid Entry Keyboard
4 Sulfur Entry Keyboard
5 Hydrogen Entry Keyboard
6 Prompt for Bomb ID ON
7 Use Long Sample IDs OFF
8 AutoSampleID Controls ON
9 Auto Controls ON
0 Weight Warning above 2.0
Page 6.9
Sample ID Controls
1 Automatic Preweigh ID ON
2 Preweigh ID Increment 1.0
3 Preweigh ID Number 1.0
Page 7
Reporting Controls
1 Printer Controls
2 Report Dest Printer
3 Automatic Reporting ON
4 Individual Reports OFF
5 Report Format Text
6 Overwrite Final Reports OFF
7 Edit Final Reports OFF
8 Recalc Final Reports OFF
9 Use New EE Values OFF
Page 8
Communication Controls
1 Smart Link Controls
2 Printer Port (RS232C)
3 Balance Port (RS232C)
4 Terminal Port (RS232C)
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Page 8.1
Smart Link Controls
1 Smart Link ID (0-15) 0
2 Baud Rate 9600
3 Report Type Short Report
4 Timeout (x 0.01 s) 50
5 Smart Link Termination OFF
6 Use a 4 digit year OFF
Page 8.2
Printer Port
Communications CAL I
1 Data Bits 8
2 Parity None
3 Stop Bits 1
4 Handshaking Xon/Xoff
5 Baud Rate 9600
Page 8.3
Balance Port Communications
1 Data Bits 7
2 Parity Even
3 Stop Bits 1
4 Handshaking None
5 Baud Rate 24006 Balance type Mettler 011
7 Data Char 9
8 Log to Printer
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
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 9.2
I/O Diagnostics
1 Activate Ignition Circuit
2 Test 02 Fill Function
3 I/O Driver Diagnostic
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Parameter Description
D0 Calorimeter drift rate (10s time base)
corrected for systematic heat leaks.
Tsum The accumulated temperature rise after the sample is
ignited. This value is the temperature rise for an
Equilibrium Method test.C0 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.
T1 This value is the extrapolated portion of the temperature
rise for a Dynamic Method test.
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
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
1266 Calorimeter Operating Instruction Manual
4-6
Fig.4.1Factory Default
SettingsContinued
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%
Page 9.7
Data Logger Controls
1 Data Logger OFF
2 Interval In Seconds 10
3 Data Log Items
4 Computer Format OFF
5 Destination Printer
6 Process Log Dest Printer
7 Process Log Items
8 Print Ram Buffer
9 Clear Ram Buffer
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Alternate Report
Destination Setup
Alternate Menu 2 (Access by Shift 2)
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 and line
feed characters.
Dry Calculation Setup
Alternate Menu 3 (Access by Shift 3)
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
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1266 Calorimeter Operating Instruction Manual
5-1
OPERATING INSTRUCTIONS 5
Operatingthe FillingConnection
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.
Operating the1108 OxygenBomb
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.
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5
All operations required to
standardize the 1266 Calorimeter, or
test an unknown sample, should
proceed step-wise in the following
manner:
1. Turn on the calorimeter and
activate the pump and heater
using Line 3 of Page 1, Calorimeter
Operations. Allow at least 20
minutes for the controller to warm
up and the jacket temperature to
stabilize. Once the jacket
temperature comes within 0.5 of
35 C, the calorimeter is ready to
begin testing. The bomb parts
should be wetted and then dried in
the manner used at the conclusion
of a test. This serves to wet all
sealing parts, as well as leaving
the bomb with the same amount
of residual water which will exist
in all subsequent testing. If the
calorimeter takes longer than 20
minutes to heat up 6 C, either the
flow rate of the cooling water is
too high or the temperature of the
incoming water is too low. If the
calorimeter jacket temperature
stays higher than the set point
(normally 35 C), then the opposite
of the above conditions exist.
Keep in mind that the product
of the cooling water flow as read
in liters/min and the absolutedifference between the jacket set
point (normally 35 C) and the inlet
water temperature in C should be
between 2 and 4 liter
degrees/minute. These settings
will maintain heater duty cycles of
between 30% and 60%.
2. Prepare the sample and charge the
oxygen bomb as described in
Operating Instructions No. 205M,
the Filling Connection Section.
The throughput of the 1266
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 3 to 5 C below the
jacket temperature. It is not
necessary to use exactly 2000
grams, but the amount selected
must be duplicated within +/-0.5gram 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
Operating theCalorimeter
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Operating theCalorimeterContinued
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.
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 thermistorprobe 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 residualgas 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
1266 Calorimeter Operating Instruction Manual
5-3
5
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5
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.
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.
Note:
Particle size is important because
it influences the reaction rate.
Compression into a pellet is
recommended because the pressuredeveloped during combustion can be
reduced as much as 40% when
compared to the combustion of the
material in the powder form. In
addition in giving controlled burn
rates, the pelletizing of samples keeps
the sample in the fuel capsule during
combustion.
Materials, such as coal, burn well
in the as-received or air-dry condition,
but do not burn completely dry
samples. A certain amount of moisture
is desirable in order to control the
burning rate. Moisture content up to
20% can be tolerated in many cases,
but the optimum moisture is best
determined by trial combustion.
If moisture is to be added to
retard the combustion rate, drop waterdirectly 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.
OperatingSuggestions
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1266 Calorimeter Operating Instruction Manual
5-5
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.
CombustionAids
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 oxidefilm. 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 moisturecontent 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.
CombustionCapsules
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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.
CoarseSamples
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 trimmingthe 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 thedetermination. 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.
VolatileSamples
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
Explosives andHigh EnergyFuels
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1266 Calorimeter Operating Instruction Manual
5-7
5
VolatileSamples
Continued
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
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.
Fig 5-7 Combustion Capsule with Adhesive Tape Seal
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The 1266 Calorimeter has been
designed to operate with an oxygen
filling pressure of 30 atm. Significant
changes from this value are not
recommended.
OxygenChargingPressure
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 non-
combustible 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.
PoorCombustion
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1266 Calorimeter Operating Instruction Manual
6-1
CORRECTIONS & FINAL REPORTS 6
EnteringCorrections
and Obtainingthe FinalReport
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
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.
Manual Entry During the reporting process, thecontroller 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
press the ENTER key. The default
setting for this value is to be
entered in milliliters of standard
alkali required to titrate total acidor calories.
Sulfur Correction
Key in the Sulfur Correction and
press the ENTER key. The default
setting for this value is to be
entered as percent sulfur in the
sample.If fixed values for fuse, acid
and sulfur are turned OFF on 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 correc-
tions are not available, the opera-
tor can use the SKIP key to bypassany of the corrections, however, a
Final Report will not be printed
until an entry is made for fuse,
acid and sulfur.
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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.
FixedCorrections
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.
AutomaticData Transfers
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1266 Calorimeter Operating Instruction Manual
7-1
7
Report OptionSelection
The 1266 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 Al