No.

299M

1281 OXYGEN BOMB

CALORIMETER

Operating Instruction Manual

 1994 Parr Instrument Company
All Rights Reserved
Preface

Scope ...........................................................................................................I-I
Getting Started .............................................................................................I-I

Concept of Operation
A Highly Automated Procedure ....................................................................1-1
New Convenience - New Technology...........................................................1-1

Installation

Required Consumables and Power Requirements.......................................2-1

Installing the Calorimeter..............................................................................2-1
Instructions for Installation & Use of the 1281 Bomb Rinse Container
Sub-assembly (A1050DD) ............................................................................2-8
Overview ......................................................................................................2-8
Concept of Operation ...................................................................................2-8
Installation ....................................................................................................2-8
Disabling the Divert Valve ............................................................................2-8
Connecting the A1050DD Rinse Container Assembly..................................2-9
Adjusting the Bomb Rinse Parameters.........................................................2-9
Operation......................................................................................................2-9

Instrument Description
Page and Line No. Selection ........................................................................3-1
Types of Controls .........................................................................................3-1
Keyboard ......................................................................................................3-2

Program Installation & Control

Software Installation .....................................................................................4-1

Default Settings ............................................................................................4-1
Revised Default Settings ..............................................................................4-1

Operating Instructions
1136 Oxygen Bomb Operating Instructions ..................................................5-1
A Chlorine-Resistant Bomb ..........................................................................5-1
Allowable Sample Size .................................................................................5-3
Attaching the Cotton Thread.........................................................................5-3
Fill Cycle .......................................................................................................5-5
Pre-Period ....................................................................................................5-5
Bomb Firing ..................................................................................................5-5

Post-Period...................................................................................................5-5
Drain.............................................................................................................5-7
Closing the Bomb .........................................................................................5-7
Closing the Calorimeter Cover......................................................................5-7
Samples and Sample Holders ......................................................................5-7

i-i
Table of Contents

Operating Suggestions .................................................................................5-12

1552 Water Cooler Operating Instructions ...................................................5-12

Corrections & Final Reports

Entering Corrections and Obtaining the Final Report ...................................6-1

Manual Entry ................................................................................................6-1
Fixed Corrections .........................................................................................6-2
Automatic Data Transfers.............................................................................6-2

Reporting Instructions
Report Option Selection ...............................................................................7-1
Report Destination........................................................................................7-1
Report Generation ........................................................................................7-1
Net Heat of Combustion ...............................................................................7-2

Memory Management
Clearing Memory ..........................................................................................8-1
Editing Memory.............................................................................................8-1

Maintenance & Troubleshooting

Bomb Maintenance.......................................................................................9-1
Bomb Pressure Release...............................................................................9-2
Visual Confirmation of the Piston Movement ................................................9-2
Confirming Correct Operation of the 934DD Solenoid Valve Assembly .......9-2
Further Troubleshooting ...............................................................................9-4
Filling and Exhausting the Bomb Using the I/O Diagnostics.........................9-4
Hall Effect Sensor Check/Adjustment...........................................................9-5
Oxygen Bomb Removal and Replacement...................................................9-5
Parr 1281 Calorimeter Error List...................................................................9-6

Appendix A - Menu Operating Instructions

Calorimeter Operation Page 1 ......................................................................A-1
Operating Controls Page 2 ...........................................................................A-1
Program Information and Control Page 3 .....................................................A-3

Calibration Data and Controls Page 4 ..........................................................A-4

Thermochemical Calculations Page 5 ..........................................................A-5
Data Entry Controls Page 6 ..........................................................................A-7
Reporting Controls Page 7 ...........................................................................A-8
Communication Controls Page 8 ..................................................................A-9
Diagnostics Page 9.......................................................................................A-10

Appendix B - Calculations

Calculating the Heat of Combustion .............................................................B-1

General Calculations ....................................................................................B-1

i-ii
Thermochemical Corrections........................................................................B-1
ASTM and ISO Methods Differ .....................................................................B-2
Thermochemical Calculation Details ............................................................B-3
ASTM Treatment for Acid and Sulfur............................................................B-5
ISO Calculations...........................................................................................B-5
Spiking Samples...........................................................................................B-6
Conversion to Other Moisture Bases............................................................B-6
Conversion to Net Heat of Combustion ........................................................B-6

Appendix C- Standardization

Standardizing the Calorimeter ......................................................................C-1

Standard Materials .......................................................................................C-1
Automatic Statistical Calculations.................................................................C-2

Appendix D - Communication Interfaces

Required Software Versions .........................................................................D-1

Required Hardware ......................................................................................D-1
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

Appendix E - Technical Service

Return for Repair ..........................................................................................E-1

Appendix F - Parts List

1281 Calorimeter Parts List ..........................................................................F-1

1281 Calorimeter Parts List Continued.........................................................F-2
1281 Calorimeter Cover Parts List................................................................F-3
1281 Bucket and Stirrer Tube Assembly Parts List ......................................F-4
1281 Air Can Assembly Parts List ................................................................F-5
1288 Accessory/Installation Kit Parts List.....................................................F-5
1136 Oxygen Bomb Parts List .....................................................................F-6
1136CL Oxygen Bomb Parts List ................................................................F-7
1289 (1281) Spare Parts List .......................................................................F-8

Appendix G - Bomb Rinse Container Assembly

Concept of Operation ...................................................................................1-1

Installation ....................................................................................................1-2
Operation......................................................................................................1-2

i-iii
Table of Contents

Figures

2-1 1552 Water Cooler Electric Circuits ...................................................2-2

2-2 1552 Water Cooler Front View...........................................................2-2
2-3 1552 Water Cooler Top View.............................................................2-2
2-4 1281 Calorimeter External Plumbing .................................................2-4
2-5 1281 Calorimeter Electrical Hookup ..................................................2-5
2-6 1281 Calorimeter Rear Panel ............................................................2-6
3-1 1281 Calorimeter Keyboard ...............................................................3-2
4-1 1281 Factory Default Settings............................................................4-2
5-1 Oxygen Bomb Assembly....................................................................5-1
5-2 Fill Flow Diagram ...............................................................................5-2
5-3 Attaching the Cotton Thread ..............................................................5-3
5-4 Pre-Period - Post-Period....................................................................5-4
5-5 Rinse and Cool Flow Diagram ...........................................................5-6
5-6 Drain Flow Diagram ...........................................................................5-8
5-7 Combustion Capsule With Adhesive Tape Seal ................................5-11
9-1 Lid Removal.......................................................................................9-14
9-2 1281 Housing Removal......................................................................9-15
9-3 1281 Wiring Diagram .........................................................................9-16
9-4 1281 Switch Wiring Diagram..............................................................9-17
9-5 1281 Solenoid Wiring Diagram ..........................................................9-18
9-6 1281 Power Supply............................................................................9-19
9-7 1281 Pneumatic Diagram ..................................................................9-20
9-8 1281 Valve Assembly ........................................................................9-21
9-9 1281 N2 Solenoid Valve Assembly....................................................9-22
9-10 1281 Solenoid Valve Assembly .........................................................9-23
9-11 1281 Water Solenoid Assembly.........................................................9-24
9-12 Air Cylinder Assembly........................................................................9-25
9-13 1281 Internal Plumbing Diagram .......................................................9-26
9-14 Internal Tubing Reference .................................................................9-27
9-15 1281 Propeller Assembly ...................................................................9-28
9-16 1281 Bucket Assembly ......................................................................9-29
9-17 1281 Air Can Assembly .....................................................................9-30
9-18 Solenoid Valve Assembly ..................................................................9-31
F-1 Oxygen Bomb Head Assembly ..........................................................F-9
F-2 Oxygen Bomb Head Assembly ..........................................................F-10

Tables

B-1 Settings for ISO & BSI Methods.........................................................B-4

D-1 Software Required .............................................................................D-2
D-2 Smart Link Cables .............................................................................D-3
D-3 1281 Terminal Port ............................................................................D-6
D-4 1281 Balance Port .............................................................................D-6
D-5 1281 Printer Port................................................................................D-7
D-6 Calorimetry Run Storage Definitions..................................................D-8
D-7 Data Entered - Bit Definitions.............................................................D-8

i-iv
i-v
Preface

Scope Additional instructions concerning the

This manual contains instructions for
installing and operating the Parr 1281
Calorimeter. For ease of use, the manual is
divided into ten chapters.
installation and operation of various
component parts and peripheral items
used with the 1281 Calorimeter have been
included and made a part of these
instructions.

Concept of Operation Installation No. Description

Instrument Description Program 201M Limited Warranty
Installation and Control 202M Introduction to Bomb
Operating Instructions Corrections & Calorimetry
Final Reports Reporting Instructions 207M Analytical Methods for
Memory Management Maintenance Oxygen Bombs
Instructions Appendices 245M 1552 Water Cooler

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 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
Getting Started
These steps are offered to help the user
become familiar with, install, operate and
develop the full capabilities of the Parr
1281 Calorimeter.

CUSTOMER SERVICE

Questions concerning the installation

or operation of this instrument
can be answered by
the Customer Service Department of
Parr Instrument Company
(309) 762-7716 (800) 872-7720
Fax: (309) 762-9453

http://www.parrinst.com parr@parrinst.com

I
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 under-
stand the operating instructions which
follow.
3. Turn the power switch ON (located at
the back, right of the controller). 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 final reports, 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 1281
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 1281
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 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
1281 Calorimeters will have an energy
equivalent of approximately 800
calories per ºC. The runs for
standardization and determinations are
identical, except for the setting of the
instrument to the standardization or
determination mode.
9. Review the Communication Interfacing,
Appendix D, for the correct installation
of any Smart Link peripherals to the
1281 Calorimeter.
10. After successful standardization, the
1281 Calorimeter should be ready for
testing samples.
II
Concept of Operation
A Highly Automated Procedure
Parr proudly introduces a new Oxygen
Bomb Calorimeter, No. 1281, 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.
In the 1281 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 - New Technology
The 1281 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.
1-1
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,
cools the system and empties the bucket.
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, 40
characters wide, 15 lines high, prompts the
operator through all setup and operating
steps with on-screen menus which make
user training quite simple.
1-2
Installation

Required Consumables and Power

Requirements

The 1281 Calorimeter System requires

availability of the following compressed gas
cylinders:

1. Oxygen, 99.5% purity, with CGA 540

connection, 2500 psig, maximum.

2. Nitrogen or air, oil and water free, with

CGA 580 connection, 2500 psig,
maximum.

Approximately 16 liters of distilled water

are required to fill the calorimeter rinse
tank.

Approximately 9 liters of tap water, with a

total hardness of 85 ppm or less, are
required for filling the Closed Water Installing the Calorimeter
Handling System.
Each Parr 1281 Calorimeter was
The power requirements for the sub- completely assembled and thoroughly
assemblies of the 1281 Calorimeter are: tested prior to shipment. The following
stepwise procedure will guide the user
• Calorimeter 10A @ 120VAC through the installation process.
5A @ 230VAC
1. Unpack the calorimeter and carefully
• Printer check the individual parts against the
2A @ 120 packing list. If shipping damage is
1A @ 230 discovered, report it immediately to the
delivering carrier. The calorimeter will
• Water Cooler need to be filled with water, connected
5.0A @ 120VAC 60Hz to the water cooler, gas supplies and an
2.5A @ 230VAC 50 Hz electrical outlet. Set the calorimeter on

WARNING - DO NOT OVERFILL THE BOMB

The safety relief valve on the regulator should protect the system from an over fill.
If for any reason, the bomb should accidentally be charged to more than 600 psig (40 atm),
Do not fire 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-filled, stop the filling operation immediately, exhaust the bomb and
open it to check for any loss of sample before repeating the filling procedure.

2-1
a sturdy, level, bench or table, free from
drafts, vibration and sources of radiant
heat.

Note:

When Swagelok Tube Fittings are used,

the instructions for installation are:

1. Simply insert the tubing into the

Swagelok Tube Fitting. Make sure that
the tubing rests firmly on the shoulder
of the fitting and that the nut is finger-
tight.

2. Before tightening the Swagelok nut,

scribe the nut at the 6 o’clock position.

3. While holding the fitting body steady

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 o’clock position.

For 3/16" and 4mm or smaller tube fittings,

tighten the Swagelok nut 3/4 turns from
finger-tight.

2. Remove the cap plug on the water

filling elbow and fill the calorimeter
water tank with good quality tap water
or distilled/deionized water until the
water level is at the bottom of the filling
elbow. The calorimeter water tank will
initially accept about 8 liters. Fill the
external calorimeter rinse tank with
about 16 liters of distilled/deionized
water through the large opening at the
top of the tank. The cover for this
opening is removed by lifting up on the
handle, pushing down on the lid, tilting
and removing. Replace and close the
cover after filling.

3. Make the connections to the water

cooler at this time. Refer to figure 2-4.
Install the 1552 Water Cooler so that

2-2
Installation
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
241VB Union Male Elbows on the water
inlet and outlet connections of the
cooler (see figure 2-3). Connections
between the calorimeter and the cooler
should be made with the furnished 3/8"
tubing. Install 183VB inserts at each
end of the two lengths of tubing prior to
inserting the tubing into the
compression fitting. A temperature
adjustment screw is located in an
opening on the front end of the cooler.
Set this adjustment at the coldest
setting (7/8 clockwise - see figure 2-2).
Note:
Do not plug in the cooler at this time.
4. Connections 5 and 6 between the
calorimeter and the 1575 Rinse Tank
should be made with two pieces of 1/8"
nylon pressure hose. These tubing
lengths should be limited to a maximum
length of 10 feet.
5. Make the connections to the oxygen
and nitrogen supplies at this time
(connections 3 and 4). Refer to figure 2-
4. Quarter inch O.D. nylon pressure
hose is used to connect the nitrogen
supply. Eighth inch O.D. nylon pressure
hose is used to connect the oxygen
supply. The delivery pressure for
oxygen should be set at 450 psig. The
nitrogen delivery pressure should be
set to 80 psig. To install the regulators,
unscrew the protecting cap from the
tank and inspect the threads on the
2-3
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 both
tank valves and check for leaks.
Note:
The cause of any leaks must be
corrected before proceeding.
A hissing sound will occur while the
rinse tank is being pressurized. This is
normal. Adjust the pneumatic supply
regulator to 80 psig as needed.
Note:
During extended periods of inactivity
(overnight or longer), close the tank valves
to prevent depleting the tanks in the event
of a leak. When changing tanks, close the
tank valve prior to removing 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 recommended 450 psig oxygen
filling pressure is slightly higher than
the 30 atmospheres prescribed in other
Parr bomb and calorimeter manuals.
This difference is insignificant. Higher
or lower settings may be used, but the
bomb must never be filled to more than
600 psig (40 atm). Filling pressures
below 28 atm (400 psig) will result in a
low oxygen pressure error message.
6. An A1108DD strainer is furnished with
each calorimeter and the strainer is
placed in the bottom of the bomb above
the 668DD check valve. The strainer
prevents large particles of ash from
impeding the operation of the check
valve and the 966DD release shaft.
Periodically remove and clean strainer.
 Figure 2-4
1281 Calorimeter External Plumbing

2-4
Installation
Connections 7 and 8, 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 10liter
carboy (231C2). The carboy should be
placed at or below the level of the
calorimeter to facilitate complete
draining of these lines.
Note:
Step 6 is optional for use with A1050DD.
See Appendix G for A1050DD2 Bomb
Rinse Container Installation and Use.
7. The balance port connection, if needed,
should be made at this time. Refer to
figure 2-5 for the correct cable to
connect the balance to the calorimeter.
2-5
8. 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 switches for the Smart Link
connection are set to the CLOSED or
ON position at the factory. If only one
Smart Link cable is plugged into the
rear of the calorimeter (end of link
position), no changes to the switch
settings are required. If two cables are
used (middle of link position), then all
switch levers will need to be set to the
OPEN or OFF position. The termination
switch for the Smart Link is located
between the two nine pin Smart Link
connectors.
9. Connect the printer power cable and
the printer communications cable
between the 1756 printer and the
connections at the rear of the
calorimeter.
Note:
Apply power to the calorimeter and turn on
the printer.
Install the printer ribbon, paper holders,
re-roll prevention guard and printer
paper at this time. Press the PRINT
SCREEN key on the calorimeter front
panel to insure correct printer
operation.
10. Go to the Calorimeter Main Menu and
press 1, Calorimeter Operation. Press
the down arrow key twice and press the
YES key to activate the calorimeter
water pump and heater. Loosen
connection #1 at the rear of the
calorimeter to purge the air from the
water cooler holding tank. Refill the
calorimeter water tank as required in
order to maintain the water level at the
bottom of the filling elbow. If the low
2-6
Installation
water error message is reported, press
the CLEAR key to acknowledge the
message, refill the tank as required and
reactivate the heater and pump.
Tighten the connection and connect the
cooler to the electrical supply when the
cooler holding tank is free of any
trapped air.
11. Wait for the calorimeter jacket
temperature to stabilize within a half a
degree of 30 C. 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 5 -1 on
page 5-1.
12. Lock the head in the bomb cylinder,
close the lid and while applying a slight
downward pressure press the F2 key to
initiate a pre-test cycle. 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.
13. Assemble the bomb head stand,
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 on page 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
2-7
displayed sample ID number followed
by SKIP and then ENTER to store the
default sample mass of 1 gram. This
test should go through Fill, Pre-period,
Post-period and Cool/Rinse Cycles and
yield a printed calorimetry report. The
calorimeter is now ready to be
standardized.
14. 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, Item 1, Operating Mode. The
YES/NO keys are used to select the
desired operating mode. 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, Line 2, using the
YES/NO keys. 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 2 to 3 calories per
degree, centered around 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.

Instructions for Installation and Use of
the 1281 Bomb Rinse Container
Assembly (A1050DD)
Overview
The A1050DD Bomb Rinse Assembly is
provided as an accessory to the
1281Calorimeter. This device allows for
complete and systematic recovery of the
bomb combustion products. These
combustion products include that portion
which is released during the initial bomb
exhaust, followed by the portion expelled
during the bomb rinse cycle.
Concept of Operation
The 1281 Bomb Rinse Container Assembly
is connected to the rear of the calorimeter,
in place of the portion of the waste tube
assembly that is connected to the bomb
exhaust fitting. The divert valve, at the right
hand side of the calorimeter, is disabled to
allow the bomb exhaust and the bomb
washings to be collected in the 1053DD,
HDPE 500 ml bottle, provided with the
A1050DD. The objective is to capture and
retain all of the combustion products which
have been dissolved in the residual water
present in the bomb prior to combustion as
well as any water formed during the
combustion process. The most common
examples of these combustion products
include:
Sulfate, derived from any sulfur containing
materials in the original sample.
Chloride, from organic samples containing
chlorine.
These combustion products are discharged
from the bomb in two steps. The first step
occurs during the initial rapid release of the
residual bomb gases. The 1053DD bottle
has sufficient strength and volume to deal
effectively with this sudden pressure
release. Gas is expelled from the four
holes on the perimeter of the 1052DD
bottle cap, leaving any discharged liquid in
the bottle. As an additional safety measure,
the bottle is supported in a 1054DD acrylic
cylinder which serves to keep the bottle
upright and contained in the unlikely event
the bottle ruptures. At the end of the bomb
exhaust step the aqueous combustion
products reside in the bomb, associated
tubing as well as the 1053DD bottle. The
bomb rinse step flushes these combustion
products from the bomb and the tubing into
the 1053DD bottle. The bottle can then be
unscrewed from the assembly and capped,
until the sample is to be analyzed. Some
users find it useful to add the contents of
the rinsed combustion capsule to the
washings collected in the bottle. Three
1053DD bottles are provided with the
assembly. Additional bottles may be
ordered separately from Parr.
Installation
Disabling the Divert Valve
The bomb rinse divert valve should be
disabled to permit the bomb washings to
be discharged out the rear of the 1281
Calorimeter. Disconnect the power cord at
the rear of the instrument and remove the
rear cover plate. Next, locate the
pneumatic solenoid responsible for piloting
the divert valve. This solenoid is the lower
of two identical solenoids, with yellow caps,
mounted to a common manifold on the
center bulkhead inside the calorimeter. The
upper solenoid operates the lid locking
mechanism. Remove one wire from the
lower solenoid. This prevents the divert
value from activating during the bomb rinse
sequence. Replace the rear cover and
apply power to the calorimeter.
2-8
Installation

Connecting the A1050DD Rinse Samples to be analyzed for chlorine should

Container Assembly
Break the connection at the rear of the
1281 calorimeter to the bomb exhaust
hose. In place of this, connect the “ tube
and 3/8” compression fitting provided as
part of the A1050DD.
be spiked in a manner to insure that the
sample as-burned contains less than 10%
chlorine and liberates at least 5000
calories. Five thousand calories
corresponds to roughly a 6.4 C
temperature rise in a 1281 Calorimeter.

Adjusting the Bomb Rinse Parameters At the completion of the test, the collection
The bomb rinse parameters are factory set bottle should be unscrewed from the
to provide approximately 50 ml of bomb 1052DD Bottle Cap and the contents of the
washings. This amount was chosen in combustion capsule added to the collected
order to rinse the bomb as quickly as washings. The bottle then may be capped
possible in order to prepare the calorimeter and labeled until the contents can be
for the next test. More quantitative rinsing analyzed.
can be realized, at the expense of time, by
increasing the volume of washings.
Experience has demonstrated that for a
bomb of this volume, wash volumes on the
order of 100 ml are required for
quantitative recovery. Doubling either the #
of rinse cycles or the rinse time on menu
page 2.4.5 from the default value of 5 to 10
will provide a volume of washing better
suited for precise analytical work. The
volume of washing can be easily verified
by performing a calorimeter pretest
sequence (F2).

Operation

Place the bottle end of the rinse assembly

in the 1054DD Bottle Support and orient in
such a way to minimize any undesirable
effects by the bomb exhaust discharge
from the four holes in the 1052DD bottle
cap. Analyze the sample in the calorimeter
in the usual fashion, using the following
guidelines in order to insure quantitative
conversion to the proper ionic form of the
analyte:

Samples containing sulfur should contain

no more than 5% sulfur as-burned in the
calorimeter and have a heat of combustion
of at least 9000 Btu/lb.

2-9
2-10
Instrument Description
All 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 which
comprise 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
Page and Line No. Selection
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 ENTER.
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 ENTER. (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.
3-1
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 arrow keys 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 displayed 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 calorimeter and are
informational only. Certain ones 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).
 these keys and their functions. Instructions
Note: in later chapters provide detailed operating
To return to previous pages from a sub- instructions.
menu, press ESCAPE. To return to the
Main Menu, press SHIFT, ESCAPE. Key Description
Remember, no value or setting chosen is
stored in the program until the ENTER key
is pressed. ↑ Moves the cursor UP on any
of the menu pages.
Keyboard
← NO Changes menu functions that
Before using the 1281 Calorimeter, the are either an ON/OFF or
operator should understand the various YES/NO toggle to OFF,NO,
keys on the keyboard (see Figure 3-1). The or to select an option from
brief descriptions given here will identify the list provided.

Figure 3-1. 1281 Calorimeter Keyboard

3-2
Instrument Description
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 on
any 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 Initiates a preconditioning
cycle which will lock the
cover, fill the bucket, fill the
bomb, drain the bucket, vent
the bomb, rinse the bomb
and open the cover. In
addition to confirming that all
systems are working
properly, it will bring the
calorimeter to operating
equilibrium after it has been
standing for a while. It is
recommended that this cycle
be run if the calorimeter has
been idle for 15 minutes or
longer. The controller will
automatically prompt the
operator to run a pretest if the
START button has not been
pressed for 15 minutes.
F3 This key is used to initiate
edit capabilities for sample
weight, spike weight, cal ID
3-3
number, fuse, acid, sulfur or
hydrogen values.
F4 Not applicable.
CLEAR Clears tests from the
MEM. memory. When it is pressed,
the controller will prompt for
the beginning and ending
Sample IDs to be deleted
from memory.
PRINT Prints information (except
SCREEN 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 function
keys (F1-F4) can be used
with the SHIFT key to provide
a total of eight programmed
functions on the four keys.
0-9 The DECIMAL and 0-9 keys
& are 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
required. It is entered before
the digits and also used to
indicate that the numbers are
being entered in scientific
notation.

CLEAR Erases incorrect values and
ENTRY 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.
← The ENTER key is used in
ENTER 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 ENTER 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.)
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 SHIFT,
ESCAPE to return directly to
the main menu from a sub-
menu.
SHIFT F1 This key activates the on / off
Function of the data logger.

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

3-4
Program Installation & Control interrupted or the unit is turned off. If the
unit experiences an intentional or
unintentional “Cold Restart”, the controller
Software Installation will return to its default settings.

The program in the 1281 Calorimeter can Revised Default Settings

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.
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
The default parameters of the 1281
Calorimeter can be changed to guarantee
that the 1281 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 Page 3, Line 9 - Save User
Default Settings, and press ENTER.
• Press YES, the controller will prompt
the user for a “User Rev.”. This can be
any number that is helpful in identifying
the user’s setup. Enter number and
press ENTER.
To re-load the user default setting, go to
Page 3, Line 8 - Re-load User Default
Settings, press ENTER and YES.

Units are preprogrammed with DEFAULT

SETTINGS. See Figure 4-1 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

4-1
4-2
Program Installation & Control

4-3
4-4
Program Installation & Control

The above menu is accessed

with Shift 3

4-5
Operating Instructions

• Stand away from the calorimeter during

To begin a test:
• Weigh the sample to 0.1 mg.
• Gently tap the capsules that contain
powdered samples to compact the
material.
• Carefully place the capsule into the
capsule holder.
• Attach 10 cm of ignition thread (see
Figure 5-3).
• Install bomb head in calorimeter.
• Close calorimeter cover.
• Select determination or standardization
as appropriate on Page 1 - Calorimeter
Operations, Line 1 - Operating Mode,
using the NO key.
• Press START to begin the test.
Calorimeter will prompt operator for
Sample ID numbers and weights in
accordance with operating modes set
into the instrument.
1136 Oxygen Bomb Operating
Instructions
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.
firing and for at least 20 seconds after
firing.
• Keep the bomb in good condition at all
times. Any parts that show signs of
weakness or deterioration must be
replaced promptly.
• Read the maintenance and safety
instructions before starting to use the
bomb, and urge all operating personnel
to read these instructions often.
A Chlorine-Resistant Bomb
The 1136CL bomb is the same as the
standard 1136 model, but with a head and
cylinder made of an alloy with superior
corrosion resistance to the free chlorine
and halogen acids released when burning
chlorinated samples. Users who intend to
test waste materials and combustible
solvents are urged to use the 1136CL
Bomb instead of the 1136 for its longer
service life under extreme corrosive
conditions. Bomb maintenance is also
improved.

Note:
The following precautions must always be
observed when using this equipment:

• Do not overcharge the bomb with

sample or with a sample which might
react with explosive violence.
• Do not overcharge the bomb with
oxygen. The initial charging pressure
should not exceed 40 atm (590 psig).

• Do not fire the bomb if there is any

indication that it is leaking.
5-1

4-6
5-2
Operating Instructions

Allowable Sample Size

Note:
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.
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
Note:
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 5-3).
Ten centimeters 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.

5-3
5-4
Operating Instructions
Fill Cycle
Once the calorimeter is started and the
cover is closed, the fill sequence begins
(see Figure 5-2).
1. The calorimeter locks the cover and
checks the bomb ignition circuitry for
continuity.
2. The water fill solenoid opens and water
is pumped from the closed water supply
tank into and through the bucket that
surrounds the bomb. Overflow from the
bucket is returned to the closed water
tank. Because the jacket and bucket
are both filled with water from the
closed water tank, initial equilibrium will
be reached quickly.
3. The oxygen fill solenoid is opened and
oxygen is added slowly to the bomb to
bring its pressure to approximately 30
atm.
Pre-Period
At the completion of the fill sequence, the
pre-period begins (see Figure 5-4).
1. The water fill solenoid valve closes and
isolates the water in the bucket from the
rest of the system. Water within this
bucket is circulated by the pump. Water
continues to circulate from the closed
water system through the jacket
surrounding the bucket.
2. The gas pressure is checked, the
oxygen filling valve closes and the
pressure in the filling line is vented. The
automatic check valve at the top of the
bomb closes and isolates the bomb
from the oxygen filling line.
5-5
3. The controller monitors the operating
temperature until it confirms that the
initial equilibrium has been established.
Bomb Firing
Once the initial equilibrium is confirmed,
the controller initiates the firing sequence.
There are no changes to the circulation
pattern, as shown in Figure 5-4, from the
pre-period through the bomb firing and
post-period.
1. A warning of five short beeps is
sounded indicating the bomb is about to
be fired.
2. Current is passed through the electrical
leads to ignite the ignition thread.
3. The controller monitors the temperature
in the bucket to establish that a
temperature rise actually occurs. If no
temperature rise occurs, the misfire
message is displayed on the controller
and the abort sequence is initiated.
Post-Period
After firing is confirmed, the post-period
begins (see Figure 5-4).
1. The controller monitors the temperature
rise and determines the final
temperature rise by either the dynamic
or equilibrium criteria as established by
the user.
2. Once the final temperature rise is
determined, it is recorded with the test
results.
5-6
Operating Instructions
At the completion of the post-period, the
rinse and cool sequence begins (see
Figure 5-5).
1. Water from the cooler via the closed
water tank is circulated through the
bucket to cool the bomb to the starting
temperature. The cooling water is
returned to the closed water tank. The
temperature of the closed water system
is maintained by the 1552 Water Cooler
and immersion heater.
2. The release valve in the bottom of the
bomb is opened and the residual
pressure is released through the bomb
exhaust line.
3. Once the excess oxygen is vented, the
bomb wash water from the pressurized
rinse water tank is admitted through the
bomb wash solenoid valve and the
check valve at the top of the bomb. The
bomb wash water is released to the
wash bottle. Several rinse patterns may
be configured by the user to meet
various operational and analytical
requirements.
4. The bomb is filled one more time with
oxygen to help flush the water residue
from the interior of the bomb.
Drain
At the completion of the bomb rinse
sequence, the drain sequence begins (see
Figure 5-6).
1. The water in the bucket is drained out
of the bucket and back into the closed
water tank.
2. Once the bucket is drained, the cover is
unlatched and may be opened to
remove the bomb head and load the
next sample.
5-7
Closing the Bomb
Care must be taken not to disturb the
sample when moving the bomb head from
the support stand to the bomb cylinder in
the calorimeter. Check the sealing ring to
be sure that it is in good condition and
moisten it with a bit of water so that it will
slide freely into the cylinder.
Notice that the bomb head grounding lug
extends beyond the outside diameter of the
bomb head. A slot for this lug is cut into the
top of the calorimeter bucket which holds
the bomb cylinder. Position this lug
approximately 20 degrees to the operators
right and slide the head into the cylinder
and push it down as far as it will go. Now
rotate the bomb head 20 degrees to the left
until the lug contacts the left edge of the
cut out and is pointed at the front of the
calorimeter.
Closing the Calorimeter Cover
After the bomb head is installed, lower the
cover of the calorimeter. When the
calorimeter operating sequence is initiated,
an air operated cylinder will lock the cover
closed and will not release it until the
operating sequence is completed and it is
safe to open the bomb.
Samples and Sample Holders
Particle Size and Moisture Content.
Solid samples burn best in an oxygen
bomb when reduced to 60 mesh, or
smaller, and compressed into a pellet with
a 2811 Parr Pellet Press.
Large particles may not burn completely
and small particles are easily swept out of
the capsule by turbulent gases during rapid
combustion.
5-8
Operating Instructions
Note:
Particle size is important because it
influences the reaction rate. Compression
into a pellet is recommended because the
pressure developed 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 combustions.
If moisture is to be added to retard the
combustion rate, drop water directly 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.
Combustion Aids. 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.
5-9
Note:
It must be remembered, however, that a
combustion aid adds 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.
Combustion Capsules. 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 oxide
film. 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
480ºC 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 analytical 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 moisture content 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.
Coarse Samples. 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 1136 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 than20 mg of
chlorine samples with high sulfur contents
will greatly accelerate corrosion of the
bomb. An alternate 1136CL 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
1136CL Bomb offers significantly
enhanced corrosion resistance for this
service.
Explosives and High Energy Fuels. The
1136 and 1136CL Bombs used in the 1281
Calorimeter have been designed to provide
highly automated testing of routine
samples. Materials which release large
volumes of gas which detonate with
explosive force or burn with unusually high
energy levels, should not be tested in this
calorimeter.
Rather, they should be tested in a model
1261 Calorimeter which can be equipped
with an 1104 High Pressure Oxygen Bomb
designed specifically for these types of
samples.
Volatile Sample Holders. Volatile
samples 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 trimming the
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.
5-10
Operating Instructions
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, are
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 the determination. 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.
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:
5-11
• Weigh the empty cup or capsule; then
cover the top with tape, trim with a knife
and press the trimmed edge firmly
against the metal rim. 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 180ºC 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.
Operating Suggestions
Poor Combustion. 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 combustions 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 containing coarse
particles which will 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 amounts to approximately
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.
Oxygen Charging Pressure. The 1281
Calorimeter has been designed to operate
with an oxygen filling pressure of 30 atm.
Significant changes from this value are not
recommended.
1552 Water Cooler Operating
Instructions
The 1552 Water Cooler is intended to
provide a uniform water supply in the
temperature range from 7º to 10ºC for
maintaining the desired bucket and jacket
temperatures for each run and cooling the
oxygen bomb after each test.
The cold water needed for cooling the
bomb is determined by the controller, and
the amount of cold water needed for the
water handling system is determined by
the temperature that is monitored and
maintained by the controller.
5-12
Corrections & Final Reports

Entering Corrections and

Obtaining the Final Report
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.
Sulfur Key in the Sulfur Correction
Correction and press the ENTER key.
The default setting for this
value is to be entered as
percent sulfur in the sample.
If fixed values for fuse, acid and sulfur are
turned OFF on 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.

Refer to the Reporting Instructions,
Chapter 7, for the steps necessary to
initiate a report from the controller.
Manual Entry
During the reporting process, the controller
will prompt the user to enter the following
values:
If values for these corrections are not
available, the operator can use the SKIP
key to bypass any of the corrections,
however, a Final Report will not be printed
until an entry is made for fuse, acid and
sulfur.

Fuse Key in the Fuse/Heat Wire

Correction Correction and press the
ENTER key. The default
setting for this value is to be
entered in calories. The fuse
correction has two
components and these are
explained in Appendix B,
Page B-2.

Acid Key in the Acid Correction

Correction and press the ENTER key.
The default setting for this
value is to be entered in
milliliters of standard alkali
required to titrate total acid or
calories.

6-1
Fixed Corrections

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.

Automatic Data Transfers

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.

6-2
Reporting Instructions

Report Option Selection pressing the DOWN arrow, UP arrow or

The 1281 Calorimeter can transmit data
two ways:
• There are two kinds of calorimeter reports;
RS232C port to a 40 or 80 column
printer to provide a printed report.
• Preliminary reports are generated at the
Smart Link which formats and prints the
data on another calorimeter with an
attached printer.
After the cabling and communication
requirements are completed in the
Installation, Chapter 2, the calorimeter
must be programmed to format and direct
the report. This option is on Page 7 -
Reporting Controls, Line 1 - Printer
Controls.
Report Destination
Report(s) can be directed to a printer, null
device or display. This selection is on Page
7 - Reporting Controls, Line 2 - Report
Destination. The default is selected by
pressing the YES or NO key.
Note:
The default setting sends the calorimetric
reports to the printer until changed by the
user.
ESCAPE to clear.
Report Generation
preliminary and final.
conclusion of a test when one or more of
the calorimeter corrections (fuse, acid,
sulfur or spike) are not fixed. If a
preliminary report is requested, the Sample
ID will be displayed and prompt the user
for a correction value for fuse, acid, sulfur
or spike before providing the report. If
Smart Link Communication is enabled for
acid, sulfur or a fixed fuse correction, this
prompting for information is eliminated. To
provide a report with the information “as
is”, press SHIFT and REPORT. Preliminary
reports will remain preliminary and the
energy equivalent or heat of combustion
value reports will reflect the user’s setup on
Page 5 - Thermochemical Corrections.
Final reports contain all of the final or fixed
calorimetric corrections needed to give an
energy equivalent or a heat of combustion
value.

Printer Reports - Are printed on the

selected printer. The ID No. of the report
being printed will be briefly displayed on
the screen while printing.

Null Device Reports - If previously

completed tests require changes, the null
device default is used to recalculate the
test results without printing.

Displayed Reports - Are shown on the

calorimeter screen. The report is viewed by

7-1
To start a report:

• Press the REPORT key.

• Calorimeter will prompt “From ID>”.

Enter beginning ID of the test(s) to be
reported and press ENTER.

• Calorimeter will prompt “To ID>”. Enter

final ID of the test(s) to be reported and
press ENTER. The reporting process
begins.

To stop printing:

• Press RESET - The calorimeter will

reset and printing will stop after the
buffer is cleared.

• Press SHIFT and RESET - Clears

buffer and stops printing immediately.

Net Heat of Combustion

To have the Net Heat of Combustion print

as part of preliminary and final reports, go
to Page 5 - Thermochemical Corrections
and turn ON Line 8 - Calculate Net Heat of
Combustion. During the reporting process,
the controller will prompt for the hydrogen
(H) value. This information will not transfer
over the Smart Link.

7-2
Memory Management
The calorimeter will hold data for tests
within its memory. These tests may be
either preliminary, final, determination, or
calibration reports. Once the memory of
the controller is filled, any attempt to start a
new analysis will cause the controller to
display “RUN, LIST, FULL”. The user must
then clear some of the memory before
proceeding or use the overwrite capability
on Page 7, Line 6.
Clearing Memory
This capability allows the operator to delete
Sample ID numbers (and all related data
and results) for a single report, sequence
of reports or for all reports.
To clear some or all memory:
• Press CLEAR MEM.
• Calorimeter will prompt “From ID>”.
Enter beginning ID of the Test(s) to be
deleted and press ENTER.
• Calorimeter will prompt “To ID>”. Enter
final ID of the test(s) to be deleted and
press ENTER.
Note:
A single test can be deleted by entering the
same Sample ID No. for the “From ID>”
and “To ID>”. To clear all reports, enter 1
for the “From ID>” and 999999 for the “To
ID>”.
Editing Memory
The user can add or change previously
gathered test information. This feature is
provided principally to permit editing of
sample weights or other information to
preliminary tests.
8-1
To revise the sample weights, spike
weights, Cal ID number, fuse, acid, sulfur
or hydrogen values on final reports:
• Go to Page 7 - Reporting Controls, Line
7 - Edit Final Reports and select ON.
• Go to Page 7 - Reporting Controls, Line
2 - Report Destination and select
Display.
To edit a report:
• Press the F3 key.
• Calorimeter will prompt “From ID>”.
Enter beginning ID of the Test(s) to be
edited and press ENTER.
• Calorimeter will prompt “To ID>”. Enter
final ID of the test(s) to be edited and
press ENTER. (The calorimeter will
identify the report(s) as either
preliminary or final.)
• Highlight the data field to be edited by
pressing the UP or DOWN arrow key
• Press the CLEAR key, enter the new
value on the keyboard and press
ENTER. The report will immediately
recalculate the heat of combustion
when a new value is entered.
Note:
This sequence can be canceled by
pressing the RESET key.
Maintenance & Troubleshooting

9-0
Maintenance & Troubleshooting

Remove, inspect and clean cylinder

Bomb Maintenance sealing/pressure release pin and
corresponding sealing area in the bomb
Daily Maintenance cylinder. In extreme cases, i.e. a spilled
(Before Testing) sample, use soap and water.

Note: Clean 986DD Electrode Contact Pins with

Clean small quad-ring that seals the bomb mild abrasive, such as a pencil eraser,
head and cylinder by wiping with a tissue. clean bomb head electrode points in a
Wet this sealing area with water prior to similar fashion, tighten screws holding
starting a series of tests. Clean heating wire in place.
corresponding sealing area in cylinder in a
similar fashion. Both surfaces must be free 50 to 100 Tests-Replace heating wire, with
of any accumulated foreign matter, such as 1.5” of 840DD2.
unburned sample material or combustion
by-products. Wet the hole in the center of Semiannual - Change water in the Water
the head which contains the check valve. Handling System and replace 149C Inline
Water Filter.
With a tissue, clean the head where the
large bucket quad-ring contacts the head 500 Tests - Replace O-rings listed.
perimeter. Wet this sealing area with water
prior to starting a series of tests. 659DD 969DD
667DDJV 1081DD
2-821DD 394HC
882DD 1374HCJV

Table 9-1
Fuse Assignments

Output OP/LED # Fuse # Part No.

Bomb Cool 2
H2O Fill 3
Drain 4
O2 Fill 5
O2 Dump 6
Bomb Rinse 7
Pressure Rel 8
Lid Lock 9
Bomb Seal 10
Divert 11
Heater NA F1-7A 959E4
Pump NA F3-1A 959E
Board NA F2

Note: The LEDs on the back panel indicate when a particular device has been turned on by the microprocessor
or manually activated by inserting a small screw driver across the test pins.
9-1
Lubricate 659DD and 357HCJB O-rings in
bomb release cylinder with 811DD
Lubricant. All O-rings are in the head
except for 1-821DD, 882DD, 969DD and
1081DD O-rings. Clean ignition contacts
and check water level.
Note:
Installation instructions for the 667DDJV
Quad-Ring - these quad-rings are identified
with a yellow mark on the outside
perimeter. This mark must be visible on the
outside perimeter after installation in order
to insure that the quad-ring has not been
“rolled”. A quad-ring that is rolled or twisted
will not seal properly.
Inspection of Critical Sealing Surfaces
The sealing grooves and related surfaces
for most of the Parr bombs are machined
to tolerances as small as +/- 0.001"
(0.03mm). As a result, any imperfection in
a sealing surface resulting from either
normal use or carelessness in handling the
bomb, can cause the bomb to leak. If the
damage or accumulated wear is much less
than 0.001" (0.03mm), then careful
polishing will restore the bomb sealing to
an as new condition. Imperfections that
penetrate the sealing surface more than
one or two thousandths of an inch (0.03-
0.06mm) may render the seal surface
unserviceable.
Any surface that comes in contact with an
elastomer seal should be carefully
examined for imperfections that would
compromise its ability to seal. A freshly
sharpened pencil can be used to probe the
metal sealing surfaces for significant
imperfection. If the pencil point hangs up in
the imperfection, further attention is
warranted. An attempt should be made to
polish (remove) any significant
imperfections. This operation generally
requires the use of a lathe in order to
guarantee that the sealing surface to be
repaired remains concentric with the
mating surface. Knowledge of the
dimensional tolerances and the ability to
accurately measure or gauge the affected
area is required in order to insure that too
much polishing (metal removal) has not
taken place. We recommend that bombs
with significant imperfection of this nature
be serviced at Parr.
Caution!
Avoid Prying Elastomer Seals (O-Rings
and Quad-Rings) from Seal Grooves
with Metallic Tools.
The use of dental picks and other metallic
tools to pry the seals from their grooves is
strongly discouraged. These hard steel
tools, if misused, can leave permanent tool
marks on the sealing surface which are
difficult or impossible to remove. These
blemishes are hidden by the seal during
normal use and as a result, are not readily
apparent as the cause of a leaking bomb.
Larger size seals (0.8" or 20 mm O.D.),
typically used to seal the bomb head, can
be extracted from its groove using either of
the following two methods:
• Grasp the outer circumference of the
seal with the thumb and forefinger and
slide them together while applying
sufficient pressure on the seal to cause
it to pucker out of the groove. With the
other hand, grab the exposed, pinched
section and pull the seal from the
groove.
• Use a non-metallic object, such as the
rounded corner of a plastic credit card,
to simply pry the seal from its groove.
9-2
Maintenance & Troubleshooting
Smaller diameter seals usually require a
different approach. A portion of the seal
should be carefully pulled, not pried, from
the groove with a small pair of pliers or a
hemostat. The exposed portion of the seal
can then be cut, or pulled further to remove
the seal. The pliers or hemostat should
never contact the sealing surface, only the
seal.
5000 Tests - Return the oxygen bomb to
factory for hydrostatic and proof testing.
Bomb Pressure Release
The bomb exhaust and sealing is
controlled by movement of the 966DD
piston inside of the 961DD bomb
seal/release cylinder. This assembly is
mounted on the bottom of the calorimeter
air can. The piston is driven to the up
position (bomb release) by applying
oxygen to 30 atm to the 1/8 male
connector (344VB). The piston is driven
down (bomb seal) by applying pressure to
the 376VB elbow. The application of the
oxygen pressure is controlled by the
934DD two station solenoid valve. There is
a flow restrictor, 381VB (0.006) on the inlet
side of this solenoid which limits the
maximum flow rate of oxygen which in turn
creates a gradual increase in pressure at
the 961DD bomb seal/release cylinder
when the solenoid is turned on. Failure of
the bomb to exhaust in a timely fashion
can have more than one cause. Certain
causes can be eliminated systematically by
checking the bomb exhaust diffuser, at the
end of the bomb exhaust line, for any
restrictions in the six small cross drilled
holes. This fitting should be removed from
the tubing, inspected thoroughly and
cleaned as required.
9-3
Visual Confirmation of the Piston
Movement
• Remove the head and the cylinder
sealing pin (668DD) from the bottom of
the cylinder.
• From the calorimeter main menu, press
923 and YES at the warning prompt.
• Down arrow to the entry called bomb
release and turn it on by pressing YES.
• One should observe the 966DD piston
move to the up position. Press NO to
turn this output off.
• Press the down arrow key twice to
bomb seal and press YES. The 966DD
piston should now be in the down or
retracted position. Press NO to turn this
output off.
Repeat this on and off sequence for each
of the outputs as necessary in order to
confirm the correct piston movement with
no applied bomb pressure.
Keep in mind that only one of these
outputs should be on at any given time. If
both are on, the piston will default to the up
position due to the size difference and
location of the two bores in the cylinder.
Confirming Correct Operation of the
934DD Solenoid Valve Assembly
If the piston does not move it is worthwhile
at this point to confirm that both sections of
the 934DD are working properly. To do
this, remove the power cord from the rear
of the instrument and separate the rear
calorimeter cover from the unit. Locate the
934DD valve assembly on the left side of
the instrument, looking from the rear.
Disconnect the 1/8 nylon pressure hose at
the upper outlet connection using a
7/16wrench. Apply power to the unit and
re-enter the I/O diagnostics page 9.2.3.
Turn the bomb release output on. Oxygen
should flow from this upper port on the
934DD. Turn the bomb release output off
and re-connect the nylon pressure hose.
Disconnect the 1/8 nylon pressure hose at
the lower outlet connection. Activating the
bomb seal output should produce a flow of
oxygen at this lower port. Turn off the
bomb seal output and reconnect the nylon
pressure hose.
If neither solenoid produces a flow of gas
when activated and other outputs are
known to be functional, then, in all
likelihood, the 381VB flow restrictor is
plugged and should be replaced. If only
one of the solenoids sources gas when
activated, then the problem must be further
diagnosed as either being electrical (I/O
board or external wiring) vs. mechanical (in
the valve) and dealt with in an appropriate
manner.
If either solenoid sources gas when it is off
(i.e. leaks) then replacement of the entire
934DD solenoid assembly is indicated. It is
worthwhile to note that if the lower outlet
port leaks and keeps the space between
the two O-rings on the piston pressurized,
the effective upward thrust on the piston
will be diminished by 40%. In this situation,
a fully pressurized bomb will not exhaust.
For reference purposes, the normal
upward thrust generated by the 966DD
piston is 50 pounds. The downward thrust
is 20 pounds. Far less than 20 pounds are
required to move the piston in either
direction when the bomb is not
pressurized.
Servicing the O-rings
on the 966DD Piston
If both solenoid positions source gas
properly and the piston remains stationary
with no applied bomb pressure, the piston
should be extracted from the cylinder and
serviced. Turn off the oxygen service
before servicing the valve. There is a
large hole on the base of the 1281
Calorimeter that is used to provide access
to the bottom of the bomb seal/release
cylinder. Disconnect the power cord from
the unit and remove the four screws that
fasten the 962DD cover plate to the bottom
of the 961DD cylinder. Extract the piston
and carefully examine the two O-rings for
wear and/or cuts. A cut or slice, especially
on the larger seal (357HCJV) will greatly
reduce the amount of upward force which
can be generated. It is worthwhile to note
that even in the complete absence of the
smaller O-ring seal, the piston can be
moved to the up or bomb release (exhaust)
position. What this means is that the
condition of the smaller O-ring will have
nothing to do with bomb exhaust problems.
The bomb may not seal properly, but it will
exhaust. Light scoring above the smaller
O-ring (659DD) is normal as long as the
diameter of the piston, adjacent to the
smaller O-ring does not exceed 0.272.
Polishing this area with Crocus cloth, by
hand, is very effective at removing
excessive scoring. Renew the O-ring seals,
apply a light coat of silicone lubricant, and
reverse the above procedure to install the
piston. These O-ring seals should be
renewed at 500 combustion test intervals.
9-4
Maintenance & Troubleshooting
Further Troubleshooting
If the piston moves properly with no
applied bomb pressure, but still fails to
initiate an exhaust of a pressurized bomb
in a timely fashion, at least one of the
following conditions exist:
• The 381VB restrictor is partially
blocked.
• There is a gas leak between the outlet
of the solenoid and the 961DD cylinder.
This also includes the 357HCJV O-ring
seal on the piston inside of the cylinder.
The latter condition can be eliminated by
following the procedure outlined in the
section servicing the O-rings on the 966DD
piston and carefully inspecting the 1/8
nylon pressure hose and associated
compression fittings for leaks while this
circuit maintained at operating pressure,
using calorimeter the I/O diagnostics on
page 9.2.3. A minute leak will result in a
significant reduction in upward thrust.
The first condition can be eliminated by
replacing the 381VB restrict.
Filling and Exhausting the Bomb Using
the I/O Diagnostics
In order to recede the amount of time it
takes to duplicate and troubleshoot this
type of situation, the I/O diagnostics can be
used to pressurize and exhaust the bomb
without having to run lengthy combustion
or pre-tests.
• Make sure the 668DD bomb sealing pin
is installed at the bottom of the cylinder.
• Lock the head into the cylinder and
close the calorimeter lid.
9-5
• Enter the I/O diagnostics and turn lid
lock on.
• Confirm bomb release is off.
• Turn bomb seal on then off to retract
the 966DD piston.
• Turn on O2 dump to seal the vent line.
• Turn on O2 fill to begin filling the bomb.
The bomb will be completely filled in
one minute, at which time O2 fill should
be turned off. Turn off O2 dump to
exhaust the fill line. This seats the
check valve in the head which in turn
seals the contents of the bomb.
• The calorimeter lid can be unlocked at
this time.
• Activating bomb release should initiate
a bomb exhaust within two seconds. If it
takes much longer than two seconds
before the bomb begins to vent, then at
least one of the conditions outlined
under further troubleshooting exist.
• If the bomb exhaust is initiated in a
timely manner but fails to complete in
10 seconds, a blockage or restriction in
the bomb exhaust circuit is indicated.
This must be investigated and
corrected.
• If the bomb fails to exhaust, a 3/32
Allen wrench (or equivalent) should be
inserted into the center opening on the
bomb head to unseat the check valve.
Up to 50 pounds of force will be
required to unseat the check valve in a
bomb that is fully pressurized.
Hall Effect Sensor
Check/Adjustment
There is one pneumatic cylinder in the
1281 Calorimeter that locks the lid at the
beginning of a test sequence. The sensor
is used to indicate that the lid is in the
locked position. The failure of the sensor to
operate properly can result from an
electrical failure of the switch or because it
is incorrectly positioned on the pneumatic
cylinder.
Checking the Lid Lock Sensor
(A1010DD, Figure 9-4). Select 9.2.3, I/O
Diagnostics, from the Main Menu.
WARNING:
This screen allows unconditional and
arbitrary output control for testing
purposes. Be aware that all user and
instrument protection is disconnected while
on this screen. This is very important and
you should take proper pre-caution.
Press ENTER to continue or ESCAPE to
exit.
Down-arrow to “LID LOCK” and turn it on.
The input image should have an “8" in the
left most position which indicates that the
sensor is on and the lid is locked. See the
HELP screen associated with the I/O
diagnostics for this and other related input
bit assignments. If the input image shows
”0" then the sensor is not coming on. The
next section will describe how to adjust the
position of the sensor.
Sensor Alignment. Exit the I/O Diagnostic
routine. Remove the 887DD Fiberglas
calorimeter lid. Select 9.2.3 from the Main
Menu to enter the I/O Diagnostic routine
again. Turn on the lid lock output. The
sensor has a built in light which illuminates
when the switch is on. The sensor is
activated when a magnet, attached
internally to the gas cylinder piston, is
directly underneath the sensor. Loosen the
clamp with an Allen wrench and slide the
sensor and clamp as a unit to the middle of
the active magnetic area on the gas
cylinder. The light should come on and the
screen should indicate an “8" in the left
most input image position. If the sensor
light comes on but the controller diagnostic
screen does not respond correctly, the
sensor should be replaced.
The center of the active magnetic area can
be easily determined as follows:
With the sensor light on, slide the sensor
forward until the light goes off and mark
this position on the gas cylinder with a
pencil, where the top of the sensor meets
the cylinder. Then slide the sensor and
clamp back, turning the light on and then
off. Mark this lower position where the light
turns off. The center of the active magnetic
area is halfway between these two marks.
Move the top of the sensor to this midpoint
position and tighten the clamp.
After the sensor has been tightened in
place, exit the I/O Diagnostics, and reverse
the cover disassembly procedure to install
the instrument cover.
Oxygen Bomb Removal and
Replacement
To service or remove the bomb cylinder
from the bucket assembly, remove the
941DD Wedge with needle nose pliers.
Remove the 668DD Check Valve from the
bomb cylinder. Remove the two
SA1631RD018 Machine Screws (see
Figure 9-16). Then remove the 942DD
Bushings and the 1081DD Quad-ring.
9-6
Maintenance & Troubleshooting
Carefully lift the bucket and bomb
assembly out of the air chamber and
position horizontally on the calorimeter to
remove the 925DD Oxygen Bomb Retainer
Nut (see Figure 9-15). Now the A890DD
Cylinder can be removed from the bucket
assembly. Note the position of the locating
pin.
To replace follow these steps in reverse.
Parr 1281 Calorimeter Error List
Error: 40
Cold Restart - The instrument has just
completed a cold restart. All memory and
calibration data has been reset to their
default values. This could have been
caused by initial startup, disconnection of
the CPU board, or a failure of the battery
backup.
Error: 41
Low Battery Voltage - The CPU battery
backup needs replacement.
Error: 42
Mux Hardware Error, See Error 48
Error: 43
Mux Communications Error, See Error 48
Error: 44
I/O Board Not Responding, See Error 48
Error: 45
Mux Master Time-out Error, See Error 48
Error: 46
Mux Slave Time-out Error, See Error 48
9-7
Error: 47
Mux Master Communications Error, See
Error 48
Error: 48
Mux Slave Communications Error - Errors
42-48 will result in the event of faulty CPU
to I/O board communication.
Error: 56
User Defaults Bad Write, See Error 59
Error: 57
User Defaults Bad Checksum, See Error
59
Error: 58
User Defaults Out of Sync, See Error 59
Error: 59
Bad Upload Checksum - Errors 56-59 will
result if the user default setup can’t be
stored to nonvolatile memory, or has
become corrupted.
Error: 62
Bad State Value - This error will result if a
check of the input and output images
results in an ambiguous condition.
Error: 64
Open Fuse Connection - The controller has
detected an open firing circuit prior to firing
the bomb. Check and/or replace the bomb
fuse wire.

Error: 68
Pre-period Time-out - The calorimeter has
failed to establish an acceptable initial
temperature, prior to firing the bomb, within
the time allowed.
Possible causes for this error are listed
below:
• 907DD breaking (check valve head)
• Poor jacket water circulation due to a
kinked hose or insufficient water in the
tank.
• A bomb leak.
• Poor bucket stirring.
• Leaking bucket water solenoid.
• Metal to metal contact between the
bucket and the jacket.
• Lid not tight may be high in back.
Error: 70
Post-period Time-out - The calorimeter has
failed to establish an acceptable final
temperature within the time allowed.
Possible causes for this error are listed
below:
• Poor jacket water circulation due to a
kinked hose or insufficient water in the
tank.
• A bomb leak.
• Poor bucket stirring.
• Leaking bucket water solenoid.
Error: 72
Run Aborted - This message is issued if
the operator presses the RESET key while
a test run is in progress.
Error: 76
O2 Bad Pressure Sensor - The oxygen
pressure switch was found to be closed
prior to filling the bomb. Replace the
pressure switch.
Error: 78
O2 Low Pressure - The oxygen filling
system was unsuccessful in filling the
bomb to the minimum required pressure,
400psig. This indicates low pressure in the
filling tank, a leak in the bomb or in some
other part of the filling system. Check
659DD on 966DD Release.
Error: 80
O2 Leak - The controller has detected a
leak in the oxygen bomb prior to entering
the pre-period. Check and/or replace all
bomb related pressure seals.
Error: 82
H2O Fill Time-out - The calorimeter has
failed to establish an acceptable initial
temperature (29.5 to 30.5), prior to entering
pre-period, within the time allowed. Check
the water level in the calorimeter jacket
and the internal water filter, or possible
kinked tubing.
Error: 84
Cool Down Time-out - The calorimeter has
failed to establish the desired cool down
temperature within the time allowed. The
water cooler may not be functioning or the
flow rate of cold water may not be
sufficient.
Check the water cooler, the level of water
in the calorimeter jacket, and the internal
water filter.
Error: 86
Drain Time Out
Maintenance & Troubleshooting
Error: 102
Run in Progress - An attempt was made to
start a test run or perform diagnostics while
a test run is in progress.
Error: 104
Tank - Low Water Level - The water tank in
the calorimeter needs refilling. This error
also results in the pump and heater being
turned off.
Error: 106
Motor Over Current - The stirrer motor is
drawing too much current from its power
supply. Check to see that the motor shaft
turns freely.
Error: 108
Bomb Firing Count Exceeds Limit - The
calorimeter controller keeps track of how
many times the bomb has been fired.
When this count exceeds a preset limit
(usually 500) this message will be issued
each time the bomb is used for a test.
Perform bomb maintenance and reset
counter on Menu Page 4 for appropriate
bomb number.
Error: 113
Bomb 1 EE Std. Dev. Exceeds Limit, See
Error 116
Error: 114
Bomb 2 EE Std. Dev. Exceeds Limit, See
Error 116
Error: 115
Bomb 3 EE Std. Dev. Exceeds Limit, See
Error 116
Error: 116
Bomb 4 EE Std. Dev. Exceeds Limit - The
relative standard deviation for the
calibration runs in memory for the indicated
bomb exceeds the preset limit.
Error: 117
Temperature Rise Exceeds Limit - The
temperature rise of the test exceeded the
warning limit. This indicates that the
maximum loading limit of 8000 calories has
been exceeded.
Error: 119
Heater and Pump are OFF - An attempt
was made to start a test run without the
water circulating pump and heater being
turned on.
Error: 121
Jacket Temperature out of Tolerance - A
test run can’t be started unless the jacket
temperature is within the range of 29.5 to
30.5C.
Error: 123
Jacket Temperature Exceeds Limit - The
jacket temperature has exceeded the high
limit value of 40C. This usually indicates a
problem with the heater control circuitry.
Error: 126
S-Record: Bad Record Number
Error: 127
S-Record: Bad Byte Count
Error: 128
S-Record: Bad Address
9-8
Error: 129 Error: 138

S-Record: Bad Data Spike Weight Already Entered

Error: 130 Error: 139

S-Record: Bad Checksum Acid Value Already Entered

Error: 131 Error: 140

Bad Remote Data Request Sulfur Value Already Entered

Errors 126-131 Error: 141

Will be issued if information downloaded to Hydrogen Value Already Entered - An

the memory of the Controller CPU is attempt was made to re-enter a value
determined to be invalid during the which is already present in the test report.
download procedure.
Error: 142
Error: 132
Balance - Data is Not (0-9,+,-,e,E)
Weight Not Found
Error: 143
Error: 133
Balance - Data Does Not Match Template
Spike Weight Not Found
Error: 144
Error: 134
Balance - Data is Unstable
Acid Value Not Found
Error: 142 – 145
Error: 135
Balance - Weight is Negative - These
Sulfur Value Not Found errors will result during a balance transfer if
the datum is not within the expected range
Error: 136 or can’t be interpreted properly

Hydrogen Value Not Found - The controller Error: 146

has not found the desired datum for the
sample ID entered. This error results
during a Smart-Link transfer if the datum or
ID can’t be located on the Smart-Link
network.
Error: 137
Invalid Password - This error will result if
an incorrect password is given at a prompt
for a password. If the password is
forgotten, the entire CPU program will
need to be reloaded.

Weight Already Entered

9-8
Maintenance & Troubleshooting
Error: 149
Password Protected - This error will result
if an attempt is made to access a menu
that has been password protected.
Error: 150
Weight is Zero - A sample mass of zero is
not an allowed value.
Error: 163
Cool Down Set Point Low Limit
Error: 165
Cool Down Set Point High Limit
Error: 166
The bomb cool down set point is
dynamically adjusted during each test to
minimize the time the calorimeter spends
in pre-period. An error will result if this
incremental adjustment process results in
a cool down set point outside the range of
20 to 40C.
Error: 168
Run List Erased - The stored test data run
list has been deleted and reinitialized. This
error will occur as a result a loss of battery
backup to the CPU board.
Error: 169
Run List Modified - On power up, the CPU
scans the run list and validates each run
area. This error will result if one or more of
these areas is found to be corrupted.
Corrupted run areas are cleared.
9-11
Error: 170
Run List Full - This error will be issued
when the memory set aside for test runs is
exhausted. The operator must either clear
space in the memory or enable automatic
overwriting of the oldest FINAL report.
Error: 171
Duplicate Sample ID - This error will be
generated if an attempt is made to use an
ID number that already exists in the
memory of the controller.
Error: 172
Sample ID Not Found - This error will be
generated during the reporting or clearing
of memory if the requested ID can’t be
found.
Error: 173
Bad Bomb ID - This error will be issued if a
bomb ID outside the range of 1-4 is given
at the prompt for a bomb ID.
Errors: 174 - 182
Will result if the controller encounters an
error during a Smart Link transaction. The
specific type of error may be useful in
determining the exact nature of the fault.
Error: 174
Smart Link - Master Arbitration Error
Error: 175
Smart Link - Slave Arbitration Error
Error: 176
Smart Link - Bad Packet Checksum
Error: 177 the cause of the problem (probe or
electronics). The valid working range of
Smart Link - Unit Did Not Respond probe resistance is 1000 to 5000 ohms.

Error: 178 Error: 191

Smart Link - Output Buffer Overrun RTS/CTS Handshake Error, See Error 194

Error: 179 Error: 192

Smart Link - Slave Release Time-out Transmitter Error, See Error 194

Error: 180 Error: 193

Smart Link - Master Release Time-out Receiver Error, See Error 194

Error: 181 Error: 194

Smart Link - No Data Available Corrupted Data - These errors will result if
the controller detects an error during a
Error: 182 serial communication exchange.

Smart Link - No Response Error: 195

Error: 183 Refill Bomb Rinse Tank - The controller

decrements the rinse tank counter each
Shorted Bucket Probe time the bomb is rinsed. This message will
be issued when the counter is at or below
Error: 184 zero when the bomb rinse sequence is
executed. This message is a reminder that
Shorted Jacket Probe the rinse tank needs refilling, followed by a
manual resetting of the bomb rinse
Error: 187 counter.

Open Bucket Probe - 1416E left side of Error: 197

bucket at bottom:
Data Log Buffer Full - This message is
• Check Connection to board. issued when RAM allocated for
• Check quick disconnect. data/process logging is exhausted. Any
• Replace probe. logging in progress is halted.

Error: 188 Error: 198

Open Jacket Probe - These errors will Master Transmitter Error

result if the temperature probe response is
not within the expected range. Probe
substitution can be useful in determining

9-12
Maintenance & Troubleshooting
Error: 199
Slave Transmitter Error
Error: 200
Master Receiver Error
Error: 201
Slave Receiver Error
Error: 202
Master to Slave Busy Error
Error: 203
Slave to Master Busy Error
Error: 198 – 204
These errors are hardware level Smart
Link fault messages.
Error: 206
Factory Defaults Bad Checksum, See
Error 207
Error: 207
Factory Defaults Out of Sync - One of
these errors will be generated when an
attempt is made to reload the factory
defaults, and a check indicates that the
factory defaults are not valid.
Error: 208
Edit Final NOT Enabled - An attempt was
made to edit a final report.
Error: 209
Divide by Zero Error - The controller
attempted to do a mathematical calculation
with a divisor of zero.
9-13
Error: 240
Lid Failed to Lock - The sensor used to
indicate that the calorimeter lid is in the
locked position failed to show a closed
condition within the required time period.
The lid may not be firmly pressed to the
closed position at the start of the test, the
nitrogen pressure may be too low to
properly activate the lid lock air cylinder, or
the sensor may be bad or mis-adjusted.
Error: 242
Solenoid in Over Current - Each solenoid
driver stage is overload protected, and has
the ability to detect intermittent connections
when the output is active. If either of these
situations are present, this message is
generated along with an indication of the of
the defective output.
Error: 245
Misfire - Fuse Burned, See Error 247
Error: 246
Misfire - Fuse Intact, See Error 247
Error: 247
One of these errors will be generated, in
the event the total temperature rise fails to
exceed 0.5 C after the first minute of the
post-period. The qualifier “Fuse Intact”
indicates ignition circuit continuity, and
“Fuse Burned” indicates an open circuit. In
either event, the test run is aborted. If
when the bomb head is extracted, the
auxiliary cotton thread is gone, the thread
simply failed to ignite the sample. In most
cases, the sample can be re-run with a
new thread. If the thread is present, make
sure it is dry.
If it is wet, replace it and re-run the sample
if no sample has adhered to the wet
thread. If the thread is dry, it is best to
check and/or change the metal heating
wire.

Error: 250

Hyper-link Slave Failed to Start

Error: 251

Hyper-link Slave Command Time-out

Error: 252

Hyper-link Slave Bad Initialization - These

errors will result if the CPU detects faulty
communication between the the CPU and
the I/O board.

Error: 260

IO Download: Bad Record Count

Error: 261

IO Download: No Response

Error: 262

IO Download: Transfer Failed - These

errors result if the CPU fails to initialize the
I/O board during power up.

9-14
Maintenance & Troubleshooting

9-15
9-16
Maintenance & Troubleshooting

9-17
9-18
Maintenance & Troubleshooting

Figure 9-5
1281 Solenoid Wiring Diagram

9-19
9-20
Maintenance & Troubleshooting

9-21
 Figure 9-8
A1013DD Valve Assembly

9-22
Maintenance & Troubleshooting

9-23
 Figure 9-10
A1012DD Solenoid Valve Assembly

9-24
Maintenance & Troubleshooting

Figure 9-11
A1014DD Water Solenoid Assembly

9-25
9-26
Maintenance & Troubleshooting

9-27
Tubing OD Tubing Total
No. Size Part No. Length (in) Notes
1 .562 JT0056TB062A 2.5
2 .375 JT0038TB062A 23.0
3 .375 JT0038TB062A 19.0
4 .375 JU0038TB062A 23.0 Use 379E Cable Tie
5 .562 JT0056TB062A 2.5 Use 998DD Hose Clamp
6 .562 JT0056TB062A 1.75 Use 998DD Hose Clamp
7 .375 JT0038TB062A 16.0

9 .375 JT0038TB062A 16.0

10 .375 JT0038TB062A 6.0 Use 379E Cable Tie
11 .125 HA0012TB031 6.0
12 .375 JT0038TB062A 13.0
13 .375 JU0038TB062A 7.0 Use 183VB Tubing Insert
14 .375 JU0038TB062A 8.5 Use 183VB Tubing Insert
15 .375 JU0038TB062A 24.0 Use 379E Cable Tie
16 .125 HX0012TB024 16.0
17 .375 JT0038TB062A 7.5
18 .250 HV0025TB065 13.0
19 .125 HX0012TB024 12.0
20 .125 HX0012TB024 12.0

22 .125 HX0012TB024 5.0

23 .125 HX0012TB024 8.0
24 .125 HX0012TB024 7.0
25 .125 HX0012TB024 9.0
26 .562 JT0056TB062A 14.0

9-28
Maintenance & Troubleshooting

9-29
9-30
Maintenance & Troubleshooting

Figure 9-17
1281 Air Can Assembly

9-31
9-32
Appendix A – Menu Operating Instructions
When the START key is pressed, the
calorimeter will prompt the user for the
Sample ID number. If the automatic
Sample ID is turned ON, the next sample
will be displayed and if it is correct, press
ENTER. If it is not correct, press CLEAR
ENTRY and key in the correct identification
number followed by ENTER. The
instrument will then prompt for sample
weight, if set up for keyboard entry. Again,
key in the weight followed by ENTER. If the
weight is set up for automatic transfer, the
value will be displayed and entered
directly. Spiking, if activated, is entered the
same as the sample weights.
The settings and controls are organized
into nine main sections or pages which
comprise the Main Menu. This appendix
describes all pages of the menu-based
operating system of the 1281 Calorimeter.
Calorimeter Operation
Page 1
The calorimeter will normally be operated
from Page 1, although tests can be started
from many Main Menu pages. The number
of free areas in the memory and the
number of rinses left in the wash tank are
always displayed at the top of this page.
At the bottom of the page is a “status bar”.
This bar provides the current status of the
calorimeter and a graphical representation
of where the instrument is in its operating
cycle.
Line 1 - Operating Mode. Sets the
operating mode by toggling between
standardization and determination.
A-1
Line 2 - Bomb Installed/EE. Used to
identify the bomb presently installed in the
calorimeter and its EE value.
Note:
The heater and pump must be turned ON
to bring jacket to the correct starting
temperature before testing can commence.
Operating Controls
Page 2
Line 1 - Method of Operation. Offers an
operating mode of either dynamic or
equilibrium. In most cases, the dynamic
mode with its curve matching capability will
save approximately 3-4 minutes per test
and will produce the same operating
precision as the slower equilibrium mode.
Line 2 - Reporting Units. Offers a choice
of Btu/lb, Cal/g, J/kg or MJ/kg for the
reporting units.
Line 3 - Use Spiking Correction.
Accesses sub-menu, Page 2.3 - Spiking
Controls. Spiking is the material addition,
such as benzoic acid or mineral oil, to
samples which are difficult to burn in order
to drive the combustion to completion.
Spike Controls
Page 2.3
Line 1 - Use Spiking. When set to
ON, the calorimeter will prompt for
the weight of the spike added and
will compensate for the heat of
combustion in the calculations.
Line 2 - Heat of Combustion of
Spike. The heat of combustion of
spike is entered here, Cal/g.
 Line 3 - Use Fixed Spike. When set
to ON, a constant amount of spike is
to be added to each test.
Line 4 - Weight of Fixed Spike. The
weight of the fixed spike is entered
here. Normally the calorimeter will
prompt the user for the weight of the
sample and then the weight of the
spike.
Line 5 - Prompt for Spike before
Weight. When set to ON, the above
sequence will be reversed.
Note:
The precision of tests with fixed spikes can
be no better than the repeatability of the
spike weight.
Line 4 - Bomb Rinse Tank Controls.
Accesses sub-menu, Page 2.4 - Bomb
Rinse Tank Control. Wash water for the
bomb is drawn from the 1575 Bomb Rinse
Tank. Users who wish to collect the bomb
washings for acid titrations or further
analysis will want to fill it with distilled or
other suitable water.
Bomb Rinse Tank Control
Page 2.4
Line 1 - Use Bomb Rinse Tank.
ON/OFF toggle for the bomb rinse
tank. A full tank will contain enough
rinse water for approximately 150
tests.
Line 2 - Rinse Tank Capacity. Sets
the number of tests available from a
tank refill. If rinse timing controls
have been changed, then the value
must be changed proportionally.
Line 3 - Reset Rinse Tank Counter.
Resets the counter when the rinse
tank has been refilled. This counter
must be reset after the rinse tank is
refilled. Line 4 - Not used.
Line 5 - Rinse Timing. Accesses
sub-menu, Page 2.4.5 - Rinse
Timing. Keeps track of the number
of times the rinse, flush, clear and
rinse cycles are run and informs the
user when the tank needs to be
refilled.
Rinse Timing
Page 2.4.5
Line 1 - Rinse Time(s). This value
establishes the time that the rinse water
solenoid is turned ON for each rinse cycle.
When the rinse water solenoid is ON,
distilled water from the rinse tank is forced,
under pressure, into the bomb cylinder.
This rinses the cylinder walls and the bomb
head. These rinsings are then pooled and
collected at the exhaust port of the
calorimeter. The factory default value is 3s.
This value, along with the # of rinse cycles,
determines the total volume of recovered
rinsings. These default values will yield a
total of 50 ml (approx.) at bomb washings.
Line 2 - Rinse Flush Time(s). This
value is used to establish a time
between rinse cycles. During this
time the rinse solenoid is turned
OFF. This off time permits the rinse
water to drain out before the next
rinse cycle begins. The factory
default value is 1s.
Line 3 - Clear Time(s). This time
value is used to establish a post-
rinse oxygen filling time for the
bomb. This step is used to clear the
lines and valves of any residual
rinse water prior to the next test.
The factory default value is 10s.
A-2
Appendix A – Menu Operating Instructions
Line 4 - # of Rinse Cycles. This
value establishes the number of
distinct rinse cycles used to rinse
the bomb. The factory default value
is 3 rinse cycles.
Line 5 - Other Multiplier
Line 6 - LCD Contrast. Controls the liquid
crystal display on the calorimeter. The
number entered sets the back lighting
intensity in values between 1 and 100.
Higher numbers provide brighter back
lighting. Most users will want to set to 100
for maximum back lighting.
Line 7 - LCD Backlight Time-out. The
unit is equipped with an automatic circuit to
shut-off the backlight when it is not being
used. The back light will shut-off if there is
no keyboard activity for the number of
seconds entered. Pressing any key will
automatically turn the back lighting ON. A
setting of 0 will keep the backlight ON at all
times.
Line 8 - Print Error Messages. When
turned ON, all error messages will be
printed on the printer and displayed on the
screen.
Line 9 - Display Stored Samples.
Displays a listing of all Sample ID’s stored
in the memory of the calorimeter.
Line 0 - Language Options are English or
German.
Program Information
and Control
Page 3
Line 1 - Date. Used to enter the current
date.
A-3
Line 2 - Time. Used to enter the current
military time.
Line 3 - Software Version. Displays the
current version of software installed in the
calorimeter.
Line 4 - User Setup ID. Displays the last
user entered ID number for the setup
stored in the calorimeter.
Line 5 - Factory Hardware Version.
Displays the current version of hardware
installed in the calorimeter.
Line 6 - Password Protection. Provides
password protection for the program
options and settings on the menus. If this
feature is turned ON, the user will be
prompted for a number, up to six digits
long, which will be the password for all
protected settings. Once protected, any
attempts to change a setting will be met
with a prompt for the password. The
program revision will only be made after
the correct password has been entered. If
access is required to sensitive areas
protected by password and the password
is not known, new Eproms will be required.
Line 7 - Re-load Factory Default
Settings. Used to erase all of the settings
and restore the factory default settings.
Line 8 - Re-load User Default Settings.
Used to restore the user’s setup should the
program in the instrument be corrupted for
any reason.
Line 9 - Copy Current Setup to Memory.
Used to record the setup to the memory
once the user has configured the
instrument to their operating requirements.
Note:
Lines 6 thru 9 make global changes to the
setup of the calorimeter and, therefore,
contain a YES or NO response to make
certain that the user wishes to proceed.
This two step entry is intended to prevent
inadvertent global program changes.
Line 0 - Cold Restart. Returns the
instrument to its initial state. It will re-load
from the memory the user’s setup if it was
saved using Line 9 - Copy Current Setup to
memory, and all valid test data will be
retained during this cold restart procedure.
Otherwise the instrument will return to the
factory default settings.
Calibration Data and Controls
Page 4
Line 1 - Calibration Run Limit.
Establishes the maximum number of runs
that will be included in determining the EE
value of a bomb and bucket combination.
Most test methods suggest 10 tests. If
more than the set maximum are present,
the most recent tests will be used; if fewer
than the limit are present, all available tests
will be used.
Line 2 - EE Max Std Deviation.
Establishes the maximum relative standard
deviation in percent that will be permitted
for any EE value calculated by the
calorimeter. If this value is exceeded, the
user will be warned to take corrective
action before proceeding with testing. This
calorimeter is capable of achieving a value
of .15 or better.
Line 3 - Heat of Combustion of
Standard. Contains the heat of
combustion in calories per gram for the
material used to standardize the
calorimeter. For benzoic acid, this value is
6318 calories per gram.
Line 4 - Bomb Service Interval.
Establishes the maximum number of times
a bomb may be fired before it is flagged as
due for service.
Line 5 - Use Bomb. Used to enter the
bomb number of the bomb currently
installed in the calorimeter. The left and
right arrow keys are used to toggle through
the bomb identification numbers available
for each bomb.
Line 6 - Not used.
Line 7 - Bomb 1. Leads to sub-menu,
Page 4.7 - Bomb 1. Contains the
standardization information for bomb and
bucket combinations. While only one bomb
and bucket is installed in the calorimeter at
a time, a spare may be used for servicing
and the respective EE values for each
bomb can be stored in memory.
For rapid turn around between tests, user
may wish to use two bomb heads on the
cylinder installed in the calorimeter. Each
head and cylinder combination can be
assigned a bomb number if the EE Values
are significantly different. Use Page 1, Line
2 to enter the bomb combination being
used in the test before the test is started,
or set prompt for bomb ID to “ON”.
A-4
Appendix A – Menu Operating Instructions
Bomb 1
Page 4.7
Line 1 - EE Value. Contains the
calculated EE value for the
corresponding bomb.
Line 2 - Protected EE Value. When
set to ON, protects the EE values if
the user does not wish to have the
calorimeter automatically update its
own EE value. Enter into Line 1 the
determined EE value and it will not
change unless revised through the
keyboard.
Line 3 - Number of Runs. Shows
how many runs have been used to
determine the EE value.
Line 4 - Relative Standard
Deviation. Reports the relative
standard deviation for the series of
tests used to determine the current
EE value.
Line 5 - Bomb Firing Count.
Contains the current bomb firing
count or the number of times the
bomb has been fired since it was
last serviced. When this count
matches the limit set on Page 4 -
Calibration Data & Controls, Line 4 -
Bomb Service Interval, the user will
be informed that the bomb is ready
for service.
Line 6 - Print Standardization Runs.
Will print all of the tests that have
been incorporated into the
calculated EE value. This will be
helpful in evaluating a series of tests
which fail to produce a satisfactory
EE value and relative standard
deviation.
A-5
Line 7 - Update Statistics. This code
will cause the EE Value for this
calorimeter ID to be updated using
all standardization runs currently in
memory. (5)
Line 8 - Bomb 2. Accesses sub-menu,
Page 4.8 - Bomb 2. Provides the same
controls as Page 4.7 - Bomb 1, Lines 1-7.
Line 9 - Bomb 3. Accesses sub-menu,
Page 4.9 - Bomb 3. Provides the same
controls as Page 4.7 - Bomb 1, Lines 1-7.
Line 0 - Bomb 4. Accesses sub-menu,
Page 4.0 - Bomb 4. Provides the same
controls as Page 4.7 - Bomb 1, Lines 1-7.
Thermochemical Calculations
Page 5
Note:
To access the numeric field from the
ON/OFF toggle position, press the SKIP
key. The SKIP key will also return you to
the ON/OFF choices.
Line 1 - Fixed Fuse Correction
(Standardization). Turns ON/OFF the
fixed fuse corrections for standardization
runs. The actual fixed correction for this
value is entered in the second data field.
Line 2 - Fixed Acid Correction
(Standardization). Turns ON/OFF the
fixed acid corrections for standardization
runs. The actual fixed correction for this
value is entered in the second data field.
Line 3 - Fixed Sulfur Correction
(Standardization). Turns ON/OFF the
fixed sulfur corrections for standardization
runs. The actual fixed correction for this
value is entered in the second data field.
Line 4 - Fixed Fuse Correction
(Determination). Turns ON/OFF the fixed
fuse corrections for determination runs.
The actual fixed correction for this value is
entered in the second data field.
Line 5 - Fixed Acid Correction
(Determination). Turns ON/OFF the fixed
acid corrections for determination runs.
The actual fixed correction for this value is
entered in the second data field.
Line 6 - Fixed Sulfur Correction
(Determination). Turns ON/OFF the fixed
sulfur corrections for determination runs.
The actual fixed correction for this value is
entered in the second data field.
Note:
When fixed corrections are turned ON, the
value in the attached field will be used in
both the preliminary and final reports. The
calorimeter will not prompt for actual
corrections. If all corrections are fixed, then
preliminary and final reports will be
identical. If values for these corrections are
entered into these lines, and the toggle is
set to OFF, then the fixed value will be
used in the preliminary report, but not in
the final report.
Line 7 - Calculation Factors. Accesses
sub-menu, Page 5.7 - Calculation Factors
which sets a number of options for the way
the thermochemical corrections are
applied.
Calculation Factors
Page 5.7
Line 1 - Acid Value is Nitric Acid
Only. When set to ON, the acid
value is nitric acid only. When set to
OFF, it represents both nitric and
sulfuric acid.
Line 2 - Acid Multiplier. The
multiplier is the normality of the
sodium carbonate used to titrate for
the acid correction.
Line 3 - Sulfur Value is Percent.
When set to ON, the sulfur value is
being entered as weight percent
sulfur. If another system is to be
used, this must be turned OFF and
the sulfur multiplier on Line 4 set
accordingly.
Line 4 - Sulfur Multiplier. Values
entered by the user to be used for
the sulfur correction are multiplied
by this value to get the product into
units of milliequivalents. The default
number here requires that the sulfur
value be entered in weight percent.
Line 5 - Fuse Multiplier. The fuse
corrections represent the number of
calories liberated by the burning
thread used to ignite the sample. If
another measurement is used, the
correction factor must be entered
here.
Line 6 - Use Offset Correction (ISO).
The thermochemical calculations
used for treatment of nitric acid and
sulfuric acid corrections in the ISO
and B. S. methods require an offset
correction to compensate for the
back titravtion that is made. To use
these calculations, set to ON and
enter the appropriate value on
Line 7.
Line 7 - Offset Value. Entry for the
value when Line 6 above is turned
ON.
A-6
 Appendix A – Menu Operating Instructions
Line 8 - Calculate Net Heat of
Combustion. Turns ON/OFF the
calculations for the net heat of combustion
for materials with significant hydrogen
content. When set to ON, the calorimeter
will prompt for hydrogen content during the
reporting data entry steps.
Data Entry Controls
Page 6
Line 1 - Weight Entry Mode. This data
field contains options for entering the
sample weight through the keyboard,
instruments connected via the Smart Link
port or through the balance port
connection.
Line 2 - Spike Weight Entry Mode. This
data field contains options for entering the
spike weight value through the keyboard,
instruments connected via the Smart Link
port or through the balance port
connection.
Line 3 - Acid Entry Mode. This data field
contains options for entering the acid
correction value through the keyboard,
instruments connected via the Smart Link
port or through the balance port
connection.
Line 4 - Sulfur Entry Mode. This data field
contains options for entering the sulfur
correction value through the keyboard,
instruments connected via the Smart Link
port or through the balance port
connection.
Line 5 - Hydrogen Entry Mode. This data
field contains options for entering the
hydrogen content for calculating the net
heat of combustion through the keyboard,
instruments connected via the Smart Link
port or through the balance port
connection.
A-7
Line 6 - Prompt for Bomb ID. In the ON
position the controller will prompt for a
Bomb ID(1-4) when a test is started.
Line 7 – Long Sample ID. Long sample
ID = can be entered, ie. XXXXXX.XXX 6
digits must precede the decimal.
Line 8 - Automatic Sample ID Increment.
Establishes the increment between sample
number. (1 = 1, 2, 3; 10 = 10, 20, 30)
Line 9 - Automatic Sample ID Controls.
Displays the next Sample ID which will be
assigned and is used to enter the
beginning Sample ID of any series. The
user can always override the automatic
Sample ID by entering the desired no. and
pressing ENTER.
Line 10 – Auto Controls Preweigh.
Accesses sub-menu, Page 6.9 - Preweigh
Sample ID Controls used to automatically
assign Sample ID numbers when a series
of samples are preweighed ahead of the
time they are actually tested.
Preweigh Sample ID Controls
Page 6.9
Line 1 - Automatic Preweigh ID.
ON/OFF toggle for this feature.
Line 2 - Automatic Preweigh ID
Increment. Establishes the
increment between samples.
Line 3 - Automatic Preweigh ID
Number. Shows the next Sample ID
which will be assigned and is used
to enter the beginning Sample ID of
any series.
Reporting Controls
Page 7
Line 1 - Printer Controls. Accesses sub-
menu, Page 7.1 - Printer Type which
contains the printer selection and controls.
Printer Controls
Page 7.1
Line 1 - Printer Type. Toggles
between a Parr 1756 and a generic
printer. When set for the 1756
Printer, all of the features of this
printer, such as red/ black printing,
will be activated.
Line 2 - Printer Connection. Sets the
printer location. The printer can be
connected directly to the printer port
or to another device connected via
the Smart Link.
Line 3 - Remote Printer Unit ID (0-
15). If printer is attached to another
device on the Smart Link, the
address of the device must be
entered here.
Line 4 - Report Width. The column
width of the printer being used can
be set to 20, 40 or 80.
Line 2 - Report Destination. Directs the
reports to the Printer Port, the Smart Link
Port, Display or Null Device.
Line 3 - Automatic Reporting.
Preliminary reports will be generated at the
conclusion of the test and final reports will
be generated as soon as all of the
thermochemical corrections are available
when this automatic reporting feature is
turned ON. When this is turned OFF,
reports will only be generated through the
reporting controls.
Line 4 - Individual Reports. When set to
ON, will generate header information for
each report printed. In the OFF position,
only one header will be printed for a series
of tests.
Line 5 - Report Format. Offers a choice of
text or data for the report format. The data
format is intended for rapid transmission to
an attached computer.
Line 6 - Overwrite Final Reports.
Establishes what the calorimeter will do
when its memory is full of tests. In the ON
position it will automatically erase the
oldest test and replace it with the new one.
In the OFF position it will not proceed until
the user has cleared memory space using
the memory management system.
Lines 7 - Edit Final Reports. When set to
ON and F3 is pressed, enables the user to
revise sample weight and thermochemical
corrections.
Line 8 - Recalculate Final Reports. When
set to ON, causes a recalculation of stored
final reports using calibration data and
menu settings currently in the calorimeter.
Line 9 - Use New EE Value in
Recalculation. When set to ON, the
recalculation made on Line 8 will use the
most recent EE value in the calculations. In
the OFF position, all calculations will be
made using the EE value which was
effective when the test was originally run.
A-8
Appendix A – Menu Operating Instructions
Communication Controls
Page 8
Line 1 - Smart Link Controls. Accesses
sub-menu, Page 8.1 - Smart Link Controls
which set the unit ID, baud rate and report
type.
Smart Link Controls
Page 8.1
Line 1 - Smart Link Unit ID (0-15).
Sets the Smart Link address. If only
one calorimeter is installed on the
link, the address is 0. If more than
one is installed refer to the Smart
Link instructions in Appendix D.
Line 2 - Smart Link Baud Rate. Sets
the baud rate. Smart Links normally
run at 9600 baud unless unusual
circumstances dictate slower
speeds.
Line 3 - Smart Link Report Type.
Toggles between short report and
long report.
Line 2 - Printer Port (RS232). Accesses
sub-menu, Page 8.2 - Printer Port
Communications.
Printer Port Communications
Page 8.2
Line 1 - Number of Data Bits.
Standard options for data bits.
Toggles between 7 and 8.
Line 2 - Parity. Standard options for
parity. Choose from None, Odd,
Even, Mark or Space.
Line 3 - Number of Stop Bits.
Standard options for stop bits.
Toggles between 1 and 2.
A-9
Line 4 - Handshaking. Standard
options for handshaking. Choose
from Xon/Xoff, RTS/CTS and None.
Line 5 - Baud Rate. Standard
options for baud rate. Choose from
9600, 4800, 2400, 2000, 1800,
1200, 600, 300, 150, 134.5, 110, 75
and 19.2K.
Line 3 - Balance Port (RS232). Accesses
sub-menu, Page 8.3 - Balance Port
Communications. Sets the communication
parameters for the RS232 ports used for a
balance port. Standard options for data
bits, parity, stop bits, handshaking, baud
rate and balance type are provided to
match any devices that might be
connected to these ports.
Balance Port Communications
Page 8.3
Line 1 - Number of Data Bits.
Standard options for data bits.
Toggles between 7 and 8.
Line 2 - Parity. Standard options for
parity. Choose from None, Odd,
Even, Mark or Space.
Line 3 - Number of StopBits.
Standard options for stop bits.
Toggles between 1 and 2.
Line 4 - Handshaking. Standard
options for handshaking. Choose
from Xon/Xoff, RTS/CTS and None.
Line 5 - Baud Rate. Standard
options for baud rate. Choose from
9600, 4800, 2400, 2000, 1800,
1200, 600, 300, 150, 134.5, 110, 75
and 19.2K.
Line 6 - Balance Type. Choose from
Mettler 011, Mettler 03, Sartorious,
Ohaus or Generic.
Line 4 - Terminal Port (RS232). Accesses
sub-menu, Page 8.4 - Terminal Port
Communications. Sets the communication
parameters for the RS232 ports used for a
terminal port. Standard options for data
bits, parity, stop bits, handshaking, baud
rate, terminal type and remote terminal are
provided to match any devices that might
be connected to these ports.
Terminal Port Communications
Page 8.4
Line 1 - Number of Data Bits.
Standard options for data bits.
Toggles between 7 and 8.
Line 2 - Parity. Standard options for
parity. Choose from None, Odd,
Even, Mark or Space.
Line 3 - Number of Stop Bits.
Standard options for stop bits.
Toggles between 1 and 2.
Line 4 - Handshaking. Standard
options for handshaking. Choose
from Xon/Xoff, RTS/CTS and None.
Line 5 - Baud Rate. Standard
options for baud rate. Choose from
19.2k, 9600, 4800, 2400, 2000,
1800, 1200, 600, 300, 150, 134.5,
110, and 75.
Line 6 - Terminal Type. Standard
options for terminal. Choose from
ADM-31 or VT100.
Line 7 - Remote Terminal. When set
to ON, a remote terminal can be
used for diagnostic purposes.
Diagnostics
Page 9
Provides the user with the means to test
many of the components and subsystems
of the calorimeter. These capabilities must
be used in conjunction with the
Maintenance Instructions, Chapter 9, to
obtain the maximum benefits from these
capabilities.
Line 1 - Self-Test. Initiates a test of first
the ROM and then the RAM section of the
calorimeter controller. A message line at
the bottom of this test screen reports
whether each section passed this test.
Line 2 - I/O Diagnostics. Accesses sub-
menu, Page 9.2 - I/O Diagnostics. Allows
the user to test the ignition circuit, pump
motor and the input/output drivers in the
Calorimeter.
I/O Diagnostics
Page 9.2
Line 1 - Activate Ignition Circuit.
Activates the ignition circuit. A volt
meter can be placed across the
firing connections on the cover plate
assembly to ensure that the actual
firing charge is reaching these
contacts.
Line 2 - Motor Diagnostics.
Accesses sub-menu, Page 9.2.2 -
Motor Diagnostics. Selects the
pump motor test routines and offers
the user the opportunity to test the
motor in all four of its operating
modes.
A-10
Appendix A – Menu Operating Instructions

Line 3 - I/O Driver Diagnostic. Leads Line 6 - EEPROM Up/Down Load.

to sub-menu, Page 9.2.3 - I/O
Diagnostics. This is a very valuable
diagnostic tool which lets the user
step through all of the inputs/outputs
and manually turn them ON/OFF to
confirm that they are working
properly or to locate operating
problems. At the top of this page will
be listed the current I/O function to
be tested. The YES/NO keys are
used to turn this function ON or
OFF. The UP and DOWN arrow
keys are used to scroll through the
I/O functions to be tested.
Supplemental diagnostic information
is shown on the lower section of
these screens. Use the help screen
to view the bit definitions of the I/O
functions.
Line 3 - Thermometry Diagnostics.
Accesses sub-menu, Page 9.3. The user
can use this page to confirm that valid
temperature values are being generated by
the bucket and jacket thermistors.
Line 4 - Communication Diagnostics.
Primarily for factory testing and will not be
useful to most users, unless special
diagnostic equipment is used.
Primarily for factory testing and will not be
useful to most users, unless special
diagnostic equipment is used.
Line 7 - Basic Calorimeter Functions.
Accesses sub-menu, Page 9.7 - Basic
Calorimeter Functions.
Basic Calorimeter Functions
Page 9.7
Line 1 - Rinse Bomb. Will rinse the
bomb.
Line 2 - Pretesting Cycle. Will run
the bomb through its full pretest
cycle to ensure that all systems are
functioning and have reached
operating equilibrium. This pretest
cycle can also be initiated by
pressing the F2 key.
Line 8 - Data Logger Menu. Primarily for
factory testing and will not be useful to
most users, unless special diagnostic
equipment is used.
Line 9 - Print Error List. Provides a list of
all error messages.

Line 5 - Keyboard Diagnostics. Accesses

sub-menu, Page 9.5 - Keyboard
Diagnostics.

Keyboard Diagnostic
Page 9.5

Displays a diagram of the controller

keyboard. When a key is pressed,
its corresponding block on the
display will turn dark to confirm that
the key is actually working. To
return to Page 9, the ESCAPE key
must be pressed two times (once to
test and a second to ESCAPE).

A-11
A-12
Appendix B – Calculations
Appendix B - Calculations
Calculating the Heat of
Combustion
The 1281 Calorimeter will automatically
make all of the calculations necessary to
produce a gross heat of combustion for the
sample. However, it is important that the
user understand these calculations to
ensure the instrument is set up so the
calculations match the procedures and the
units are consistent throughout the
process.
General Calculations
The calculation for the gross heat of
combustion is done by:
WT- e1 – e2 – e3
Hc =
m Thermochemical Corrections
Where:
Hc = Gross heat of combustion. T
= Observed temperature rise.
W = Energy equivalent of the cal-
orimeter being used.
e1 = Heat produced by burning the
nitrogen portion of the air
trapped in the bomb to form
nitric acid.
e2 = The heat produced by the
formation of sulfuric acid from
the reaction of sulfur dioxide,
water and oxygen.
e3 = Heat produced by the heating
wire and cotton thread.
m = Mass of the sample.
These calculations are made in calories,
grams, and degrees Celsius, and then
converted to other units if required.
B-1
Temperature Rise. The 1281 Calorimeter
produces a corrected temperature rise
reading automatically. Corrections for heat
leaks during the test are applied. (For a
complete discussion of this process see
Introduction to Bomb Calorimetry, Manual
No. 202M).
Energy Equivalent. The energy equivalent
(represented by W in the above formula, or
abbreviated as EE) is determined by
standardizing the calorimeter as described
in Appendix C - Standardization. It is an
expression of the amount of energy
required to raise the temperature of the
calorimeter one degree. It is commonly
expressed in calories per degree Celsius.
Since it is directly related to the mass of
the calorimeter, it will change whenever
any of the components of the calorimeter
(i.e. the bomb, bucket or amount of water)
is changed.
Nitric Acid Correction. In the high
pressure oxygen environment within the
oxygen bomb, nitrogen that was present as
part of the air trapped in the bomb is
burned to nitric oxide which combines with
water vapor to form nitric acid. All of this
heat is artificial since it is not a result of the
sample burning. The nitric acid correction
removes this excess heat from the
calculation.
Sulfur correction. In the oxygen rich
atmosphere within the bomb, sulfur in the
sample is oxidized to sulfur trioxide which
combines with water vapor to form sulfuric
acid. This liberates additional heat over the
normal combustion process which converts
sulfur to sulfur dioxide. The sulfur
correction removes this excess heat from
the calculation.
Fuse Correction. The fuse correction in
the 1281 Calorimeter is significantly
different than the correction used in earlier
model Parr calorimeters where the
correction was made to compensate for the
amount of fuse wire burned in the test.
There are two components to the fuse
correction in the 1281 Calorimeter:
1. The heat introduced by heating the wire
used to ignite the cotton thread.
2. The heat of combustion of the cotton
thread used to ignite the sample.
The semi-permanent heating wire is
heated by dissipating an electrical charge
from a capacitor. Since this charge is
controlled by the size of the capacitor and
the charging voltage, and because the
capacitor is fully discharged for each test,
the energy released can be calculated. In
the 1281 Calorimeter this is a fixed
correction of 10 calories per test.
Cotton has a heat of combustion of 4000
calories per gram. The actual thread being
used should be weighed to see how much
is being burned. Ten centimeters of a fine
thread will weigh approximately 0.003
grams which would release 12 calories as
it burns. Heavier threads weigh up to 0.010
grams per 10 centimeters and increase this
correction to 40 calories per test. The finer
the thread, the smaller errors will be if the
thread is not exactly ten centimeters in
length. Polyester thread is not
recommended for use in the bomb
because it has a tendency to melt and fall
away from the heating wire before it
ignites.
Using the fine thread mentioned above, the
fuse correction for the calorimeter would be
the 10 calories from electrical heating plus
12 calories from the burning thread for a
total of 22 calories per test. The thread
supplied by Parr has a mass of
approximately 1 milligram per centimeter.
This results in a total fuse correction of 50
calories.
ASTM and ISO Methods Differ
Current ASTM, ISO, and British Standard
Methods differ on their treatment of the
nitric and sulfuric acid thermochemical
corrections. ASTM Methods call for titrating
the bomb washings to determine the total
acid present. This is assumed to be all
nitric acid with a heat of combustion of
_14.1 Kcal per mole. The amount of sulfur
is then determined and converted to
equivalents of sulfuric acid. The difference
between the heat of formation of sulfuric
acid (_72.2 Kcal per mole or _36.1 calories
per milliequivalent) and nitric acid is then
subtracted as the sulfur correction.
Most other test methods treat nitric and
sulfuric acid corrections as entirely
separate values instead of combined
values. This eliminates the requirement for
a total acid determination and permits the
nitric acid correction to be handled in a
variety of ways, including the assumption
of a fixed nitric acid correction.
The 1281 Calorimeter can be set up to
apply the acid correction by either the
ASTM or ISO convention, as the user
prefers. Care must be used to ensure the
proper corrections are applied, and the
calculations made are consistent with the
procedure used.
Note:
Please review the following section on Acid
and Sulfur Corrections. Different standard
test methods use different values for the
heat of formation of sulfuric acid. These
differences are generally insignificant. The
1281 Calorimeter uses the most recent,
published values for all thermochemical
data.
B-2
Appendix B– Calculations
Thermochemical Calculation
Details
Traditionally, standard solutions and
procedures have been established to
simplify the calculations related to the
thermochemical corrections. The 1281
Calorimeter has been programmed to
permit the user to use standard solutions
and units which are most convenient, since
the microprocessor can easily apply any
conversion factors required.
FUSE Correction. The fuse correction
applied by the calorimeter is calculated as:
e3 = (fuse value)(fuse multiplier)
= (entered value)(Page 5.7
Line 5, )
“Fuse Value” is the number entered by the
user and the value which appears in the
test report.
Note:
Page 5.7 - Calculation Factors, Line 5 -
Fuse Multiplier is normally set to 1.0 so the
entered value is in calories (Press SKIP to
add the fixed value).
Users may find it convenient to enter a
fixed value for the fuse correction and
avoid the need to determine this correction
for each test.
Fixed fuse corrections can be entered
when Page 5 - Thermochemical
Corrections, Line 1 or 4 is set to ON. By
default a fixed fuse correction of 50
calories is applied to all tests. Total errors
of more than 5 calories will seldom occur
when using a fixed fuse correction and the
ignition thread supplied by Parr.
B-3
ACID and SULFUR Corrections.
• Total acid is the amount of base
required to titrate the bomb washings
(milliliters).
• Nitric acid is that portion of the total
acid in the bomb washings that result
when the nitrogen in the air that is
trapped in the bomb is burned at high
pressure. Since this nitric acid does not
result from the sample, and the
combustion conditions are reasonably
constant from test to test, the amount of
nitric acid formed is also constant.
• Acid multiplier is multiplied by the user
entered acid value to arrive at the
number of milliequivalents of acid. This
value is normally the concentration
(normality) of the base in equivalents
per liter (N).
• Percent sulfur is the concentration of
sulfur in the sample (weight %).
• Molecular weight of sulfur is 32.06.
• Equivalent weight of sulfur in H2SO4
is 16.03 (one half of the molecular
weight).
• Heat of formation of nitric acid is
14.1 calories/milliequivalent.
• Heat of formation of sulfuric acid
(from SO2) is 36.1 calories/millie-
quivalent.
• Sample mass is the mass of sample
burned in the bomb (grams).
• Sulfur multiplier is multiplied by the
product of the user entered sulfur value
and the sample mass to arrive at the
number of milliequivalents of sulfuric
acid in the bomb washings.
Example:
(Percent Sulfur) x (Sample Mass) x
10 = milligrams of sulfur
(milligrams of sulfur) / (equivalent wt. of S
in H2SO4) = milliequivalents of H2SO4
Sulfur Multiplier is then 10 / equivalent wt.
of S in H2SO4 or 10/16.03 = 0.6238
e1 is the nitric acid portion of the total
acid correction.
e2 is the sulfuric acid portion of the total
acid correction.
e1 + e2 is the total bomb acid correction.
Calculation for e1 when entered acid value
is total acid:
[((total acid) (acid mult))-(percent sulfur)
(sample mass) (sulfur mult) ] (heat of
formation of HNO3)
Total acid milliequivalents - milliequivalents
of H2SO4 = milliequivalents of HNO3.
(milliequivalents of HNO3) (heat of
formation of HNO3) = heat (in calories) due
to HNO3 produced.
Calculation for e1 when entered acid value
is nitric acid only:
(nitric acid) (acid multiplier) (heat of
formation of HNO3).
Calculation of e2 when entered sulfur value
is % sulfur:
e2 = (percent sulfur) (sample mass) (sulfur
multiplier) (heat of formation of H2SO4).
Users may find it convenient to enter a
fixed value for the acid correction and
avoid the need to determine this correction
for each test. Use of a fixed value for the
acid correction is highly recommended.
Fixed acid corrections can be entered
when Page 5 - Thermochemical
Corrections, Line 2 or 5 is set to ON. A
correction of 10 calories is a good number
for the fixed nitric acid value. For most
work, it is recommended to set “Acid Value
is Nitric Acid Only”, Page 5.7, Line 1 to ON.
Total errors of more than 3 calories will
seldom occur when using fixed nitric acid
corrections.
Fixed sulfur corrections can be entered if a
series of samples contain a constant
amount of sulfur. Fixed sulfur corrections
can be entered when Page 5 -
Thermochemical Corrections, Line 3 or 6 is
set to ON and then enter percent sulfur as
indicated on this line. Any errors will be
proportional to the difference between the
actual and assumed value for sulfur.
For ordinary work where benzoic acid is
used, or standardizing the calorimeter, the
Fixed Sulfur Correction, Page 5, Line 3
should be ON applying a fixed value of 0.0
to all standardization tests. Benzoic acid
contains no sulfur.
Page Line Setting Value
5 2 Off 13
3 Off 7
5 Off 13
6 Off 7
5.7 1 On
2 0.154
3 Off
4 0.1
6 On
7 -43.5
Table B-1
Settings for ISO & BSI Methods
B-4
Appendix B– Calculations
Please note that the values entered into
the test report appear as entered in the
report. Values for e1, e2 and e3 are
calculated and used as energy corrections
in accordance with the formulas and
settings given above. The formulas used
above to arrive at e1 or e2 are not the same
as the formulas used for e1 and e2 which
appear in most ASTM bomb calorimetric
procedures. However, the sum of e1 and
e2, above, is equal to the sum of the ASTM
treatment of e1 and e2.
ASTM Treatment for Acid and Sulfur
In the ASTM treatment, the correction for
acid formation assumes that all the acid
titrated is nitric acid. Obviously, if sulfur is
present in the sample, which in turn
produces sulfuric acid, part of the
correction for the sulfuric acid formed is
already included in the ASTM nitric acid
correction (e1). This is adjusted by a
separate computation based upon the
sulfur content of the sample. An additional
correction of 1.37 Kcal must be applied for
each gram of sulfur converted to sulfuric
from sulfur dioxide. This is based upon the
heat of formation of sulfuric acid, from
sulfur dioxide, under bomb conditions,
which is -72.2 Kcal per mole or -36.1
calories per milliequivalent. But remember,
a correction of 14.1 calories per
milliequivalent of sulfuric acid is already
included in the ASTM nitric acid correction
(e1). Therefore the additional correction
which must be applied for sulfur will be the
difference between 36.1 and 14.1 or 22.0
calories per milliequivalent (44.0 Kcal per
mole). For convenience, this is expressed,
in the ASTM e2 formula, as 13.7 calories
(44.0/32.06) for each percentage point of
sulfur per gram of sample.
B-5
ISO Calculations
Both the ISO 1928 and BSI 1016: Part 5
methods for testing the calorific value of
coal and coke, deal with acid and sulfur
corrections in a manner which is somewhat
different than ASTM procedures. Provision
has been made in the 1281 Controller for
dealing with these different procedures.
The analysis of bomb washings in these
methods call for a titration, first using O.1N
barium hydroxide (V2) followed by filtering,
and a second titration using 0.1N HC1(V1)
after 20 ml of a 0.1N sodium carbonate has
been added to the filtrate. Table B-1 gives
the settings which allows the results of the
two titrations, V1 and V2, to be entered into
the controller directly for the calculation of
the total acid correction. V1 should be
entered at the prompt for acid and V2 is
entered at the prompt for sulfur. The
settings in Table B-1 assume that the
same procedure is carried out for both
standardization and determination.
The offset value is the product of -1, the
Heat of Formation of Nitric Acid, the acid
multiplier, and the 20 ml of 0.1 N sodium
carbonate used in the analysis.
The formula used to get the total correction
in calories is as follows:
V1(Acid Multiplier)(Heat of
Formation of Nitric Acid)V2(Sulfur
Multiplier)(Heat of Formation of
Sulfuric Acid)+offset value.
The values for fixed acid and sulfur, which
are used in preliminary reports, will reflect
a sulfur correction of 0, and a nitric acid
correction of 10 calories.
Spiking Samples
It is sometimes necessary to add a spiking
material to samples which are very small,
have a low heat of combustion, or have a
high moisture content to add sufficient heat
to drive the combustion to completion.
Benzoic acid is an excellent material for
spiking for all of the same reasons it is a
good standard material. White oil is also an
excellent material, particularly for liquid
samples. The 1281 Calorimeter can
automatically compensate for the addition
of spiking materials to these samples. The
calculations are modified in these cases as
follows:
WT- e1- e2- e3- (Hcs)(Ms)
Hc =
m The calorific value obtained in a bomb
where Hcs = Heat of combustion of
the spiking material
(cal/gm)
Ms = Mass of spiking material
This factor is added to the calculations
when Page 2.3 - Spike Controls, Line 1 -
Use Spiking is set to ON. Line 2 - Heat of
Combustion of Spike is entered as calories
per gram. The controller will prompt the
user to enter the weight of spiking material.
Fixed spikes can be used when Line 3 -
Use Fixed Spike is set to ON and entering
the mass of the spike on Line 4 - Weight of
Fixed Spike.
Conversion to Other Moisture Bases
The calculations described above give the
calorific value of the sample with moisture
as it existed when the sample was
weighed. For example, if an air-dried coal
sample was tested, the results will be in
terms of heat units per weight of air-dry
sample. This can be converted to a
moisture free or other basis by determining
the moisture content of the air-dry sample
and using conversion formulae published
in ASTM Method D3180 and in other
references on fuel technology.
Conversion to Net Heat of Combustion
calorimeter test represents the gross heat
of combustion for the sample. This is the
heat produced when the sample burns,
plus the heat given up when the newly
formed water vapor condenses and cools
to the temperature of the bomb. In nearly
all industrial operations, this water vapor
escapes as steam in the flue gases and
the latent heat of vaporization, which it
contains, is not available for useful work.
The net heat of combustion obtained by
subtracting the latent heat from the gross
calorific value is therefore an important
figure in power plant calculations. If the
percentage of hydrogen H, in the sample is
known, the net heat of combustion, Hnet
Btu per pound can be calculated as
follows:
Hnet = 1.8Hc - 92.7H
(Solid fuels, ASTM D2015)
Hnet = 1.8Hc - 91.23H
(Liquid fuels, ASTM D240)
B-6
Appendix C - Standardization
Appendix C- Standardization
Standardizing the Calorimeter
The Energy Equivalent Factor. The term
“standardization”, as used here, denotes
the operation of the calorimeter on a
standard sample from which the energy
equivalent or effective heat capacity of the
system can be determined. The energy
equivalent, W or EE of the calorimeter is
the energy required to raise the
temperature one degree, usually
expressed as calories per degree Celsius.
Standardization tests should be repeated
after changing any parts of the calorimeter,
and occasionally as a check on both the
calorimeter and operating technique.
Standardization Procedure. The
procedure for a standardization test is
exactly the same as for testing a fuel
sample. Use a pellet of calorific grade
benzoic acid weighing not less than 0.9 nor
more than 1.25 grams. The corrected
temperature rise, T, is determined from the
observed test data and the bomb washings
are titrated to determine the nitric acid
correction. The energy equivalent is
computed by substituting the following
equation:
Hm + e1 + e2 + e3
W=
T
Where:
W = Energy equivalent of the cal-
orimeter in calories per
degree Celsius.
H = Heat of combustion of the
standard benzoic acid
sample in calories per gram.
m = Mass of the standard benzoic
acid sample in grams.
T = Temperature rise in ºC.
C-1
e1 = Correction for heat of
formation of nitric acid in
calories.
e2 = Correction for sulfur which is
usually 0.
e3 = Correction for heating wire
and combustion of cotton
thread.
Standard Materials
A bottle of 100 one-gram benzoic acid
pellets (Part No. 3415) is furnished with
each calorimeter for standardizing
purposes. The Parr benzoic acid has been
calibrated against NIST benzoic acid.
Additional benzoic acid pellets can be
obtained from Parr. For very high precision
measurements, a primary standard
benzoic acid powder can be purchased
from the National Institute of Standards &
Technology, Washington, D.C.
It is not common to have sulfur in standard
materials, or to use spikes in
standardizations, but the capabilities have
been included in this calorimeter.
Users should take great care to ensure that
the conditions during standardization runs
and determinations are as identical as
possible.

CAUTION:
BENZOIC ACID MUST ALWAYS BE
COMPRESSED INTO A PELLET BE-
FORE IT IS BURNED IN AN OXYGEN
BOMB TO AVOID POSSIBLE DAM-
AGE FROM RAPID COMBUSTION OF
THE LOOSE POWDER. THIS IS
BEST ACCOMPLISHED BY USING A
PARR 2811 PELLET PRESS.
Automatic Statistical Calculations
The 1281 Calorimeter includes a provision
for calculating and using a mean energy
equivalent for each of up to 4 separate
bomb and bucket combinations. ASTM
procedures recommend that the energy
equivalent be determined by averaging ten
tests. The 1281 Calorimeter automatically
determines and uses up to 10 tests in its
memory and will update the EE Value as
additional standardizations are run. Only
Final Tests will be used in determining and
updating EE values. These values, the
number of tests, and the relative standard
deviation for the tests used in determining
the EE value are stored on Pages 4.4 thru
4.7, Line 1 - EE Value.
Any outliers or other tests which should not
be included in the average EE Value must
be deleted from the memory using the
memory management procedures (see
Chapter 8). A list of all tests associated
with any Cal ID can be printed from Page
4.7 - 4.0, Line 6 - Print Standardization
Runs.
The user can elect to have any number of
stored standardization runs used in
determining the EE value by entering this
number on Page 4 - Calibration Data &
Controls, Line 1 - Calibration Run Limit.
Line 2 - EE Max Std Deviation on this
same page establishes the maximum
allowable standard deviation for the EE
Value before an error condition is reported.
The default value is zero and the ASTM
limit is .15%, but the user should enter a
value appropriate for the test being made.

The user can chose to turn off the

automatic averaging and updating
procedure and protect the EE Values by
turning ON the protection feature for the
appropriate bomb on Pages 4.7 thru 4.0,
Line 2 - Protected EE Value.

C-2
Appendix D– Communication Interfaces
The Parr Smart Link is designed to
facilitate the connection and control of a
network of equipment which can include
the 1281 Calorimeter,1271 Calorimeter,
1261 Calorimeter, 1760 Sulfur Analyzer,
1720 or 1730 Calorimeter Controllers,
1741 Balance Interfaces and 1750
Proximate Analyzers with attached
analytical balances, 1745 Computer
Interface and/or the 1747 PC Smart Link
Board and associated computer, and 1742
Sulfur Interface for automatically entering
and storing sulfur values.
Successful installation of the Smart Link
network will depend upon all elements of
the communications network (Smart Link)
being preset, properly configured and
connected. A step-by-step review of the
Smart Link communications network and
the configuration requirements for all
devices installed on the Link is provided in
this chapter (see Smart Link Configuration
Checklist) to ensure that the system is
properly addressed before attempting to
use it.
The Parr Smart Link is a combination of
the hardware (circuit board, connectors
and cables) used to interconnect these
devices and the software (programs)
required to identify the devices on the
network and control the bi-directional
transfer of data between these devices.
Inherent in the programs which are an
integral part of the Smart Link are the
protocols for sending and receiving data,
avoiding interference when the network is
busy and ensuring the security and validity
of the data.
In addition to the intelligent network control
feature of the Smart Link, there are two
additional important advantages offered by
the communications link when compared
D-1
with more conventional direct coupling
methods such as multiple RS232C
connectors. Since devices can be
connected in series (or daisy-chained)
there is no practical limit to the number of
devices that can be connected and only a
single connection port is required for each
device. The Smart Link is also capable of
communicating with devices up to 1000
meters away as opposed to the 50 foot
restriction for RS232C lines.
Required Software Versions
Before proceeding with the installation of
the 1281 Calorimeter on the Parr Smart
Link, the user must ensure that all of his
devices have the versions of software
capable of communicating over the Smart
Link and have been configured for the
intended network (see Table D-1).
The version of software installed in a Parr
device can be determined by performing
the self-test procedure and checking the
printed or displayed message. Users who
do not have the required software installed
should contact the Technical Service
Department at Parr Instrument Company.
Required Hardware
This 1281 Calorimeter is fully equipped for
operation on the Smart Link. The 1760
Sulfur Analyzer, as well as 1720 and 1730
Controllers must have the optional 1722
Smart Link board installed to communicate
on the Smart Link. The 1750 Proximate
Analyzer and the 1741, 1742, 1745 and
1747 Interfaces include all of the required
Smart Link hardware. If a 1760 Sulfur
Analyzer or 1720 or 1730 Controller will be
used in the installation and the 1722 Board
has not already been installed, it must be
installed at this time.
Smart Link Configurations
Each device on the Smart Link has several
parameters associated with it which help
to: 1) identify the instrument and, 2) control
the flow of information to and from
instruments on the link.
Each category of device has its own fixed
identification which automatically identifies
it on the Smart Link. Addresses of
individual instruments within a class, such
as calorimeter controllers, must be
changed from the default setting only if
more than one device in the same category
is installed on the link. The second device
within the category must have its address
set to one, and the third set to two, etc.
All devices on the Smart Link are set, by
default, to communicate at a rate of 9600
baud. All devices on the Smart Link must
communicate at the same transmission
speed.
Device
1281 Calorimeter
1271 Calorimeter
1261 Calorimeter
1720 Controller
1730 Controller
1741 Balance Interface
1745 Computer Interface
1747 PC Interface
1750 Proximate Analyzer
1760 Sulfur Analyzer
Table D-1
Software Required
Smart Link Configuration Checklist
1. Software versions verified for all
devices connected on the Smart Link.
2. Any devices which are not the only
device within their category have had
their addresses changed to 1, 2 or
higher as needed.
3. The two devices at the ends of the
Smart Link have had all levers of the
terminator switches closed as viewed
from the rear of the calorimeter; open is
to the left and closed is to the right.
4. All other devices, other than the ones
on the ends, have all levers of the
terminator switches open.
5. All devices have been checked to see
that a transmission rate of 9600 baud
has been set.
6. All devices on the Link have been
turned ON.
Software Version
81.0 or Higher
71.0 or Higher
61.0 or Higher
20.4S or Higher
30.2S or Higher
41.3 or Higher
45.1S or Higher
1.0 or Higher
50.2 or Higher
60.1 or Higher
D-2
Appendix D – Communication Interfaces

Smart Link Configuration Cabling

Smart Link devices, including the 1281
Controller, can be connected using any of
the cables listed in Table D-2.
Smart Link cables can be linked as
extension cords. If a device is removed
from the link, the two cables should be
connected to each other to maintain the
continuity of the link. All devices should be
turned off before cables are connected or
disconnected.
Parr offers the 1454E Connecting adapter
for connections from the identified RS232C
port to devices located within five feet of
the calorimeter. Users may have longer
cables designed to match their devices and
installations using these specifications.
RS232C ports are not designed for
communicating over distances greater than
50 feet.

Cable Cable Length

A597E4 10 Feet
A597E 25 Feet
A597E2 100 Feet
A597E3 Custom to 1000 Feet Maximum

Table D-2
Smart Link Cables

RS232C Connection

The 1281 Calorimeter is also equipped

with an RS232C port for connection to
either a 40 or 80 column printer and/or a
computer (see Figure 2-5). Before making
either of these connections the data
transmission rate of the calorimeter and
the printer or computer must be matched.
Generally the baud rates on either device
can be changed to achieve this match.
Printer Port Communications for the 1281
Controller are on Page 8.2 -Printer Port
Communications, Lines 1-5.

The default parameters for the 1281

Calorimeter are set up for use with the Parr
1756 Printer. Table D-3 identifies and
describes the pinout for the RS232C port.

D-3
Terminal Port Connections same for both the balance and the
calorimeter.
All report transmissions to a computer
must be initiated at the calorimeter Mettler 011/012 Interface
controller.
Field Length
Run area data consists of 22 fields with ID 2
commas separating each field. space 1
data 9
Each calorimeter is furnished with 1454E space 1
Adapter for attaching 9 pin female g 1
connector to computer with 8 pin opening. CR 1
The RJ45 female and RJ45 male LF 1
connector may be obtained from an
electronic supply store. The ID field must contain “S_” to indicate a
stable mass. The data field contains the
Balance Input Driver Specifications current mass, right justified, with a decimal
point. The balance should be configured to
The 1281 Calorimeter supports input from send continuously.
the four balance types indicated below.
Additionally, a generic input driver is Mettler 03 Balance Interface
provided for communications with balances
that do not conform to the four supported Field Length
protocols. A new feature supported by all NULL 1
five balance input drivers is the ability to ignored 6
change the expected number of characters space 1
in the data field. The number of data data 9
characters indicated for each of the drivers, space 1
below, are default values. This feature ignored 3
virtually eliminates the need for balance CR 1
input drivers to be re-written in the event LF 1
the balance manufacturer elects to alter
the output string of a balance when new Leading zeros and the “+” sign in the data
models are introduced. field are suppressed. The NULL character
is used to indicate a stable mass. The
The format of an unknown balance can be balance should be configured to send
determined by logging the balance output continuously.
to the printer attached to the calorimeter.
Those protocols which send a command Sartorius Balance Interface
string to the balance will do so while
logging is active. In order for the logging to Field Length
produce meaningful results, the cable polarity 1
connecting the balance to the balance space 1
input port of the calorimeter must be data 8
correctly wired or configured. In addition, space 1
the specifics of the data frame, such as the stability 2
baud rate, # of data bits, parity, # of stop CR 1
bits and handshaking (if used) must be the LF 1

D-4
Appendix D – Communication Interfaces

The polarity field must contain either a “+” this command once every few seconds
or a space. Leading zeros in the data field after the ENTER key has been pressed
are blanked, except for the one to the left during a mass entry sequence. The
of the decimal point. The stability field must ENTER key should only be pressed when
contain “g_” for the calorimeter to accept a the mass reading is stable. However,
mass. The balance should be configured to unstable readings will be rejected and a
transmit data upon receipt of the following warning will be issued. Acknowledging the
command string: warning by pressing the CLEAR ENTRY
key will re-issue the command string to the
[ESC] [CR] [LF] balance on a periodic basis. The auto print
feature is also compatible with this
Note: The automatic data output option calorimeter input balance driver routine.
should not be used.
Generic Interface
The calorimeter will send this command
string once every few seconds after the Field Length
ENTER key has been pressed during a data 9
mass entry sequence. The ENTER key CR 1
should only be pressed when the mass
reading is stable. However, unstable The data field should consist of 9 numeric
readings will be rejected and a warning will characters (0 through 9, +, - and space)
be issued. Acknowledging the warning by terminated with a carriage return (CR).
pressing the CLEAR ENTRY key will re- Leading zeros may be blanked as spaces
issue the command string to the balance and are counted. Non-numeric characters
on a periodic basis. are ignored and will reset the input buffer if
the data field has not been filled. Any
Ohaus Balance Interface characters received after filling the data
field and before the carriage return are
Field Length ignored.
polarity 1
data 7
space 1
mode 5
stability 1
address 2
CR 1
LF 1

The single character polarity field should

contain a space. The Data field contains
the current display mass, right justified,
with a decimal point. The contents of the
mode and address field are ignored by the
calorimeter. The stability field must be
blank for the calorimeter to accept a mass.
The balance should be configured to send
its data upon receipt of the P9print display
data) command. The calorimeter will send

D-5
 Table D-3
1281 Terminal Port
10 Pin 8 Pin Direction
RJ-45 Pin # RJ-45 Pin # Pin Description 1281 - Terminal
1 Spare Output (Not Used) →
2 1 Carrier Detect (DCD) ←
3 2 Frame Ground ←→
4 3 Received Data ←
5 4 Transmitted Data →
6 5 Data Set Ready (DSR) ←
7 6 Ready to Send (RTS)
→
8 7 Signal Ground
←→
9 8 Clear to Send (CTS)**
10 Data Terminal Ready ←
→
** Held at +12V (space or logic 0) while the 1281 is on.

Table D-4
1281 Balance Port
10 Pin 8 Pin Direction
RJ-45 Pin # RJ-45 Pin # Pin Description 1281 - Terminal
1 Carrier Detect (DCD) ←
2 1 Spare Output (Not Used) →
3 2 Frame Ground ←→
4 3 Transmitted Data →
5 4 Received Data ←
6 5 Data Terminal Ready (DTR) →
7 6 Clear to Send (CTS)**
←
8 7 Signal Ground
←→
9 8 Ready to Send (RTS)
10 Data Set Ready (DSR) →
←
** Held at +12V (space or logic 0) while the 1281 is on.

D-6
Appendix D – Communication Interfaces

Table D-5
1281 Printer Port
10 Pin 8 Pin Direction
RJ-45 Pin # RJ-45 Pin # Pin Description 1281 - Terminal
1 Spare Output (Not Used) →
2 1 Not Used
3 2 Frame Ground ←→
4 3 Received Data ←
5 4 Transmitted Data →
6 5 Data Set Ready (DSR) ←
7 6 Carrier Detect (DCD) ←
8 7 Signal Ground
←→
9 8 Clear to Send (CTS)**
←
10 Data Terminal Ready
→
** Held at +12V (space or logic 0) while the 1281 is on.

D-7
 Table D-6
Calorimetry Run Storage Definitions

No. Field Comments

1 Mode 0=determination, 1=standardization
2 Method 0=equilibrium, 1=dynamic
3 Status 0=preliminary, 1=final
4 Units 0=MJ/Kg, 1=Btu/lb, 2=Cal/g, 3=J/Kg
5 Data Entered See table below
6 Date Date of run
7 Time Time of run
8 Channel Channel that this was run
9 Cal ID Calorimeter ID
10 Samp ID Sample ID number
11 Weight Sample weight
12 Starting Temp. Initial temperature
13 Jacket Temp. Jacket temperature
14 Delta Temp. Temperature rise
15 Fuse Fuse value
16 Acid Acid value
17 Sulfur Sulfur value
18 Energy Equivalent Heat capacity of calorimeter
19 Heat of Combustion H value
20 Net Heat Comb Net heat of combustion
21 Spike Weight Weight of spike material
22 Hydrogen Amount of hydrogen in sample

Table D-7
Data Entered - Bit Definitions
Description Bit Position
1 = Calorimetry completed f
1 = Initialized e
X = Unused d,c,b,a,9,8
1 = Hydrogen value entered 7
1 = Spike value entered 6
1 = Sulfur value entered 5
1 = Acid value entered 4
1 = Fuse value entered 3
1 = Cal ID entered 2
1 = Weight value entered 1
1 = Sample ID entered 0

D-8
Appendix E – Technical Service

Appendix E - Technical Service

Should you need assistance in the

operation or service of your instrument,
please contact the Technical Service
Department.

Telephone (309)762-7716
1-800-872-7720
Fax (309)762-9453

When calling, please make note of and

have available the following:

1. The serial # of the calorimeter

2. Date purchased
3. Software Version (Page 3, Line 3)
4. User Setup ID (Page 3, Line 4)
5. Factory Default Version (Page 3,Line 5)
6. The number and type of any SmartLink
peripherals and their software revisions.

It is also helpful if the person calling is

close to the 1281 Calorimeter to implement
any changes recommended by the
Technical Service Department.

Return for Repair

To return the instrument for repair, please

call the Technical Service Department for
shipping instructions and a RETURN
AUTHORIZATION NUMBER. This number
must be clearly shown on the outside of
the shipping carton or it will be refused.
Ship repair to:

Parr Instrument Company

Attn: Service Department
211- 53rd Street
Moline, Illinois 61265

E-1
E-2
 Appendix F – Parts List

1281 Calorimeter Parts List

Item Description Item Description
359VB Filter 909E Switch, Power
574DD Clamp, Capacitor 908E Relay, Solid State
576DD Spacer, .25L, Male/Female 911E Filter, Interface, 10 amp
A598DD Switch, Pressure;400 psi 1181E Connector, Female
799DD Bushing,2” Snap 1203EEE Cordset, 10A/220V CE Plug
809DD Plug, Screw 10-32 w/GSK Brass 1400E Power supply, Output Switching
A864DDEB Heater, 500W, 120V, 3/8NPT A1401E2 Circuit Board, CPU
A864DDEE Heater, 500W, 230V, w3/8NPT A1402E Circuit Board, Driver
A866DD Valve assy, Solenoid 24VDC 1404E Battery, Lithium 3.6V, w/Plug
886DD Housing, Calorimeter 1406E Connector, thru 18 Ga, 5 Pos
894DD Foot, Plastic 1407E Connector, thru 18 Ga, 10 Pos
908DD Water Tank 1408E Connector, end 18 Ga, 14 Pos
909DD Arm Assembly 1409E Connector, Female, 8 Pos
910DD Anchor Block 1410E Connector, Female, 12 Pos
911DD Pivot Block 1411E Connector, Female, 13 Pos
912DD Base, Calorimeter 1414E Keypad
913DD Base Plate, Calorimeter A1415E Display Keyboard Assembly
914DD Back Angle A1418E Harness, Power Supply
915DD Support, Outer, Right A1419E Printer Power Cable
916DD Support, Center 1412E Connector, Female, 17 Pos
917DD Support, Outer, Left 1417E Thermistor, Jacket
918DD Angle, Air Can Mounting 1451HC Pad, Heat Transfer
919DD Angle, Divert Valve 79HW2 Plug, Socket Head, 1/8NPT
921DD Bracket, Pump Support 117HW3 Elbow, Male, 1/4T x 1/8NPTM
922DD Backplate, Calorimeter 179VB Tee, Street, 1/8NPTM-F-F Brass
923DD Backplate, Air Can 180VB Elbow, Male, 1/8T x 1/8NPTM
A924DD Manifold Assembly 206VB Elbow, Male, 1/4T x 1/8NPTM
927DD Receptacle, In-Line 214VBAD Ferrule, 1/8”
928DD Adapter, Barbed1/4 NPTMx1/4 ID 244VB Union, Bulkhead, 1/8T, Brass
929DD Adapter, Barbed ¼ NPTMx1/2 ID 300VB Tee, 1/4NPTF Brass
931DD Elbow, Barbed ¼ NPTM x ¼ ID 311VB Fitting, Mini Hose
A932DD Tee Tube Assembly, Soldered 315VB Fitting, Barbed, Rt Angle
935DD Bracket, LCD Mount Aluminum 321VB Valve, bucket
997DD Backplate, Calorimeter 328VB Union, Bulkhead 1/4T Brass
998DD Clamp, Hose, Snap 5/8 Nylon 329VB Union, Bulkhead 3/8T Brass
A1011DD Switch Assy, Liquid Level 329VBAD Union, Bulkhead 3/8T T316
A1012DD Valve Assy, Solenoid, O2/Rinse 332VB Elbow, Male 3/8Tx1/8NPTM Brass
A1013DD Solenoid Valve Assy, Bomb Release 345VB Reducer, Tube 1/4T x 1/8T Brass
A1014DD Valve, Water Handling Solenoid 346VBAD Nipple, Close 1/4NPT T316
A1015DDEA Pump Motor Assy, 115V/60Hz 367VB Elbow, Street ½NPT Brass
A1015DDEF Pump Motor Assy, 230V/50Hz 368VB Elbow, Male 3/4T x 1/2PTM Brass
A1050DD Bomb Rinse Container Assy 369VB Plug, Tube 3/4T
A1108 Strainer 370VB Plug, Pipe 1/2NPTM
A1145DD Motor Cable 371VB Adapter, Barbed 1/2NPTM x ½ ID
1053DD Bottle, 500 mL 372VB Union, Barbed, HDPE 1/2T x 1/4T
1054DD Bottle Support 379VB Union Tee, Barbed HDPE 1/2T ID
A719E Cordset, 115V Plug 411VBAD Reducer 1/4T x 3/8T x SS
897E Capacitor, 40 V 182VB Male Connector, 1/8T – 1/8NPT
A1016DD Motor

F-1
 1281 Calorimeter Parts List Continued
Item Description
A1064DD 1281 Software Update Disk
HA0012TB031 Tubing, TFE, 6”
HX0012TB024 Pressure tubing, 1/8”OD, Nylon
HX0025TB062 Tubing, Plastic, ¼”OD x 1/8” ID
HX0038TB062 Tubing, Bev-A-Line, 3/8” OD x ¼” ID
JT0038TB062A Tubing, Tygon, 3/8” OD x ¼” ID
JU0038TB062A Tubing, Polyurethane, ¼” ID x 1/16W
SA1332RD06 6-32 x 3/8 RHMS
SA1932FT08 10-32 x ½ FHMS
SB1932BT04 10-32 x ¼ BHSCS
SN1332HLHJ Nut, 6-32 Hex Lock Nylon
SN1632HLHJ Nut, 8-32 Hex Lock Nylon
SN1932HLHJ Nut, 10-32 Hex Lock Nylon
SW13NL Lock Washer
SW39FT .625 x .390 x .063 Washer
SW44FT06 7/16 Flat Washer
TN1332HL 6-32 Hex Nut
TN1632HL 8-32 Hex Nut
TN1932HL 10-32 Hex Nut
TW56FT Bolt Washer

F-2
Appendix F – Parts List

1281 Calorimeter Cover Parts List

Item Description
887DD Cover, Calorimeter
973DD Bracket, Motor Mount
A975DD Lid Assembly
976DD Seal, Lid
977DD Block, Cylinder Mounting
978DD Shaft, Latch
979DD Pin, Spring 1/8 x ¾ SS
980DD Arm, Latch Pivot
981DD Cylinder, Air 5/8 Bore
982DD Clevis, Rod, with Nut
983DD Spring, Compression
985DD Guide Pin, Lid
986DD Pin, Contact
987DD Block, Contact Pin
988DD Spring, Compression .03 x 7/16
989DD Ring, Retaining
990DD Sensor, Clamp
991DD Bulkhead, Lift support
992DD Block, Hinge
993DD Arm, Left Lift
994DD Arm, Right Lift
995DD Rod, Lift Arm
996DD Cam, Lid
A1010DD Sensor Assy, Hall Effect Switch
A1016DD Motor Assy, Pump 6 Watt, 12 Volt
214VBHJ Ferrule Set
243VB2 Conn, Male 1/8T x 1/8NPT
311VB Fitting, Mini Hose
390VBHJ Union
SA1332FS06 6-32 x 3/8 FH Socket
SA1632FS06 8-32 x 3/8 FH Socket
SA1932FT08 10-32 x ½ FHMS
SA1932RD06 10-32 x 3/8 RHMS
SA1932RD08 10-32 x ½ RHMS
SA1932RD16 10-32 x 1 RHMS
SB1932SC10 10-32 x 5/8 SHCS
SG1140FT06ST No 4 x 3/8 Flat Hd Slot
TN1332HL 6-32 Hex Nut
TN1932HL 10-32 Hex Nut
SW25FT ¼ Bolt Washer

F-3
 1281 Bucket and Stirrer Tube Assembly Parts List

Item Description
925DD Retainer, Oxygen Bomb
A940DD Tube Assy, Bucket; Solered
941DD Wedge, Bucket
942DD Bushing, Bucket Retaining Delrin
943DD Fitting, Drain; Bucket Brass
944DD O-Ring, Buna-N .237 ID
946DD Seal ¼ SS
947DD Bearing, Ball; Plastic
A950DD Coupler, Magnetic; Assembly
951DD Housing, Bearing; Delrin
A955DD Propeller Assembly, Stirrer
988DD Spring, Compression
1135E Adapter, 16 Pin Stick
1416E Thermistor, Bucket
1462E Extension Cable
715HC O-Ring, Buna-N, 1-1/4 ID
SC1332SC03 6-32 x 3/16 SHSS 18-8 SS
SN1140HLHJ Nut, 4-40 Hex Lock Nylon
SW31FT06 5/16 Flat Washer 18-8 SS

F-4
Appendix F – Parts List

1281 Air Can Assembly Parts List

Item Description
659DD O-Ring, Buna-N .145 ID
857DD O-Ring, Buna-N 3/8 ID
882DD O-Ring, Buna-N .487 ID
A960DD Air Can Assembly
961DD Cylinder, Bomb Release
962DD Cap, Bomb Release Cylinder
963DD Retainer, Bomb
964DD Spacer, Bomb
965DD Adapter, Air Can
966DD Shaft, Pin Release
967DD Seal, Air Can
969DD O-Ring, Buna-N, ¼ ID
970DD Retaining Ring SS
972DD Cam, Lid
328E Hole Plug, 3/8
357HCJB O-Ring, Buna-N, ¼ ID
A92HWAD Male Connector, 1/4T – 1/8NPT
344VB Connector, Male 1/8T x 1/16NPTM
376VB Elbow, Male 1/8T x 1/16NPTM
SA1632FS06 8-32 x 3/8 FH Socket
SA1632RD18 8-32 x 1-1/8 RHMS 18
SB1632SC06L 8-32 x 3/8 SHCS SS
SN1632HLHJ Nut, 8-32 Hex Lock
TA1332RD08L 6-32 x ½ RHMS w/Ext.
TE1320PP06ST No 6 x 3/8 Pan Head
XB0130 ½” Wire Loom, Flex

1288 Accessory / Installation Kit Parts List

Item Description
43AS Capsule, SS
149C In-Line Filter
231C2 Container, PP 10L Foldable
A570DD Regulator Assembly, Oxygen
811DD Lube/Sealant
840DD2 Heating Wire
845DD Ignition Wire
649DD O-Ring, Buna-N .070 ID
A812DD Regulator Assembly, N2
876DD Cutter, Plastic Tubing
A1050DD Bomb Rinse Container
A1419E Cable, Printer Power
1454E Adapter, 9 Pin (F)
3415 Benzoic Acid Pellets 100 Gram Bottle

F-5
 1136 Oxygen Bomb Parts List

Parr Part No. Description

882DD O-Ring, Buna-N, .487 ID x .102 CS
1081DD Quad-Ring, Buna-N
A890DD Oxygen Bomb Cylinder Assembly
647DD Bracket, Anti-Rotation
888DD Cylinder
889DD Outer Ring
SA1332FP04 6-32 x ¼ Flat Head
SC1332SC02 6-32 x 1/8 SHSS 18-8
A895DD Oxygen Bomb Head Assembly
654DD Electrode Washer
655DD Electrode Spacer
658DD Insulator, TFE
659DD O-Ring, Buna-N
663DD Contact Bushing
667DDJV Quad-Ring, FKM
645DD Water Diffuser
821DD O-Ring, .056 x .060
840DD2 Heating Wire
896DD Bomb Head 1136/1281
898DD Locator, Bomb Cap
899DD Handle, Bomb Head
901DD Funnel, O2 Line T303
902DD Ground Stud, Bomb Head
904DD Standoff, SS
905DD Standoff, SS
906DD Holder, Capsule
907DD Check Valve, Head
1094DD Electrode Long
1095DD Electrode
394HC O-Ring, Viton 3/8 ID
1374HCJV O-Ring, Viton 1/8 ID
PA1332RD04 6-32 x ¼ RHMS, T316SS
SA1632FS06 8-32 x 3/8 FH Socket
SA1632RD06 8-32 x 3/8 RHMS 18-8
SN1632HX 8-32 Hex Nut 18-8 SS

F-6
Appendix F – Parts List

1136CL Oxygen Bomb Parts List

Parr Part No. Description

882DD O-Ring, Buna-N, .487 ID x .102 CS
1081DD Quad-Ring, Buna-N
A890DDCL Oxygen Bomb Cylinder Assembly
647DD Bracket, Anti-Rotation
888DDCL Cylinder
889DD Outer Ring
SA1332FP04 6-32 x ¼ Flat Head
SC1332SC02 6-32 x 1/8 SHSS 18-8
A895DDCL Oxygen Bomb Head Assembly
645DD Water Diffuser
654DD Electrode Washer
655DD Electrode Spacer
658DD Insulator, TFE
659DD O-Ring, Buna-N
663DD Contact Bushing
667DDJV Quad-Ring, FKM
645DD Water Diffuser
821DD O-Ring, .056 x .060
840DD2 Heating Wire
896DDCL Bomb Head 1136/1281
898DD Locator, Bomb Cap
899DD Handle, Bomb Head
901DD Funnel, O2 Line T303
902DD Ground Stud, Bomb Head
904DD Standoff, SS
905DD Standoff, SS
906DD Holder, Capsule
907DD Check Valve, Head
1094DD Electrode Long
1095DD Electrode
394HC O-Ring, Viton 3/8 ID
1374HCJV O-Ring, Viton 1/8 ID
PA1332RD04 6-32 x ¼ RHMS, T316SS
SA1632FS06 8-32 x 3/8 FH Socket
SA1632RD06 8-32 x 3/8 RHMS 18-8
SN1632HX 8-32 Hex Nut 18-8 SS

F-7
 1289 (1281) Spare Parts List

Item Description
1081DD Quad Ring NBR 2.88 ID x .125 CS
653DD Nut, Electrode
654DD Electrode Washer, Ceramic
655DD Electrode Spacer
656DD Reducer Bushing
658DD Insulator, TFE
659DD O-Ring, NBR, .145 ID x .070 CS
663DD Contact Bushing, Delrin
667DDJV Quad Ring NBR 1.48 ID x .139 CS
668DD Check Valve
821DD O-Ring .056 ID x .060 CS
822DD O-Ring, NBR, .487 ID x .102 CS
840DD2 Heat Wire 60”L
843DD Holder Wire
845DD Thread, Ignition; Spool
882DD O-Ring, NBR, .487 ID
897DD Electrode Core 1136
906DD Holder, Capsule
907DD Check Valve, Head
969DD O-Ring, NBR, .484 ID x .139 CS
1002DD Electrode, Straight
394HC O-Ring FKM 3/8 ID x 1/16 CS
1374HCJV O-Ring FKM 1/8 ID x 1/16 CS
PA0948RD04 3-48 x ¼ RHMS T316 SS

F-8
F-9
Appendix G – Bomb Rinse Container Assembly
The A1050DD2 Bomb Rinse Assembly
is available as an accessory to the 1281
Calorimeter. This device allows for
complete and systematic recovery of
the bomb combustion products. These
combustion products include that
portion which is released during the
initial bomb exhaust, followed by the
portion expelled during the bomb rinse
cycle. The A1050DD2 Assembly is
similar to the A1050DD Assembly,
except that 1/8" tube construction is
used instead of 1/4" tubing. The
A1050DD2, with its 1/8" tube
construction, is suitable for use with
calorimetric samples that do not
produce appreciable amounts of ash or
other incombustible material that could
become lodged in the 1/8" tubing. The
sole benefit of the 1/8" construction is a
longer bomb exhaust release time.
Some users find this feature desirable.
Note:
The A1050DD2 should not be used in
routine coal testing applications.
Concept of Operation
The 1281 Bomb Rinse Container Assembly
is connected to the rear of the calorimeter,
in place of the portion of the waste tube
assembly that is connected to the bomb
exhaust fitting. The divert valve, at the right
hand side of the calorimeter, is disabled to
allow the bomb exhaust and the bomb
washings to be collected in the 1053DD,
HDPE 500 ml bottle, provided with the
A1050DD2. The objective is to capture and
retain all of the combustion products which
have been dissolved in the residual water
present in the bomb prior to combustion as
well as any water formed during the
combustion process. The most common
examples of these combustion products
include:
G-1
• Sulfate, derived from any sulfur
containing materials in the original
sample.
• Chloride from organic samples
containing chlorine.
These combustion products are discharged
from the bomb in two steps. The first step
occurs during the initial rapid release of the
residual bomb gases. The 1053DD Bottle
has sufficient strength and volume to deal
effectively with this sudden pressure
release. Gas is expelled from the four
holes on the perimeter of the 1052DD
Bottle Cap, leaving any discharged liquid in
the bottle. As an additional safety measure,
the bottle is supported in a 1054DD
Cylinder (acrylic) which serves to keep the
bottle upright and contained in the unlikely
event the bottle ruptures. At the end of the
bomb exhaust step the aqueous
combustion products reside in the bomb,
associated tubing as well as the 1053DD
Bottle. The bomb rinse step flushes these
combustion products from the bomb and
the tubing into the 1053DD Bottle. The
bottle can then be unscrewed from the
assembly and capped until the sample is to
be analyzed. Some users find it useful to
add the contents of the rinsed combustion
capsule to the washings collected in the
bottle. Three 1053DD Bottles are provided
with the assembly. Additional bottles may
be ordered separately from Parr.
Installation
Note:
By-passing the divert valve (if present) -
1281 Calorimeters built after September
6, 1995, have the 320VB Divert Valve
removed. The bomb rinse divert valve
must be by-passed to permit the bomb
washings to be discharged out the rear
of the 1281 Calorimeter. Disconnect the
power cord at the rear of the instrument
and remove the rear cover plate.
Disconnect the 1/4" line at the divert valve
and the 3/8" line at bulkhead connection #8
at the rear of the instrument. Connect the
1/4" line to the #8 bulkhead connection
using a 411VBAD Reducer along with a
211VBAD Nut and 222VBAD Ferrule Set.
Replace the rear cover and apply power to
the calorimeter.
Connection to the A1050DD2 Rinse
Container Assembly - break the
connection at the rear of the 1281
Calorimeter to the bomb exhaust hose. In
place of this, connect the 1/8" tube and
3/8" compression fitting adapter provided
as part of the A1050DD2.
Adjusting the bomb rinse parameters -
The bomb rinse parameters are factory set
to provide approximately 50 ml of bomb
washings. This amount was chosen in
order to rinse the bomb as quickly as
possible in order to prepare the calorimeter
for the next test. More quantitative rinsing
can be realized, at the expense of time, by
increasing the volume of washings.
Experience has demonstrated that for a
bomb of this volume, wash volumes on the
order of 100 ml are required for
quantitative recovery. Doubling the rinse
time on Menu Page 2.4.5 from the default
valve of 5 to 10 will provide a volume of
washing better suited for precise analytical
work. The volume of washing can be easily
verified by performing a calorimeter pretest
sequence (F2).
Operation
Place the bottle end of the rinse assembly
in the 1054DD Bottle Support and orient in
such a way to minimize any undesirable
effects by the bomb exhaust discharge
from the four holes in the 1052DD Bottle
Cap. Analyze the sample in the calorimeter
in the usual fashion, using the following
guidelines in order to insure quantitative
conversion to the proper ionic form of the
analyze:
• Samples containing sulfur should
contain no more than 5% sulfur as-
burned in the calorimeter and have a
heat of combustion of at least 9000
Btu/lb.
• Samples to be analyzed for chlorine
should be spiked in a manner to insure
that the sample as-burned contains less
than 10% chlorine and liberates at least
5000 calories. Five thousand calories
corresponds to roughly a 6.4 C
temperature rise in a 1281 Calorimeter.
At the completion of the test, the collection
bottle should be unscrewed from the
1052DD bottle cap and the contents of the
combustion capsule added to the collected
washings. The bottle then may be capped
and labeled until the contents can be
analyzed.
G-2
 PARR INSTRUMENT COMPANY

211 Fifty - Third Street

Moline, Illinois 61265 USA
309 / 762-7716 800 / 872-7720
Fax 309 / 762-9453

http://www.parrinst.com parr@parrinst.com

Printed in USA
4/16/02