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.

Preface
5
Explanation of Symbols
IOn Position
OOff Position
~Alternating Current
This CAUTION symbol may be present on the Product Instrumentation
and literature. If present on the product, the user must consult the
appropriate part of the accompanying product literature for more
information.
ATTENTION, Electrostatic Discharge (ESD) hazards. Observe precautions
for handling electrostatic sensitive devices.
Protective Earth (PE) terminal. Provided for connection of the protective
earth (green or green/yellow) supply system conductor.
Chassis Ground. Identifies a connection to the chassis or frame of the
equipment shall be bonded to Protective Earth at the source of supply in
accordance with national and local electrical code requirements.
Earth Ground. Functional earth connection.This connection shall be
bonded to Protective earth at the source of supply in accordance with
national and local electrical code requirements.
Safety Information
To avoid electrical shock, always:
1. Use a properly grounded electrical outlet of
correct voltage and current handling capability.
2. Ensure that the equipment is connected to
electrical service according to local national
electrical codes. Failure to properly connect
may create a fire or shock hazard.
3. For continued protection against possible
hazard, replace fuses with same type and
rating of fuse.
4. Disconnect from the power supply before
maintenance or servicing.
To avoid personal injury:
1. Do not use in the presence of flammable or
combustible materials; fire or explosion may
result.This device contains components which
may ignite such material.
2. Refer servicing to qualified personnel.
General Specifications
Electrical Ratings
120VAC, 5.0 Amps. 50/60 Hz
240VAC, 3.0 Amps. 50/60 Hz
Before connecting the calorimeter to an electrical
outlet, the user must be certain that the electrical
outlet has an earth ground connection and that the
line, load and other characteristics of the installa-
tion do not exceed the following limits:
Voltage: Fluctuations in the line voltage should not
exceed 10 % of the rated nominal voltage shown
on the data plate.
Frequency: Calorimeters can be operated from
either a 50 or 60 Hertz power supply without affect-
ing the operation or calibration.
Current:The total current drawn should not exceed
the rating shown on the data plate on the calorim-
eter by more than 10 percent.

Preface
6
Environmental Conditions
Operating: 15 ºC to 30 ºC; maximum relative
humidity of 80 % non-condensing. Installation Cat-
egory II (over voltage) in accordance with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25 ºC to 65 ºC; 10 % to 85 % relative
humidity.
Provisions for Lifting and Carrying
Before moving the instrument, disconnect all
connections from the rear of the apparatus. Lift the
instrument by grabbing underneath each corner.
Cleaning & Maintenance
Periodic cleaning may be performed on the ex-
terior surfaces of the instrument with a lightly
dampened cloth containing mild soap solution.
All power should be disconnected when cleaning
the instrument.There are no user serviceable parts
inside the product other than what is specifically
called out and discussed in this manual. Advanced
troubleshooting instructions beyond the scope of
this manual can be obtained by calling
Company in order to determine which part(s)
may be replaced or serviced.
Getting Started
These steps are offered to help the user become
familiar with, install, operate and develop the full
capabilities of the 6400 Calorimeter.
1. Review the Concept of Operations, Chapter 1,
to get an understanding of the overall capabili-
ties of the calorimeter and microprocessor
control.
2. Unpack and install the calorimeter in accor-
dance with the Installation, 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. Review the Program Installation and Control,
Chapter 3, to match the factory settings to
the intended mode of operation. Any required
changes can be made to the program param-
eters located in the Main Menu.
4. Turn the power switch ON (located on the
back). Turn to the Menu Description, Chap-
ter5, to review the touchscreen controls the
menu functions used to modify the program
contained in the 6400 Calorimeter. A review
of the menus will provide a good idea of the
capabilities and flexibility designed into this
instrument.
5. Review Standardization, Chapter 6. This
will serve two important functions. First, it
provides instructions on generating the energy
equivalent factor required to calculate the heat
of combustion of unknown samples. Secondly,
it will give the user the opportunity to run tests
on a material with a known heat of combustion
to become familiar with the instrument and
confirm that the instrument and operating
procedures are producing results with accept-
able precision. Most 6400 Calorimeters will
have an energy equivalent of approximately
940 cal/ºC.The runs for standardization and
determinations are identical, except for the
setting of the instrument to the standardization
or determination mode.
6. Review the Calculations, Chapter 7. This pro-
vides information about calculations performed
by the 6400 Calorimeter.
7. Review the Reporting Instructions, Chapter 9,
to become familiar with the manner in which
calorimetry corrections are entered. Also
discussed are generating final reports, editing
and clearing memory.
8. Review the Communication Interfacing,
Chapter 12, for the correct installation of any
peripherals connected to the 6400 Calorimeter.
9. After successful standardization, the 6400 Calo-
rimeter should be ready for testing samples.

Concept of Operation
1
8
chaPter 1
Concept of Operation
A Highly Automated Procedure
ynapmoC proudly introduces a new Oxygen Bomb
Calorimeter, No. 6400, in which new technol-
ogy is combined with time-proven calorimetric
techniques to produce a completely automatic
system for measuring the heat of combustion of
solid and liquid fuels, combustible wastes, foods,
feeds and other oxygen combustible materials.
This new approach to bomb calorimetry results in
a remarkable simplification of the steps required
for a calorimetric test without compromising the
need for complete combustion, rapid heat flow
and precise thermometry which are essential in a
combustion calorimeter.
In the 6400 Oxygen Bomb Calorimeter most of the
manual operations in conventional bomb calorim-
etry have been eliminated by a new technology
centered around a semi-automatic bucket handling
mechanism and an automatic bomb filling, vent-
ing and rinsing design.To perform a test the user
simply loads a sample into a holder, attaches a
short auxiliary fuse, places the head into the cyl-
inder, seals with a 1/16 of a turn, closes the cover
and presses the START key to begin the procedure.
New Convenience and New Technology
The 6400 Calorimeter represents a blending of
some new unique design features with some long
proven ynapmoC calorimetric technology to dramati-
cally simplify the user’s tasks during a calorimetric
determination.
In this new design the bomb cylinder and bucket
are mounted in the calorimeter.The bomb is com-
pletely surrounded by a bucket chamber, sealed
co-axially with the bomb head. After the bomb and
bucket are closed and sealed, the bomb is filled
with oxygen, the bucket chamber is filled with
water, initial equilibrium is established, the bomb
is fired and the temperature rise is monitored and
recorded - all under automatic microprocessor
control.Then, at the completion of a test, auto-
matic control releases the residual pressure in
the bomb, rinses the bomb, cools the system and
empties the bucket.
These new mechanical features support an es-
tablished technology in which water is circulated
around the bomb to bring all inner parts of the
calorimeter to a uniform temperature rapidly, while
true isoperibol operating conditions are main-
tained by an outer water jacket. Microprocessor
based, real time heat leak corrections are applied
to implement the isoperibol jacketing method
and to support the ynapmoC rapid dynamic method for
predicting the final temperature rise. Precise tem-
perature measurements are made with thermistor
thermometry providing 0.0001ºC resolution over
the operating range of the calorimeter.
In addition to handling all test sequence opera-
tions, the microprocessor makes all calculations
and reports and stores all results, as provided in
earlier ynapmoC isoperibol and adiabatic calorimeters.
A bright, backlit liquid crystal display, prompts the
operator through all setup and operating steps
with on-screen menus which make user training
quite simple.
Isoperibol Operation
In Isoperibol operation, the calorimeter jacket is
held at a constant temperature while heat from
the burning sample causes the bomb and bucket
temperature to rise.The small heat flow between
the bucket and its surroundings during a test is
monitored by a microprocessor in the calorimeter,
which continuously determines the effect of any
heat leak and applies the necessary correction
automatically.This system differs from adiabatic
operation in which the jacket temperature must be
adjusted continuously to match the bucket temper-
ature 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.

Concept of Operation
6400 1
9
Dynamic Operation
In its Dynamic Operating Mode, the calorimeter
uses a sophisticated curve matching technique to
compare the temperature rise with a known ther-
mal curve to extrapolate the final temperature rise
without actually waiting for it to develop. Repeated
testing, and over 30 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.
Full Microprocessor Based Process Control
The microprocessor controller in this calorim-
eter has been pre programmed to automatically
prompt the user for all required data and control
input and to:
• Generate all temperature readings in the
calorimeter.
• Monitor jacket as well as bucket temperature.
• Confirm equilibrium conditions.
• Fire the bomb.
• Confirm that ignition has occurred.
• Determine and apply all necessary heat leak
corrections.
• Perform all curve matching and extrapolations
required for dynamic operation.
• Terminate the test when it is complete.
• Monitor the conditions within the calorimeter
and report to the user whenever a sensor or
operating condition is out of normal ranges.
Full Microprocessor Based Data Acquisition
& Handling
In addition to its process control functions, the
microprocessor in the calorimeter has been pre-
programmed to:
• Collect and store all required test data.
• Apply all required corrections for combustion
characteristics.
• Compute and report the heat of combustion for
the sample.
Flexible Programming
The fifth generation software built into this calo-
rimeter and accessed through the screen menus
permit the user to customize the operation of the
calorimeter to meet a wide variety of operating
conditions including:
• A large selection of printing options.
• Choice of accessories and peripheral equipment.
• Multiple options in regard to handling thermo-
chemical corrections.
• Choice of ASTM or ISO correction procedures.
• A variety of memory management and reporting
procedures.
• Complete freedom for reagent concentrations and
calculations.
• Unlimited choice of reporting units.
• Automatic bomb usage monitoring and reporting.
• A choice of Equilibrium or Dynamic test methods.
• Automatic statistical treatment of calibration runs.
• Enhanced testing and trouble shooting procedure.
The 6400 Calorimeter is equipped with a USB
connection plus an Ethernet port for direct commu-
nication with attached peripherals and a computer
or network.

Installation
2
10
chaPter 2
Installation
Note: Some of the following manual sections con-
tain information in the form of warnings, cautions
and notes that require special attention. Read and
follow these instructions carefully to avoid personal
injury and damage to the instrument. Only person-
nel qualified to do so, should conduct the installa-
tion tasks described in this portion of the manual.
Environmental Conditions
The 6400 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 user’s laboratory.
This apparatus is to be used indoors. It requires at
least 0.4 m
2
(4 sq ft) of workspace on a sturdy bench
or table in a well-ventilated area with convenient
access to an electric outlet, running water and a drain.
Required Consumables, Utilities & Power
Requirements
The 6400 Calorimeter requires availability of
oxygen, 99.5 % purity, with appropriate connec-
tion, 17 MPa (2500 psig), maximum.
The 6400 Calorimeter requires availability of
nitrogen or air, oil and water free, with appropriate
connection, 17 MPa (2500 psig), maximum.
Approximately 16 L of distilled water are required
to fill the external pressurized rinse tank.
Approximately 2 L of distilled, de-ionized, or tap
water, with a total hardness of 85 mg/kg (85 ppm)
or less, are required for filling the internal cooling
reservoir.
The power requirements for the sub-assemblies of
the 6400 Calorimeter are:
Calorimeter
120 VAC, 5.0 Amps. 50/60 Hz
240 VAC, 3.0 Amps. 50/60 Hz
1759 Printer
100 to 240 VAC, 1.4 Amps 50/60 Hz
1759 Printer Supplies
334C Printer Paper
381C Printer Ribbon
Electrical Connection
Plug the power line into any grounded outlet
providing proper voltage that matches the
specification on the nameplate of the calorimeter.
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.
Turn the power switch to the ON position. After
a short time, the ynapmoC logo will appear on the LCD
display followed by a running description of the in-
strument boot sequence. When the boot sequence
is complete, the Main Menu is displayed.
Front Panel Meter
The panel meter on the front of the calorimeter
controls the temperature of the water in the in-
ternal cooling resorvoir. The setpoint is locked at
15°C. A red light will flash in the upper left corner
of the display when the water is being cooled.