587M Parr 6400 Calorimeter After 10 2010 Inst
587M Parr 6400 Calorimeter After 10 2010 Inst
587M Parr 6400 Calorimeter After 10 2010 Inst
6400
6400
Table of Contents
Preface 4
Scope 4
Related Instructions 4
Purpose 4
Explanation of Symbols 5
Safety Information 5
Intended Usage 5
General Specifications 6
Environmental Conditions 6
22
Cool/Rinse
26
Drain
Fill Cycle
23
Pre-Period
24
Bomb Firing
25
Post-Period
25
Chapter 428
Menu Descriptions
28
Main Menu 28
Calorimeter Operation Menu 28
Chapter 18
Installation
Environmental Conditions 8
Swagelok Tube Fittings 8
Required Consumables, Utilities and Power Requirements 9
Electrical Connection 9
Front Panel Meter 9
Water Connection 11
Gas Connection 12
Bomb Exhaust Connections 12
Communication Connections 13
Printer Connections 13
Balance Connections 13
Chapter 216
29
29
30
31
32
User/Factory Settings
33
35
35
37
38
39
39
Initial Fill 16
40
Quick Start 16
40
Quick Start
16
Chapter 318
Operation
18
Menu System 18
Menu Keys 18
Control Keys 18
Programming 19
Default Settings 19
Sample Preparation 19
Test Process 22
41
42
43
Diagnostics Menu 44
Data Logger Controls
44
45
45
I/O Diagnostics:
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Table of Contents
Chapter 546
Chapter 10 70
Reports
Maintenance
46
Reports 46
70
Chapter 648
Standardizations
48
Chapter 752
Calculations
52
Fuses 71
Daily Maintenance 71
Quarterly Maintenance 71
50 to 100 Test Maintenance 71
500 Test Maintenance 71
5000 Test Maintenance 72
6400 Maintenance Checklist 73
Chapter 1174
Troubleshooting
74
Chapter 1278
ISO Calculations 56
Technical Service
Spiking Samples 57
78
Chapter 858
Chapter 1380
Parts Lists
80
58
Computer Connections 58
Computer Communications
Chapter 9 68
Memory Management
68
Chapter 14 82
Clearing Memory 68
Drawings
Removable SD Memory 68
82
Chapter 15 104
Tables
104
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Table of Contents
Figures
Figure 1-1
Figure 14-11
Figure 14-12
Wiring Diagram
92
92
93
94
95
96
97
98
99
100
Figure 14-21
Wiring Diagram
101
Figure 14-22
Fuse Diagram
102
82
84
Tables
Table 6-1
85
86
87
88
88
89
90
91
49
Table 6-2
50
Table 6-3
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51
66
67
104
106
Preface
Preface
Related Instructions
Scope
This manual contains instructions for installing and
operating the Parr 6400 Calorimeter. For ease of
use, the manual is divided into 15 chapters.
1. Installation
2. Quick Start
3. Operation
4. Menu Descriptions
5. Reports
6. Standardizations
7. Calculations
8. Computer Communications
9. Memory Management
10. Maintenance
11. Troubleshooting
12. Technical Service
13. Parts Lists
14. Drawings
15. Tables
Description
Limited Warranty
207M
230M
483M
Purpose
Customer Service
Questions concerning the installation or operation of this instrument
can be answered by the Parr Customer Service Department:
1-309-762-7716 1-800-872-7720 Fax: 1-309-762-9453
E-mail: [email protected] http://www.parrinst.com
4
6400
Preface
Explanation of Symbols
I
On Position
Off Position
Alternating Current
This CAUTION symbol may be present on the Product Instrumentation and literature. If present on the product, the user must consult
the appropriate part of the accompanying product literature for more
information.
ATTENTION, Electrostatic Discharge (ESD) hazards. Observe precautions for handling electrostatic sensitive devices.
Protective Earth (PE) terminal. Provided for connection of the protective earth (green or green/yellow) supply system conductor.
Chassis Ground. Identifies a connection to the chassis or frame of the
equipment shall be bonded to Protective Earth at the source of supply
in accordance with national and local electrical code requirements.
Earth Ground. Functional earth connection. This connection shall be
bonded to Protective earth at the source of supply in accordance with
national and local electrical code requirements.
Safety Information
To avoid electrical shock, always:
1. Use a properly grounded electrical outlet of
correct voltage and current handling capability.
2. Ensure that the equipment is connected to
electrical service according to local national
electrical codes. Failure to properly connect may
create a fire or shock hazard.
3. For continued protection against possible
hazard, replace fuses with same type and rating
of fuse.
4. Disconnect from the power supply before
maintenance or servicing.
Intended Usage
If the instrument is used in a manner not specified
by Parr Instrument Company, the protection provided by the equipment may be impaired.
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Preface
General Specifications
Electrical Ratings
120VAC, 5.0 Amps. 50/60 Hz
240VAC, 3.0 Amps. 50/60 Hz
Before moving the instrument, disconnect all connections from the rear of the apparatus. Lift the
instrument by grabbing underneath each corner.
Environmental Conditions
Operating: 15 C to 30 C; maximum relative humidity of 80% non-condensing. Installation Category II
(over voltage) in accordance with IEC 664. Pollution
degree 2 in accordance with IEC 664.
Altitude Limit: 2,000 meters.
Storage: -25 C and 65 C; 10% to 85% relative humidity.
6400
Notes
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1 Installation
Chapter 1
Installation
Figure 1-1
Swagelok Tube Fittings
Environmental Conditions
The 6400 Calorimeter is completely assembled and
given a thorough test before it is shipped from the
factory. If the user follows these instructions, installation of the calorimeter should be completed with
little or no difficulty. If the factory settings are not
disturbed, only minor adjustments will be needed to
adapt the calorimeter to operating conditions in the
users laboratory.
This apparatus is to be used indoors. It requires at
least 4 square feet of workspace on a sturdy bench
or table in a well-ventilated area with convenient
access to an electric outlet, running water and a
drain.
6400
The type of tubing and the wall thickness also has
an effect on the amount of tightening required.
Plastic tubing requires a minimal amount of additional tightening while heavy wall metal tubing
may require somewhat more tightening. In general,
the nut only needs to be tightened about 1/8 turn
beyond finger tight where the ferrule seats in order
to obtain a tight seal.
Over tightening the nut should be avoided. Over
tightening the nut causes distortion (flaring) of the
lip of the tube fitting where the ferrule seats. This
in turn causes the threaded portion of the body to
deform. It becomes difficult to tighten the nut by
hand during a subsequent re-tightening when the
fitting body becomes distorted in this manner.
Installation
Electrical Connection
Plug the power line into any grounded outlet providing proper voltage that matches the specification on
the nameplate of the calorimeter. Grounding is very
important not only as a safety measure, but also to
ensure satisfactory controller performance. If there
is any question about the reliability of the ground
connection through the power cord, run a separate
earth ground wire to the controller chassis.
Turn the power switch to the ON position. After
a short time, the Parr logo will appear on the LCD
display followed by a running description of the instrument boot sequence. When the boot sequence
is complete, the Main Menu is displayed.
The 6400 Calorimeter requires availability of nitrogen or air, oil and water free, with appropriate
connection, 2500 psig, maximum.
Approximately 16L of distilled water are required to
fill the external pressurized rinse tank.
Approximately 2L of distilled, de-ionized, or tap
water, with a total hardness of 85 ppm or less, are
required for filling the internal cooling reservoir.
The power requirements for the sub-assemblies of
the 6400 Calorimeter are:
Calorimeter
5.0 Amps @ 120 VAC
3.0 Amps @ 240 VAC
Printer
(100 to 240 VAC, 50/60 Hz) 0.35 Amps
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1 Installation
Figure 1-2
6400 Calorimeter Back Panel
10
6400
Installation
Water Connection
Remove the cap plug on the water filling elbow and
fill the internal reservoir tank with water having a
total hardness of 85 ppm or less, until the water level
is at the bottom of the filling elbow. The calorimeter
water tank will initially accept about 2 liters.
Fill the external rinse tank with about 16 liters of
distilled water through the large opening at the top
Figure 1-3
6400 External Plumbing
06-05-07
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HJA
11
1 Installation
Gas Connection
Alternatively:
The A1050DD Bomb Rinse Container Assembly is
available as an accessory to the 6400 Calorimeter.
See Figure 14-19. This device allows for complete
and systematic recovery of the bomb combustion
products. These combustion products include the
initial line exhaust after the fill cycle and the portion expelled during the bomb rinse cycle. The
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. 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.
6400
Communication Connections
There is a Universal Serial Buss (USB) port at the
rear of the calorimeter.
The USB port is used to connect to external devices
such as a printer or balance. Multiple devices can be
attached by installing a USB hub.
The 6400 Calorimeter is also equipped with an RJ45
Ethernet port for connection to a computer.
The 6400 will also allow the user to specify the
IP addresses of one or more Balance Interface
devices on the network by selecting the Network
Data Device menu in the Communications Controls
menu. Balance Interface devices are polled from
device 1 to 15 for sample and/or spike weights when
the weight entry mode is set to Network.
Printer Connections
The printer settings are on the Communication
Controls Menu. The default parameters for the 6400
are set up for use with the Parr 1758 Printer.
Balance Connections
The 6400 Calorimeter supports input from multiple
balance types. Additionally, a generic input driver
is provided for communications with balances that
do not conform to the eight supported protocols.
A new feature supported by all balance input drivers is the ability to change the expected number
of characters in the data field. The number of data
characters indicated for each of the drivers, below,
are default values. This feature virtually eliminates
the need for balance input drivers to be re-written
in the event the balance manufacturer elects to alter
the output string of a balance when new models are
introduced.
Installation
Mettler 011/012 Interface
The ID field must contain
S_ to indicate a stable
mass. The data field contains the current mass, right
justified, with a decimal
point. The balance should
be configured to send continuously.
Field
ID
space
data
space
g
CR
LF
Length
2
1
9
1
1
1
1
Sartorius Interface
Field
Length
The polarity field must conpolarity
1
tain either a + or a space.
space
1
Leading zeros in the data
data
8
field are blanked, except
space
1
for the one to the left of the
stability
2
decimal point. The stability
CR
1
field must contain g_ for
LF
1
the calorimeter to accept a
mass. The balance should
be configured to transmit data upon receipt of
the following command string:
[ESC] P [CR] [LF]
Note: The automatic data output option
should not be used.
Generic Interface
Field
Length
The data field should condata
8
sist of 9 numeric characters
CR
1
(0 through 9, +, - and space)
terminated with a carriage
return (CR). Leading zeros may be blanked as
spaces and are counted. Non-numeric characters are ignored and will reset the input buffer if
the data field has not been filled. Any characters
received after filling the data field and before the
carriage return are ignored.
The format of an unknown balance can be determined by logging the balance output to the printer
attached to the calorimeter. Those protocols which
send a command string to the balance will do so
while logging is active. In order for the logging to
produce meaningful results, the cable connecting
the balance to the balance input port of the calorimeter must be correctly wired or configured. In
addition, the specifics of the data frame, such as the
baud rate, # of data bits, parity, # of stop bits and
handshaking (if used) must be the same for both the
balance and the calorimeter.
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13
1 Installation
Figure 1-4
6400 Calorimeter Peripherals
Figure 1-5
Multiple Alternate Configurations
14
6400
Notes
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15
Quick Start
Chapter 2
Quick Start
Initial Fill
When you first fill the calorimeter with water the
main reservoir will be filled. There is also a cooling
water reservoir that is filled from the main reservoir.
Once the calorimeter has been filled with water and
all external connections made:
1. Turn on the calorimeter.
2. Once at the Main Menu go to the Calorimeter Operation screen and turn ON the heater and pump.
Water should start to circulate in the tubing.
Quick Start
1. Turn on the heater and pump in the Calorimeter
Operation menu. Allow at least 20 minutes for
the calorimeter to warm up.
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6400
Notes
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17
3 Operation
Chapter 3
Operation
Menu System
All configurations and operations are handled by
a menu-driven system operated from the bright
touch screen display. The settings and controls are
organized into ten main sections as displayed on the
MAIN MENU.
Control Keys
There are five control keys which always appear
in the right column of the primary displays. These
keys are unavailable when they are gray instead of
white.
1. Escape. This key is used to go up one level in
the menu structure.
Note: Keys with a double box in the upper
left hand corner lead to sub-menus.
Menu Keys
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. Simply touching the key on the
screen toggles the choice to the other option.
The current setting is displayed in the lower
right corner of the key.
2. Option Selection. These data fields contain a list
of options. Touching the key on the screen steps
the user through the available choices. The current setting is displayed in the lower right corner
of the key.
3. Value Entry Fields. These data fields are used to
enter data into the Calorimeter. Touching the key
on the screen brings up a sub-menu with a key
pad or similar screen for entering the required
18
This key appears in the Escape key location when the main menu is displayed. This key
is used to shut down the calorimeter program
before turning off the power.
6400
Operation
Programming
Sample Preparation
The program in the 6400 Calorimeter can be extensively modified to tailor the unit to a wide variety
of operating conditions, reporting units, laboratory
techniques, available accessories and communication modes. In addition, the calculations, thermochemical corrections and reporting modes can be
modified to conform to a number of standard test
methods and procedures. Numerous provisions are
included to permit the use of other reagent concentrations, techniques, combustion aids and short cuts
appropriate for the users work.
Sample Size
To stay within safe limits, the bomb should never be
charged with a sample which will release more than
8000 calories when burned in oxygen. The initial
oxygen pressure is set at 30 atmospheres (450 psig).
This generally limits the mass of the combustible
charge (sample plus benzoic acid, gelatin, firing oil
or any combustion aid) to not more than 1.1 grams.
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.
Default Settings
Units are pre programmed with default settings.
See Table 15-1 for a listing of the factory default
settings. A more in-depth explanation of these parameters is found on the corresponding parameter
group help pages. These default settings remain
in effect until changed by the user. Should the user
ever wish to return to the factory default settings, go
to the Program Info and Control Menu, User/Factory
Settings, touch Reload Factory Default Settings and
YES. Non-volatile memory is provided to retain any
and all operator initiated program changes; even
if power is interrupted or the unit is turned off. If
the unit experiences an intentional or unintentional
Cold Restart, the controller will return to the last
known settings.
The default parameters of the 6400 Calorimeter can
be changed to guarantee that the 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:
To re-load the user default setting, go to the Program Info and Control Page, User/Factory Settings,
Re-load User Default Settings, and YES.
When starting tests with new or unfamiliar materials, it is always best to use samples of less than 0.7
grams with the possibility of increasing the amount if
preliminary tests indicate no abnormal behavior and
the sample will not exceed the 8000 calorie limit.
Samples containing sulfur should contain no more
than 50 mg of sulfur and liberate at least 5000
calories.
Samples containing chlorine should be spiked to
insure that sample contains no more than 100 mg of
chlorine and liberates at least 5000 calories
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.
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 to giving controlled
burn rates, the formation of pellets from
sample material 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
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19
3 Operation
combustions. If moisture is to be added to retard
the combustion rate, drop the water directly onto
the loose sample or onto a pellet after the sample
has been weighed. Then let the sample stand to
obtain uniform distribution. Low volatile samples
with 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.
Sample Types
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:
The combustion must produce sufficient turbulence within the bomb to bring oxygen into
the fuel cup for burning the last traces of the
sample.
The use of a sample which contains coarse particles will not burn readily. Coal particles which
are too large to pass a 60 mesh screen may not
burn completely.
20
6400
Operation
Figure 3-1
Volatile Sample Technique
Use the following procedure when filling and handling any of these tape-sealed sample holders:
1. 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
3-1).
2. Puncture the tape at a point below the flag, then
re-weigh the empty cup with its tape cover.
3. Add the sample with a hypodermic syringe;
close the opening with the flag and re-weigh the
filled cup.
4. Set the cup in the capsule holder and arrange
the auxiliary fuse so that it touches the center of
the tape disc.
5. 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.
6. Fill the bomb with the usual oxygen charging
pressure.
7. The calorimeter will fire the bomb and complete
the test in the usual manner.
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 white oil or other
suitable material of known purity can be mixed with
the sample. Ethylene glycol, butyl alcohol or decalin
may be used for this purpose.
Note: It must be remembered, 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.
When benzoic acid is combusted for standardization
runs, 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.
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21
3 Operation
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, fused quartz, and platinum alloyed with
3-1/2% rhodium.
Stainless steel capsules (43AS) are furnished with
each calorimeter. 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. New
capsules are heated in a muffle furnace at 500 C for
24 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. Capsules should
be monitored for wear. Do not use the capsule if the
wall or base thickness is less than 0.025.
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.
When combusting samples that contain metal
particles such as aluminum or magnesium, the nonmetallic 43A3 Fused Silica or 43A3KQ Fused Quartz
Capsule is required.
When superior corrosion resistance is needed, the
43A5 Platinum Rhodium Capsule or 43A3KQ Fused
Quartz is required.
Test Process
Loading the sample
Prepare and weigh the sample to 0.0001g. Gently
tap capsules that contain powdered samples to
compact the material. (Pellets are easier to handle
than loose samples and they burn slower in the
bomb, thereby reducing the chances for incomplete
combustion).
22
6400
Operation
Fill Cycle
Once the calorimeter is started and the cover is closed, the fill sequence begins.
Figure 3-3
Bucket Fill Flow Diagram
3. The oxygen fill solenoid is opened and oxygen is added slowly to the bomb to bring its pressure to
approximately 30 atm.
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23
3 Operation
Pre-Period
At the completion of the fill sequence, the pre-period begins.
Figure 3-4
Pre-Period/Post-Period Flow Diagram
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 stirrer. Water continues to circulate from the closed water
system through the jacket surrounding the bucket.
2. 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.
3. The controller monitors the operating temperature until it confirms that the initial equilibrium has been
established.
24
6400
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 3-4, from the pre-period through the bomb
firing and post-period. A warning of short beeps is
sounded indicating the bomb is about to be fired.
Operation
Post-Period
A minimal temperature rise will confirm that the
sample has ignited. After this verification, the postperiod begins. See Figure 3-4.
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.
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25
3 Operation
Cool/Rinse
At the completion of the post-period, the rinse and cool sequence begins.
Figure 3-5
1. Chilled water is circulated through the bucket
to cool the bomb to the
starting temperature.
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 rinse
water from the rinse
water tank is admitted
through the bomb rinse
solenoid valve and the
check valve at the top
of the bomb. The bomb
rinse water is released to
the wash bottle.
Note: 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.
26
6400
Operation
Drain
At the completion of the bomb rinse sequence, the drain sequence begins.
Figure 3-6
Drain Flow Diagram
The water in the bucket is drained out of the bucket and routed to the drain connection. Once the bucket is
drained, the calorimeter may be opened to remove the bomb head and load the next sample.
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27
4 Menu Descriptions
Chapter 4
Menu Descriptions
Main Menu
6400
Temperature vs. Time Plot
Menu Descriptions
Bucket Plot Symbol: Toggles between No Point
Small Dot
Round
Square
Up Triangle
Down Triangle
Diamond
Bucket Min Value: Press this key to access its
numeric dialog box to set a minimum bucket
value.
Jacket Plot Symbol: Toggles between (same as
Bucket Plot Symbol, above).
Setup: Press the Setup key to access the Temperature Plot Setup Menu, which has many
keys that permit the user to fully customize
both the x (time) axis and the scaling of the y
axis.
Temperature Plot Setup Menu
29
4 Menu Descriptions
Operating Controls Menu
Spiking Controls
30
6400
Bomb Rinse Tank Controls
Menu Descriptions
Rinse Flush Time: 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 2s.
Clear Time: 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.
# 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
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31
4 Menu Descriptions
Program Information and Control Menu
Date & Time: Accesses a sub-menu to set the current date and time.
Date: Displays current date and accesses
sub-menu on which date is set in (YY/MM/DD)
format.
Time: Displays current time and accesses submenu on which time is set in (HH:MM) format.
Time Zone: Displays the selected time zone
in relation to Greenwich Mean Time. Pressing
this key will step through the time zones and
automatically adjust the time setting.
Volume Level Adjust: Opens a window with a slide
adjustment to set the volume of the key cliks and
alarms of the calorimeter. Default is 85%.
32
6400
User/Factory Settings: This key leads to a submenu that allows the user to save or recall user
defined instrument settings. Additionally, factory
pre installed settings supporting different bombs or
special operating modes can also be recalled.
User/Factory Settings
Menu Descriptions
Reload User Default Settings: Used to restore
the user setup ID settings should the program
in the instrument be corrupted for any reason.
Save User Default Settings: Used to record the
setup to the memory once the user has configured the instrument to their operating requirements.
Compare Settings With Factory Defaults: This
button will bring up a screen that will show the
differences in the current settings of the calorimeter with the factory defaults.
Feature Key: This key displays a screen which
allows the user to input a code to access special
calorimeter features such as the bar code capabilities, remote calorimeter operation or Samba server
feature.
User Setup ID: Used to enter a unique identifier for recalling user settings. Parr offers a
unique program within the 6400 identified as
64-FAST. The program will overlay the
factory settings and shorten the run time by
approximately 2 minutes however the user
should be aware that a loss of precision may
occur.
Reload Factory Default Settings: Used to erase
all of the settings and restore the factory default settings.
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33
4 Menu Descriptions
Calibration Data and Controls Menu
Bomb 1 - Bomb 4: Leads to sub-menu, Bomb 1 Bobm 4. Displays 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 for
more rapid turn-around. The respective EE values
for each bomb can be stored in memory.
34
6400
Bomb 1
Menu Descriptions
Manual EE Entry: This key allows the user to
manually enter an EE or calibration factor for
a given calorimeter ID or bomb head. If an EE
value is manually entered, it is necessary to
turn the Protect EE Value ON in order to prevent this value from being overwritten by an
automatic update.
Print Standardization Runs: This key 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.
Reset Bomb Fire Count: After bomb service,
press this key to reset the fire count to zero.
Rel. Std. Dev.: Displays the relative standard deviation for the series of tests used to determine
the current EE value in percent of the EE value.
Control Chart Plot: Displays the current standardization runs being used to calculate the
Bomb EE Value. The display will either chart
the value of the Heat of Combustion (HOC) of
the Standard or the Energy Equivalent (EE) depending on the selection on the Control Chart
Parameters menu (see Calibration Data and
Controls menu).
Control Plot Chart Plot
You can display the information used for each test
by selecting the appropriate dot.
35
4 Menu Descriptions
Thermochemical Corrections Menu
36
Determination Corrections
Fixed Fuse Correction: Press this key on the LEFT
side to toggle ON or OFF the fixed fuse correction
for determination runs. Press it on the RIGHT side
to access the Fixed Fuse numeric dialog box on
which the value can be set. An appropriate fixed
fuse value is 50 calories.
Acid Correction: Press this key on the LEFT side
to toggle between Fixed HNO3, Calculated HNO3 ,
Entered Total, Entered HNO3, and Fixed Total for the
acid correction for determination runs. Press it on
the RIGHT side to access the Acid Correction numeric dialog box on which the value can be set.
Fixed Sulfur Correction: Press this key on the LEFT
side to toggle ON or OFF the fixed sulfur correction
for determination runs. Press it on the RIGHT side
to access the Fixed Sulfur numeric dialog box on
which the value can be set.
Note: When fixed corrections are turned ON,
the value in the specified field will be used
in both the preliminary and final reports.
The calorimeter will not prompt for actual
corrections. If all corrections are fixed, only
final reports will be generated. If any correction value is entered and the toggle is set to
OFF, then the preliminary report will use the
displayed fixed value, but the final report will
use the value entered when prompted during
the reporting process.
6400
Calculation Factors: Accesses the Calculation Factors sub-menu, which provides for setting a number
of options for the way the thermochemical corrections are applied.
Calculation Factors Menu
Menu Descriptions
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 (0.6238)
requires that the sulfur value be entered in
weight percent.
Fuse Multiplier: The fuse corrections represent the number of calories liberated by the
burning fuse wire used to ignite the sample. If
another measurement is used, the correction
factor must be entered here. Press this key to
access the Fuse Multiplier numeric dialog box
and enter this multiplier value.
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 titration that
is made. To use these calculations, toggle this
to ON and enter the appropriate value as the
offset value.
Offset Value: The value used when Offset
Correction is turned ON. Press this key to access the Offset Value numeric dialog box and
change its value.
Heat of Formation Sulfuric Acid: Different
methods use different values for the heat of
formation of sulfuric acid. The value can be set
to match the specific method being followed.
Default = 36.1.
Heat of Formation Nitric Acid: Different
methods use different values for the heat of
formation of nitric acid. The value can be set
to match the specific method being followed.
Default = 14.1.
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37
4 Menu Descriptions
Net Heat/Dry Factors: Accesses the Net Heat/Dry
Factors sub-menu, which provides for setting the net
heat of combustion and Dry Factors Thermochemical
Corrections.
38
6400
Hydrogen Entry Mode: This key steps through
the options for entering hydrogen content for
calculating the net heat of combustion either
manually through the touch screen or automatically through the balance (USB) port.
Oxygen Entry Mode: This key steps through
the options for entering oxygen content for
calculating the net heat of combustion either
manually through the touch screen or automatically through the balance (USB) port.
Nitrogen Entry Mode: This key steps through
the options for entering nitrogen content for
calculating the net heat of combustion either
manually through the touch screen or automatically through the balance (USB) port.
Auto Sample ID Controls: Accesses sub-menu for
controlling the automatic assignment of sample
identification numbers.
Auto Sample ID Controls
Menu Descriptions
Next Auto Sample ID Number: Establishes the
initial sample number for a series of tests and
then shows the next sample ID which will be
assigned. Used when the Automatic Sample
ID is set to ON. Press this key to access a submenu for entering a numeric increment.
Auto Sample ID Increment: Establishes the increment between sample numbers; used when
the Automatic Sample ID is set to ON. Press
this key to access a sub-menu for entering a
numeric increment.
Sample Weight Warning Above: This key displays
and leads to a sub-menu used to set the maximum
allowable sample weight (including spike) in grams.
A warning will be given if sample weights above
this value are entered.
Spike Weight Entry Mode: This key steps through
the options for entering spike weights either manually through the touch screen, balance (USB) port or
network.
Sulfur Entry Mode: This key steps through the options for entering the sulfur correction value either
manually through the touch screen or automatically
through the balance (USB) port.
Moisture Entry Mode: This key steps through the
options for entering the moisture percentage whether manually through touch screen or automatically
through the balance (USB) port.
Moisture Data Entry Controls
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39
4 Menu Descriptions
Moisture as Determined (MAD) Entry Mode:
This key steps through the options for entering
the moisture as determined correction value
either manually or through the touch screen or
automatically through the balance (USB) port.
40
6400
Communication Controls Menu
Menu Descriptions
Customize Balance Setting. Sets the communication parameters for the 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 Settings
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41
4 Menu Descriptions
42
6400
Menu Descriptions
Diagnostics Menu
The white upper portion of the Run Data File Manager screen presents all tests in memory in a scrollable
window. Test attributes include filename (sample
ID), test type, status, and date. Touching anywhere in
the column related to a given test attribute will sort
the file list by that attribute. Successive touches will
toggle between an ascending and descending sort.
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43
4 Menu Descriptions
Data Logger Controls
44
6400
User Defined Buttons
Combine Det. Reports: Pressing this key combines all determination reports into a single
file named /tmp/bigdetfile.txt.
Combine Std. Reports: Pressing this key combines all determination reports into a single
file named /tmp/bigstdfile.txt.
Logged Data to SD: Pressing this key copies
the log file to an SD memory card inserted into
the back of the controller.
Rinse Bomb: This key initiates a bomb rinse. This
function can be used to clean out the cylinder in the
event a sample is spilled inside the cylinder.
Menu Descriptions
I/O Diagnostics:
Press this key to display the I/O Diagnostics submenu, which allows the user to manipulate digital
outputs for troubleshooting. The I/O Diagnostics
screen is used to display the digital outputs at a
basic level for troubleshooting. Both the bucket
and jacket temperatures are also displayed on this
screen. Any output can be selected using the left
and right arrow keys. The selected output is turned
ON (1) or OFF (0) using the 1 and 0 keys. Prior
to entering the Diagnostics Menu, the controller
stores the present state of the outputs. This state is
restored when you exit this screen. Digital outputs
cannot be manipulated while a test is in progress.
Memory
Mass Storage
Network
45
5 Reports
Chapter 5
Reports
Reports
The 6400 Calorimeter can transmit its stored test
data in either of two ways. The AUTO REPORT
DESTINATION key on the Reporting Controls Menu
toggles the report destination between the display
and an optional printer connected to the USB port
of the calorimeter. This menu also selects the type
of reports that are generated automatically by the
calorimeter.
Preliminary Reports are generated at the conclusion of a test. They are intended to confirm to
the operator that the results of the test fell within
the expected range.
Final reports are generated once all of the thermochemical corrections have been entered into
the file. If fixed corrections are used for all of the
thermochemical corrections, a preliminary report
will not be generated. The report will automatically become finalized.
46
6400
Notes
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47
6 Standardizations
Chapter 6
Standardizations
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 1.1 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:
W=
Hm + e1 + e2 + e3
T
Where:
W = Energy equivalent of the calorimeter in
calories per C.
H
= Heat of combustion of the standard
benzoic acid sample in calories per
gram.
m = Mass of the sample.
T
e1
e2
e3
48
= Temperature rise in C.
= Correction for heat of formation of
nitric acid in calories. The default value
in the 6400 is 8.
= Correction for sulfur which is usually 0.
= Correction for heating wire and combustion of cotton thread. The default
value in the 6400 is 50 cal.
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 before it is burned in an oxygen
bomb to avoid possible damage from rapid
combustion of the loose powder. This is best
accomplished by using a Parr 2811 Pellet Press.
6400
Standardizations
Table 6-1
Calorimeter Control Limit Values in J/g When Benzoic Acid is Used as a Test Sample
MAXIMUM PERMISSIBLE
DEVIATION OF THE GROUP MEAN
FROM THE ACCEPTED VALUE OR
GRAND MEAN
79.4
56.1
45.8
39.7
35.5
32.4
30.0
28.1
26.5
25.1
23.9
22.9
22.0
21.2
20.5
19.8
19.2
18.7
18.2
17.7
17.3
16.9
16.5
16.2
15.9
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49
6 Standardizations
Table 6-2
Calorimeter Control Limit Values in cal/g When Benzoic Acid is Used as a Test Sample
50
MAXIMUM PERMISSIBLE
DEVIATION OF THE GROUP MEAN
FROM THE ACCEPTED VALUE OR
GRAND MEAN
19.0
13.4
10.9
9.5
8.5
7.7
7.2
6.7
6.3
6.0
5.7
5.5
5.3
5.1
4.9
4.7
4.6
4.5
4.3
4.2
4.1
4.0
4.0
3.9
3.8
6400
Standardizations
Table 6-3
Calorimeter Control Limit Values in BTU/lb When Benzoic Acid is Used as a Test Sample
MAXIMUM PERMISSIBLE
DEVIATION OF THE GROUP MEAN
FROM THE ACCEPTED VALUE OR
GRAND MEAN
34.1
24.1
19.7
17.1
15.3
13.9
12.9
12.1
11.4
10.8
10.3
9.8
9.5
9.1
8.8
8.5
8.3
8.0
7.8
7.6
7.4
7.3
7.1
7.0
6.8
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51
7 Calculations
Chapter 7
Calculations
Energy Equivalent
The energy equivalent (represented by W in the
formula, or abbreviated as EE) is determined by
standardizing the calorimeter as described in Chapter 6 - 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.
Thermochemical Corrections
General Calculations
The calculation for the gross heat of combustion is
done by:
Hc =
WT-e1 - e2 - e3
m
Where:
Hc
= Gross heat of combustion.
T
= Observed temperature rise.
W
= Energy equivalent of the
calorimeter 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 cal/g and degrees
Celsius and then converted to other units if required.
Temperature Rise
The 6400 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. 483M.
52
6400
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 Thermochemical
Corrections, is set to ON.
By default a fixed fuse correction of 50 calories
is applied to all tests. Total errors of more than 3
calories will seldom occur when using a fixed fuse
correction and the thread supplied by Parr.
When using the 6400, there are two components to
the fuse correction:
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 6400 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.
Calculations
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 6400 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
6400 Calorimeter uses the most recent, published values for all thermochemical data.
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53
7 Calculations
Thermochemical Calculation Details
Traditionally, standard solutions and procedures
have been established to simplify the calculations
related to the thermochemical corrections. The 6400
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.
54
Sulfur Correction:
e2 = (percent sulfur)(sample mass)(sulfur multiplier)(heat of formation of H2SO4).
Acid Correction:
In the 6400 there are a number of settings for the
acid correction.
e1 is the nitric acid portion of the correction.
Fixed HNO3: The Acid Correction is a fixed value set
by the operator.
The calculation is:
e1 = (nitric acid value)(acid multiplier)(heat of
formation of nitric acid)
For an 1138 bomb the default nitric acid value is 8
and acid multiplier is .0709. The heat of formation
of nitric acid is 14.1 calories/milliequivalent so the
calculation is:
e1 = (8)(.0709)(14.1) or e1 = 7.9975 (rounds to 8)
When the Acid Correction is set to Fixed HNO3 the
value is considered a final value and the operator is
not prompted for an acid value when reporting the
results.
Entered HNO3: The Acid Correction is entered by the
operator when reporting the results.
The calculation is the same as Fixed HNO3 above.
The value listed on the Acid Correction button is
used for preliminary calculations. When finalizing
the report the operator will be prompted for the acid
value.
Fixed Total: The Acid Correction represents the total
base required to titrate the bomb washings (in milliliters). This includes both nitric and sulfuric acid.
The correction is a fixed value set by the operator.
The calculation is:
e1 = [((total acid)(acid multiplier)) (% sulfur)
(sample mass)(sulfur multiplier)](heat of formation of nitric acid)
6400
Using the default acid and sulfur multipliers as well as
a heat of formation of nitric acid of 14.1 cal/milliequivalent a 1 gram sample with 25 ml of washings and 2
% sulfur would result in the following calculation:
e1 = [((25)(.0709)) (2)(1)(.6238)] 14.1
e1 = [(1.7725) (1.2476)] 14.1
e1 = [.5249] 14.1
e1 = 7.40
When the Acid Correction is set to Fixed Total the
value is considered a final value and the operator is
not prompted for an acid value when reporting the
results.
Entered Total: The Acid Correction represents the
total base required to titrate the bomb washings
(in milliliters). This includes both nitric and sulfuric
acid. The correction is entered by the operator when
reporting the results.
The calculation is the same as the Fixed Total above.
The value listed on the Acid Correction button is
used for preliminary calculations. When finalizing
the report the operator will be prompted for the acid
value.
Calculated HNO3: In ASTM D5865 there are provisions for calculating the nitric acid contribution.
For test samples that contain no nitrogen, the
quantity of nitric acid formed during the combustion
process is a function of the volume of the bomb, the
oxygen filling pressure, and the quantity of energy
released.
For the calculated nitric acid method:
e1 = (nitric acid factor/1000) x (Energy Equivalent) x (corrected temperature rise)
Example: For a test run with energy equivalent of
927.40 and a corrected temperature rise of 6.892
would result:
Calculations
The calculated nitric acid method can be applied
to samples containing up to 2% nitrogen without
introducing a significant error in the resulting heat
of combustion value.
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 Acid Correction - Thermochemical Corrections,
is set to Fixed HNO3. A correction of 8 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, in Calculation Factors 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 Fixed Sulfur
- Thermochemical Corrections, 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, for
standardizing the calorimeter, the Fixed Sulfur Correction, for Standardizations should be ON applying
a fixed value of 0.0 to all standardization tests.
Benzoic acid contains no sulfur.
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.
e1 = (1.58/1000)(927.4022)(6.892)
e1 = 10.10 calories
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7 Calculations
ASTM Treatment for Acid and Sulfur
ISO Calculations
56
6400
Calculations
Spiking Samples
Hc =
WT-e1 - e2 - e3 - (Hcs)(Ms)
m
Where:
Hcs = The spiking material (cal/g)
Ms = Mass of spiking material
This factor is added to the calculations when Spike
Controls, Use Spiking is set to ON. 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,
Use Fixed Spike is set to ON and entering the mass
of the spike on - Weight of Fixed Spike.
1.8Hc - 91.23H
(Liquid fuels, ASTM D240)
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57
Computer Communications
Chapter 8
Computer Communications
Computer Connections
If the 6400 Calorimeter is to be connected to a
computer, the Ethernet connection should be used.
Test data can be transferred to an Ethernet network
connected computer using the FTP File Transfer
Protocol. First, you must know the IP address of
the network-connected calorimeter. The network
DHCP (Dynamic Host Configuration Protocol) server
provides this address shortly after the calorimeter is
turned on or a static IP address can be assigned. The
address can be seen on the Software & Hardware
Info screen, under Program Info and Control Menu
(see the example screenshot on page 41). Users
who dont have a network infrastructure can create
a simple network by connecting a router with DHCP
server capability to the calorimeter using an ordinary CAT 5 network cable. The calorimeter should
The following screenshot illustrates the contents of the calorimeter data directory as presented by a web browser.
You can drag and drop or copy and paste test data files (with the csv suffix) from the web browser window
to any convenient folder or directory on the PC.
58
6400
Samba Server Feature (Optional)
Samba was originally developed as an implementation of the SMB (Server Message Block) protocol.
The most common use of SMB is in Microsofts CIFS
(Common Internet File System) implementation. As
a result, Samba has become a de facto Microsoft
network compatibility tool. In relation to CIFS,
Samba allows non-Microsoft operating systems to
enjoy effectively seamless server and client operation in networks catering to the needs of Windows
computers. It is an open standard and defined in
IETF RFC1001 and RFC1002.
The Samba server feature option in the Parr 6400
Calorimeter offers seamless file services to Windows based clients. It allows the calorimeter to
interact with a Microsoft Windows client as if it is
a Windows file server. The Samba server feature
can be used to facilitate data file transfer from a
Computer Communications
calorimeter or proximate interface to a PC running
the Windows operating system. This method of file
transfer, for some users, may be less cumbersome
and more intuitive than using a web browser as an
FTP client program to retrieve or log files.
When purchasing this feature, the user must supply
Parr with the MAC address of the calorimeter (found
in the Software & Hardware Info menu screen). This
allows Parr to activate the feature key. In order to
enable the calorimeter to use the bar code feature, the
feature key needs to be entered into the instrument.
Select the PROGRAM INFORMATION AND CONTROL
key from the Main Menu. Next, select FEATURE
KEY and enter the feature key purchased from Parr
Instrument Company into the instrument by using the
touchpad. Pressing the key labeled ABC allows the
user to switch from upper case letters, to lower case
letters, to numerals, and finally to symbols.
To access the test data open the run data folder. To access the log file open the log data folder.
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59
Computer Communications
The calorimeter offers a web server service. Test reports can be viewed with a web browser using a URL of
the following form.
http://10.1.5.10
Where 10.1.5.10 is the IP address of the calorimeter. The following screenshot illustrates the calorimeter
home page.
60
6400
Computer Communications
Clicking on the Config button will display the screen below. Changes made on this screen will change the
settings in the calorimeter.
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61
Computer Communications
Clicking on the Run Data button displays a list of reports currently in the instrument memory.
Clicking on a test under the select sample ID box will display the data for the selected sample ID.
62
6400
Computer Communications
Clicking on the System Info button will display the screen below.
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63
Computer Communications
Clicking on the LCD Snap Shot button will display the current menu screen displayed by the calorimeter. If
the backlight is not on, this screen will display a blank blue square.
Note: This is a picture only. The calorimeter cannot be remotely operated from this screen. Remote
operation requires the appropriate Feature Key.
Please contact Parr Instrument Company for more details about available Feature Keys.
64
6400
Computer Communications
Clicking on the Documentation button will display the screen below. Clicking on any of the links will open the
corresponding web page.
Note: Connection to the internet is required for these links.
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65
Computer Communications
Bar Code Port
The use of barcodes in the laboratory has become
a highly accurate, rapid and inexpensive way to
identify samples. When purchasing this feature,
the user must supply Parr with the MAC address of
the calorimeter (found in the Software & Hardware
Info menu screen). This allows Parr to activate the
feature key. In order to enable the calorimeter to
use the bar code feature, the feature key needs to
be entered into the instrument. Select the Program
Information and Control key from the Main Menu.
Next, select Feature Key and enter the feature key
purchased from Parr Instrument Company into the
instrument by using the touchpad.
Pressing the key labeled ABC allows the user
to switch from upper case letters, to lower case
letters, to numerals, and finally to symbols. A CD
containing all the necessary documentation and
setup information for using both the scanner and
the printer is provided at the time of purchase. A PC
based program used for printing bar coded labels is
also provided on this CD.
66
Table 8-1
6400 Data File Naming Convention
Filename
<ID>.std.plim.csv
<ID>.std.finl.csv
<ID>.det.plim.csv
<ID>.det.finl.csv
<ID>.---.pwgh.csv
6400
Computer Communications
Table 8-2
6400 Calorimeter Run Data Template
Field
SampleID
Timestamp
Mode
Method
State
Units
UnitMultIfOther
BombID
BombEE
SampleWt
SpikeWt
Fuse
FuseFinal
Acid
AcidFinal
Sulfur
SulfurFinal
Hydrogen
HydrogenFinal
MAD
MAD Final
JacketTemp
InitTemp
DeltaT
HOC
NetHOC
DryHOC
DryNetHOC
Oxygen
Description
char[16]
MM/DD/YY HH:mm:ss
0 = determination, 1 = standardization
0 = equilibrium, 1 = dynamic
0 = preweigh, 1 = preliminary, 2 = final
0 = MJ/kg, 1 = BTU/lb, 2 = cal/g, 3 = J/kg, 4 = other
unit multiplier in effect at time of report
[1,4]
bomb energy equivalent
sample weight
spike weight
fuse value
fuse value is final
acid value
acid value is final
sulfur value
sulfur value is final
hydrogen value (net calc option)
hydrogen value is final (net calc option)
moisture as determined value (dry calc option)
moisture as determined is final
jacket temperature
initial temperature
temperature rise
gross heat of combustion
dry net HOC (net calc options enabled)
dry gross HOC (if dry calc option enabled)
dry net HOC (if both dry and net calc options enabled)
oxygen value (net calc option)
Oxygen Final
Nitrogen
Nitrogen Final
MAR
MAR Final
Dry Net HOC_AR
Bomb Name
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67
Memory Management
Chapter 9
Memory Management
The 6400 Calorimeter will hold data for 1000 tests
in its memory. These tests may be pre weights,
preliminary or final reports for either standardization or determination runs. Once the memory of the
controller is filled, the controller will not start a new
analysis until the user clears some of the memory.
Clearing Memory
The FILE MANAGEMENT key on the main menu
leads to the file management sub-menu. The RUN
DATA FILE MANAGER key leads to a listing of the
files.
Removable SD Memory
The controller of the 6400 Calorimeter can accept
SD memory cards, Parr part number 2201E. These
cards can be used to:
68
6400
Notes
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69
10 Maintenance
Chapter 10
Maintenance
Bomb Removal
To service or remove the bomb cylinder from
the bucket assembly, remove the 668DD Check
Valve from the bomb cylinder. Remove the 941DD
Wedge with needle nose pliers. Remove the two
SA1632RD18 Machine Screws (see Figure 14-16),
then remove the 942DD plastic bushings and the
1071DD Quad-ring.
The entire bucket can be removed by disconnecting
the bucket probe at the quick disconnect. 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 14-14). Now the cylinder can be
removed from the bucket assembly. Note the position of the locating pin.
To replace, follow these steps in reverse.
6400
Maintenance
10
Fuses
Type
Ratings
139E23
Lines Protective
Fuses
Fast-Acting
15 Amps,
250Vac
1641E2
Fast-Acting
2.5 Amps,
250VAC
1641E
Fast-Acting
1 Amp,
250VAC
997E5
Slo-Blo
5 Amps,
250VAC
Daily Maintenance
Clean the 1444DDJB O-ring that seals the bomb
head and cylinder by wiping with a tissue. Wet this
sealing area with water prior to starting a series of
tests. Clean the corresponding sealing area in the
cylinder in a similar fashion. Both surfaces must
be free of any accumulated foreign matter, such as
unburned sample material or combustion by-products. Wet the hole in the center of the head which
contains the check valve.
With a tissue, clean the head where the large bucket
quad-ring (1071DD) contacts the head perimeter.
Wet this sealing area with water prior to starting a
series of tests.
Remove, inspect and clean the cylinder check
valve (668DD) and corresponding sealing area in
the bomb cylinder. In extreme cases, i.e. a spilled
sample, use soap and water to clean the area.
Quarterly Maintenance
Change water in the Water Tank and replace the 149C
water filter. Clean the grill on the heat sink at the
rear of the calorimeter.
Periodic cleaning may be performed on the exterior
surfaces of the instrument with a damp cloth. All
power should be disconnected when cleaning the
instrument.
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71
10 Maintenance
The 1140DD Seal/Release mechanism should be serviced with the same frequency as the bomb head.
This includes the replacement and lubrication of the
659DDJU (2), 1138DD, 1143DD and 357HCJB O-rings
with 811DD lubricant. See Figure 14-15 and Figure
14-16 for O-ring locations. The tools required are:
screwdriver, snap ring pliers and needle nose pliers.
1. Turn off the gas supply to the calorimeter. Raise
the lid. Go to the I/O Diagnostics Screen and
turn on the bomb seal command. Turn on the O2
Fill Command. Wait for the oxygen tube in the
lid to stop hissing. These steps are necessary
to release the gas pressure in the seal/release
mechanism before disassembling.
2. Turn off the calorimeter.
Proof testing
Hydrostatic testing
6. Remove the vessel spacer, 964DD and the associated O-ring, 969DD.
There are no user serviceable parts inside the product other than what is specifically called out and discussed in this manual. Advanced troubleshooting
instructions beyond the scope of this manual can be
obtained by contacting Parr Instrument Company in
order to determine which part(s) may be replaced or
serviced.
72
6400
Maintenance
10
Date
Quarterly Maintenance
Date
Date
Date
Date
Date
1. Change water
2. Replace 149C
3. Clean grill on
heat sink.
1. Replace 8400DD2
Heating Wire
2. Clean 986DD
Electrode Contact
Pins
500 Test Maintenance
Replace the following:
Date
Date
Date
Date
Head:
1374HCJV (2) O-rings
394HC O-ring
694DD O-ring
519AJV O-ring
659DD O-ring
1444DDJB O-ring
Cylinder:
1071DD Quad ring
821DD O-ring
882DD O-ring
Bucket and Bomb Seal/Exhaust area:
969DD O-ring
1143DD O-ring
1138DD O-ring
659DDJU (2) O-rings
357HCJB O-ring
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73
11 Troubleshooting
Chapter 11
Troubleshooting
74
6400
Troubleshooting 11
Caution!
Turn off the power to the calorimeter prior
to attempting to reset the thermostat. The
temperature control assembly can become
very hot. Use caution when servicing this
area of the calorimeter.
If line voltage (115V or 230V) is present across the
heater cartridge connection, check the resistance
across the heater cartridge. Approximately 70 ohms
will be seen with a 115V calorimeter. Approximately
140 ohms will be seen with a 230V calorimeter. If
the resistance is not correct the heater may have
failed.
If the voltage is not present, then examine the 2040E
thermostat reset button. If the reset button extrudes
this means that the temperature in the temperature
control assembly has exceeded 75C. Confirm that
water is flowing through the system, turn off the
power and then reset the switch by depressing the
button. If the thermostat continues to trip even
though water is flowing through the system, refer to
the error code There Is A Problem With The Jacket
Thermistor for further troubleshooting.
If there is no voltage present, and the reset button
on the thermostat is not tripped, refer to the error
code There Is A Problem With The Jacket Thermistor for further troubleshooting. There may also
be a problem with the calorimeter controller,
A1250DD2, and Parr service should be contacted.
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75
11 Troubleshooting
Error List
The calorimeter will run a number of diagnostic
checks upon itself and will advise the operator if it
detects any error conditions. Most of these errors
and reports will be self-explanatory. The following
list contains errors that are not necessarily selfevident and suggestions for correcting the error
condition.
A bomb leak
A bomb leak
A bomb leak
76
Replace probe
Replace board
Replace probe
Replace board
Troubleshooting 11
6400
Bomb ID Has Been Fired Times Which Exceeds the Bomb
Service Interval.
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
Calibration Data and Control page for appropriate
bomb number.
The heater loop break limit has been detected. The heater
will now be shutdown.
This error means that the calorimeter is trying to
heat the water in the unit for an extended period of
time. When the heater and pump are initially turned
on the heater will be at 100% power until the jacket
temperature approaches 29.5 C. Once it gets close
the power being applied to the heater will be cut
back to avoid overshooting the target of 30 C.
You Have Exceeded the Run Data File Limit (1000 Files).
The memory set aside for test runs has been filled.
Use the memory management techniques to clear
out non-current tests.
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77
12 Technical Service
Chapter 12
Technical Service
Should you need assistance in the operation or service of your instrument, please
contact the Technical Service Department.
Telephone: (309) 762-7716
Toll Free: 1-800-872-7720
Fax: (309) 762-9453
E-mail: [email protected]
Any correspondence must include the following basic information:
78
Notes 12
6400
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79
13 Parts Lists
Chapter 13
Parts Lists
Description
1138/1138CL
1795E
1796E
897E
A1250DD2
A1251DD
A1447DD
A1448DD
A1449DD
A1254DD2EB
A1254DD2EE
A1255DD
1433DD
A1449DD
A1456DD
A1275DDEB
A1275DDEE
139E23
Caution!
For continued protection against possible
hazard, replace fuses with same type and
rating of fuse.
80
Description
Film Guard, LCD 1802E
Speaker Assembly with Cable
Power Cable Assembly
A1823E
A2140E
A2141E
A2154E6
A2163E
A2164E
A2166E
A2167E
1477DD
2147E
1472DD
Description
O-ring, Buna-N .237 ID
Seal SS
Pin, Anti-rotating (A940DD)
1416E
1462E2
A940DD
A1255DD
659DD
Thermistor, Bucket
Thermistor Cable
Tube Assy, Bucket; Soldered
Bucket Stirrer Assembly
O-ring NBR 5/32 ID x 1/16 CS
6400
Parts Lists
Description
Snap Ring, Internal .50
Wave Spring, .50 OD
Ball Bearing, .50 OD
690DD
715HC
954DD
1029DD
1242DD2
SA1140RD04
SN1140HLHJ
1327DD
V-Seal, Nitrile
O-ring NBR 1-1/4 ID
Propeller
Baffle Assembly
Pulley, Timing
4-40 X RHMS 18-8 SS
Nut, 4-40 Hex Lock
Housing, Bearing Brass
1030DD
Shaft, Stirrer
13
Description
Container, PP 10L Foldable
Benzoic Acid Pellets 100 Gram Bottle
Pliers for Snap Ring
Capsule, SS
Lube/Sealant
Heating Wire
Ignition Thread, 4
876DD
1005DD
A1006DD
A38A
TX03SKMM
TX14SK
149C
1344DD
1889E
HJ0025TB035
HX0012TB024
Spring Compression
Snap Ring External .219
Bushing 0.125 ID
6-32 Hex Nut 18-8 SS
Plunger/Knob Assembly
Cover, Air
Plate
Friction Hinge
Latch Block
Post, Latch Locking
Cover/Tubing Assembly
Tubing PTFE
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81
14 Drawings
Chapter 14
Drawings
Figure 14-1
1138 Parts Diagram
82
Drawings 14
6400
1138 Parts Diagram Key
Key
Item
Description
888DD2
Cylinder
889DD
Outer Ring
821DD
668DD
Check Valve
882DD
925DD
Bomb Retainer
SA1632RD06 (2)
902DD
899DD
Head Handle
10
1454DD
Funnel
11
904DD (2)
12
905DD
13
SA1632FT06 (2)
14
898DD
Locator Cap
15
SN1632HX
16
1374HCJV (2)
17
394HC
18
663DD
Contact Bushing
19
1071DD
20
1444DDJB
21
1452DD
Head
1452DDCL
22
655DD (2)
Electrode Spacer
23
1095DD
Electrode
24
PA1332RD04 (2)
25
656DD
Reducer Bushing
26
653DD
Electrode Nut
27
43AS
Capsule
28
906DD
Capsule Holder
29
658DD
Insulator
30
654DD
Electrode Washer
31
1094DD
Electrode
32
643DD
Check Valve
33
645DD
Water Diffuser
34
647DD
Anti-Rotator
35
SC1332SC02 (3)
36
SA1332FP04
37
659DD
38
840DD2
39
694DD
40
1453DD
41
519AJV
Item
Complete Assemblies
A1450DD
A1450DDCL
A890DD2
Cylinder Assembly
A890DD2CL
83
14 Drawings
Figure 14-2
6400 Cutaway Right
84
Drawings 14
6400
Figure 14-3
6400 Cutaway Left
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85
14 Drawings
Figure 14-4
6400 Cover Open
1324DD2
Locking
Post
86
A2140E
IO BOARD
P6
P8
USB PORT
A2154E
CPU BOARD
www.parrinst.com
J10
J1
J9
J8
J4
TOLERANCES
IN INCHES
UNLESS OTHERWISE SPECIFIED
J100
J17
PROPRIETARY
J6
J5
2147E
LCD DISPLAY
REVISIONS
FOR
J8
J2
J9
BACK PANEL
USB PORT
6300/6400 CALORIMETER
J19
A1823E TOUCH
SCREEN CABLE ASSY
A1821E
SPEAKER
CABLE
ASSEMBLY
Electrostatic Discharge
(ESD)
UNMARKED
RADII .03" hazards. Observe precautions for
MACHINED SURFACES:
handling electrostatic 64sensitive
devices. DRAWN IN 3rd ANGLE PROJECTION DO NOT SCALE DRAWING
OR BETTER
ATTENTION:
PIN #1
PIN #1
1472DD
LCD ENCASEMENT
J6
J1
SCALE
APPROVED
NTS
02-26-10
02-22-10
MAW
SIZE
BY
SHEET 1 OF *
A1250DD2
DWG NO.
CONTROLLER SCHEMATIC
A2165E
REF
DETAIL "A"
CONTACTS ARE
EXPOSED
IN THIS VIEW
DRAWN
DATE
DATE
J1
DESCRIPTION
J10
A2165E
TRANSITION
BOARD TO
DISPLAY CABLE
A2141E
LCD TRANSISTION
BOARD
(SEE SHEET 2 FOR INSTALLATION
ON ENCASEMENT)
6400
Drawings 14
Figure 14-5
87
14 Drawings
Figure 14-6
A1251DD Oxygen Solenoid Assembly
Figure 14-7
A1447DD Water Solenoid Assembly
88
Drawings 14
6400
Figure 14-8
A1456DD Rinse Valve Assembly
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89
14 Drawings
Figure 14-9
6400 Internal Plumbing Diagram
90
Drawings 14
6400
Figure 14-10
6400 Water Tank and Jacket Cooling Solenoid
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91
14 Drawings
Figure 14-11
A1455DD Propeller Assembly
Apply thread sealant (Locktite or equivalent to set screw in 1242DD2 pulley before installing.
Figure 14-12
A1448DD Temperature Control Assembly
92
Drawings 14
6400
Figure 14-13
A1268DD Stirrer Motor and Mount
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93
14 Drawings
Figure 14-14
6400 Bucket Assembly
94
Drawings 14
6400
Figure 14-15
6400 Air Can Assembly, Cutaway Left
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95
14 Drawings
Figure 14-16
6400 Air Can Assembly, Cutaway Front
96
Drawings 14
6400
Figure 14-17
A1450DD Bomb Head Assembly, View 1
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97
14 Drawings
Figure 14-18
A1450DD Bomb Head Assembly, View 2
98
Drawings 14
6400
Figure 14-19
1.50
1052DD
BOTTLE CAP
TOLERANCES
....
....
....
1/64
.010
.003
ANGULAR .. 1/2
UNMARKED RADII .03"
1/X
.00
.000
IN INCHES
UNLESS OTHERWISE SPECIFIED
HX0025TB062
1/4" TUBING X 4 FT LG
411VBAD REDUCER
(1/4T-3/8Tx)
1051DD
EXHAUST DIFFUSER
FOR
REVISIONS
1281 CALORIMETER
R1 ADDED NOTE 4; 7-19-95 PJC
R2 WAS BOMB; 10-15-97 TVK
R2
MOLINE, ILLINOIS
A1050DD
DESCRIPTION
VESSEL RINSE CONTAINER ASSY
PART NO.
7-17-95 BY PJC
7-17-95 BY DGM
CAD
CK
FULL
DATE
DRAWN
DATE
CHECKED
SCALE
99
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14 Drawings
Figure 14-20
Wiring Diagram
100
Drawings 14
6400
Figure 14-21
Wiring Diagram
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101
14 Drawings
Figure 14-22
Fuse Diagram
102
6400
Notes
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14
103
15
Tables
Chapter 15
Tables
Table 15-1
Factory Default Settings
Calorimeter Operations
Operating Mode
Bomb Installed/EE
Heater and Pump
Operating Controls
Method of Operation
Reporting Units
Use Spiking Correction
OTHER Multiplier
Calibrate Touchscreen
LCD Backlight Timeout(s)
LCD Backlight Intensity
Print Error Messages
Language
Spike Controls
Use Spiking
Heat of Combustion of Spike
Use Fixed Spike
Weight of Fixed Spike
Prompt for Spike before Weight
Bomb Rinse Tank Control
Report Rinse Tank Empty
Rinse Tank Capacity
# Rinses Left
Reset Rinse Tank Counter
Rinse Time
Rinse Flush Time
Clear Time
# of Rinse Cycles
104
Dynamic
BTU/lb
OFF
4.1868
1200 S
70%
ON
English
OFF
6318.4
OFF
0.0
OFF
ON
150
150
25
20
100
3
Date
Time
Volume Level Adjust
Software and Hardware Info
Settings Protect
User/Factory Settings
Feature Key
Bomb Type Select
User Function Setup
Cold Restart
User/Factory Settings
User Setup ID
Reload Factory Default Settings
Reload User Default Settings
Save User Default Settings
Calibration Data & Controls
Calibration Run Limit
EE Max Std Deviation
Heat of Combustion of Standard
Bomb Service Interval
Use Bomb
Bomb 1 Through 4
EE Value
Protected EE Value
XX/XX/XXXX
XX:XX
85%
OFF
64-1138
10
0.0
6318.4
500
1
940
OFF
6400
Determination
Fixed Fuse Correction
Acid Correction
Fixed Sulfur Correction
Net Heat/Dry Factors
Tables
15
Calculation Factors
Nitric Acid Factor
Acid Multiplier
Sulfur Value is Percent
Sulfur Multiplier
Fuse Multiplier
Use Offset Correction (ISO)
Offset Value
Heat of Formation Sulfuric Acid
Heat of Formation Nitric Acid
Net Heat/Dry Factors
Fixed Hydrogen
Fixed Oxygen
Fixed Nitrogen
Calculate Net Heat of Combustion
Fixed Moisture as Determined
Fixed Moisture as Received
Dry Calculation
Data Entry Controls
Prompt for Bomb ID
Weight Entry Mode
Acid Entry Mode
Net Heat Entry Modes
Auto Sample ID Controls
Sample Weight Warning above
Spike Weight Entry Mode
Sulfur Entry Mode
Moisture Entry Modes
Auto Preweigh Controls
1.58
0.0709
ON
0.6238
1.0
OFF
0.0
36.1
14.1
Automatic Sample ID
Automatic Sample ID Number
Automatic Sample ID Increment
Auto Preweigh Controls
Automatic Preweigh ID
Automatic Preweigh ID Increment
Automatic Preweigh ID Number
ON
1
1
ON
1
1
Reporting Controls
Report Width
40
Automatic Reporting
ON
Auto Report Destination
Printer
Individual Printed Reports
OFF
Edit Final Reports
OFF
Recalculate Final Reports
OFF
Use New EE Values in Recalculation
OFF
Report Schedule
End of Cool/Rinse
OFF 0.0
ON 0.0
ON 0.0
OFF
OFF 0.0
OFF 0.0
OFF
Communication Controls
Printer Type
Balance Port
Network Interface
Printer Destination
Bar Code Port
Network Data Devices
Parr 1758
Local USB
ON
Touch Screen
Touch Screen
Generic
ON
2.0
Touch Screen
Touch Screen
8
None
1
None
9600
8
4
10
ON
Touch Screen
Touch Screen
Touch Screen
Touch Screen
Touch Screen
Data Logger
Data Logger
Interval in Seconds
Data Log Destination
OFF
12
Log File and Printer
Text
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105
15
Tables
Table 15-2
Settings for ISO & BSI Methods
Page
Thermochemical
Corrections
Line
Setting
Value
Entered HNO3
13
Off
Entered HNO3
13
Off
Acid Multiplier
Sulfur Value is Percent
Calculations Factors
Off
Sulfur Multiplier
Use Offset Correction
Offset Value
106
0.154
0.1
On
-43.5