1271 Oxygen Bomb Calorimeter: Operating Instruction Manual
1271 Oxygen Bomb Calorimeter: Operating Instruction Manual
284MM
S/N 1 - 999
1992 Parr Instrument Company
All Rights Reserved
Table of Contents
Preface I
Scope .................................................................................................................................. I
Getting Started .................................................................................................................... I
Installation 2-1
i-i
Table of Contents
MAINTENANCE
Access to the Interior of 1271 Work Station (A750DD2)..................................................... 9-1
Time/Test Scheduled Maintenance for A750DD2 Calorimeter Mechanism........................ 9-2
Daily Maintenance (Before Testing).................................................................................... 9-2
50 to 100 Tests ................................................................................................................... 9-3
Semiannual ........................................................................................................................ 9-3
500 Tests ............................................................................................................................ 9-3
5000 Tests .......................................................................................................................... 9-7
TROUBLESHOOTING
O2 Low Pressure ................................................................................................................ 9-7
A865DD Pump Service ....................................................................................................... 9-8
Shaft Replacement.............................................................................................................. 9-8
Pneumatic Solenoid Replacement ...................................................................................... 9-9
I/O Driver Board (A1490E) Troubleshooting ....................................................................... 9-9
Sample Does Not Burn ....................................................................................................... 9-10
Open Fuse Correction......................................................................................................... 9-10
Head Extraction Procedure ................................................................................................. 9-10
1271 Head Timing Procedure ............................................................................................. 9-12
Pneumatic Cylinder Check.................................................................................................. 9-13
1271 Error Messages.......................................................................................................... 9-15
i-ii
Appendix A - Menu Operating Instructions A-1
i-iii
Table of Contents
Figure
i-iv
5-1 Cotton Thread Assembly......................................................................................... 5-1
5-2 Fill Flow Diagram..................................................................................................... 5-2
5-3 Pre-Period - Post-Period ......................................................................................... 5-4
5-4 1131 Oxygen Bomb................................................................................................. 5-5
5-5 Rinse and Cool Flow Diagram................................................................................. 5-6
5-6 Drain Flow Diagram................................................................................................. 5-8
5-7 Heat Wire Assembly................................................................................................ 5-9
5-8 Combustion Capsule with Adhesive Tape Seal ...................................................... 5-13
9-1 1271 Outer Shell Disassembly ................................................................................ 9-5
9-2 A750DD2 Work Station Wiring Diagram ................................................................ 9-20
9-3 Solenoid Wiring Schematic ..................................................................................... 9-21
9-4 Switch Wiring Schematic......................................................................................... 9-22
9-5 Pneumatic Diagram................................................................................................. 9-23
9-6 Jacket Plumbing Diagram ....................................................................................... 9-24
9-7 Plate Assembly........................................................................................................ 9-25
9-8 Internal Plumbing Diagram...................................................................................... 9-26
9-9 Loader Assembly..................................................................................................... 9-27
9-10 Controller Power Supply.......................................................................................... 9-28
9-11 Valve Assembly....................................................................................................... 9-29
F-1 Pump & Motor Assembly......................................................................................... F-8
F-2 Bomb Head Assembly............................................................................................. F-9
F-3 Pump Block Assembly............................................................................................. F-10
F-4 Oxygen Bomb Vessel Assembly ............................................................................. F-11
Tables
9-1 Fuse Assignments................................................................................................... 9-7
B-1 Settings for ISO & BSI Methods .............................................................................. B-4
D-1 Software Required................................................................................................... D-2
D-2 Cables ..................................................................................................................... D-3
D-3 Terminal Port Specifications.................................................................................... D-4
D-4 Printer Port Specifications ....................................................................................... D-4
D-5 Balance Port Specifications..................................................................................... D-5
D-6 Calorimetry Run Storage Definitions ...................................................................... D-6
D-7 Data Entered - Bit Definitions .................................................................................. D-6
i-v
Preface
To assure successful installation and These steps are offered to help the user
operation, the user must study all become familiar with, install, operate
instructions carefully before starting to and develop the full capabilities of the
use the calorimeter to obtain an Parr 1271 Calorimeter.
understanding of the capabilities of the
equipment and the safety precautions to 1. Review the Concept of Operations,
be observed in the operation. Chapter 1, to get an understanding
of the overall capabilities of the
Additional instructions concerning the calorimeter and microprocessor
installation and operation of various control.
component parts and peripheral items
CUSTOMER SERVICE
http://www.parrinst.com [email protected]
I
2. Unpack and install the calorimeter in capabilities and flexibility designed
accordance with the Installation into this instrument.
Instructions, Chapter 2. This simple,
step-wise procedure will acquaint 7. Review the Calculations, Appendix
the user with the various parts of the B. This provides information about
calorimeter and make it easier to calculations performed by the 1271
understand the operating Calorimeter.
instructions which follow.
8. Review Standardization, Appendix
3. With the tank link connection cord C. This will serve two important
between the controller and the functions. First, it provides
calorimeter disconnected, turn the instructions on generating the
power switch ON (located at the energy equivalent factor required to
back, right of the controller). Turn to calculate the heat of combustion of
the Instrument Description, Chapter unknown samples. Secondly, it will
3, to review the keyboard controls. give the user the opportunity to run
tests on a material with a known
4. Review the Program Installation and heat of combustion to become
Control, Chapter 4, to match the familiar with the instrument and
factory settings to the intended confirm that the instrument and
mode of operation. Any required operating procedures are producing
changes can be made to the results with acceptable precision.
program parameters located in the Most 1271 Calorimeters will have an
Main Menu. energy equivalent of 635 +/- 5
calories per °C. The runs for
5. Review the Reporting Instructions, standardization and determinations
Chapter 7, to become familiar with are identical, except for the setting of
the manner in which calorimetry the instrument to the standardization
corrections are entered. Also or determination mode.
discussed are generating final
reports, editing and clearing 9. Review the Communication
memory. Interfacing, Appendix D, for the
correct installation of any Smart Link
6. Turn to the Menu Operating peripherals to the 1271 Calorimeter.
Instructions, Appendix A, to review
the menu functions used to modify 10. After successful standardization, the
the program contained in the 1271 1271 Calorimeter should be ready
Calorimeter. A review of the menus for testing samples.
will provide a good idea of the
II
Concept of Operation
In the 1271 Oxygen Bomb Calorimeter, These new mechanical features support
most of the manual operations in an established technology in which
conventional bomb calorimetry have water is circulated around the bomb to
been eliminated by a new technology bring all inner parts of the calorimeter to
centered around an automatic bomb a uniform temperature rapidly, while true
and bucket loading mechanism. To isoperibol operating conditions are
perform a test, the user simply loads a maintained by an outer water jacket.
sample into a holder, attaches a short Microprocessor based, real time heat
auxiliary fuse, lowers the protective leak corrections are applied to
shield and presses the START key to implement the isoperibol jacketing
begin the procedure. method and to support the Parr rapid
dynamic method for predicting the final
New Convenience - New temperature rise. Precise temperature
Technology measurements are made with thermistor
thermometry providing 0.0001°C
The 1271 Calorimeter represents a resolution over the operating range of
blending of some new unique design the calorimeter.
features with some long proven Parr
calorimetric technology to dramatically In addition to handling all mechanical
simplify the user’s tasks during a operations, the microprocessor makes
calorimetric determination. all calculations and reports and stores
all results, as provided in earlier Parr
In this new design the bomb cylinder isoperibol and adiabatic calorimeters. A
and bucket are mounted permanently in bright, backlit liquid crystal display, 40
the calorimeter, with the bomb cylinder characters wide, 15 lines high, prompts
held in an inverted position. A loading the operator through all setup and
mechanism raises the head and sample operating steps with on-screen menus
into the open bottom of the cylinder and which make user training quite simple.
seals the bomb with a 23-degree twist,
1-1
1-2
Installation
2-1
Installing the Calorimeter detected must be stopped before
proceeding.
Set the calorimeter mechanism on a
level, sturdy bench or table in a location The fill cycle is described in the
that is reasonably free from drafts and is Operating Instructions, Chapter 5, Page
protected from sources of radiant heat, 5-2.
preferably in an air-conditioned room.
The regulator was set at the factory to
The closed water handling system and deliver oxygen at 450 psig, the re-
water cooler may be placed on the commended charging pressure, and
same working surface as the calorimeter should be checked before using the
mechanism, or below it. system by observing the pressure
attained during an actual filling
Note: operation.
There is a five foot restriction on the
interconnecting tubing between To do this, cycle the calorimeter without
each of these three sub-assemblies. a charge and observe the delivery
pressure as shown on the 0-600 psi
Installing the Oxygen Filling gage while the bomb is charging. Adjust
System the regulator, if necessary, to bring the
pressure to 450 psig. If there is any
The 1271 Calorimeter is equipped with doubt about the setting, release the gas
an automatic bomb filling system. It from the bomb and run a second check.
consists of a pressure regulator
(A570DD) which is mounted on the Note:
oxygen tank and a control and During extended periods of inactivity
measurement system mounted in the (overnight or longer), close the tank
calorimeter case. valve to prevent leakage. When
changing oxygen tanks, close the
To install the regulator, unscrew the tank valve and pull the relief valve to
protecting cap from the oxygen tank and exhaust the system. Do not use oil or
inspect the threads on the tank outlet to combustible lubricants on this filling
be sure they are clean and in good system or on any devices handling
condition. oxygen under pressure. Keep all
threads, fittings and gaskets clean
Place the ball end of the regulator in the and in good condition.
outlet and draw up the union nut tightly,
keeping the gages tilted slightly back The recommended 450 psig filling
from an upright position. pressure is slightly higher than the
30 atm prescribed in Parr bomb and
Connect the regulator so that the arrow calorimeter instruction manuals.
of filter is pointing toward the tower if This difference is insignificant.
only one tower is used. Otherwise, Higher or lower settings can be
connect the regulator so that the arrow used, but the bomb must never be
is pointing to one leg of the 353VB male filled to more than 600 psig (40atm).
tee connector and attach the other two If pressures below 28 atm are used,
legs of the tee to towers one and two the low pressure warning will always
with high pressure, 1/8" diameter, nylon occur.
tubing. All connections should be
checked for leaks and any leaks
2-2
Installation
Plumbing
2-3
Figure 2-1
1271 Calorimeter External Plumbing – 1 System
2-4
2-5
Note:
When only one tower is connected, the tower. Connection 12 (see Figure 2-
make loop connections from 1 and 2-8) should be made with tubing
connection 5 to connection 6, and packaged with the nitrogen gas
from connection 2 to connection 4 regulator. The nitrogen tank must have
on the Water Handling System. the CGA-580 fitting.
Install the 1551 Water Cooler so that Two Tower Setup. Connection 12
heat from the compressor will not should be made with tubing packed with
produce adverse effects on the the nitrogen regulator and teeing into
calorimeter. one leg of the 354VB (1/4" tee), and the
other two legs of the tee should be
In any installation, allow a minimum connected to the towers. The nitrogen
clearance of 6 inches in front of the unit, tank must have the CGA-580 fitting.
3 inches in the rear and at least 1 inch
on the sides for circulation. Caution:
USE DISTILLED WATER ONLY
Set the cooler on a firm base and slide
the two 7-1/2" edge strips onto the steel The rinse tank should now be filled with
housing at the base of the unit. 16 liters of distilled water through the
large opening at the top of the tank. The
Install the two 362VB Union Elbows on cover for this opening is removed by
the water inlet and outlet tubes on the lifting up on the handle, lowering lid,
cooler (see Figure 2-3). All water tilting and removing. Replace and close
connections should be made with the the cover after filling with water.
furnished 3/8" tubing. Install 3/8" inserts
(183VB) in all ends of tubing. Both the oxygen and pneumatic
supplies should be turned on at this
Note: time. A hissing sound will occur for
Do not connect power to the several minutes as the rinse tank is
cooler at this time. pressurized. The pneumatic supply
regulator should be adjusted to 100
Connect Line No. 7 and 8 of the closed psig.
water handling system to the water
cooler.
2-6
Installation
Note:
To refill the rinse tank after the (left rear) of the water handling system
calorimeter has been placed into is up or floated.
service, the tank must be
depressurized by first turning off the The amount of wetting agent added will
pneumatic supply and then opening depend on the type of water used for
the toggle valve on top of the rinse filling the reservoir. Tap water would
tank. require about 30mL, and de-ionized or
distilled water would require about .3
Connections 13-15 (see Figure 2-1 and mL. All make-up water used thereafter
2-8) are made with the three tube should have the same concentration of
assemblies, each containing: the wetting agent. There should be a
thin layer of suds across the entire
• 10 feet of 1/8" O.D. nylon tubing, surface of water in the Water Handling
(oxygen fill vent connection #13) System. Add wetting agent sparingly as
• it requires 24 hours for wetting agent to
3/8" O.D. “Bev-A-Line” tubing with mix with all the water in the system.
the bomb exhaust diffuser assembly
at one end.(Bomb Vent, connection Electrical Connections
#14)
Refer to Figure 2-4 for the 1271
• 5/8" O.D. “Bev-A-Line” tubing.(Drip Calorimeter System electrical hookup.
Pan, connection #15).
Link Connections
The end of the assembly with the
exhaust diffuser should be inserted into Connect the A1570E Control Link Cable
the 10 liter carboy (231C2) which should between the controller and the
be placed on the floor or a level lower calorimeter mechanism (see Figure 2-8
than the tower mechanism. and 2-9).
The optional connection for “make-up Connect the A1330E Tank Link Cable
water in” on the closed water handling between the calorimeter mechanism
system may be made at this time. This and the closed water handling system
connection requires 1/4" tubing (not (see Figure 2-5 and 2-8).
supplied). The small daily of loss of
water from the 1271 Calorimeter System For thermometry connections, connect
can usually be conveniently made up by one A1335E Cable between the closed
filling directly through the large opening water handling system and the controller
on top of the closed water handling to establish the calorimeter jacket
system. The latter method is preferred. temperature probe connection (see
Figure 2-5 and 2-9).
The 20 liter reservoir of the closed water
handling system should be filled through Connect the remaining A1335E Cable
the top opening at this time. The between the calorimeter mechanism
reservoir should be filled until the top and the controller to establish the
level switch located on the inside cover calorimeter temperature probe
connection.
2-7
For power connections, connect the
supplied power cord to the calorimeter
mechanism. Plug the power cord into
the proper 110 or 220 VAC power
source. The power switch at the rear of
the calorimeter mechanism may be
turned on at this time. Connect the
supplied power cord to the controller.
Plug the power cord into the proper 110
or 220 VAC power source.
Note:
Do not power up the controller at
this time.
2-8
Installation
2-9
If only one Smart Link cable is plugged
into the rear of the controller, (end of link If you purchased a two tower system
position) no changes of the switch you may begin the power up sequence
settings are required. of the controller as the controller has
been configured with both A/D boards at
If two cables are required, (middle of link the factory. If you are installing a
position) then the switches will need to recently added second tower, you must
be set to the OPEN or OFF position, install the second A/D board in the
down = off. This may be done by controller. Remove screws from the rear
removing the two screws (controller location of cover assembly and pivot the
rear) securing the cover of the cover assembly forward to reveal card
controller. Swing the cover, which is cage assembly which has slot three
hinged at the front, to the fully upright available for the A/D board. Carefully
position. insert the A/D board and attach the
polarized ribbon connector, the black
The termination switches for the Smart polarized line connector and the six pin
Link are located at the center, top edge connectors from the thermistor BNC
of the circuit board, immediately behind connector to location F on the board,
the communication connectors on the close the cover and proceed with the
rear of the controller. The switch is power-up sequence.
labeled SW1.
The ON switch of the controller is
Change the switch settings as required located at the back, right of the
and close the cover, taking care not to controller. The Parr logo and firmware
pinch any wires or cables. Install the two revision will be shown briefly, and then
screws to re-secure the case. the Main Menu will be displayed. Press
the PRINT SCREEN key to verify
Printer correct printer operation.
Initial Calorimeter System Startup Fully lower and latch the Lexan plastic
guard around the sample loading area.
Note: The shield should pop back to the raised
At this time power-up the A750DD position after 10 seconds. This
workstation(s) prior to power-up of operation verifies the presence of
the A800DD Controller to ensure pneumatic pressure.
proper I/O download to the tower.
2-10
Installation
2-11
2-12
Instrument Description
Any page or line number on a page can 3. Value Entry Fields. These data
be selected by: fields are used to enter data into the
calorimeter. Most data fields will accept
Cursor Control - The up and down any value entered by the user through
arrow keys can be used to move the the keyboard. Certain data fields may
reverse video to the desired page/line only accept certain values from a table
number. Once the desired page/line built into the menu similar to the option
number is highlighted, press ENTER. selection described above. Once the
correct value is displayed in the field,
Note: press the ENTER key to record the
When the cursor highlights the line value.
number and title, as opposed to the
data field, a page or sub-menu can 4. Data Displays. Most of these data
be accessed by pressing ENTER. fields display values that have been
(See Command Codes in this calculated by the calorimeter and are
chapter.) informational only. Certain ones can be
overridden by the user entering a
Number Control - Page/Line numbers desired value through the keyboard.
can also be selected by simply pressing
3-1
5. Command Codes. Line numbers
that access sub-menus or statements Key Description
initiating an action (the controller will
ask, “Do you wish to continue (Yes or ↑ Moves the cursor up on
No?” to prevent accidental disruptions to any of the menu pages.
the program and/or stored data).
← NO Changes menu functions
Note: that are either an
To return to previous pages from a ON/OFF or YES/NO
submenu, press ESCAPE. To return toggle to OFF, NO, or to
to the Main Menu, press SHIFT, select an option from the
ESCAPE. list provided.
3-2
Instrument Description
3-4
Program Installation & Control
Software Installation
Revised Default Settings
The program in the 1271 Controller can
be extensively modified to tailor the unit The default parameters of the 1271
to a wide variety of operating conditions, Controller can be changed to guarantee
reporting units, laboratory techniques, that the 1271 Calorimeter, when cold
available accessories and restarted, will always be in the desired
communication modes. configuration before beginning a series
of tests.
In addition, the calculations,
thermochemical corrections and Users who wish to permanently revise
reporting modes can be modified to their default settings may do so using
conform to a number of standard test the following procedure:
methods and procedures.
Establish the operating parameters to
Numerous provisions are included to be stored as the user default settings.
permit the use of other reagent
concentrations, techniques, combustion Go to Page 3, Line 9 - Copy Current
aids and short cuts appropriate for the Setup to EEPROM, and press ENTER.
user’s work.
Press YES, the controller will prompt the
Note: user for a “User Rev.”. This can be any
Changes to the program are made number that is helpful in identifying the
by use of the menu structure user’s setup. Enter number and press
described in Appendix A of this ENTER.
manual. Any of these items can be
individually entered at any time to To re-load the user default setting, go to
revise the operating program. Page 3, Line 8 - Re-load User Default
Settings, press ENTER and YES.
Default Settings
4-1
4-2
Program Installation & Control
4-3
4-4
Program Installation & Control
4-5
4-6
Operating Instructions
5-1
5-2
Operating Instructions
5-3
5-4
Operating Instructions
Drain
1. The controller monitors the
temperature rise and determines the At the completion of the bomb rinse
final temperature rise by either the sequence, the drain sequence begins
dynamic or equilibrium criteria as (see Figure 5-6).
established by the user.
1. The water in the bucket is pumped
2. Once the final temperature rise is out of the bucket and back into the
determined, it is recorded with the closed water system.
test results.
2. Once the bucket is pumped dry, the
At the completion of the post-period, the bomb head is opened and lowered
rinse and cool sequence begins for the preparation of the next
(see Figure 5-5). sample.
5-5
5-6
Operating Instructions
• Do not overcharge the bomb with To avoid damage to the bomb and
too much oxygen. The initial calorimeter, and possible injury to
charging pressure should not the operator, it should be a standing
exceed 40 atm (590 psig). rule in each laboratory that the bomb
must never be charged with more
• Do not fire the bomb if there is than 1.5 grams of combustible
any indication that it is leaking. material.
5-7
5-8
Operating Instructions
Note:
This wire needs to be 1.5 inches or 4
cm long. Longer lengths will not get
hot enough to ignite the thread and
shorter lengths will get too hot and
will have a short service life.
5-9
Samples and Sample Holders in order to control the burning rate.
Moisture content up to 20% can be
Particle Size and Moisture Content. tolerated in many cases, but the
Solid samples burn best in an oxygen optimum moisture is best determined by
bomb when reduced to 60 mesh, or trial combustions.
smaller, and compressed into a pellet
with a 2811 Parr Pellet Press. Combustion Aids. Some samples may
be difficult to ignite or they may burn so
Large particles may not burn completely slowly that the particles become chilled
and small particles are easily swept out below the ignition point before complete
of the capsule by turbulent gases during combustion is obtained. In such cases
rapid combustion. powdered benzoic acid, white oil or any
other combustible material of known
Note: purity can be mixed with the sample.
Particle size is important because it Ethylene glycol, butyl alcohol or decalin
influences the reaction rate. may also be used for this purpose.
Compression into a pellet is
recommended because the pressure Note:
developed during combustion can be It must be remembered, however,
reduced as much as 40% when that a combustion aid adds to the
compared to the combustion of the total energy released in the bomb
material in the powder form. In and the amount of sample may have
addition to giving controlled burn to be reduced to compensate for the
rates, the pelletizing of samples added charge.
keeps the sample in the fuel capsule
during combustion. Also, when benzoic acid is
combusted for standardization runs
Materials, such as coal, burn well in the or for combustion aid purposes, it
as-received or air-dry condition, but do should be in the form of a pellet to
not burn completely dry samples. A avoid possible damage to the bomb
certain amount of moisture is desirable which might result from high
in order to control the burning rate. pressures developed by the rapid
Moisture content up to 20% can be combustion of the loose powder.
tolerated in many cases, but the
optimum moisture is best determined by Combustion Capsules. Non-volatile
trial combustions. samples to be tested in Parr oxygen
bombs are weighed and burned in
If moisture is to be added to retard the shallow capsules measuring
combustion rate, drop water directly into approximately 1" diameter and 7/16"
a loose sample or onto a pellet after the deep. These are available in stainless
sample has been weighed. Then let the steel, fused silica and platinum alloyed
sample stand for awhile to obtain with 3-1/2% rhodium.
uniform distribution.
5-10
Operating Instructions
Stainless steel capsules (43AS) are is heat sensitive and cannot be dried, a
furnished with each calorimeter. When water soluble combustion aid such as
combusting samples that contain metal ethylene glycol can be added to
particles such as aluminum or promote ignition.
magnesium, the non-metallic (fused
silica) 43A3 Capsule is required, or Coarse Samples. In most cases it may
where the superior corrosion resistance be necessary to burn coarse samples
of a Pt-Rh, the 43A5 Capsule is without size reduction since grinding or
required. The stainless steel capsules drying may introduce unwanted
will acquire a dull gray finish after changes. There is no objection to this if
repeated use in an oxygen bomb due to the coarse sample will ignite and burn
the formation of a hard, protective oxide completely. Whole wheat grains and
film. This dull finish not only protects the coarse charcoal chunks are typical of
capsule, but it also promotes materials which will burn satisfactorily
combustion and makes it easier to burn without grinding and without additives or
the last traces of the sample. a special procedure.
5-11
Rather, they should be tested in a model Note:
1261 Calorimeter which can be Tape should always be stored in a
equipped with an 1104 High Pressure sealed container to minimize
Oxygen Bomb designed specifically for changes in its moisture and solvent
these types of samples. content.
Volatile Sample Holders. Volatile Use the following procedure when filling
samples can be handled in a Parr 43A6 and handling any of these tape-sealed
Platinum Capsule with a spun rim, or in sample holders:
a Parr 43AS Alloy Capsule which has a
sturdy wall with a flat top rim. These • Weigh the empty cup or capsule;
holders can be sealed with a disc of then cover the top with tape, trim
plastic adhesive tape prepared by with a knife and press the trimmed
stretching tape across the top of the cup edge firmly against the metal rim.
and trimming the excess with a sharp Also cut and attach a small flag to
knife. The seal obtained after pressing the disc (see Figure 5-8).
this disc firmly against the rim of the cup
with a flat blade will be adequate for • Puncture the tape at a point below
most volatile samples. the flag, then re-weigh the empty
cup with its tape cover.
The tape used for this purpose should
be free of chlorine and as low in sulfur • Add the sample with a hypodermic
as possible. Borden Mystic Tape, No. syringe; close the opening with the
M-169-C or 3M Transparent Tape, No. flag and re-weigh the filled cup.
610, are recommended for this purpose.
The 3M Transparent Tape can be • Set the cup in the loop electrode and
ordered through Parr, Part No. 517A. arrange the auxiliary fuse so that it
touches the center of the tape disc.
The weight of the tape disc must be
determined separately and a correction • Just before starting the test, prick
applied for any elements in the tape the disc with a sharp needle to make
which might interfere with the a small opening which is needed to
determination. This can be done by prevent collapse of the disc when
running a blank test with tape alone pressure is applied.
using a sample weighing 1.0 gram. The
compensation for heat of tape may be • Fill the bomb with the usual oxygen
done through the spike option; see Page charging pressure.
2.3 - Spike Controls, Line 2 - Heat of
Combustion of Spike.
• The calorimeter will fire the bomb
and complete the test in the usual
manner.
5-12
Operating Instructions
Low volatile samples with a high water • The combustion must produce
content, such as urine or blood, can be sufficient turbulence within the bomb
burned in an open capsule by absorbing to bring oxygen into the fuel cup for
the liquid on filter paper pulp or by burning the last traces of the
adding a combustion aid, such as sample.
ethylene glycol.
• Loose or powdery condition of the
Operating Suggestions sample which will permit unburned
particles to be ejected during a
Poor Combustion. Because of the violent combustion.
difference in combustion characteristics
of the many different materials which • The use of a sample containing
may be burned in an oxygen bomb, it is coarse particles which will not burn
difficult to give specific directions which readily. Coal particles which are too
will assure complete combustions for all large to pass a 60 mesh screen may
samples. not burn completely.
5-13
1551 Water Cooler Operating
Instructions
5-14
Corrections & Final Reports
Fuse Correction
Key in the Fuse/Heat Wire 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 Correction
Key in the Acid 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
6-2
Reporting Instructions
The 1271 Controller can transmit data There are two kinds of calorimeter
two ways: reports; preliminary and final.
7-1
To stop printing:
7-2
Memory Management
The controller will hold data for 500 tests Editing Memory
within its memory. These tests may be
either preliminary, final, determination, The user can add or change previously
or calibration reports. Once the memory gathered test information. This feature is
of the controller is filled, any attempt to implemented with the F3 key principally
start a new analysis will cause the to permit editing of sample weights or
controller to display “RUN, LIST, FULL”. other information.
The user must then clear some of the
memory before proceeding or use the To revise the sample weights, spike
overwrite capability on Page 7, Line 6. weights, Cal ID number, fuse, acid,
sulfur or hydrogen values on final
Clearing Memory reports:
Note:
This sequence can be canceled by
pressing the RESET key.
8-1
8-2
Maintenance & Troubleshooting
9-1
Time/Test Scheduled Maintenance Excessive use of the 811DD lubricant
for A750DD Calorimeter will diminish the cleanliness of the
Mechanism bucket interior. This results in a
reduction in instrument precision.
Note: Finally, clean the perimeter of the head.
Does not include 1131 bomb cylinder Note: do not allow any lubricant to
and head pressure retaining parts come in contact with the interior
which have a maintenance interval of portion of the combustion bomb or
500 firings. any of its sealing surfaces! Possible
ignition of the lubricant and
Daily Maintenance (Before subsequent damage to the
instrument may result.
Testing)
Clean and re-lubricate the 857DD O-ring
Note:
on the head loader rod.
Remove the head from the loader
rod. Clean small quad-ring that seals
Clean electrode contact strips with mild
the bomb head and cylinder by
abrasive, such as a pencil eraser.
wiping with a tissue. Wet this sealing
area with water prior to starting a
Clean bomb head electrode points in a
series of tests. Clean corresponding
similar fashion. Tighten screws holding
sealing area in cylinder in a similar
fuse wire in place.
fashion. Both surfaces must be free
of any accumulated foreign matter,
such as unburned sample material or
combustion by-products. Clean the
hole in the center of the head which
accepts the loader rod. With a
tissue, clean the head where the
large bucket quad-ring contacts the
head perimeter. Wet this sealing
area with water prior to starting a
series of tests. Remove, inspect and
clean head sealing/pressure release
pin and corresponding sealing area
in the bomb head. In extreme cases,
i.e. a spilled sample, use soap and
water.
9-2
Maintenance & Troubleshooting
50 to 100 Tests
Semiannual
500 Tests
9-3
9-4
Maintenance & Troubleshooting
9-5
9-6
Maintenance & Troubleshooting
Note: TROUBLESHOOTING
Installation Instructions for the
667DDJV Quad-Ring - These quad- O2 Low Pressure
rings are identified with a yellow
mark on the outside perimeter. This This message indicates the bomb has
mark must be visible on the outside not filled to 400 psig within 40 seconds.
perimeter after installation in order Possible causes are the oxygen tank
to insure that the quad-ring has not may have insufficient oxygen pressure,
been “rolled”. A quad-ring that is the regulator is not set to deliver 450
rolled or twisted will not seal psig, the pin valve in the bomb head has
properly. not seated properly due to foreign
matter around the pin, an oxygen leak is
5000 Tests in the oxygen control solenoids or in the
oxygen feed tubing between the
Replace gear pump assembly and solenoids and the bomb cylinder, or the
center plastic portion of motor coupler. vent solenoid on the 322VB Valve
Assembly may be leaking on the fill
Replace large quad ring that seals cycle. The oxygen solenoid is
bucket. Lube 719DD slide rod at rear of accessible by following instructions for
loader mechanism with light machine oil. step 1 and 2/3 in Access to the Interior
Return the 1131 bomb to the factory for of 1271 Tower (A750DD) section of this
recertification. chapter.
Table 9-1
Fuse Assignments
9-7
A865DD Pump Service 4. Remove the pump seal (690DD)
using a pair of locking forceps,
Parr recommends that the A865DD taking care not to mar or gouge the
pump assembly be replaced or serviced pump cover (681DD). Discard the
at a 5000 test interval in order to old pump seal.
maintain reliable operation. This
replacement is necessitated due, in 5. Remove the snap ring (682DD)
large part, to wear of the water seal using snap ring pliers (Parr part no.
used in this assembly. Parr has 356HCW) and the wave spring
provided this assembly as a complete (683DD).
tested unit to end users due to the
involved nature of fitting a new seal into 6. Pull the shaft (685DD) and bearings
the assembly. A recent modification to a (684DD) from the pump cover as a
part used in this assembly has greatly unit.
simplified the installation and
replacement of the water seal, thus 7. Remove the bearings from the old
making field installation practical. This shaft and fit them on the new shaft.
improvement may result in lower cost of Discard the old shaft. Old shafts can
ownership for those users capable of not be modified to incorporate the
performing the service, outlined below, new groove detail.
on the water pump assembly. Original
1271 Calorimeter pump assemblies 8. Reverse the above procedure to
required that the seal be cemented in reassemble the pump assembly,
place in order to restrict the movement fitting a new water seal to the shaft.
of the seal during calorimeter operation.
New pump assemblies use a modified Seal replacement in pumps that
pump shaft (685DD), incorporating a incorporate a new shaft involves simply
recessed area for the seal. This pulling the old seal from the shaft, with
modification has been demonstrated to small tipped locking type forceps, and
be effective at properly holding the seal fitting a new one in its place. Make sure
in place during calorimeter operation. that the new seal is properly aligned in
Old pump assemblies can be upgraded the groove behind the driven gear.
to use this new shaft using the following
procedure. Caution:
Fitting a new seal, as described
Shaft Replacement above, to an old shaft, without the
new groove detail, will result in
1. Parts required are 685DD shaft and erratic calorimeter operation.
690DD seal.
Heavily worn pumps may have a grove
2. Remove the plastic gears (689DD) worn into the pump cover where the
and shaft key (688DD). seal lip contacts the cover. Fitting a new
seal to an excessively worn cover may
3. Remove the motor coupler (869DD) not result in a reliable, long lasting seal.
using a 1/32" Allen wrench (Parr part If this is the case, replacement of the
no. TX03SK). pump cover (681DD), with the 687DD
idler shaft cemented in place, is the only
recourse.
9-8
Maintenance & Troubleshooting
9-9
Problem - All Hall Effect switch inputs a wire or screwdriver. If the beeping
are not being sensed properly, stops and the display says
producing head up/down/open/closed “charging”, then the internal circuitry
errors. is ok. If ok, proceed with step three.
9-10
Maintenance & Troubleshooting
9-11
It is recommended that O-rings,
gaskets and seals be replaced by the Indications - Head is slightly mistimed.
user after 500 firings or at more
frequent intervals if the bomb has Solution - Manually load and unload the
been subject to heavy usage or bomb head to and from the cylinder by
shows any evidence of damage from direct manipulation of the loader
over pressure or other causes. mechanism. Head open, head up, head
closed, head open, head down.
1271 Head Timing Procedure
Determine whether the head is under or
Goal - To position the head so that over rotated at the head down step.
there is no mechanical interference of
the lugs on the head with the Loosen the SB2520SC12 fastener that
corresponding lugs of the cylinder locks the 739DD to the 733DD rod,
during a head up and/or head while the head is up, and adjust the
extraction. position (extension) of the open/ closed
air cylinder to eliminate the under/over
Preliminary Steps - Refer to figure 9-9. rotation.
First, check that the sets screws that
hold the 734DD to the 733DD are tight. Firmly tighten the SB2520SC12 fastener
Loose set screws here will result in that locks the 739DD to the 733DD rod.
symptoms (head down errors) that
otherwise would require re-timing. Repeat the manual loading
Tighten as required and check by doing operation/adjustment to obtain smooth
a head-up/get head cycle on page 9.7. If operation.
the problem persists, remove the front
cover assembly. Confirm correct timing by doing head
up/get head cycle(s) via the 9.7 menu.
Go to the Controller Main Menu and
press SHIFT 1. Make sure that the Problem - Head will not go into the
loader mechanism can fully rotate the cylinder (Head lugs hit cylinder lugs).
1/16th of a turn (22.5 degrees) as
indicated by the Input Image on the Indications - Head is grossly mistimed.
SHIFT 1 screen. The Input Image on the
SHIFT 1 screen will read 6 in the left Solution - Loosen socket head set
most position with the loader rod down screw in the 739DD (Arm). This is
and open. In the down and closed located at the bottom of the 733DD twist
position the screen will read 5. Failure to tube. This should allow the 734DD
achieve full rotation will result in head rotator collar to spin freely.
insertion/withdraw problems. Identify the
cause of the under-rotation and correct With the bomb head on the 734DD
as required. rotator collar, and the open/closed air
cylinder in the open (extended) position,
Problem - Head up operation works fine the loop electrode should be on the right
and get head operation produces head and the straight electrode should be on
down errors, with the loader rod “stuck” the left.
in the up position.
9-12
Maintenance & Troubleshooting
Manually lift the loader mechanism up to fully penetrates the cylinder, the input
put the head in the cylinder, keeping the image should have an “a” in the left
open/closed air cylinder in the extended most position, which indicates the head
position. Rotate the head, slightly, as is up and open (8 hex plus 2 hex equals
needed to center the head lugs between “a” hex). See the HELP screen
the cylinder lugs. associated with the I/O Diagnostics for
this and other related input bit
Firmly tighten the SB2520SC12 fastener assignments. If the input image shows 2
that locks the 739DD to the 733DD twist then the head up sensor is not coming
tube. on. The next section will describe how to
adjust the position of the head up
Manually load and unload the bomb sensor.
head to and from the cylinder by direct
manipulation of the loader mechanism. Head Up Sensor Alignment - Exit the
Put the head into the following positions: I/O Diagnostic routine. Remove the
Head open, head up, head closed, head head and the drip pan. Unscrew the
open and head down. bomb rinse fitting, where the bomb
washings exit the instrument. Follow
Repeat the manual loading steps 1 thru 4 on page 9-1 of the 1271
operation/adjustment to obtain smooth Operating Instruction Manual to remove
operation. the front cover assembly. Press 9, 2, 3
from the main menu to enter the I/O
Confirm correct timing by doing head Diagnostic routine again. Install the
up/get head cycle(s) via the 9.7 menu. bomb head onto the loading rod. Turn
on head open followed by head up to
Pneumatic Cylinder Check drive the head into the cylinder. There
are two sensors which are clamped to
There are two pneumatic cylinders in the gas cylinder to indicate the position
the 1271 Calorimeter that control head of the cylinder to the controller. The
operations, head open/close and head lower sensor is the head up sensor. The
up/down (see figure 9-5). There is a sensors have a built in light which
sensor for indicating each of the four illuminates when the switch is on. The
possible head positions: head up, head sensor is activated when a magnet,
down, head open and head closed (see attached internally to the gas cylinder
figure 9-5). The failure of any given piston, is directly underneath the sensor.
sensor to operate properly can result Loosen the clamp with an Allen wrench
from an electrical failure of the switch or and slide the sensor and clamp as a unit
because it is incorrectly positioned on to the middle of the active magnetic
the pneumatic cylinder. area on the gas cylinder. The light
should come on and the controller
Checking the Head Up Sensor - Press should indicate an “a” in the left most
9, 2, 3 from the main menu to enter the input image position. If the sensor light
I/O Diagnostics. Arrow down to head comes on but the controller diagnostic
open and turn it on. Arrow up to head up screen does not respond correctly, the
and turn it on. Assuming that the head sensor should be replaced.
9-13
The center of the active magnetic area the instrument tools provided, remove
can be easily determined as follows: the 7/16" compression nut that secures
the oxygen filling line to the 338VBAD
With the sensor light on, slide the connection which is threaded into the
sensor up until the light goes off, and top of the bomb cylinder. Remove the
mark this position on the gas cylinder 338VBAD connector, and with tweezers
with a pencil where the top of the sensor remove the 643DD check valve.
meets the cylinder. Then slide the Remove the 642DD nut with socket
sensor and clamp down, turning the light wrench and with free hand grasp the
on and off. Mark this lower position bottom of the cylinder via the loading
where the light just turns off. The center chamber so as to catch the cylinder
of the active magnetic area is halfway when free from bucket chamber.
between these two marks. Move the top
of the sensor to this midpoint position Note:
and tighten the clamp. Withdraw the bomb cylinder and
note the position of the notch in the
Make sure the sensor is rotated to the 646DD Brass Outer Ring. Insert the
right, and not positioned toward the front replacement bomb with the notch of
of the instrument. If the sensor is the ring in the correct position to
positioned (rotated) to the front of the engage the pin in the front and
instrument, it will rub on the inside of the center of the bucket chamber and
front cover assembly when the head secure cylinder with 642DD Nut.
goes up and down, and will become
mis-adjusted. Bomb Repairs and Proof Tests. Parr
oxygen bombs can be returned to the
Other Sensors - The other three factory at any time for repair and testing
sensors can be checked and adjusted in in accordance with ANSI/ ASTM E144-
a similar fashion, by positioning the 94, “Recommended Practice for Safe
head in the appropriate position and Use of Oxygen Combustion Bombs”.
observing the correct response. The
head down sensor (upper) can be Ship prepaid to Parr Instrument
checked or aligned in a manner similar Company, ATTN: Repair Department,
to that used for the head up sensor, 211-53rd Street, Moline, IL, 61265.
except that the loader rod is in the idle
(down) position. The head open and Send a Purchase Order with the
head close sensors may be checked by shipment, provide return shipping
manually rotating the head open and instructions and the name and
closed. The input image on the I/O telephone number of the person to be
Diagnostic screen will read 6 in the left contacted if questions arise concerning
most position with the loader rod down repair costs or other problems.
and open. In the down and closed
position the screen will read 5. The Note:
alignment procedure is similar to that No repairs will be started without a
used for the head up/down sensors. purchase order.
Oxygen Bomb Service. Follow steps 1 Individual repair parts can be ordered
and 5 in Access to the Interior of 1271 from any Parr dealer or direct from the
Work Station (A750DD). Remove the factory.
head from the loader mechanism. With
9-14
Maintenance & Troubleshooting
Error: 60/61
Cal Not Ready - The calorimeter is busy
performing another function i.e. a
pretest cycle.
9-15
Error: 78/79 either because the switch has failed, the
02 Low Pressure - The pressure in the switch is not positioned correctly or the
oxygen feed line to the bomb is less cylinder is not moving to the down
than 400 psig (see Troubleshooting position.
Chapter).
Error: 92/93
Error: 80/81 Up Position Sensor Error - The up
02 Leak - The system did reach the switch on the up/down pneumatic
correct oxygen pressure. However, cylinder for the head is not functioning
before starting the test procedure, a either because the switch has failed, the
recheck of oxygen pressure to bomb switch is not positioned correctly or the
indicated the oxygen pressure was less cylinder is not moving to the up position.
than 450 psi which indicates a leak.
Check all internal oxygen feed lines for Error: 94/95
leaks. Open Position Sensor Error - The head
open switch on the head open/ close
Error: 82/83 pneumatic cylinder is not functioning
H20 Fill Time-out - The bucket did not fill either because the switch has failed, the
with water in the allotted time as switch is not positioned correctly, or the
indicated by the motor current. The pneumatic cylinder is not moving to the
water filter in the water feed line open position.
connected to connector No. 2 may need
replacement. A visual check of the water Error: 96/97
lines for the bucket will confirm that Closed Position Sensor Error - The
water is entering the bucket. Check the head closed switch is not functioning
859DD coupler to see that it is still either because the switch has failed, the
functioning between the motor and the switch is not positioned correctly or the
stirrer assembly (see Figure F-1). pneumatic cylinder is not moving to the
closed position.
Error: 84/85
Cool Down Time-out - The temperature Error: 102/103
in the bucket did not reach the Run In Progress - The calorimeter is not
necessary temperature for starting the available to do another function as it is
next test in the allotted time. The filter in busy running a test.
the cold water line to connector No. 1
may be plugged or the cooler may not Error: 104
be functioning properly, i.e. insufficient Error Tank - Low Water Level - The
coolant. level switch in the water handling
system indicates that the water level
Error: 86/87 dropped and more water needs to be
Drain Time-out - The calorimeter was added. After adding more water add
unable to drain in the allotted time as more photoflow to maintain 50% surface
indicated by the motor current. The area with bubbles.
controller will not allow automatic
extraction of the bomb head if this
message occurs.
Error: 90/91
Down Position Sensor - The head down
switch on the up/down pneumatic
cylinder for the head is not functioning
9-16
Maintenance & Troubleshooting
9-17
Error: 140 below 100 psig. The problem is
Sulfur Value Already Entered - Indicates insufficient pressure at the pneumatic
that the sulfur correction is in the source, the regulator is not set to 100
controller’s memory for the Sample ID psig, or a filter is plugged to the work
entered. station.
9-18
Maintenance & Troubleshooting
Error: 187/189
Open Bucket Probe - The controller has
sensed a very low temperature in the
bucket probe. The probe has an open
circuit and needs to be replaced. The
internal cable from BNC connector at
the rear chassis is not attached to
connector H on the DIO board inside the
controller.
Error: 188/190
Open Jacket Probe - The controller has
sensed a very low temperature in the
bucket probe. The probe has an open
circuit and needs to be replaced.
Error: 195/196
Refill Bomb Rinse Tank - The counter
for rinse washing is at zero. Refill the
rinse tank. Reset the bomb rinse
counter after refilling rinse tank (see
Page 2.4).
9-19
9-20
Maintenance & Troubleshooting
9-21
Figure 9-4
Switch Wiring Schematic
9-22
Maintenance & Troubleshooting
Figure 9-5
Pneumatic Diagram
9-23
9-24
Maintenance & Troubleshooting
9-25
9-26
Maintenance & Troubleshooting
9-27
9-28
Maintenance & Troubleshooting
9-29
9-30
Appendix A - Menu Operating Instructions
When the START key is pressed, the Line 1 - Operating Mode. Sets the
calorimeter will prompt the user for the operating mode by toggling between
Sample ID number. If the automatic standardization and determination.
Sample ID is turned ON, the next
sample will be displayed and if it is Line 2 - Bomb Installed/EE. Used to
correct, press ENTER. If it is not correct, identify the bomb presently installed in
press CLEAR ENTRY and key in the the calorimeter and its EE value.
correct identification number followed by
ENTER. The instrument will then prompt Line 3 - Heater and Pump. Used to
for sample weight, if set up for keyboard switch ON and OFF the heater and
entry. Again, key in the weight followed pump in the water handling system.
by ENTER. If the weight is set up for
automatic transfer, the value will be Note:
displayed and entered directly. Spiking, The heater and pump must be turned
if activated, is entered the same as the ON to bring jacket to the correct
sample weights. starting temperature before testing
can commence.
The settings and controls are organized
into nine main sections or pages which Operating Controls
comprise the Main Menu. This chapter Page 2
describes all pages of the menu-based
operating system of the 1271 Controller. Line 1 - Method of Operation. Offers
an operating mode of either dynamic or
Calorimeter Operation equilibrium. In most cases, the dynamic
Page 1 mode with its curve matching capability
will save approximately 3-4 minutes per
The calorimeter will normally be test and will produce the same operating
operated from Page 1, although tests precision as the slower equilibrium
can be started from many Main Menu mode for most samples.
pages. If the second calorimeter
(Calorimeter II) is installed, the data will Line 2 - Reporting Units. Offers a
be displayed automatically in the second choice of Btu/lb, Cal/g, J/kg or MJ/kg for
data field column. If only Calorimeter I is the reporting units.
present, the display is simplified
accordingly. The number of free areas in Line 3 - Use Spiking Correction.
the memory and the number of rinses Accesses sub-menu, Page 2.3 - Spiking
left in the wash tank are always Controls. Spiking is the material
displayed at the top of this page. addition, such as benzoic acid or
mineral oil, to samples which are difficult
At the bottom of the page is a “status to burn in order to drive the combustion
bar”. This bar provides the current to completion.
status of the calorimeter and a graphical
representation of where the instrument
is in its operating cycle. Error messages
will appear below the “status bar”.
A-1
Spike Controls Bomb Rinse Tank Control
Page 2.3 Page 2.4
Line 1 - Use Spiking. When set to Line 1 - Use Bomb Rinse Tank.
ON, the calorimeter will prompt for ON/OFF toggle for the bomb rinse
the weight of the spike added and tank counter. A full tank will contain
will compensate for the heat of enough rinse water for
combustion in the calculations. approximately 150 tests.
A-2
Appendix A - Menu Operating Instructions
A-3
Line 7 - LCD Contrast. Controls the
liquid crystal display on the calorimeter. Line 5 - Factory Hardware Version.
The number entered sets the contrast in Displays the current version of hardware
values between 1 and 100. Higher installed in the controller.
numbers provide greater contrast.
Numbers in the 60’s provide excellent Line 6 - Password Protection.
contrast for most lighting conditions. Provides password protection for the
program options and settings on the
Line 8 - LCD Backlight Time-out. The menus. If this feature is turned ON, the
unit is equipped with an automatic circuit user will be prompted for a number, up
to shut-off the backlight when it is not to six digits long, which will be the
being used. The back light will shut-off if password for all protected settings.
there is no keyboard activity for the Once protected, any attempts to change
number of seconds entered. Pressing a setting will be met with a prompt for
any key will automatically turn the back the password. The program revision will
lighting ON. A setting of 0 will keep the only be made after the correct password
backlight ON at all times. has been entered. If access is required
to sensitive areas protected by
Line 9 - Print Error Messages. When password and the password is not
turned ON, all error messages will be known, new Eproms will be required.
printed on the printer and displayed on
the screen. Line 7 - Re-load Factory Default
Settings. Used to erase all of the
Line 0 - Display Stored Samples. settings and restore the factory default
Displays a listing of all Sample ID’s settings.
stored in the memory of the controller.
Line 8 - Re-load User Default
Program Information and Control Settings. Used to restore the user’s
Page 3 setup should the program in the
instrument be corrupted for any reason.
Line 1 - Date. Used to enter the current
date. Line 9 - Copy Current Setup to
EEPROM. Used to record the setup to
Line 2 - Time. Used to enter the current the EEPROM once the user has
military time. configured the instrument to their
operating requirements.
Line 3 - Software Version. Displays the
current version of software installed in Note:
the controller. Lines 6 thru 9 make global changes
to the setup of the calorimeter and,
Line 4 - User Setup ID. Displays the therefore, contain a YES or NO
last user entered ID number for the response to make certain that the
setup stored in EEPROM. user wishes to proceed. This two
step entry is intended to prevent
inadvertent global program changes.
A-4
Appendix A - Menu Operating Instructions
A-5
Line 3 - Number of Runs. Shows
how many runs have been used to Thermochemical Calculations
determine the EE value. (Only final Page 5
reports are included in these
calculations.) Note:
To access the numeric field from the
Line 4 - Relative Standard Deviation. ON/OFF toggle position, press the
Reports the relative standard SKIP key. The SKIP key will also
deviation for the series of tests used return you to the ON/OFF choices.
to determine the current EE value.
Line 1 - Fixed Fuse Correction
Line 5 - Bomb Firing Count. (Standardization). Turns ON/OFF the
Contains the current bomb firing fixed fuse corrections for standardization
count or the number of times the runs. The actual fixed correction for this
bomb has been fired since it was value is entered in the second data field.
last serviced. When this count
matches the limit set on Page 4 - Line 2 - Fixed Acid Correction
Calibration Data & Controls, Line 4 - (Standardization). Turns ON/OFF the
Bomb Service Interval, the user will fixed acid corrections for standardization
be informed that the bomb is ready runs. The actual fixed correction for this
for service by error 108. value is entered in the second data field.
A-6
Appendix A - Menu Operating Instructions
Line 1 - Acid Value is Nitric Acid Line 7 - Offset Value. Entry for the
Only. When set to ON, the acid value when Line 6 above is turned
value is nitric acid only. When set to ON.
OFF, it represents both nitric and
sulfuric acid. Line 8 - Calculate Net Heat of
Combustion. Turns ON/OFF the
Line 2 - Acid Multiplier. The calculations for the net heat of
multiplier is the normality of the combustion for materials with
sodium carbonate used to titrate for significant hydrogen content. When
the acid correction. set to ON, the calorimeter will
prompt for hydrogen content during
Line 3 - Sulfur Value is Percent. the reporting data entry steps.
When set to ON, the sulfur value is
being entered as weight percent Line 9 - Calorimeter II same as I.
sulfur. If another system is to be Establishes that all corrections will
used, this must be turned OFF and be handled in the same manner for
the sulfur multiplier on Line 4 set Calorimeter II when it is installed. If
accordingly. this is turned OFF, controls for
Calorimeter II are set on sub-menu,
Line 4 - Sulfur Multiplier. Values Page 5.9 - Thermochemical
entered by the user to be used for Corrections. This sub-menu is the
the sulfur correction are multiplied by same as Page 5 - Thermochemical
this value to get the product into Corrections, Lines 1-9.
units of milliequivalents. The default
A-7
Data Entry Controls
Page 6 Line 8 - Automatic Sample ID
Number. Displays the next Sample ID
Line 1 - Weight Entry Mode. This data which will be assigned and is used to
field contains options for entering the enter the beginning Sample ID of any
sample weight through the keyboard, series. The user can always override the
instruments connected via the Smart automatic Sample ID by entering the
Link port or through the balance port desired number and pressing ENTER.
connection.
A-8
Appendix A - Menu Operating Instructions
A-9
Line 2 - Printer Port (RS232).
Accesses sub-menu, Page 8.2 - Line 3 - Number of Stop Bits.
Printer Port Communications. Standard options for stop bits.
Toggles between 1 and 2.
Printer Port Communications
Page 8.2 Line 4 - Handshaking. Standard
options for handshaking. Choose
Line 1 - Number of Data Bits. from Xon/Xoff, RTS/CTS and None.
Standard options for data bits.
Toggles between 7 and 8. Line 5 - Baud Rate. Standard
options for baud rate. Choose from
Line 2 - Parity. Standard options for 9600, 4800, 2400, 2000, 1800,
parity. Choose from None, Odd, 1200, 600, 300, 150, 134.5, 110, 75
Even, Mark or Space. and 19.2K.
A-10
Appendix A - Menu Operating Instructions
A-11
Keyboard Diagnostic useful to most users, unless special
Page 9.5 diagnostic equipment is used.
A-12
Appendix B - Calculations
B-1
Fuse Correction. The fuse correction in per test. The thread supplied by Parr
the 1271 Calorimeter is significantly has a mass of approximately 1 milligram
different than the correction used in per centimeter. This results in a total
earlier model Parr calorimeters where fuse correction of 50 calories.
the correction was made to compensate
for the amount of fuse wire burned in the ASTM and ISO Methods Differ
test. There are two components to the
fuse correction in the 1271 Calorimeter: Current ASTM, ISO, and British
Standard Methods differ on their
1. The heat introduced by treatment of the nitric and sulfuric acid
heating the wire used to ignite thermochemical corrections. ASTM
the cotton thread. Methods call for titrating the bomb
washings to determine the total acid
2. The heat of combustion of the present.
cotton thread used to ignite the
sample. This is assumed to be all nitric acid with
a heat of combustion of _14.1 Kcal per
The permanent fuse wire is heated by mole. The amount of sulfur is then
dissipating an electrical charge from a determined and converted to
capacitor. Since this charge is controlled equivalents of sulfuric acid. The
by the size of the capacitor and the difference between the heat of formation
charging voltage, and because the of sulfuric acid (_72.2 Kcal per mole or
capacitor is fully discharged for each _36.1 calories per milliequivalent) and
test, the energy released can be nitric acid is then subtracted as the
calculated. In the 1271 Calorimeter this sulfur correction.
is a fixed correction of 10 calories per
test. Most other test methods treat nitric and
sulfuric acid corrections as entirely
Cotton has a heat of combustion of separate values instead of combined
4000 calories per gram. The actual values. This eliminates the requirement
thread being used should be weighed to for a total acid determination and
see how much is being burned. Ten permits the nitric acid correction to be
centimeters of a fine thread will weigh handled in a variety of ways, including
approximately 0.003 grams which would the assumption of a fixed nitric acid
release 12 calories as it burns. Heavier correction.
threads weigh up to 0.010 grams per 10
centimeters and increase this correction The 1271 Calorimeter can be set up to
to 40 calories per test. The finer the apply the acid correction by either the
thread, the smaller errors will be if the ASTM or ISO convention, as the user
thread is not exactly ten centimeters in prefers. Care must be used to ensure
length. Polyester thread is not the proper corrections are applied, and
recommended for use in the bomb the calculations made are consistent
because it has a tendency to melt and with the procedure used.
fall away from the heating wire before it
ignites. Note:
Please review the following section
Using the fine thread mentioned above, on Acid and Sulfur Corrections.
the fuse correction for the calorimeter Different standard test methods use
would be the 10 calories from electrical different values for the heat of
heating plus 12 calories from the formation of sulfuric acid. These
burning thread for a total of 22 calories differences are generally
B-2
Appendix B - Calculations
B-3
at the number of milliequivalents of Example:
sulfuric acid in the bomb washings.
(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 or10/16.03 = 0.6238
Table B-1
Settings for ISO & BSI Methods
B-4
Appendix B - Calculations
B-5
ISO Calculations Spiking Samples
Both the ISO 1928 and BSI 1016: Part 5 It is sometimes necessary to add a
methods for testing the calorific value of spiking material to samples which are
coal and coke, deal with acid and sulfur very small, have a low heat of
corrections in a manner which is combustion, or have a high moisture
somewhat different than ASTM content to add sufficient heat to drive
procedures. Provision has been made in the combustion to completion. Benzoic
the 1271 Controller for dealing with acid is an excellent material for spiking
these different procedures. for all of the same reasons it is a good
standard material. White oil is also an
The analysis of bomb washings in these excellent material, particularly for liquid
methods call for a titration, first using samples. The 1271 Calorimeter can
O.1N barium hydroxide (V2) followed by automatically compensate for the
filtering, and a second titration using addition of spiking materials to these
0.1N HC1(V1) after 20 ml of a 0.1N samples. The calculations are modified
sodium carbonate has been added to in these cases as follows:
the filtrate. Table B-1 gives the settings
which allows the results of the two Hc = WT − e1 − e2 − e3 − (Hcs)(Ms)
titrations, V1 and V2, to be entered into m
the controller directly for the calculation
of the total acid correction. V1 should be where Hcs= Heat of combustion of
entered at the prompt for acid and V2 is the spiking material
entered at the prompt for sulfur. The
settings in Table B-1 assume that the Ms = Mass of spiking material
same procedure is carried out for both
standardization and determination. This factor is added to the calculations
when Page 2.3 - Spike Controls, Line 1 -
The offset value is the product of -1, the Use Spiking is set to ON. Line 2 - Heat
Heat of Formation of Nitric Acid, the acid of Combustion of Spike is entered as
multiplier, and the 20 mL of 0.1 N calories per gram. The controller will
sodium carbonate used in the analysis. prompt the user to enter the weight of
spiking material. Fixed spikes can be
The formula used to get the total used when Line 3 - Use Fixed Spike is
correction in calories is as follows: set to ON and entering the mass of the
spike on Line 4 - Weight of Fixed Spike.
• V1(Acid Multiplier)(Heat of Formation
of Nitric Acid)V2 (Sulfur Multiplier)
(Heat of Formation of Sulfuric
Acid)+offset value.
B-6
Appendix B - Calculations
B-7
B-8
Appendix C - Standardization
C-1
CAUTION:
C-2
Appendix D - Communication Interfaces
The Parr Smart Link is designed to to the number of devices that can be
facilitate the connection and control of a connected and only a single connection
network of equipment which can include port is required for each device. The
the 1271 Calorimeter, 1261 Calorimeter, Smart Link is also capable of
1266 Calorimeter, 1351 Calorimeter, communicating with devices up to 1000
1356 Calorimeter, 1760 Sulfur Analyzer, meters away as opposed to the 50 foot
1720 or 1730 Calorimeter Controllers, restriction for RS232C lines.
1741 Balance Interfaces and 1750
Proximate Analyzers with attached Required Software Versions
analytical balances, 1745 Computer
Interface and/or the 1747 PC Smart Link Before proceeding with the installation
Board and associated computer, and of the 1271 Calorimeter on the Parr
1742 Sulfur Interface for automatically Smart Link, the user must ensure that all
entering and storing sulfur values. of his devices have the versions of
software capable of communicating over
Successful installation of the Smart Link the Smart Link and have been
network will depend upon all elements configured for the intended network (see
of the communications network (Smart Table D-1).
Link) being preset, properly configured
and connected. A step-by-step review of The version of software installed in a
the Smart Link communications network Parr device can be determined by
and the configuration requirements for performing the self-test procedure and
all devices installed on the Link is checking the printed or displayed
provided in this chapter (see Smart Link message. Users who do not have the
Configuration Checklist) to ensure that required software installed should
the system is properly addressed before contact the Technical Service
attempting to use it. Department at Parr Instrument
Company.
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.
D-1
The second device within the category
Required Hardware must have its address set to one, and
the third set to two, etc.
This 1271 Calorimeter is fully equipped
for operation on the Smart Link. The All devices on the Smart Link are set, by
1760 Sulfur Analyzer, as well as 1720 default, to communicate at a rate of
and 1730 Controllers must have the 9600 baud. All devices on the Smart
optional 1722 Smart Link board installed Link must communicate at the same
to communicate on the Smart Link. The transmission speed.
1750 Proximate Analyzer and the 1741,
1742, 1745 and 1747 Interfaces include Smart Link Configuration
all of the required Smart Link hardware. Checklist
If a 1760 Sulfur Analyzer or 1720 or
1730 Controller will be used in the 1. Software versions verified for all
installation and the 1722 Board has not devices connected on the Smart
already been installed, it must be Link.
installed at this time.
2. Any devices which are not the only
Smart Link Configurations device within their category have
had their addresses changed to 1, 2
Each device on the Smart Link has or higher as needed.
several parameters associated with it
which help to: 1) identify the instrument 3. The two devices at the ends of the
and, 2) control the flow of information to Smart Link have had all levers of the
and from instruments on the link. terminator switches closed.
Termination switches are located on
Each category of device has its own the rear of the controller.
fixed identification which automatically
identifies it on the Smart Link. 4. All other devices, other than the
Addresses of individual instruments ones on the ends, have all levers of
within a class, such as calorimeter the terminator switches open.
controllers, must be changed from the
default setting only if more than one 5. All devices have been checked to
device in the same category is installed see that a transmission rate of 9600
on the link. baud has been set.
Table D-1
Software Required
D-2
Appendix D - Communication Interfaces
Smart Link Configuration Cabling The default parameters for the 1271
Calorimeter are set up for use with the
Smart Link devices, including the 1271 Parr 1756 Printer. Table D-3 identifies
Controller, can be connected using any and describes the pinout for the
of the cables listed in Table D-2. RS232C port.
Smart Link cables can be linked as Parr offers the A643E2 Connecting
extension cords. If a device is removed Cable for connections from the identified
from the link, the two cables should be RS232C port to devices located within
connected to maintain the continuity of five feet of the calorimeter. Users may
the link. All devices should be turned off have longer cables designed to match
before cables are connected or their devices and installations using
disconnected. these specifications. RS232C ports are
not designed for communicating over
RS232C Connection distances greater than 50 feet.
D-3
Direction
Pin No. Name ← ←→ →
1271 Terminal
1 Frame Ground ←→
2 Transmitted Data →
3 Received Data ←
4 Request to Send (RTS) →
5 Clear to Send (CTS) ←
6 Data Set Ready (DSR) ←
7 Signal Ground
←→
8 Data Carrier Detect
←
20 Data Terminal Ready
→
Connector: 25pin, D type, female
Table D-3
Terminal Port Specifications
Direction
Pin No. Name ← ←→ →
1271 Terminal
1 Frame Ground ←→
2 Received Data ←
3 Transmitted Data →
4 Clear to Send (CTS)* ←
5 Request to Send (RTS) →
6 Data Set Ready (DSR) ←
7 Signal Ground
←→
20 Clear to Send (CTS)
←
* Held at +12V (space or logic 0) while the 1271 is ON.
Connector: 25 pin, D type, female
Table D-4
Printer Port Specifications
D-4
Appendix D - Communication Interfaces
Direction
Pin No. Name ← ←→ →
1271 Terminal
1 Frame Ground ←→
2 Received Data ←
3 Transmitted Data →
4 Clear to Send (CTS) ←
5 Request to Send (RTS) →
6 Data Terminal Ready →
7 Signal Ground
←→
20 Data Set Ready
←
Connector: 25 pin, D type, female
Shift 2 accesses the alternate menu so that reports can be sent direct to
null modem.
Table D-5
Balance Port Specifications
D-5
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-6
Calorimetry Run Storage Definitions
Table D-7
Data Entered - Bit Definitions
D-6
Appendix E - Technical Service
E-1
E-2
Appendix F - Parts List
F-1
1271 Calorimeter Controller Parts List
Item Description
573DD Filter Fan Guard Assembly
614DD Guard, Wire
756DD Keyboard Overlay
A800DD Controller Assembly
A861DD Fan, 12 VDC
A999DD Display Board Package (includes *)
A719E Cordset, 120V
A719EEE Cordset, 240V
1264E Power Supply, Output Switching
A1266E Display, Graphic LCD Module*
A1267E Circuit Board, Display Driver
A1268E Circuit Board, Comm Fanout
A1269E Circuit Board, DIO
A1326E CPU Board, w / Eproms
A1386E Firmware, English (Set of 7 Eproms)
A1387E Firmware, German (Set of 7 Eproms)
1520E Battery, Lithium 3V
1668E Bulb
Item Description
189A2 Gage
A165VB2 Pressure Regulator (Go)
359VB Filter
A383VB Pressure Regulator (Concoa)
HX0012TB024 Tubing, Pressure 1/8" OD
F-2
Appendix F - Parts List
Item Description
A670DD Bucket Assembly
692DD Spacer, Mtr Mtg
694DD O-ring, Buna-N 0.301 ID
698DD Shaft, ISO Valve
699DD O-ring, Buna-N, 0.112 ID
703DD Coupling, Complete
809DD Screw Plug, 10-32
A856DD Pump Cover Assembly
859DD Coupling, Nylon Center Piece
1071DD Quad Ring, Buna-N 2.88 ID
1096DD Quad Ring, NBR
1096HC O-ring, Buna-N, 0.864 ID
309VB Male Connector, 1/8T x 1/8NPT
311VB Fitting, Mini Hose
314VB Fitting, Barbed 1/4 T ID
338VBAD Male Connector 1/8 T
SA1140FT06 FHMS, 4-40 x 3/8
SA1140RD04 RHMS, 4-40 x 1/4
SB1140BT04 BHSCS, 4-40 x 1/4
SC1140SC08 SHSS, 4-40 x 1/2
WB3118HX20 HHCS Nylon, 5/16 - 18 x 1-1/4
Item Description
694DD O-ring, Buna-N .301 ID
A702DD Top Plate Assembly, Jacket
A704DD Jacket Tube Assembly, Soldered
A707DD Plate Assembly, Cool Loop Rear
708DD Spacer, Jacket Mounting
A767DD Bottom Plate Assembly, Jkt
769DD Plate, Shield Mounting LH
798DD Pin, Shield Pivot
819DD Isolator, Contact Strip
825DD Plate, Shield Mounting RH
1341E Ignition Contact Strip
314VB Fitting Barbed 1/4T ID
SA1632RD04 RHMS, 8-32 x 1/4
SB1932BT04 BHSCS, 10-32 x 1/4
SC0948SC02 BHSCS, 3-48 x 1/8
F-3
1131 Oxygen Bomb Parts List (Cylinder)
Item Description
650DD Bomb Head
651DD Electrode Straight
652DD Electrode, Loop
653DD Nut, Electrode
654DD Electrode Washer, Ceramic
655DD Electrode, Spacer
656DD Reducer Bushing
657DD Electrode Core
658DD Insulator, TFE
659DD O-ring, Buna-N, .145 ID
663DD Contact Bushing, Delrin
666DD Pin, Rotator
667DDJV Quad Ring, FKM, 1.484 ID
668DD Check Valve Head
821DD O-ring, Buna-N, .056 ID
840DD2 Heat Wire, 60" L
843DD Wire Holder
845DD Thread, Ignition (Spool), 563 yards
851DD Oxygen Bomb Head Assembly
PA0948RD04 RHMS, 3-48 x 1/4 T316SS
SN1632HX Hex Nut, 8-32
F-4
Appendix F - Parts List
Item Description
189A2 Oxygen Gage
189AP2BE Gage, 200 psi
43AS Capsule, SS
149C In-line Filter
231C2 Carboy, 10 Liter
263C Paper, Printer; 40 Column
264C Ribbon, Replacement 1756
266C Printer, Dot Matrix; 40 Column
A570DD Regulator Assembly, Oxygen
700DD Tool, O-ring Installation
811DD Lube/Sealant
A812DD Regulator, Nitrogen Assembly
841DD Photo-flo Solution (Pint)
840DD2 Heat Wire, 60" L
845DD Thread, Ignition (Spool)
876DD Tubing Cutter
877DD Wrench, 7/16"
878DD Wrench, 11/16"
883DD Handle, Sliding "T", 3/8 Drive
884DD Socket 9/16" Deep, 3/8 DRV 6 PT
885DD Socket, 3/4" Deep, 3/8 DRV 6 PT
A962E Cable, Printer
A996E Power Cable, Printer
372HC2 Wrench, 9/16"
TX09SK 3/32 Socket Screw Key
TX12SK 1/8 Socket Screw Key
A324VBAD Toggle Valve, Rinse Tank
3415 Benzoic Acid Pellets, 100 GR
F-5
1271 Calorimeter Tubing & Connectors
Item Description
149C Filter
HX0062TB062 5/8" OD x 1/2" ID Bev-A-Line Tubing
JT0038TB062A 3/8" OD x 1/4" ID Nylon Tubing
HX0038TB062 3/8" OD x 1/4" Bev-A-Line Tubing
JU0038TB062A 3/8" OD x 1/4" ID Polyurethane Tubing
JU0012TB032 1/8" OD x 1/16" ID Polyurethane Tubing
JU0012TB032XH 1/8" OD x 1/16" ID Ribbon Tubing
X0012TB024 1/8" x .077 ID Nylon Tubing
181VB Insert Tubing, 5/8" OD, Brass
183VB Insert Tubing, 3/8" OD, T316SS
213VB Compression Nut, 1/8" OD, Brass
213VBAD Compression Nut, 1/8" OD, T316SS
214VB Ferrule Set, 1/8" OD, Brass
214VBAD Ferrule Set, 1/8" OD, Stainless
214VBHJ Ferrule Set, 1/8" OD, Nylon
217VB Compression Nut, 1/4" OD, Brass
218VB Ferrule Set, 1/4" OD, Brass
221VB Compression Nut, 3/8" OD, Brass
222VB Ferrule Set, 3/8" OD, Brass
225VB Compression Nut, 5/8" OD, Brass
226VB Ferrule Set, 5/8" OD, Brass
Item Description
A593DDEA Pump/Motor, 120V
A593DDEF Pump/Motor, 240V
A862DD Thermistor
A863DD Level Switch
A864DDEB Heater, 120V
A864DDEE Heater, 240V
A865DD Make-up Water Solenoid
A866DD Cold Water Solenoid
1351E Fuse, 10 AMP
172HW2 Receiver Cover Cap
187HW O-ring, Buna-N, 1.299 ID
A200HWEA Closed Water System Assembly, 120V
A200HWEF Closed Water System Assembly, 240V
F-6
Appendix F - Parts List
F-7
Figure F-1
Pump & Motor Assembly
Note: The coupler should be "tight" when motor shaft is pushed in toward pump. Axial
play of 0.2 to 0.3 mm in motor must be preserved. Loosen set screws on motor side
coupler only to make adjustment.
F-8
Appendix F - Parts List
Figure F-2
Bomb Head Assembly
F-9
Figure F-3
Pump Block Assembly
F-10
Appendix F - Parts List
Figure F-4
Oxygen Bomb Vessel Assembly
F-11
F-12
PARR INSTRUMENT COMPANY
http://www.parrinst.com [email protected]
Printed in USA
9/5/06