Parr Instrument 6300 User Manual
NO. 586M
Parr Instrument Company
6300
Oxygen Bomb Calorimeter
Operating Instruction Manual
For models produced after October 2010
6300
TABLE OF CONTENTS
PREFACE — 7
Scope — 7
Explanation of Symbols — 8
Safety Information — 8
Intended Usage — 8
Cleaning & Maintenance — 8
General Specifications — 9
Environmental Conditions — 9
Getting Started — 9
CHAPTER 1
ONCEPT OF OPERATION — 11
C
A Highly Automated Procedure — 11
New Convenience and New Technology — 11
Isoperibol Operation — 11
Dynamic Operation — 11
Full Microprocessor Based Process Control — 12
Full Microprocessor Based Data Acquisition and
Handling — 12
Flexible Programming — 12
CHAPTER 2
NSTALLATION — 13
I
Required Consumables, Utilities and Power
Requirements — 13
Installing the Calorimeter — 13
6300 Calorimeter External Plumbing — 17
Combustion Aids — 35
Oxygen Charging Pressure — 35
Combustion Capsules — 35
Foodstuffs and Cellulosic Materials — 36
Coarse Samples — 36
Corrosive Samples — 36
Explosives and High Energy Fuels — 36
Volatile Sample Holders — 36
Poor Combustion — 37
CHAPTER 6
ORRECTIONS & FINAL REPORTS — 39
C
Entering Corrections and Obtaining the Final Report — 39
Manual Entry — 39
Fixed Corrections — 39
CHAPTER 7
EPORTING INSTRUCTIONS — 41
R
Report Option Section — 41
Report Generation — 41
Net Heat of Combustion — 42
CHAPTER 8
ILE MANAGEMENT — 43
F
Clearing Memory — 43
Removable SD Memory — 43
CHAPTER 3
NSTRUMENT DESCRIPTION — 21
I
Types of Controls — 21
Menu Keys — 21
Control Keys — 21
CHAPTER 4
ROGRAM INSTALLATION & CONTROL — 23
P
Software Installation — 23
Default Settings — 23
Revising Default Settings — 23
CHAPTER 5
PERATING INSTRUCTIONS — 27
O
To Begin a Test — 27
Operating the Oxygen Bomb — 27
Allowable Sample Size — 29
Attaching the Cotton Thread — 29
Closing the Bomb — 31
Fill Cycle — 31
Pre-Period — 31
Bomb Firing — 31
Post-Period — 33
Cool/Rinse — 33
Drain — 33
Samples — 35
CHAPTER 9
AINTENANCE & TROUBLESHOOTING — 45
M
Routine Maintenance — 45
6300 Maintenance Checklist — 47
Inspection of Critical Sealing Surfaces — 48
Bomb Exhaust Troubleshooting — 48
Jacket Fill and Cooling Problems — 50
Bomb Removal and Replacement — 51
6300 Calorimeter Error List — 51
APPENDIX A
ENU OPERATING INSTRUCTIONS — 53
M
Main Menu — 53
Calorimeter Operation Menu — 53
Temperature vs. Time Plot — 54
Temperature Plot Setup Menu — 54
Operating Controls Menu — 55
Program Information and Control Menu — 57
Calibration and Data Controls Menu — 58
Thermochemical Calculations Menu — 60
Calculation Factors Menu — 62
Net Heat/Dry Heat Factors — 63
Data Entry Controls Menu — 63
Reporting Controls Menu — 65
Communication Controls Menu — 66
File Management — 67
Run Data File Manager — 68
Diagnostics Menu — 68
www.parrinst.com
3
TABLE OF CONTENTS
APPENDIX B
ALCULATIONS — 71
C
Calculating the Heat of Combustion — 71
General Calculations — 71
Thermochemical Corrections — 71
Fuse Correction — 73
Acid and Sulfur Corrections — 73
ASTM Treatment for Acid and Sulfur — 74
ISO Calculations — 75
Spiking Samples — 75
Conversion to Net Heat of Combustion — 75
APPENDIX C
TANDARDIZATION — 77
S
Standardizing the Calorimeter — 77
Standard Materials — 77
Automatic Statistical Calculations — 77
APPENDIX D
OMMUNICATIONS INTERFACES — 81
C
USB Port — 81
Balance and Port Input Driver Specifications — 81
Mettler 011/012 Balance Interface — 81
Sartorius Balance Interface — 81
Generic Interface — 82
Ethernet Interface — 83
Samba Server Feature (Optional) — 84
Bar Code Port — 92
Network Data Services — 92
APPENDIX E
ECHNICAL SERVICE — 93
T
Return for Repair — 93
APPENDIX F
ARTS LISTS & DRAWINGS — 95
P
Principal Assemblies in Calorimeter — 95
A1250DD2 Controller Assembly — 96
A1251DD Oxygen Solenoid Assembly — 96
A1252DD Water Solenoid Assembly — 96
A1257DD Water Regulator Assembly — 97
A1258DD Temperature Control Assembly — 97
A1260DD Water Level Assembly — 97
A1264DD Air Can Assembly — 98
A1267DD Accessory/Installation Kit — 99
A1265DD Bucket and Stirrer Tube Assembly — 99
6300 Stirrer Motor and Drive — 100
A1255DD Bucket Stirrer Assembly — 100
A1266DD Cover Assembly — 100
6309B Spare Parts Kit — 101
1136 and 1136CL Oxygen Bomb — 103
1138 and 1138CL Oxygen Bomb — 105
APPENDIX G
OMB RINSE CONTAINER ASSEMBLY — 127
B
Overview — 127
Concept of Operation — 127
Connection — 127
Operation — 127
TABLES
Table B-1
Settings for ISO & BSI Methods — 74
Table C-1
Calorimeter Control Limit Values in J/g When
Benzoic Acid is Used as a Test Sample — 78
Table C-2
Calorimeter Control Limit Values in cal/g When
Benzoic Acid is Used as a Test Sample — 79
Table C-3
Calorimeter Control Limit Values in BTU/lb When
Benzoic Acid is Used as a Test Sample — 80
Table D-1
6300 Data File Naming Convention — 82
Table D-2
6300 Calorimeter Run Data Template — 82
FIGURES
Figure 2-1
Swagelok Tube Fittings — 15
Figure 2-2
6300 Calorimeter Back Panel — 16
Figure 2-3
Closed Loop Configuration with 6520A — 17
Figure 2-4
Closed Loop Configuration with 1564 — 17
Figure 2-5
Open Loop Configuration with 1552 — 18
Figure 2-6
Open Loop Configuration — 18
Figure 4-1
6300 Factory Default Settings — 24
Figure 5-1
Fill Flow Diagram — 28
Figure 5-2
Cotton Thread Assembly — 29
Figure 5-3
Pre-period/Post-period — 30
Figure 5-4
Rinse & Cool Flow Diagram — 32
Figure 5-5
Drain Flow Diagram — 34
Figure 5-6
Combustion Capsule with Adhesive Tape Seal — 37
Figure F-1
Parts Diagram for the 1136 and 1136CL Oxygen
Bombs — 102
4
Parr Instrument Company
6300
FIGURES (CONTINUED)
Figure F-2
Parts Diagram for the 1138 and 1138CL Oxygen
Bombs — 104
Figure F-3
6300 Oxygen Bomb Calorimeter Cutaway Right —
106
Figure F-4
6300 Oxygen Bomb Calorimeter Cutaway Left —
107
Figure F-5
6300 Oxygen Bomb Calorimeter Cover Open — 108
Figure F-6
A1250DD2 Control Schematic — 109
Figure F-7
A1251DD Oxygen Solenoid Assembly — 110
Figure F-8
A1200DD Internal Plumbing Diagram — 111
Figure F-9
A1252DD Water Solenoid Assembly — 112
Figure F-10
A1416DD Bomb Wash Pump Assembly and Fittings
— 113
Figure F-11
A1254DD Circulatory Pump Assembly — 114
Figure F-12
A1255DD Bucket Stirrer Assembly — 115
Figure F-13
A1256DD Water Assembly Tank — 116
Figure F-14
A1257DD Water Regulator Assembly — 117
Figure F-15
A1258DD Temperature Control Assembly — 118
Figure F-16
Cover Contact Pin Assembly — 119
Figure F-17
Stirrer Motor and Mount — 120
Figure F-18
A1260DD Water Level Control Assembly — 121
Figure F-19
A1265DD Bucket Assembly — 122
Figure F-20
6300 Air Can Assembly — 123
Figure F-21
A1450DD Bomb Head Assembly (1) — 124
Figure F-22
A1450DD Bomb Head Assembly (2) — 125
Figure G-1
Vessel Rinse Container — 128
TABLE OF CONTENTS
www.parrinst.com
5
TABLE OF CONTENTS
This page left blank intentionally.
6
Parr Instrument Company
6300
PREFACE
PREFACE
SCOPE
This manual contains instructions for installing and
operating the Parr 6300 Calorimeter. For ease of use,
the manual is divided into nine chapters.
Concept of Operation
Installation
Instrument Description
Program Installation & Control
Operating Instructions
Corrections & Final Reports Reporting
Instructions
File Management
Maintenance & Troubleshooting
Subsections of these chapters are identified in the Table
of Contents.
No. Description
201M
207M
230M
483M
Additional instructions for the printer, cooler, and water
handling systems are found in the respective package
and should be made a part of this book.
Note:
The unit of heat used in this manual is the International
Table (IT) calorie, which is equal to 4.1868 absolute
joules.
Limited Warranty
Analytical Methods for Oxygen Bombs
Safety in the Operation of Laboratory and
Pressure Vessels
Introduction to Bomb Calorimetry
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 6300 Calorimeter have been
included and made a part of these instructions.
Customer Service:
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
1-309-762-7716 • 1-800-872-7720 • Fax: 1-309-762-9453
E-mail: parr@parrinst.com • http://www.parrinst.com
www.parrinst.com
7
PREFACE
EXPLANATION OF SYMBOLS
I On Position
O Off Position
~ Alternating Current (AC)
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:
Use a properly grounded electrical outlet of correct 1.
voltage and current handling capability.
Ensure that the equipment is connected to electrical 2.
service according to local national electrical codes.
Failure to properly connect may create a fire or
shock hazard.
For continued protection against possible hazard, 3.
replace fuses with same type and rating of fuse.
Disconnect from the power supply before 4.
maintenance or servicing.
To avoid personal injury:
Do not use in the presence of flammable or 1.
combustible materials; fire or explosion may result.
This device contains components which may ignite
such material.
Refer servicing to qualified personnel.2.
INTENDED USAGE
If the instrument is used in a manner not specified by
Parr Instrument Company, the protection provided by
the equipment may be impaired.
CLEANING & MAINTENANCE
Periodic cleaning may be performed on the exterior
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 Parr Instrument Company in order to determine
which part(s) may be replaced or serviced.
8
Parr Instrument Company
6300
PREFACE
GENERAL SPECIFICATIONS
Electrical Ratings
120VAC, 6.0 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 installation 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 affecting their
operation or calibration.
Current: The total current drawn should not exceed the
rating shown on the data plate on the calorimeter by
more than 10 percent.
ENVIRONMENTAL CONDITIONS
Operating: 15ºC to 30ºC; maximum relative
humidity of 80% non-condensing. Installation Category
II (over voltage) in accordance with IEC 664.
Pollution degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25ºC and 65ºC; 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.
GETTING STARTED
These steps are offered to help the user become familiar
with, install, operate and develop the full capabilities of
the Parr 6300 Calorimeter.
parts of the calorimeter and make it easier to
understand the operating instructions which follow.
Turn the power switch ON (located on the back). 3.
Turn to the Instrument Description, Chapter 3, to
review the touch screen controls.
Review the 4. 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.
Review the 5. Reporting Instructions, Chapter 7,
to become familiar with the manner in which
calorimetry corrections are entered. Also discussed
are generating final reports, editing and clearing
memory.
Turn to the 6. Menu Operating Instructions, Appendix
A, to review the menu functions used to modify
the program contained in the 6300 Calorimeter. A
review of the menus will provide a good idea of
the capabilities and flexibility designed into this
instrument.
Review the 7. Calculations, Appendix B. This provides
information about calculations performed by the
6300 Calorimeter.
Review 8. 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
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 6300 Calorimeters will
have an energy equivalent of approximately 940
calories per ºC with an 1138 oxygen bomb (800
calories per ºC with an 1136 oxygen bomb.) The
runs for standardization and determinations are
identical, except for the setting of the instrument to
the standardization or determination mode.
Review the 1. Concept of Operations, Chapter 1, to get
an understanding of the overall capabilities of the
calorimeter and microprocessor control.
Unpack and install the calorimeter in accordance 2.
with Installation, Chapter 2. This simple, step-wise
procedure will acquaint the user with the various
Review the 9. Communication Interfacing, Appendix
D, for the correct installation of any peripherals
connected to the 6300 Calorimeter.
After successful standardization, the 6300 10.
Calorimeter should be ready for testing samples.
www.parrinst.com
9
PREFACE
This page left blank intentionally.
10
Parr Instrument Company
6300
CHAPTER 1
CONCEPT OF OPERATION
A HIGHLY AUTOMATED PROCEDURE
Parr proudly introduces a new Oxygen Bomb
Calorimeter, No. 6300, in which new technology 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.
CONCEPT OF OPERATION
These new mechanical features support an established
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 maintained by an outer water
jacket. Microprocessor based, real time heat leak
corrections are applied to implement the isoperibol
jacketing method and to support the Parr rapid dynamic
method for predicting the final temperature rise. Precise
temperature measurements are made with thermistor
thermometry providing 0.0001ºC resolution over the
operating range of the calorimeter.
In addition to handling all test sequence operations, the
microprocessor makes all calculations and reports and
stores all results, as provided in earlier Parr 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.
1
In the 6300 Oxygen Bomb Calorimeter most of the
manual operations in conventional bomb calorimetry
have been eliminated by a new technology centered
around a semi-automatic bucket handling mechanism
and an automatic bomb filling, venting 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 cylinder, 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 6300 Calorimeter represents a blending of some
new unique design features with some long proven Parr
calorimetric technology to dramatically 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 completely
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, automatic control releases the residual pressure
in the bomb, rinses the bomb, cools the system and
empties the bucket.
ISOPERIBOL OPERATION
In Isoperibol operation, the calorimeter jacket is held
at a constant temperature while heat from the burning
sample causes the bomb and bucket temperature to
rise. The small heat flow between the bucket and
its surroundings during a test is monitored by a
microprocessor in the calorimeter, which continuously
determines the effect of any heat leak and applies
the necessary correction automatically. This system
differs from adiabatic operation in which the jacket
temperature must be adjusted continuously to match
the bucket temperature in an attempt to maintain a zero
temperature differential with no heat leaks between the
bucket and its surroundings. Calorimetrists have long
recognized the advantages of simplification and better
precision obtainable with a well designed and executed
Isoperibol system as opposed to the rapidly changing
jacket temperature required in an adiabatic calorimeter.
DYNAMIC OPERATION
In its Dynamic Operating Mode, the calorimeter
uses a sophisticated curve matching technique to
compare the temperature rise with a known thermal
curve to extrapolate the final temperature rise without
actually waiting for it to develop. Repeated testing,
and over 20 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.
www.parrinst.com
11
1
CONCEPT OF OPERATION
FULL MICROPROCESSOR BASED PROCESS
C
ONTROL
The microprocessor controller in this calorimeter has
been pre programmed to automatically prompt the user
for all required data and control input and to:
•
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.•
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 AND HANDLING
In addition to its process control functions, the
microprocessor in the calorimeter has been pre
programmed to:
The 6300 Calorimeter is equipped with a USB
connection plus an Ethernet port for direct
communication with attached peripherals and a
computer or network.
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 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 large selection of printing options.
•
Choice of accessories and peripheral equipment.•
Multiple options in regard to handling •
thermochemical corrections.
Choice of ASTM or ISO correction procedures.
•
A variety of memory management and reporting •
procedures.
12
Parr Instrument Company
6300
INSTALLATION
2
CHAPTER 2
INSTALLATION
REQUIRED CONSUMABLES, UTILITIES AND
P
OWER REQUIREMENTS
The 6300 Calorimeter System requires availability of
Oxygen, 99.5% purity, with appropriate connection,
2500 psig, maximum.
This apparatus is to be used indoors. It requires at least
4 square feet 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. The supply
voltage must be within ± 10% of marked nominal
voltage on the apparatus. The supply voltage receptacle
must have an earth ground connection.
Approximately 4 liters of tap water, with a total
hardness of 85 ppm or less, are required for filling the
calorimeter jacket reservoir. This water is provided via
the tap water connection at the rear of the calorimeter.
The inlet pressure should be in the range of 20 to 60
psig. The required flow rate is on the order of 0.5 liters/
minute. This connection also supplies cooling water
for the calorimeter. As a result, the temperature of the
water should not exceed 25 °C. The speed at which
the calorimeter will recycle between tests is a function
of the temperature of the incoming tap water. (The
performance will slow noticeably above 20 °C and will
become sluggish above 25 °C). Water consumption
is dependent on the incoming water temperature and
shouldn’t normally exceed 1.5 liters per test.
An open water drain connection is required.
INSTALLING THE CALORIMETER
Each Parr 6300 Calorimeter was completely assembled
and thoroughly tested prior to shipment. The following
stepwise procedure will guide the user through the
installation process.
Unpack the calorimeter and carefully check the
•
individual parts against the packing list. If shipping
damage is discovered, save the packing cartons
and report it immediately to the delivering carrier.
The calorimeter needs to be located near a water
drain. A cold-water tap water supply, oxygen
and an electrical outlet are also required. Set the
calorimeter on a sturdy, level, bench or table, free
from drafts, vibration and sources of radiant heat.
Make the calorimeter drain connection using the
•
provided 7/8” Tygon tubing (assembly A1336DD).
The calorimeter must be located so that the drain
tubing is always lower than the drain port at the rear
of the calorimeter. Failure to meet this requirement
will cause water to back up inside the calorimeter.
Make the tap water connection at the rear
•
of the calorimeter using 1/4” Nylon tubing
(HJ0025TB035). The inlet pressure should not
exceed 60 psig. Refer to figure 2-1 and 2-2. The inlet
connection incorporates a water filter, 1245DD,
just behind the inlet connection. When making
the water connection, a back-up wrench should
be placed on the water filter to insure a secure
connection and to prevent over tightening the filter.
NOTE:
During extended periods of inactivity (overnight or longer), shut off the tap water supply
to the calorimeter.
The power requirements for the subassemblies of the
6300 Calorimeter are:
Calorimeter
•
5A @ 120VAC
3A @ 230VAC
Printer
•
(100 to 240 VAC, 50/60 Hz) 0.35 A
Printer Supplies•
334C Printer Paper
335C Printer Ribbon
Make the connection to the rinse water source using
•
3/8” Tygon tubing (JT0038TB062A). A barbed
fitting is provided at the rear of the calorimeter
for this connection. A 10 liter carboy (231C2) is
provided as a distilled water rinse reservoir. Place a
149C in-line water filter at the end of the water line
that is inserted into the carboy.
www.parrinst.com
13
2
INSTALLATION
INSTALLING THE CALORIMETER (CONTINUED)
Make the connections to the oxygen supply at •
this time. Refer to figure 2-2 and 2-3. 1/8” O.D.
nylon pressure hose (HX0012TB024) is used to
connect the oxygen supply. The inlet connection
incorporates a flow restrictor just behind the inlet
connection. When making the oxygen connection,
a back-up wrench should be placed on the restrictor
to insure a secure connection and to prevent over
tightening the flow restrictor. The delivery pressure
for oxygen should be set at 450 psig. To install the
regulator, unscrew the protecting cap from the 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 tank outlet and
draw up the union nut tightly, keeping the gages
tilted slightly back from an upright position. Open
the tank valve and check for leaks. The bomb must
never be filled to more than 600 psig (40 atm).
Note:
The cause of any leaks must be corrected before
proceeding.
printer and the connections at the rear of the
calorimeter. Install the printer ribbon and printer
paper at this time. Apply power to the calorimeter
and turn on the printer.
SWAGELOK TUBE FITTINGS
When Swagelok Tube Fittings are used, the instructions
for installation are:
Simply insert the tubing into the Swagelok Tube 1.
Note:
During extended periods of inactivity (overnight or
longer), close the tank valve to prevent depleting the tank
in the event of a leak. When changing tanks, close the
tank valve prior to re-moving the regulator. Do not use oil
or combustible lubricants in connection with any part of
the oxygen filling system. Keep all threads, fittings and
gaskets clean and in good condition.
The exhaust and vent connections at the rear of the
•
calorimeter, are made with the dual tube A1006DD
assembly. The end of the assembly with the bomb
exhaust diffuser should be placed into the 10 liter
carboy (231C2). The carboy should be placed at
or below the level of the calorimeter to facilitate
complete draining of these lines.
Note:
This step is optional for use with A1050DD. See Appendix
G for A1050DD Bomb Rinse Container Installation and
Use.
Connect the printer USB cable between the 1758
•
14
Parr Instrument Company
6300
Fitting. Make sure that the tubing rests firmly on
the shoulder of the fitting and that the nut is fingertight.
Before tightening the Swagelok nut, scribe the nut at 2.
the 6 o’clock position.
While holding the fitting body steady with a back-3.
up wrench, tighten the nut 1-1/4 turns. Watch the
scribe mark, make one complete revolution and
continue to the 9 o’clock position.
For 3/16” and 4mm or smaller tube fittings, tighten 4.
the Swagelok nut 3/4 turns from finger-tight.
Figure 2-1
Swagelok Tube Fittings
INSTALLATION
Insert the tubing with pre-swaged ferrules into the 1.
fitting body until the front ferrule seats.
Tighten the nut by hand. Rotate the nut to the 2.
original position with a wrench. An increase
in resistance will be encountered at the original
position. Then tighten slightly with a wrench.
Smaller tube sizes (up to 3/16” or 4mm) take less
tightening to reach the original position than larger
tube sizes.
The type of tubing and the wall thickness also has an
effect on the amount of tightening required. Plastic
tubing requires a minimal amount of additional
tightening while heavy wall metal tubing may require
somewhat more tightening. In general, the nut only
needs to be tightened about 1/8 turn beyond finger tight
where the ferrule seats in order to obtain a tight seal.
2
Over tightening the nut should be avoided. Over
tightening the nut causes distortion (flaring) of the lip
of the tube fitting where the ferrule seats. This in turn
causes the threaded portion of the body to deform. It
becomes difficult to tighten the nut by hand during a
subsequent re-tightening when the fitting body becomes
distorted in this manner.
RETIGHTENING SWAGELOK TUBE FITTINGS
Swagelok tubing connections can be disconnected
and retightened many times. The same reliable leakproof seal can be obtained every time the connection is
remade using the simple two-step procedure.
www.parrinst.com
15
2
INSTALLATION
Figure 2-2
6300 Calorimeter Back Panel
16
Parr Instrument Company
6300
6300 CALORIMETER EXTERNAL PLUMBING
Figure 2-3
Closed Loop Confi guration with 6520A
O2 Regulator
DI Water
~Room Temp
5-10 °C
INSTALLATION
2
6520A
Water Recircualtion
System
Figure 2-4
Closed Loop Confi guration with 1564
O2 Regulator
DI Water
~Room Temp
5-10 °C
Rinse Collection
1552
Water
Cooler
Line 1 & 2 – Maximum length of 10 feet, 1/4” OD, Polyurethane (Part Number HJ0025TB035)
Line 3 - Maximum length of 25 feet, 1/8” OD, Nylon (Part Number HX0012TB024)
1564
Water
Recircualtion
System
Rinse Collection
www.parrinst.com
17
2
INSTALLATION
6300 CALORIMETER EXTERNAL PLUMBING (CONTINUED)
Figure 2-5
Open Loop Confi guration with 1552
O2 Regulator
Tap Water
· <25 °C
· <85 ppm
· <60 psig
1552
Water
Cooler
DI Water
~Room Temp
Drain
Figure 2-6
Open Loop Confi guration
O2 Regulator
Tap Water
· <25 °C
· <85 ppm
· <60 psig
5-10 °C
Rinse Collection
DI Water
~Room Temp
Rinse Collection
Drain
Line 1 & 2 – Maximum length of 10 feet, 1/4” OD, Polyurethane (Part Number HJ0025TB035)
Line 3 - Maximum length of 25 feet, 1/8” OD, Nylon (Part Number HX0012TB024)
18
Parr Instrument Company
6300
INSTALLATION
2
INSTALLING THE CALORIMETER (CONTINUED)
After the calorimeter displays the main menu, press •
the Calorimeter Operation button. This screen
should indicate that the jacket is filling with water.
The initial fill can take as long as 8 to 10 minutes
to complete. If the jacket filling process times out,
simply acknowledge the timeout message to resume
the jacket filling process. After the jacket is filled
press the Heater and Pump button in order to toggle
the heater and pump on.
Wait for the calorimeter jacket temperature to
•
stabilize within a half a degree of 30 °C. (When
the pump and heater are turned on after being off
for an extended period of time, it may take longer
than 10 minutes for the calorimeter warm up. This
may cause an error. Simply restart the heater and
pump.) While waiting for the jacket temperature to
stabilize, raise the calorimeter lid and remove the
bomb head by twisting 1/16 turn counterclockwise
and pulling straight up. Examine the bomb release
pin at the bottom of the combustion cylinder. If it
has become dislodged during shipping, position it
correctly using the long forceps supplied in the calorimeter accessory kit. Refer to figure F-19.
Lock the head in the bomb cylinder (see section
•
5-7), close the lid and while applying a slight
downward pressure. Press the CALORIMETER
OPERATION key on the main menu followed by
the Pretesting Cycle button to initiate a pre-test
cycle. (This button will not be available until the
jacket temperature has been stable for 15 minutes.)
During the initial portion of this cycle, check to
see that the oxygen supply pressure is set to 450
psig. Adjust as required. The calorimeter should
complete the pre-test cycle with no errors.
ENTER to store the default sample mass of 1 gram.
This test should go through Fill, Pre-period, Postperiod and Cool/Rinse Cycles without error. The
calorimeter is now ready to be standardized.
•
The calorimeter must be accurately standardized
prior to actually performing calorimetric tests on
sample materials. Review Appendix C – Standardization, in order to become familiar with the general
procedure and calculations. The user should configure the calorimeter at this time to accommodate the
desired sample weight entry mode. The calorimeter
can be placed into the standardization mode on
the Calorimeter Operation Page, by pressing the
Operating Mode button. If two bomb heads 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 by pressing the Bomb Installed/
EE key. Both bomb heads 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 calorimeter one degree.
Repeated standardization with any given bomb
head should yield an energy equivalent value with
a range of up to 4 calories per degree, centered on
the mean value for all tests using that bomb head.
The calorimeter is ready for testing samples after a
suitably constant energy equivalent value has been
obtained.
Assemble the bomb head stand (A38A), located in
•
the accessory kit. Remove the head from the calorimeter and place it on the stand. Place a 1 gram
pellet of benzoic acid in a combustion capsule
and place this unweighed sample on the capsule
holder of the bomb head. Attach 10 cm of fuse
thread as shown in figure 5-3. Install the bomb
head in the calorimeter and close the cover. Apply
a slight downward pressure on the cover and press
the START key to begin the test sequence. Press
the ENTER key to accept the displayed sample ID
number. At the sample weight prompt press 1 then
www.parrinst.com
19
2
INSTALLATION
This page intentionally left blank.
20
Parr Instrument Company
6300
CHAPTER 3
INSTRUMENT DESCRIPTION
TYPES OF CONTROLS
All calorimeter configurations and operations are
handled by a menu-driven system operated from the
bright touch screen display. The settings and controls
are organized into nine main sections or pages which
comprise the MAIN MENU.
Note:
Keys with a double box in the upper left hand corner lead
to sub-menus.
INSTRUMENT DESCRIPTION
Some keys lead to multiple choices. Always clear
the current value before entering a new value. Once
entered the screen will revert to the previous menu
and the new value will be displayed in the lower
right corner of the key.
Data Displays.4. Most of these keys display values
that have been calculated by the calorimeter and are
informational only. Certain ones can be overridden
by the user entering a desired value through a submenu. The value is displayed in the lower right
corner of the key.
Note:
Some keys will respond with an opportunity for the user
to confirm the specified action to minimize accidental
disruptions to the program and/or stored data.
CONTROL KEYS
3
MENU KEYS
The controls that change the data field information in
the menus will be one of the following:
Toggles.1. These data fields contain ON/OFF or
YES/NO choices. Simply touching the key on the
screen toggles the choice to the other option. The
current setting is displayed in the lower right corner
of the key.
Option Selection.2. These data fields contain a list
of options. Touching the key on the screen steps
the user through the available choices. The current
setting is displayed in the lower right corner of the
key.
Value Entry Fields.3. These data fields are used to
enter data into the calorimeter. Touching the key
on the screen brings up a sub menu with a key pad
or similar screen for entering the required value.
There are five control keys which always appear in the
right column of the primary displays. These keys are
unavailable when they are gray instead of white.
Escape.1. This key is used to go up one level in the
menu structure.
Main Menu. 2. This key is used to return to the main
menu touch screen from anywhere in the menu
structure.
Start.3. This key is used to start a calorimeter test.
Report.4. This key is used to access the test results
stored in the calorimeter, to enter thermochemical
corrections and to initiate report on the display,
printer or attached computer
Help. 5. This key is used to access help screens related
to the menu currently displayed on the touch screen.
Abort.6. This key appears in the Start key location
while a test or pretest is running. Pressing this key
will abort the test or pretest in progress.
7. This key appears in the Escape key location
when the main menu is displayed. This key is used
to shut down the calorimeter program before turn-
ing off the power.
www.parrinst.com
21
3
INSTRUMENT DESCRIPTION
This page left blank intentionally.
22
Parr Instrument Company
6300
PROGRAM INSTALLATION & CONTROL
4
CHAPTER 4
PROGRAM INSTALLATION &
CONTROL
SOFTWARE INSTALLATION
The program in the 6300 Calorimeter can be extensively
modified to tailor the unit to a wide variety of operating
conditions, reporting units, laboratory techniques,
available accessories and communication modes.
In addition, the calculations, thermochemical
corrections and reporting modes can be modified to
conform to a number of standard test methods and
procedures.
Numerous provisions are included to permit the use of
other reagent concentrations, techniques, combustion
aids and short cuts appropriate for the user’s work.
REVISING DEFAULT SETTINGS
The default parameters of the 6300 Calorimeter can
be changed to guarantee that the 6300 Calorimeter,
when cold restarted, will always be in the desired
configuration before beginning a series of tests.
Users who wish to permanently revise their default
settings may do so using the following procedure:
Establish the operating parameters to be stored as
•
the user default settings.
Go to the Program Info and Control Menu, User/
•
Factory Settings, User Setup ID, and enter the
desired User Setup ID.
Select Save User Default Settings
•
To re-load the user default settings, go to the Program
Info and Control Page, User/Factory Settings, Re-load
User Default Settings, and YES.
Note:
Changes to the program are made by use of the menu
structure described in Appendix A of this manual. Any
of these items can be individually entered at any time to
revise the operating program.
DEFAULT SETTINGS
Units are pre programmed with DEFAULT
SETTINGS. See pages 24 and 25 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 the Program Information
and Control Menu, then to User/Factory Settings, and
then touch Reload Factory Default Settings and YES.
Non-volatile 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.
www.parrinst.com
23
4
PROGRAM INSTALLATION & CONTROL
Figure 4-1
6300 Factory Default Settings
Calorimeter Operations
Operating Mode Determination
Bomb Installed/EE 1/940.0
Heater and Pump OFF
Operating Controls
Method of Operation Dynamic
Reporting Units BTU/lb
Use Spiking Correction OFF
“OTHER” Multiplier 4.1868
Calibrate Touchscreen
LCD Backlight Timeout(s) 1200 S
LCD Backlight Intensity 70%
Print Error Messages ON
Language English
Spike Controls
Use Spiking OFF
Heat of Combustion of Spike 6318.4
Use Fixed Spike OFF
Weight of Fixed Spike 0.0
Prompt for Spike before Weight OFF
User Function Setup
Cold Restart
User/Factory Settings
User Setup ID 63-1138
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Compare settings with Factory Defaults
Calibration Data & Controls
Calibration Run Limit 10
EE Max Std Deviation 0.0
Heat of Combustion of Standard 6318.4
Bomb Service Interval 500
Use Bomb 1
Control Chart Parameters
Charted Value HOC Standard
Process Sigma 0.1
Temp Rise High Warning 8.5
Temp Rise Low Warning 5.1
Bomb Rinse Tank Control
Report Rinse Tank Empty ON
Rinse Tank Capacity 150
# Rinses Left 150
Reset Rinse Tank Counter
Rinse Time 25
Rinse Flush Time 20
Clear Time 100
# of Rinse Cycles 3
Program Information and Control
Date & Time Settings
Volume Level Adjust 85%
Software and Hardware Info
Settings Protect OFF
User/Factory Settings
Feature Key
Bomb Type Select
Bomb 1 Through 4
EE Value 800.0
Protected EE Value OFF
Thermochemical Corrections Standardization
Fixed Fuse ON 50.0
Acid Correction Fixed HNO
Fixed Sulfur ON 0.0
Determination
Fixed Fuse ON 50.0
Acid Correction Fixed HNO
Fixed Sulfur OFF 0.0
Net Heat/Dry Factors
Calculation Factors
Nitric Acid Factor 1.58
8.0
3
8.0
3
24
Parr Instrument Company
6300
PROGRAM INSTALLATION & CONTROL
Factory Default Settings
Continued
4
Acid Multiplier 0.0709
Sulfur Value is Percent ON
Sulfur Multiplier 0.6238
Fuse Multiplier 1.0
Use Offset Correction (ISO) OFF
Offset Value 0.0
Net Heat/Dry Factors
Fixed Hydrogen OFF 0.0
Fixed Oxygen ON 0.0
Fixed Nitrogen ON 0.0
Calculate Net Heat of Combustion OFF
Fixed Moisture as Determined OFF 0.0
Fixed Moisture as Received OFF 0.0
Dry Calculation OFF
Data Entry Controls
Prompt for Bomb ID ON
Weight Entry Mode Touch Screen
Acid Entry Mode Touch Screen
Net Heat Entry Modes Touch Screen
Auto Sample ID Controls ON
Sample Weight Warning above 2.0
Spike Weight Entry Mode Touch Screen
Sulfur Entry Mode Touch Screen
Moisture Entry Modes Touch Screen
Auto Preweigh Controls ON
Auto Sample ID Controls
Automatic Sample ID ON
Automatic Sample ID Increment 1
Automatic Sample ID Number 1
Auto Preweigh Controls
Automatic Preweigh ID ON
Automatic Preweigh ID Increment 1
Automatic Preweigh ID Number 1
Reporting Controls
Report Width 40
Automatic Reporting ON
Auto Report Destination Printer
Individual Printed Reports OFF
Edit Final Reports OFF
Recalculate Final Reports OFF
Use New EE Values in Recalculation OFF
Report Schedule End of Postperiod
Communication Controls
Printer Type Parr 1758
Balance Port
Network Interface
Printer Destination Local USB
Bar Code Port
Network Data Devices
Balance Port Communications
Balance Type Generic
Balance Port Device
Customize Balance Settings
Balance Port Settings
Number of Data Bits 8
Parity None
Number of Stop Bits 1
Handshaking None
Baud Rate 9600
Data Characters from Balance 8
Data Precision 4
Transfer Timeout (seconds) 10
Balance Handler Strings
Data Logger
Data Logger OFF
Data Log Interval 12s
Data Log Destination Log File and
Printer
Select Data Log Items
Data Log Format Text Format
www.parrinst.com
25
4
PROGRAM INSTALLATION & CONTROL
This page intentionally left blank.
26
Parr Instrument Company
6300
OPERATING INSTRUCTIONS
5
CHAPTER 5
OPERATING INSTRUCTIONS
TO BEGIN A TEST
Weigh the sample to 0.1 mg. 1.
Gently tap the capsules that contain powdered 2.
samples to compact the material. (Pellets are easier
to handle than loose samples and they burn slower
in the bomb, thereby reducing the chances for incomplete combustion.)
Carefully place the capsule into the capsule holder.3.
Attach 10 cm of ignition thread (see Figure 5-2).4.
Install bomb head in calorimeter.5.
Close calorimeter cover making certain the latch is 6.
engaged
Select determination or standardization as appro-7.
priate on Calorimeter Operations Page, Operating
Mode.
Press START to begin the test. Calorimeter will 8.
prompt operator for Cal ID number, Sample ID
numbers and weights in accordance with operating
modes set into the instrument.
OPERATING THE OXYGEN BOMB
Combustion with oxygen in a sealed bomb is a very
effective and reliable method for releasing all heat
energy obtainable from a sample, and for preparing
hydrocarbon compounds and carbonaceous materials
for analysis.
Note:
The following precautions must always be observed when
using this equipment:
Do not overcharge the bomb with sample or with a 1.
sample which might react with explosive violence.
Do not overcharge the bomb with oxygen. The 2.
initial charging pressure should not exceed 40 atm
(600 psig).
Do not fire the bomb if there is any indication that 3.
it is leaking.
Stand away from the calorimeter during firing and 4.
for at least 20 seconds after firing.
Keep the bomb in good condition at all times. Any 5.
parts that show signs of weakness or deterioration
must be replaced promptly.
Read the maintenance and safety instructions before 6.
starting to use the bomb, and urge all operating
personnel to read these instructions often.
Note:
Tape should always be stored in a sealed container to
minimize changes in its moisture and solvent content.
www.parrinst.com
27
5
OPERATING INSTRUCTIONS
Figure 5-1
Fill Flow Diagram
28
Parr Instrument Company
6300
OPERATING INSTRUCTIONS
5
ALLOWABLE SAMPLE SIZE
To stay within safe limits, the bomb should never be
charged with a sample which will release more than
8000 calories when burned in oxygen.
The initial oxygen pressure is set at 30 atmospheres (450
psig). This generally limits the mass of the combustible
charge (sample plus benzoic acid, gelatin, firing oil or
any combustion aid) to not more than 1.1 grams.
When starting tests with new or unfamiliar materials, it
is always best to use samples of less than .7 gram with
the possibility of increasing the amount if preliminary
tests indicate no abnormal behavior and sample will not
exceed the 8000 calorie limit.
To avoid damage to the bomb and calorimeter, and possible injury to the operator, it should be a standing rule
in each laboratory that the bomb must never be charged
with more than 1.5 grams of combustible material.
Figure 5-2
Cotton Thread Assembly
Samples containing sulfur should contain no more than
50 mg of sulfur and have a calorific value of at least
9000 BTU/lb.
Samples containing chlorine should be spiked to insure
that sample contains no more than 100 mg of chlorine
and liberates at least 5000 calories.
ATTACHING THE COTTON THREAD
Remove any moisture from the heating wire prior to attaching the cotton thread.
A cotton thread (845DD) is used as an auxiliary fuse to
ignite the sample (See Figure 5-2).
Four inches of thread is recommended for this auxiliary
thread which is looped over the heating wire, doubled
on itself, twisted to form a single strand and fed into the
sample cup to lay on the sample.
When contact is made through the heating wire, the
thread will ignite, drop into the sample cup and ignite
the sample.
One spool of thread, part number 845DD, is 563 yards.
Part number 845DD2 contains approximately 1000
pieces of thread pre-cut to 4 inches.
www.parrinst.com
29
5
OPERATING INSTRUCTIONS
WARNING - DO NOT OVERFILL THE BOMB
The safety relief valve on the regulator should protect the system from an over fi ll. If for any reason, the
bomb should accidentally be charged to more than 600 psig (40 atm), do not fi re the bomb. The dangerous pressures which might develop under such conditions could damage the bomb and injure the operator.
If there is any reason to believe that the bomb has been over-fi lled, stop the fi lling operation immediately,
exhaust the bomb and open it to check for any loss of sample before repeating the fi lling procedure.
Figure 5-3
Pre-period/Post-period
30
Parr Instrument Company
Loading...