Bomba Cal 1266

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1266Isoperibol Bomb Calorimeter

No. 367MOperating Instruction Manual

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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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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



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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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


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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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.


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.


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.


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.


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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2-3

2

InstallationContinued

Figure 2-3 1552 Water Cooler Top View

Figure 2-4 Swagelok 1



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.


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


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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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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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


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.


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


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.


3-4

3

KeyboardContinued

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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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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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4

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


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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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 and line

feed 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

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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


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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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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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.

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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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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5

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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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



entered in milliliters of standard

alkali required to titrate total acidor calories.

Sulfur Correction

Key in the Sulfur Correction and



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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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

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