parr 6400 Instruction Manual

6400 Automatic Isoperibol Calorimeter
Operating Instruction Manual

Table of Contents
1
PREFACE
Scope 4
Related Instructions 4
Purpose 4
Intended Usage 4
Explanation of Symbols 5
Safety Information 5
General Specifications 5
Environmental Conditions 6
Provisions for Lifting and Carrying 6
Cleaning & Maintenance 6
Getting Started 6
CHAPTER 1
CONCEPT OF OPERATION 8
A Highly Automated Procedure 8
New Convenience and New Technology 8
Isoperibol Operation 8
Dynamic Operation 9
Full Microprocessor Based Process Control 9
Full Microprocessor Based Data Acquisition & Handling 9
Flexible Programming 9
CHAPTER 2
INSTALLATION 10
Environmental Conditions 10
Required Consumables, Utilities & Power Requirements 10
Electrical Connection 10
Front Panel Meter 10
Swagelok Tube Fittings 11
6400 Calorimeter Installation Guide Video 11
Water Connection 13
Gas Connection 14
Combustion Vessel Exhaust Connections 14
Communication Connections 15
Printer and Balance Connections 15
CHAPTER 3
PROGRAM INSTALLATION & CONTROL 16
Programming 16
Default Settings 16
User Default Settings 16
Factory Default Settings 16
CHAPTER 4
OPERATION 18
Initial Fill 18
Quick Start 18
Sample Preparation 19
Sample Size 19
Particle Size and Moisture Content 19
Sample Types 20
Foodstuffs and Cellulosic Materials 20
Coarse Samples 20
Corrosive Samples 20
Explosives and High Energy Fuels 20
Volatile Sample Holders 20
Combustion Aids 21
Combustion Capsules 21
Test Process 22
Loading the sample 22
Closing the Oxygen Combustion Vessel 22
Fill Cycle 23
Pre-Period 24
Oxygen Combustion Vessel Firing 24
Post-Period 24
Cool/Rinse 25
Drain 26
CHAPTER 5
MENU DESCRIPTIONS 28
Menu System 28
Menu Keys 28
Control Keys 28
Calorimeter Operation 29
Temperature vs. Time Plot 29
Temperature Plot Setup 29
Operating Controls 30
Spiking Controls 30
Bomb Rinse Tank Controls 31
Program Information & Control 32
Software & Hardware Info 32
User/Factory Settings 32
Calibration Data and Controls 33
Bomb 1 34
Control Plot Chart Plot 35
Thermochemical Corrections 35
Calculation Factors 36
Net Heat/Dry Factors 37

Table of Contents
2
Data Entry Controls 38
Net Heat Data Entry Controls 38
Auto Sample ID Controls 38
Moisture Data Entry Controls 39
Preweigh Sample ID Controls 39
Reporting Controls 40
Communication Controls 40
Balance Port Communications 40
Balance Port Settings 41
File Management 42
Run Data File Manager 42
Diagnostics 43
Data Logger Controls 43
Data Log Items 43
I/O Diagnostics: 44
CHAPTER 6
STANDARDIZATIONS 46
Standardizing the Calorimeter 46
The Energy Equivalent Factor 46
Standardization Procedure 46
Standard Materials 46
Automatic Statistical Calculations 46
Calorimeter Control Limit Values in J/g 47
Calorimeter Control Limit Values in cal/g 48
Calorimeter Control Limit Values in BTU/lb 49
CHAPTER 7
CALCULATIONS 50
Calculating the Heat of Combustion 50
General Calculations 50
Temperature Rise 50
Energy Equivalent 50
Thermochemical Corrections 50
Nitric Acid Correction 50
Sulfur Correction 50
Fuse Correction 50
ASTM and ISO Methods Differ 51
Thermochemical Calculation Details 52
Acid and Sulfur Corrections 52
Sulfur Correction: 52
Acid Correction: 52
ASTM Treatment for Acid and Sulfur 54
ISO Calculations 54
Settings for ISO & BSI Methods 54
Spiking Samples 55
Conversion to Other Moisture Bases 55
Conversion to Net Heat of Combustion 55
CHAPTER 8
CORRECTIONS & FINAL REPORTS 56
Entering Corrections and Obtaining the Final Report 56
Manual Entry 56
Fixed Corrections 56
CHAPTER 9
REPORTING INSTRUCTIONS 57
Report Options 57
Report Generation 57
Net Heat of Combustion 57
CHAPTER 10
FILE MANAGEMENT 58
Clearing Memory 58
USB Flash Drive 58
CHAPTER 11
MAINTENANCE & TROUBLESHOOTING 60
Calorimeter Maintenance 60
Quarterly Maintenance 60
Fuses 60
Oxygen Combustion Vessel Maintenance 60
Inspection of Critical Sealing Surfaces 60
Oxygen Combustion Vessel Removal 61
Daily Maintenance 61
50 to 100 Test Maintenance 61
500 Test Maintenance 61
5000 Test Maintenance 62
6400 Maintenance Checklist 63
Troubleshooting 64
Vessel Exhaust Troubleshooting 64
Service the O-rings on the 966DD2 Piston 64
Confirm function of the 966DD2 piston 64
Confirm Correct Operation of the Solenoid Valve 65
Jacket Temperature Troubleshooting 65
Error List 65
Technical Service 67
Return for Repair 67
CHAPTER 5 (CONTINUED) CHAPTER 7 (CONTINUED)

Table of Contents
3
FIGURES
Figure 2-1: Swagelok Tube Fittings 11
Figure 2-2: 6400 Calorimeter Back Panel 12
Figure 2-3: 6400 External Plumbing 13
Figure 4-1: Volatile Sample Technique 21
Figure 4-2: Bucket Fill Flow Diagram 23
Figure 4-3: Pre-Period/Post-Period Flow Diagram 24
Figure 4-4: Rinse & Cool Flow Diagram 25
Figure 4-5: Drain Flow Diagram 26
Figure 12-1: 6400 Calorimeter Peripherals 69
Figure 12-2: Multiple Alternate Configurations 69
Figure 13-1a: 1138 Parts Diagram 82
Figure 13-1b: 1138 Parts Diagram Key 83
Figure 13-2: A1450DD Vessel Head Assembly, View 1 84
Figure 13-3: A1450DD Vessel Head Assembly, View 2 85
Figure 13-4: 6400 Bucket Assembly 86
Figure 13-5: 6400 Air Can Assembly, Cutaway Left 87
Figure 13-6: 6400 Air Can Assembly, Cutaway Front 88
Figure 13-7: 6400 Cutaway Right 89
Figure 13-8: 6400 Cutaway Left 90
Figure 13-9: 6400 Cover Open, View 1 91
Figure 13-10: 6400 Cover Open, View 2 92
Figure 13-11: 6400 Internal Plumbing Diagram 93
Figure 13-12: A1251DD Oxygen Solenoid Assembly 94
Figure 13-13: A1447DD Water Solenoid Assembly 95
Figure 13-14: A1456DD Rinse Valve Assembly 96
Figure 13-15: Water Tank & Jacket Cooling Solenoid 96
Figure 13-16: A1448DD Temperature Control Assembly 97
Figure 13-17: A1050DD Rinse Collection Assembly 97
Figure 13-18: A1455DD Propeller Assembly 98
Figure 13-19: A1268DD Stirrer Motor and Mount 98
Figure 13-20: Fuse Diagram 99
Figure 13-21: A1250DD3 Control Schematic 100
Figure 13-22: Power Input & Cooling Wiring 101
Figure 13-23: Ignition Wiring Diagram 102
Figure 13-24: Heater/Pump Power Wiring Diagram 102
Figure 13-25: Solenoid Harness Wiring Diagram 103
CHAPTER 12
COMMUNICATIONS INTERFACES 68
Printer Port 68
Balance Connections 68
Ethernet Interface 70
Advanced Network Options 70
Test Data Files 71
6400 Data File Naming Convention 71
6400 Calorimeter Run Data Template 71
Optional Feature Keys 79
Remote Operation 79
Bar Code Port 79
Samba Server Feature 79
CHAPTER 13
PARTS LISTS & DRAWINGS 80
Parts Lists 80
Principal Assemblies in Calorimeter 80
A1250DD2 Controller Assembly 80
A1265DD Bucket & Stirrer Tube Assembly 80
A1455DD Bucket Stirrer Assembly 81
A1266DD Cover Assembly 81
A1457DD Accessory/Installation Kit 81
Drawings 82
1138 Oxygen Combustion Vessel 82

Preface
4
Preface
Scope
This manual contains instructions for installing and
operating the 6400 Calorimeter. For ease of
use, the manual is divided into 13 chapters.
1. Concept of Operation
2. Installation
3. Program Installation & Control
4. Operation
5. Menu Description
6. Standardization
7. Calculations
8. Corrections & Final Reports
9. Reporting Instructions
10. File Management
11. Maintenance & Troubleshooting
12. Communications Interfaces
13. Parts Lists & Drawings
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 start-
ing to use the calorimeter to obtain an understanding
of the capabilities of the equipment and the safety
precautions to be observed in the operation.
Note About Nomenclature: Historically, burning
a sample enclosed in a high pressure oxygen
environment is known as Oxygen Bomb Calo-
rimetry and the vessel containing the sample is
known as an Oxygen Bomb. The terms bomb
and vessel are used interchangeably.
Related Instructions
Additional instructions concerning the installation
and operation of various component parts and
peripheral items used with the 6400 Calorimeter
should be made a part of these instructions. Ad-
ditional instructions for the optional printer are
found in the respective printer package and should
be made a part of this book.
No. Description
201M Limited Warranty
207M Analytical Methods for Oxygen Bombs
230M Safety in the Operation of Laboratory
and Pressure Vessels
483M Introduction to Bomb Calorimetry
Note: The unit of heat used in this manual is the
InternationalTable calorie, which is equal to 4.1868
absolute joules.
Purpose
Heats of combustion, as determined in an oxygen
combustion (“bomb”) calorimeter such as the 6400
Automatic Isoperibol Calorimeter, are measured
by a substitution procedure in which the heat ob-
tained from the sample is compared with the heat
obtained from a standardizing material. In this test,
a representative sample is burned in a high-pressure
oxygen atmosphere within a metal oxygen combus-
tion vessel or “bomb”. The energy released by the
combustion is absorbed within the calorimeter and
the resulting temperature change is recorded.
Intended Usage
If the instrument is used in a manner not specified
by Company, the protection pro-
vided by the equipment may be impaired.