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VERSION 4.8
Contents
HISTORY OF DDS BOMB CALORIMETERS .................................................................................................................. 13
HOW TO USE THIS MANUAL ..................................................................................................................................... 13
WARNING SYMBOL ............................................................................................................................................... 14
INFORMATION (NOTE) SYMBOL ........................................................................................................................... 14
.............................................................................................................................................................................. 14
CALORIMETER (CAL2K-1) .......................................................................................................................................... 14
COOLER (CAL2K-2) .................................................................................................................................................... 15
FILLING STATION (CAL2K-3) ...................................................................................................................................... 15
HIGH PRESSURE OXYGEN .......................................................................................................................................... 15
VESSEL (CAL2K-4) ...................................................................................................................................................... 16
SYSTEM COMPONENTS ............................................................................................................................................. 17
THE CALORIMETER (CAL2K-1) ................................................................................................................................... 18
.................................................................................................................................................................................. 18
EXTERNAL CONNECTIONS (REAR PANEL) .............................................................................................................. 19
CALORIMETER COMPONENTS............................................................................................................................... 19
.................................................................................................................................................................................. 20
KEYPADS/KEYBOARDS........................................................................................................................................... 20
.................................................................................................................................................................................. 20
LCD DISPLAY .......................................................................................................................................................... 20
INDICATOR LAMP.................................................................................................................................................. 20
BEEPER (SITUATED BEHIND KEYBOARD) ............................................................................................................... 20
DOOR LATCH AND LID SWITCH ............................................................................................................................. 20
VESSEL CONNECTIONS .......................................................................................................................................... 21
THE COOLER CAL2K-2 ............................................................................................................................................... 21
.................................................................................................................................................................................. 21
COOLER SYSTEM COMPONENTS ........................................................................................................................... 22
COOLER INSTALLATION ......................................................................................................................................... 22
COOLER PERFORMANCE TESTING ......................................................................................................................... 22
COOLER NORMAL OPERATION ............................................................................................................................. 23
COOLER DISPLAY PANEL........................................................................................................................................ 23
SAMPLE ................................................................................................................................................................. 43
COOLING ............................................................................................................................................................... 44
EXPLANATION OF DISPLAY DURING A DETERMINATION .......................................................................................... 45
LID OPEN – NO VESSEL IN WELL ............................................................................................................................ 45
SELECT MASS & SID ............................................................................................................................................... 45
CLOSE LID .............................................................................................................................................................. 45
INITIAL .................................................................................................................................................................. 45
FIRING ................................................................................................................................................................... 46
FINAL..................................................................................................................................................................... 46
DONE .................................................................................................................................................................... 46
OPEN LID ............................................................................................................................................................... 46
DETERMINATION OF VESSEL DEVIATION FACTOR .................................................................................................... 46
DETERMINATION OF CALORIMETER DEVIATION FACTOR ......................................................................................... 46
.................................................................................................................................................................................. 47
SINGLE VESSEL SYSTEM............................................................................................................................................. 47
DUAL VESSEL SYSTEM ............................................................................................................................................... 47
TRIPLE VESSEL SYSTEM ............................................................................................................................................. 48
.................................................................................................................................................................................. 48
SAMPLE MASS ENTRY ............................................................................................................................................... 48
NORMAL DETERMINATION ....................................................................................................................................... 48
CALIBRATION ............................................................................................................................................................ 49
ENTER USER ID (NUMBER) ........................................................................................................................................ 49
RECALL DEFAULT SETUP............................................................................................................................................ 50
BA CHECK SAMPLE ON/OFF ...................................................................................................................................... 50
DISPLAY OR SET GID .................................................................................................................................................. 51
DISPLAY ACTIVE BOMB CAL. ..................................................................................................................................... 51
DISPLAY B. CAL DETAILS ............................................................................................................................................ 51
SPIKE VALUE ............................................................................................................................................................. 53
SPIKE MASS ............................................................................................................................................................... 53
SPIKING ON/OFF ....................................................................................................................................................... 53
TIME OF DAY IN HHMM ............................................................................................................................................ 54
DATE IN DDMMYY..................................................................................................................................................... 54
CLEAR HEAP .............................................................................................................................................................. 54
DISPLAY SOFTWARE VERSION ................................................................................................................................... 55
CALIBRATION VALUE OF B.A. .................................................................................................................................... 55
CALIBRATION DEVIATION ......................................................................................................................................... 55
SAVE CALIBRATION 0-9 ............................................................................................................................................. 56
RECALL CALIBRATION................................................................................................................................................ 56
INITIAL DRIFT IN DEGREE C ....................................................................................................................................... 56
INITIAL TIME IN MINUTES ......................................................................................................................................... 57
FINAL DRIFT IN CAL VALUE........................................................................................................................................ 57
FINAL DRIFT IN DEGREE C ......................................................................................................................................... 57
FINAL TIME IN MINUTES ........................................................................................................................................... 57
SET AMBIENT TEMP. OFFSET .................................................................................................................................... 57
CORRECTION #1 (SULPHUR)...................................................................................................................................... 58
CORRECTION #2 (COTTON) ....................................................................................................................................... 58
SET CALORIMETER ID 1-7 .......................................................................................................................................... 58
SET BOMB NUMBER ................................................................................................................................................. 58
SET FIRING VOLTAGE ................................................................................................................................................ 59
INITIAL COMPENS. ON/OFF ...................................................................................................................................... 59
HIGH MASS LIMIT ..................................................................................................................................................... 59
LOW MASS LIMIT ...................................................................................................................................................... 59
BALANCE MASS, PC OFF ............................................................................................................................................ 59
ENERGY UNIT : BTU, CAL, MJ .................................................................................................................................... 60
AUTOMATIC BALANCE MASS .................................................................................................................................... 60
SELECT LANGUAGE 1-4 ............................................................................................................................................. 60
LOW RISE CURVE CHANGE ........................................................................................................................................ 61
ENABLE BOMB MASS ENTRY ..................................................................................................................................... 61
RECOMMENDED VALUE FOR MJ/KG......................................................................................................................... 61
SPIKE VALUE ............................................................................................................................................................. 63
SPIKE MASS ............................................................................................................................................................... 63
STEP BY STEP ENTERING THE SPIKE VALUE ............................................................................................................... 63
SOFTWARE INTALLATION.......................................................................................................................................... 64
MINIMUM SYSTEM REQUIREMENTS .................................................................................................................... 64
STEP BY STEP INSTALLATION..................................................................................................................................... 64
INSTALLING THE CAL2K MANAGEMENT TOOL ...................................................................................................... 64
USING THE CAL2K MANAGEMENT TOOL SOFTWARE ............................................................................................... 68
FAMILIARISING THE SOFTWARE FUNCTIONS ........................................................................................................ 68
USER SECURITY MANAGER ................................................................................................................................... 70
ADMINISTRATE USERS .......................................................................................................................................... 70
AUTOMATED DOWNLOAD OF RESULTS FROM CAL2K .......................................................................................... 71
FILE MANAGEMENT .............................................................................................................................................. 71
MENU ITEMS......................................................................................................................................................... 72
DECIMAL SEPARATOR ........................................................................................................................................... 73
TOOLS ................................................................................................................................................................... 73
STATUS.................................................................................................................................................................. 73
SETUP CALORIMETER ............................................................................................................................................ 74
HELP ...................................................................................................................................................................... 74
DISPLAYED INFORMATION ITEMS ......................................................................................................................... 75
BUTTON ITEMS ..................................................................................................................................................... 75
SETTING UP THE CALORIMETER ............................................................................................................................ 76
LOADING A FILE .................................................................................................................................................... 77
UPLOADING AND RETRIEVING RESULTS ............................................................................................................... 78
VIEW VESSEL ......................................................................................................................................................... 81
TEMPERATURE GRAPH.......................................................................................................................................... 82
GRAPH EXPLANATION ........................................................................................................................................... 83
DRIFT CURVE ......................................................................................................................................................... 84
CALORIFIC CURVE ................................................................................................................................................. 84
LOAD CURVES ....................................................................................................................................................... 85
HEAP MANAGEMENT............................................................................................................................................ 86
ADVANCED CALIBRATION ..................................................................................................................................... 86
CURVES ................................................................................................................................................................. 87
SAVING OPTIONS .................................................................................................................................................. 88
................................................................................................................................................................................ 121
PRESSURE CONVERSIONS ....................................................................................................................................... 123
MJ / CAL / BTU ENERGY CONVERSIONS .................................................................................................................. 123
BALANCE SETTINGS FOR CAL2K BOMB CALORIMETER ........................................................................................... 123
DB25 CONNECTOR .............................................................................................................................................. 123
INTRODUCTION
Digital Data Systems (Pty) Ltd (dds) specializes in the design and manufacture of scientific Bomb Calorimeter systems
for various types of industries and applications from the coal mining industry to educational institutes. dds Bomb
Calorimeter systems are the most advanced bomb calorimeter systems available today. The system is used to
measure the calorific value of both solids and liquids. dds has three different Bomb Calorimeter models in their
Scientific CAL2k range:
You have chosen the CAL2k Bomb Calorimeter System, which is best suited for your calorimetry requirements.
With the processing power of the microprocessors available at the time, the CP500 Calorimeter was born with its
striking “buttercup yellow” colour. The CP500 proved to be a very fast and reliable system and was exported to the
USA, Europe, Scandinavia, Australasia, Africa and India.
In early 2002 work began on the new CAL2k model. The tried and tested DRY system was retained and only the very
latest electronic technology was used, including surface mount devices. The CAL2k is now in full production and is
sure to be an even bigger success than its predecessor, the CP500. In 2005, dds realized the need for a smaller, low
sample volume, and inexpensive calorimeter system with the same accuracy and reliability of the CAL2k. Based on
these requirements, the ECO was then created as an alternative system to the CAL2k. By 2007, due to customer
demands work began on the e2k model. The e2k was designed to be able to have two language options – one being
English and the other an alternative language for example French. The e2k was also designed to work faster than
the ECO but not as fast as the CAL2k with less features as the CAL2k to keep it cost-effective.
WARNING SYMBOL
This yellow triangle with an exclamation mark inside it, indicates a WARNING message or a message
that is instructing you NOT to do something. Please take note of this message, because if you ignore it
you could damage the Calorimeter equipment.
This white hand with a finger pointing, indicates a NOTE or INFORMATIVE message. It indicates
something that you need to pay attention to. Please take note of this message, as it provides special
or detailed information about a particular item.
SAFETY
CALORIMETER (CAL2K-1)
• Electrical Shock: There are NO user serviceable parts inside.
• Do not open the back panel unless the mains cable has been disconnected.
• Dangerous voltages will be present inside after the mains cable has been disconnected.
DO NOT TAMPER WITH THE EARTHING - CONSULT A QUALIFIED ELECTRICIAN SO THAT THE
EARTHING CAN BE CHECKED.
COOLER (CAL2K-2)
• Electrical shock: There are NO user serviceable parts inside.
• Do not open with the water hoses connected.
• Disconnect from Mains before opening the Cooler (CAL2K-2).
• Dangerous voltages will be present inside after the mains cable has been disconnected.
DO NOT TAMPER WITH THE EARTHING - CONSULT A QUALIFIED ELECTRICIAN SO THAT THE
EARTHING CAN BE CHECKED.
DO NOT USE ANY OTHER PIPE OTHER THAN THE HIGH PRESSURE PIPE SUPPLIED.
ALWAYS FILL THE VESSEL WITH OXYGEN TO A MAXIMUM PRESSURE OF 3000KPA (30 BAR).
NOTE: With some applications you may need to fill the Vessel to less than 3000KPA e.g. 1500KPA (15
bar), however this is only applicable when you have a sample which is highly combustible, for
example with wood related samples.
REMEMBER: You may fill the Vessel LESS than 3000KPA but NEVER more than 3000KPA.
NEVER use oil or oil based grease on any part of the gauge assembly or any part of the Filling Station
and Vessel for SAFETY reasons!
• Use only an approved pressure reduction valve with a safety blow valve.
• Consult your safety engineer when in doubt.
VESSEL (CAL2K-4)
• The Vessel has been pressure tested (certificate will be provided if required), at 3000 KPa according to
international standards.
• The Vessel and its Cap’s thread is subject to wear and tear, and it must be inspected regularly. Check for
excessive play.
• A Vessel with “loose” or worn threads is dangerous, and it must be repaired (reconditioned) by the dds
Factory.
• A Vessel with worn threads may cause the lid to blow off during a determination, which is extremely
dangerous and may cause injury to the operator. Vessels with worn threads which cannot be reconditioned
will be deemed unsafe and a condemnation certificate will be issued.
• Vessels should be returned to dds every 6 months for reconditioning, checking and subsequent pressure
tests. A Vessel will require reconditioning after 5000 firings; however it is this quantity could be significantly
reduced depending on the type of samples analysed. Therefore it is advisable to have your Vessel(s)
checked regularly. Vessels will need to be returned to dds for reconditioning, an agent is not authorised to
recondition a Vessel and therefore it must be sent to dds for this procedure.
• Do not extend any part of your body over the CAL2K-1 Calorimeter during the initial period.
• Consult your safety engineer or your mechanical engineer for guidelines, when in doubt.
NEVER IMMERSE THE VESSEL INTO COLD WATER WHEN COOLING. USE THE CAL2K-2 COOLER OR
ALLOW THE VESSEL TO COOL DOWN NATURALLY.
NOTE: THE MANUFACTURER (DDS) AND ITS AGENTS CANNOT BE HELD RESPONSIBLE FOR ANY LOSS
OR DAMAGE RESULTING FROM NEGLIGENCE OR INCORRECT USE OF THEIR EQUIPMENT. IT IS YOUR
DUTY AND RESPONSIBILITY TO CHECK ALL SAFETY ASPECTS OF THE CAL2K SYSTEM REGULARLY.
There are no special precautions to be taken during unpacking, other than retaining all the packaging material.
Other information and instructions when unpacking the Bomb Calorimeter System, can be found in the printed
CAL2k Handbook.
GETTING STARTED
SYSTEM COMPONENTS
Congratulations on purchasing your new CAL2k Bomb Calorimeter System!
The CAL2k System is the most advanced Calorimeter system available today and if treated with the care and respect
it deserves, it will give you years of service and satisfaction. No other calorimeter operates quite like the CAL2k and
for this reason, we ask you to spend some time learning and discovering its qualities and idiosyncrasies. The time
invested in studying this manual will provide you, the User, with the maximum usage of the machine.
LCD
Display
Numerical
Keypad/Keyboard
Indicator
Pilot Light
Operating
Keypad/Keyboard
CALORIMETER COMPONENTS
The Calorimeter comprises of the following components:
An Installation Kit is supplied with necessary accessories and spare parts. Please refer to the section on the CAL2K-1
Calorimeter Installation Kit at the back of this manual, for a list of which items are included in this kit.
SPECIAL
FUNCTION RESULT CLEAR ID ENTER
(History) Clear Screen Entry Accepts a
File or Exit from Keyboard
present Entry
operation
LCD DISPLAY
The display consists of 4 lines (rows), each has a maximum of 40 characters:
• Line #1: Calorimeter Operations
• Line #2: Result and Mass Selection
• Line #3: Faults, Warnings, Key Entry
• Line #4: Menu, Parameter Display
INDICATOR LAMP
This lamp indicates the status of the Calorimeter unit:
OFF : The unit is OFF or the Lid is OPEN.
ON : The Lid is CLOSED and a determination is IN PROGRESS.
FLASHING : The determination is COMPLETE and the Lid is CLOSED or an ERROR OCCURED during the
determination and the Lid is CLOSED.
VESSEL CONNECTIONS
These are situated inside the Vessel Well, inside the Calorimeter. There are four (4) connections between the
Calorimeter and the Vessel. Three connections are in the Base of the Well and the fourth connection is at the top of
the Vessel where the Vessel connects to the Lid Contact inside the Calorimeter’s Lid.
The ground contact is incorporated in the 3 Vessel supports. Communication with the Vessel is via the two spring-
loaded contacts in the centre of the Base board. The firing contact is in the centre of the Lid and again is a spring
contact, which only makes contact when the Lid is closed.
Door Lock
Well
Door
An Installation Kit with Accessories and Spare Parts is supplied with the Cooler. Please see the Section of CAL2K-2
Cooler Installation Kit at the back of this manual, for a list of which items are included.
COOLER INSTALLATION
• A stable, balanced workbench, near water and mains power supply is required.
• The power requirements (Mains supply) need to be the following:
o Voltage: 90 – 260 VAC, 50/60Hz
o Consumption: 150 Watts Maximum
• The CAL2K-2 needs to be positioned in a convenient place where it has access to both a mains supply and a
main water supply (please note that only a TRICKLE of water flow is required).
• Water may also be circulated through a tank system.
• Connect the water supply to the CAL2K-2 pipe marked IN using the plastic water pipe and fittings supplied.
The pipe marked OUT is to be taken to a draining point such as a sink or sump. Connect the ambient cable
between the CAL2K-1 and the CAL2K-2 to the respective plugs marked AMBIENT SENSOR. This is for the
remote temperature sensor for the Cooler. The Ambient Sensor cable is reversible.
• Plug in the Mains cable.
• Remove ambient cable and check that “AMBIENT FAULT” LED comes on. Re-insert ambient cable, and
observe that the LED switches off again.
This Cooler is designed to reduce the temperature of a recently fired Vessel to ambient temperature. The ambient
temperature reference is plugged into the CAL2K-1 Calorimeter ambient sensor. Solid state cooling is used and the
hot junction of the Peltier elements is cooled by a continuous trickle from the mains water supply.
After installation and an initial warm-up or cool-down period, the unit is designed to operate continually and will
reduce the average hot Vessel to ambient in approximately 2 minutes. This unit is suitable for high volume workload
applications.
For a small volume workload the Cooler can be set in idle mode, when it is not required.
If 0,5 grams of average coal is burnt in the CAL2K-4 Vessel, the temperature will rise by approximately 9 degrees C,
however this is not fixed and may rise above or below 9 degrees C. The energy released is approx. 220 Watt min.
This heat has to be dissipated before a new determination can be started, otherwise the Vessel would get warmer
with every determination.
The Cooler, with an effective cooling capacity of 200 Watt can cool the Vessel to its starting temperature within 2
minutes. The Vessel needs to be at ambient temperature prior to a determination.
This "cooling to ambient" is done to allow the Vessel enough time to stabilise (equalise) when it is being reloaded
and handled.
VESSEL IN WELL
This LED will be green when the Cooler recognizes that a Vessel has been inserted into the well. The LED will go off
once the Vessel has been removed.
CLOSE DOORS
This LED will be orange if the Vessel is warm, indicating that the doors need to be closed.
VESSEL COOLING
This LED will be orange if the Vessel is cooling. Once the Vessel has reached ambient temperature, the LED will go
off.
The centre column of 4 LED’s indicates the status of the Peltier elements. The elements are referenced as left and
right when the unit is viewed from the front.
POWER
This is a green LED and will be ON continuously as long as mains power is applied to the unit.
IDLE
This is an orange LED and will be ON if the unit has gone into IDLE mode.
AMBIENT FAULT
This is a red LED and will be ON if the ambient sensor is not detected. This occurs if the ambient cable is faulty or not
plugged into both the Cooler and the Calorimeter.
AUXILIARY
This LED has not been assigned to any function.
OPEN DOORS
This will open the doors before the ambient temperature has been reached.
IDLE
This will force the Cooler to go into Idle mode. The idle LED will then be switched ON (green).
WAKE-UP
This will take the Cooler out of idle mode and return it to normal operation.
LED TEST
This will illuminate all the 12 LEDs thus confirming that they are working. The test is only operative while the button
is being held down.
Lever
Nozzle
Lid Holder or
Defiller Cap or
Handling Hook
Holder
Base
A Filling Station Installation Kit is supplied. Please see the CAL2K-3 Filling Station Installation Kit at the back of this
manual for a list of the contents.
The Filling Station is packed in its own box along with the other components and Vessels, which are in their own
plastic bag. Remove the foam, which holds the Filling Station in place. Before proceeding any further, inspect the
Filling Station for any possible damages during transportation. If you find it to be damaged in any way, contact your
Agent immediately. Also, check the packing list and confirm all the contents.
The type of oxygen to be used is normal Industrial Oxygen, used for welding. A purity of 99.5% is suitable. The
oxygen bottle should be firmly secured to a wall or pillar. Using the pressure pipe and connectors supplied, connect
the Filling Station to the oxygen bottle. Slowly increase the pressure and check all connections for any possible leaks.
If a connection is leaking, turn the oxygen off and disassemble the connection to ensure that the ferrule is sealing.
Once the Filling Station is installed and ready to use, place the Vessel on the base and lower the arm, ensuring that
the Filling Station nozzle fits directly and cleanly over the Vessel’s valve. Once the arm is fully down it will latch in this
position and the Vessel will then fill, unattended. When the Vessel reaches the required pressure the arm can be
lifted and the Vessel removed.
There are 2 pressure gauges on the Filling Station. The right hand gauge indicates the bottle or incoming pressure,
and this should always be 3000Kpa. The gauge on the left indicates the Vessel or filling pressure. The rate of the
filling is clearly visible on this gauge. One can fill the Vessel to less than 3000Kpa (never more), however this will only
be applicable when one is analysing samples which are highly combustible (e.g. Wood samples) and need less
oxygen to burn. For samples such as these we recommend filling the Vessel to 1500Kpa.
During normal operation the Filling Station requires very little maintenance. However it is suggested that the ex-
centre and piston be lightly silicone greased (NOT oiled) so as to minimize wear. (See the parts detail further on in
this manual). Also, the O-ring in the nozzle should be lightly smeared with silicon grease daily, to avoid the Vessel
from sticking to the nozzle when filling. Incorporated with the Filling Station are two holders on either side – one can
be used for holding the handling hook and defiler cap, while the other is to hold the Vessel’s lid assembly.
WARNING: NEVER use any oil or oil based lubricant on the Filling Station and Vessel. A light (small)
amount of special silicone grease can be used on the Filling Station Nozzle O-Ring, Lever, Piston and
Ex-Centre. DO NOT use silicone grease on any part of the VESSEL.
ADJUSTMENTS
The Filling Station was designed to be as simple as possible to use by the Operator and to have as few adjustments
as possible. Please refer to the diagrams on the Filling Station parts under the section on “Maintenance” further on
in this Manual. There are only two adjustments which may be required on the Filling Station:
Firstly, the plastic base is adjusted so that the Vessel valve is directly under the Filling Station’s nozzle. This is
adjusted in the Factory and should not require adjustment again. However, if an adjustment is necessary, the
following procedure should be followed:
Secondly, adjustment to the rate of filling the Vessel may be needed. This is adjusted by the Flow Adjustor screw on
the right hand side of the gauge block holder, next to the bottle pressure gauge. (See the parts detail further on in
this Manual). This screw is already adjusted at the dds Factory so that a Vessel will fill up to 3000Kpa in about 20
seconds. Turning the screw inwards (clockwise) will reduce the flow and thus the Vessel will take longer to fill.
Turning the screw outwards (counter clockwise) will increase the flow enabling the Vessel to fill faster. When
turning the screw inwards, do not over tighten, as this will damage the plastic nipple inside.
When turning the screw outwards great care must be taken. The screw must NOT be turned more than 2 turns from
its original position.
WARNING: Over turning can cause the screw to be blown out of the threads by the pressure. This
can result in damage or cause injury to the Operator.
The filling time should be varied between 30 - 60 seconds only. The actual time being chosen should be in
accordance with the operator’s experience and speed.
One more adjustment which could be required is that of the Bottle Pressure. This should always be set to 3000Kpa
to allow the Vessel to fill unattended. If the pressure is set correctly the Vessel will not overfill. Please remember
that with high combustible samples which require less oxygen to burn, it is advisable to fill the Vessel to 1500Kpa.
The absolute maximum pressure to which the incoming pressure can be set is 4000Kpa.
WARNING: Any additional pressure can cause damage to the Filling Station or even injury to the
Operator. If a Vessel is filled to below 3000Kpa, and the sample being analysed does not have a high
combustion, there is a chance you will receive a misfire error as there is not enough oxygen in the
Vessel to burn the sample. However, as mentioned already this may not happen if the sample you
are analysing is highly combustible and needs less oxygen to ignite.
Cap
Lid Assembly
Lid
Centre Electrode
Top O-Ring
Lid O-Ring Bottom O-Ring
Valve Screw
Outside
Electrode
Sleeve
Deflector Plate
VESSEL BACKGROUND
The CAL2K-4 Vessel is smaller than a conventional Vessel, which results in a smaller heat capacity. Special attention
was given to a thermally balanced Vessel design that was achieved with computer aided design (CAD) and computer
simulation of heat transfer characteristics.
The Vessel has an oxygen volume of 0.2 Litre, which allows for a 0.5g sample of Coal with approx. 30MJ/Kg. The
temperature sensors are located cylindrically within the Vessel’s walls at four places and terminate on the bottom of
the Vessel PCB and subsequently onto the contact base rings.
The approx. temperature rise of the CAL2K-4 Vessel after the burning of 0.5g benzoic acid is 9 Degrees Celsius.
Practical tests have shown that up to 0.8g of benzoic acid can be burnt without affecting the accuracy. Oxygen
starvation affects the results with higher charges.
The Vessel must be cooled after a determination. This can be achieved by conventional means such as making use of
a fan or simply leaving it on the table to cool down naturally. To speed up the cooling down process, a CAL2K-2
Solid-State Cooler is recommended, and a necessity should more than 6 determinations be required in one hour. The
Cooler reduces the temperature of the warm Vessel to the starting temperature, which is also the room (or ambient)
temperature. The absolute ambient temperature is not important.
Another design feature is the “firing through the valve” concept, which is of the utmost importance for the thermal
balanced heat conductivity.
MICROPROCESSOR
The Vessel is “smart” with a microprocessor built into its base. The sensors plug directly into the microprocessor
board. All the information pertinent to a Vessel is stored permanently inside the Vessel i.e. Vessel number,
calibration curve, number of firings, date of last reconditioning, etc.
The Vessel PCB is only powered up when it is placed in the Calorimeter or the Cooler. The consequence of the Vessel
memory is that any Vessel can run in any Calorimeter without a new calibration. The Vessel’s memory can only be
accessed from the Calorimeter’s Keyboard or the PC. The electronics and sensors are fully vacuum epoxy
impregnated to prevent physical damage as well as moisture from entering the electronics.
For firing, a length of pure cotton thread (CAL2K-4-FC) is tied to the firing wire with its “tail” touching the sample.
The Firing Cotton must be pure cotton, not any blend with synthetic fibres and must be of a standard length. It is
recommended that only firing cotton supplied by DDS or its Agents should be used.
Only three connections are required: positive, ground and signal. The connections are made via slip rings between
the base of the Vessel and the base connection holders in the CAL2K-1 Calorimeter and the CAL2K-2 Cooler. Always
ensure these slip rings are clean.
A problem, however, occurs in that during the determination period (±10min) some energy may be gained from or
lost to the environment.
In the adiabatic system, the environment is controlled so that no energy is lost or gained. To achieve this state, the
calorimeter’s Vessel (bomb) and bucket are surrounded by a water jacket which is strictly temperature controlled by
a system of circulators, heaters and Coolers, so that it has the same temperature as the inner bucket.
An Isothermal calorimeter measures the effect that the environment has on the bucket before and after the
determination and corrects the result accordingly. This implies that the environment is stable during the
determination. To achieve stability a large body of water surrounds the Vessel and bucket assembly, which is
thermally stable.
DRY METHOD
In the conventional way a Vessel is placed in a water container and the water temperature is measured. Since the
water quantity and container are part of the effective heat capacity, great care must be taken not to change the
capacity. Equally important is that the water acts as a heat sink and a temperature transfer medium to the sensor.
In the dry way, the Vessel, water and container are replaced by a highly temperature conductive aluminium jacket
which is shrunk over the stainless steel body at a very high pressure and forms an integral part of the Vessel. The
temperature sensors are equally spaced around the Vessel body in between the aluminium jacket and the stainless
steel body. This method eliminates all the problems with water and results in very fast temperature equilibrium,
with a fixed heat capacity.
Since the Vessel became that much faster, the environment could affect the measurement 5 times less than with the
conventional use of a water jacket.
Also, a warm Vessel is not placed in cold water to achieve equilibrium. The solid-state CAL2K-2 Cooler reduces the
temperature from warm to ambient, after which the Vessel would be ready for firing once again.
The Vessel design was the result of a computer aided process and extensive computer simulations to predict its
temperature behaviour. The Vessel is tested and certified to international material and test requirements.
From the operator’s point of view, the Vessel is lighter, easier to handle and plated on the exterior, for easy cleaning.
The Vessel’s temperature is measured with 8 sensors and a 25% redundancy (software). The Vessel’s electronics are
vacuum epoxy sealed, and require no adjustment or maintenance.
The Vessel can be operated over a wide temperature range (+10 to +50 degrees C), but it is advised that the Vessel’s
starting temperature is the ambient (room) temperature. The “intelligent-SMART” Vessel brings other
improvements such as: firing counts, identification, history of use and reconditioning data.
CONNECTION
SYSTEM CONFIGURATIONS FOR NETWORKING
The CAL2k Calorimeter full system is ideally suited for single systems and high volume, multiple Calorimeter
networked systems. However, two basic choices must be made regardless of the number of systems in the setup.
Either use the Calorimeter with or without a PC, or make use of a Balance connection
The system configuration follows the “plug-and-play” idea and can be setup by anyone.
The Calorimeter has no printer output and if a hardcopy of the data is required, a PC should be used (at least once a
week) to retrieve and print the results.
a) The MASS is manually entered (typed in) via the Calorimeter’s Keypad.
b) A balance is connected to any CAL2K-1 Calorimeter and the mass and sample identification (SID) is
distributed to all Calorimeters within the Network.
The CAL2k is very versatile in catering for your requirements and expansions. The following maximum system
configuration shows that although it is not practical, it is still possible:
Balance
(Up to 7)
CAL2K-1 CAL2K-2
PC (Max 7)
(Max 7)
(Max 7)
Optional:
Network ……………………..
nodes Up to 255 Vessels CAL2K-4
(Max 7)
With a PC connected, Menu items 2 and 3 can be locked. For details see the section on Menu Access further on in
this Manual. Some parameters require a “once only” setting from the PC.
• A MASS and SID entry is distributed throughout the CAL2k system. That means you can see it on any
Calorimeter, and do a determination on any Calorimeter. The MASS and SID entry can come from a PC or
from a Balance connected to one of the Calorimeters.
• A Balance can be connected to a “CAL2k Docking Station”, which allows entering the MASS, SID, GID into the
bomb Vessel. See the Section: System with Docking Station at the end of this Manual.
WARNING: Just a trickle of water is required for the Cooler. Too much pressure with a full open tap
will cause leakages. The Cooler has been designed for LOW pressure!
NOTE: dds supplies a Balance Cable with a D25 connector. This Balance Cable has been
manufactured for use and compatibility with a Sartorius Balance. However, should you wish to
connect to another brand of Balance all you need to do is ensure that it has the correct connector to
the CAL2K-1 Calorimeter.
GENERAL OPERATION
Calorimeter Lid
Calorimeter Lid
Lid Contact
Well
Calorimeter
Keyboards
Microswitch
Display
TEMPERATURE MEASUREMENT
8 Calibrated sensors are embedded within the Vessel’s wall. These are averaged to determine a single temperature.
The temperature resolution on the display of the Calorimeter is limited (only shows a certain amount of characters),
so on the display it will read as 0,0001Cº. But the actual Temperature resolution of the Calorimeter is 0,000006Cº.
The temperature measuring range is from 0Cº to 65Cº. However, the actual temperature rise of a burned sample
should be in the 4 – 12Cº range, which can be anywhere in the total measuring range of 0 to 65Cº.
VESSEL IDENTIFICATION
Each Vessel has a unique number so that the Calorimeter can identify which Vessel is being used. Vessel
identification can be set by specialised PC software or from the keyboard and will be a number from 1 to 255.
VESSEL CALIBRATION
The method of determining a single Vessel factor, in the conventional sense, is not utilised by the CAL2k. It is
replaced by a "Vessel Curve" determined by many "parameters” to achieve higher accuracy and data security.
Generation and storage of these "Vessel Curves” is automatically performed during calibration runs against standard
CV values (e.g.: Benzoic Acid, Coal Standard, etc.). The CAL2k will not allow access to the calibration parameters, but
using a PC can manage the calibration.
The Vessel can retain 10 curves, made up of one “prime operating” curve and 9 “reserve” curves. The calibration
curves can be managed from a PC.
CV DETERMINATION CYCLE
When a Vessel is inserted into the measuring chamber of the Calorimeter (Well) and the Lid is closed, the following
checks are performed:
Assuming that the above checks are satisfactory, the determination cycle will automatically start and will proceed
through the following four phases:
INITIAL
A temperature stabilisation phase will be carried out. The duration of this phase is dependent on the preset initial
parameters and the stability of the Vessel prior to insertion into the CAL2K-1 Calorimeter.
FIRING
When the preset initial conditions have been met, the Vessel is automatically fired. This means that the preset firing
voltage is applied to the Firing Wire.
FINAL
This is initiated immediately after a successful firing phase. During this phase, a CV figure is calculated every 6
seconds taking into account the calibration curve, CV corrections and sample mass. The duration of this phase is
dependent on the preset final parameters. An unsuccessful firing (i.e. sample not ignited or absent) will be reported
as a “MISFIRE” fault and the determination aborted. Sometimes, a “MISFIRE” can also mean that the Lid Assembly is
at fault.
DONE
On successful completion of the FINAL phase, a final CV result is displayed and stored. The MASS and SAMPLE ID are
deleted from the heap.
WARNING – COOLING: DO NOT IMMERSE THE VESSEL INTO COLD WATER WHEN COOLING. Use the
CAL2K-2 Cooler or allow the Vessel to cool naturally.
CORRECTION FACTORS
Two corrections are possible within the operating procedure of the CAL2K-1 Calorimeter. The CAL2K-1 calculates (in
principle) the following:
Correction 2 (CORR2) is a constant for cotton, wire and nitric acid; Correction 1 (CORR1) is a constant for sulphur, or
the like.
Correction 1 is assumed to be zero during calibration. The corrections can be changed at any time without affecting
the calibration.
NOTE: Correction 2 is independent of the sample mass. Correction 1 is dependant on the sample
mass.
The access level can be changed by a keyboard operation and by a PC entry. A change or setting made using the PC
entry (setting) dominates i.e. it locks. That is to say if Menu Access 2 and 3 are enabled by the PC, the key access can
be set from the keyboard to 1, 1 and 2 or 1, 2 and 3. A PC = 1 only access, does not allow any change from the
keyboard.
MENU ACCESS
The Equals Sign key pressed repeatedly, scrolls through the available Menu Options.
The Square key will exit from the Menu Option and clear the screen.
The Menu is always displayed on line 4 of the Calorimeter’s LCD Display, while value entries are made in the Key field
of line 3.
Press to view the present value. The first Menu item will be displayed.
Press each time in order to view the next Menu item, description and value.
To change a value:
Press or until the required Menu Option and value are displayed. Type in the complete value,
followed by (ENTER) observe that the new value is displayed. It is then automatically stored.
The new value can be entered in the Keyboard entry field, then press . The new value is now displayed in the
original position and stored. The changed value is recorded in the “result memory” for further reference. Some
values are entered with the “double-confirm” feature.
, ,
To lift access restrictions one level up, provided the level is “enabled” by a PC operation, press the following:
, ,
SID and MASS entries must be done one after another as they form a single record in the HEAP. Entries can be made
at any time, even while a determination is in progress.
SID ENTRY
SID is up to 8 characters – 4 alpha followed by 4 numeric. Last 4 characters must be numeric to allow for auto
incrimination of the SID. Alpha characters can only be entered via a PC.
To change this number: Using the Keyboard, enter an 8 digit number. This will be displayed on line 3, next to SID #
→.
MASS ENTRY
KEYBOARD ENTRY
Enter the Mass via the Keyboard, this entry will be displayed next to MASS: on line 3. To accept this entry press
, and the screen will be cleared. Mass & SID are now added to HEAP and available for use.
BALANCE ENTRY
If a balance is connected and set up correctly, any stable mass will be displayed on line 4. The mass is checked
against preset limits and if it is outside of these limits, the mass is displayed with a “?” at the end.
If the mass is correct, press , and the screen will clear. MASS & SID are now added to the HEAP and available
for use.
NOTE: A Keyboard entry takes precedence over a balance entry. That is, if a balance entry is
displayed on line 4 and Keyboard entries are entered on line 3 and “enter” is pressed on the
Keyboard, then the Keyboard entry will be saved.
SYSTEM PARAMETERS
The CAL2K Calorimeter system can be setup from the Keyboard or from a PC. The PC allows editing, saving and
printing of the parameters.
1. All equipment is switched ON. Warm-up time for the Cooler is approx. 5 minutes. Oxygen pressure checked
and regulator adjusted if necessary. Cooler water flow checked and adjusted if necessary.
2. System Tests carried out.
3. Configuration parameters entered and/or checked.
4. All Vessels cleaned and O-rings checked for any damage, if damaged please change the o-rings.
5. All Vessels calibrated.
6. All Vessels checked against known CV standards and re-calibrated if necessary.
7. All Vessels checked for accurate Vessel correction factors.
8. Determine new correction factors if necessary.
Verification of the above checklist before starting a new batch of samples or after prolonged non-usage of the
Calorimeter will ensure trouble-free operation with minimum downtime.
PREPARING VESSELS
NOTE: This section MUST be read as it provides valuable information for achieving accurate results.
The art of producing highly reproducible results revolves around establishing a constant work cycle with the
minimum of interruptions. Adherence to the following Vessel preparation sequence will ensure that unexpected
breaks in routine operation will be kept to the absolute minimum.
• Depressurise the Vessel if it has just been fired using the Defiller Cap (CAL2K-4-DC).
• Place Vessel in the Cooler if it has just been fired.
• Remove Vessel from the Cooler when the Cooler doors open. (If Vessel has been standing for a while, check
that it is at ambient temperature by placing it in the Cooler.
• Open the Vessel, clean the inside of the chamber using paper towel, and ensure no fibres are left inside
the chamber. The Vessel should always be cleaned after every determination.
• Remove and clean the Crucible (CAL2K-4-CB) with a Wire Brush (CAL2K-4-WB). Old or damaged crucibles
should be discarded as they can cause damage to the Vessel during firing.
• Clean the Vessel and Vessel Cap threads with a Wire Brush.
• Remove any old Firing Cotton (CAL2K-4-FC) from the firing wire (if the Vessel was not fired recently). If the
Vessel has been fired the cotton would have burnt away with the sample so there should be no firing cotton
left on the firing wire.
• Inspect the Firing Wire (CAL2K-4-FW) and replace if necessary. Only use the dds supplied pre-cut Firing Wire.
• Insert the pre-cut length of Firing Cotton (CAL2K-4-FC) by looping it over the firing wire and then twisting the
ends together.
• Weigh the sample using a balance. Make sure you place the empty crucible on the balance weigh plate first,
then press “Tare”. Once this has been done then you may place the sample inside the crucible and weigh the
sample. By following this procedure you will cancel out the weight of the crucible and this will give you an
accurate sample mass.
• Insert weighed crucible and sample into the outside electrode’s crucible holder, ensuring that the firing
cotton touches the sample.
• Be careful as not to “flick” any sample out of the crucible with the cotton. Experience and technique practice
helps.
• Insert the electrode assembly (Lid Assembly) into the Vessel body.
• Screw the cap down until it touches the top of the lid. Tighten with quarter to half a turn. Do not over
tighten, as it will be difficult to open later. Also make sure the cap does not screw all the way down.
• Place the Vessel under the Filling Station, keeping it upright. Fill it with 3000KPA oxygen. The right hand
gauge should read 3000KPA.
• Remove from the Filling Station with the Handling Hook (CAL2K-4-HH) and let the Vessel stabilize for approx.
1 minute before inserting it into the Calorimeter.
CALIBRATION OF VESSELS
Each Vessel is calibrated before delivery and the calibration is stored in C0 and C1. C0 is the “working” calibration
curve, and C1 is one of nine additional curves available for storage.
Should it become necessary to perform a calibration, then follow the steps below:
1. Weigh a tablet of Benzoic Acid and enter the mass into the Calorimeter
2. Prepare a Vessel as per the procedure above (and place it in the Calorimeter’s Well).
3. Do not close the Calorimeter’s lid.
4. Confirm (if this is the first ever calibration) the following parameters, this can be done very conveniently from a
PC, but here the Menu Options that are used:
Calibration : ON 1
Spiking : OFF 0
Time : Check
Date : Check
6. Enter MASS.
8. Close the Calorimeter’s lid. Observe that the CAL2k goes through Initial, Fire, Final and Done stages (5 minutes
in total).
9. If you open the lid, then the calibration is saved C0 (the working curve!).
During a complete determination, each Vessel has to go through 4 distinct cycles as shown in the following
sequence. Note that the WAIT cycle does not require any work:
The above cycle sequence must be adhered to for best results. Total throughput time is improved by the use of more
Vessels. The following describes the various operational cycles in detail.
PREPARE
Prepare a Vessel as in the section Preparing Vessels.
WAIT (STABILIZE)
During this time (0.5 to 1.0 minute), the Vessel can equalize outside the CAL2K-1. If placed directly into the CAL2K-1
and the lid is closed, an erroneous firing could take place with a slightly high result. (A side effect of pressurizing is to
raise the internal Vessel temperature).
SAMPLE
1. Open the Calorimeter’s lid (if not open already).
2. Insert a prepared Vessel using the Handling Hook. It is preferable not to insert the Vessel with your hand as
you may affect the temperature of the Vessel.
3. Press and scroll through the HEAP records until the required record, i.e. MASS & SID, is located. Press
until required Mass and SID are displayed.
4. Press ENTER and the selected record will be transferred to line 1 of the display, only if the Vessel is in the
well.
5. If the MASS & SID have not been entered, then do so now.
6. If the HEAP is empty, then enter the MASS & SID now.
7. Close the Calorimeter’s lid.
8. If a fault occurs now or at any stage during the determination then refer to the section on Troubleshooting
for full details. The pilot light will flash until the lid is opened.
9. If no fault is detected then the INITIAL status will be displayed and the pilot light will be ON.
10. Drift & time will be displayed during this period depending on the initial parameters of the Calorimeter.
11. Once the initial period criteria have been met then the Vessel will be fired.
12. The FIRE status will be briefly displayed (6 seconds).
13. Immediately after firing the FINAL status will be displayed.
14. Drift or time will be displayed during this period depending on the final parameters of the Calorimeter.
15. The result will also be displayed as it develops during the final period.
16. Once the final period criteria have been met then the determination will end.
17. The DONE status will be displayed and the pilot light will flash until the lid is opened.
NOTE: If the pilot light is flashing then the Calorimeter needs attention.
1. The result that is displayed is the final result with -> inserted before the result.
2. Open the lid and the pilot light will go OFF.
3. Remove the Vessel.
4. The information contained in line 1 will be transferred to the result memory and stored.
5. Line 1 will be cleared ready for the next determination.
NOTE: The sample record, i.e. MASS and SID, is removed from the HEAP.
COOLING
• De-fill the Vessel using the Defiller Cap
• Place the Vessel in the Cooler
WARNING: DO NOT COOL VESSEL IN COLD WATER. USE THE CAL2K-2 COOLER UNIT TO COOL THE
VESSEL.
Repeat the cycle sequence above for all samples in batch using the next available Vessel.
Please note the MASS and SID will be blank until the Vessel is inserted. Once inserted you will see the following:
Temperature of Vessel
CLOSE LID
If no errors are detected the following will be displayed. The indicator lamp will go ON.
INITIAL
The initial drift is the rate in degrees C at which the Vessel temp. is drifting up or down. The timer will not start until
the drift conditions have been met.
“D” indicates the initial drift is outside limits.
“T” indicates that the timer has started.
The timer will then run for the preset initial time as long as the drift is within the preset limits. If the drift goes out of
these limits, then the timer will reset.
FIRING
Once the initial conditions have been met then the Vessel will fire.
FINAL
After firing the final phase will commence.
The timer will run for the preset final time. The temperature rise and result will be displayed dynamically.
DONE
At the end of the preset final time “DONE” will be displayed. The indicator lamp will start flashing.
OPEN LID
The lid of the Calorimeter can now be opened. The Vessel can also be removed and the next determination started.
The fiddle factor is multiplied with the calibration to affect the result. Normal entry is 1.0000. If calibration is low or
high, then the fiddle factor can be used to adjust the result.
This Vessel deviation factor can only be set by a PC. It is set to 1.0000 during the calibration.
• Balance offset.
• Moisture offset.
• Calorimeter offset (could result from a poor installation).
• Sample preparation offset.
With offset, we don’t mean a mathematical offset but rather a “constant difference”.
The deviation factor can be adjusted while the CAL2k is in “DONE” mode, and the effect of the adjustment is visible.
Otherwise the deviation can be adjusted whenever it is suitable. Normal entry is 1.0000.
OPERATING CYCLES
As explained in the previous section, a complete CV determination goes through four distinct cycles:
• Preparation
• Wait
• Sample
• Cool
The CAL2k system has been designed to operate with multiple Vessels with each Vessel in one of the above cycles
for maximum throughput. The following timing examples show the effect that the number of Vessels in the system
has on throughput:
NOTE: The Calorimeter is only 60% occupied and the Cooler 40%.
This method is somewhat difficult due to the different times, but the CAL2K-1 is almost 100% utilized.
QUICK GUIDE
This section is intended as a quick reference guide to the Operating Instructions and Menu Options:
NORMAL DETERMINATION
CALIBRATION
NOTE: Calibration will only stay ON for one sample so after a calibration it is not necessary to turn
calibration OFF.
To enter a new “User ID” – enter new “User ID” then press enter e.g.: 123.123 . The new “User ID” will now
be displayed.
E.g.: 123.123
1 is = ON
0 is = OFF
NOTE: This function only stays ON for one determination and then reverts to OFF.
Press
Active bomb
calibration
1 displays the data for calibration curve 1. (and continue this way from 1 to 9 to view all calibration curves
and their details).
Vessel No.
Above is an example and is showing the data for curve 0.
NOTE: The 3rd reconditioning of the Vessel will overwrite the first reconditioning and so on.
Customer Name
SPIKE VALUE
This is the known calorific value of the substance to be used for spiking, usually benzoic acid of approx. 26.454MJ/Kg.
On some occasions, the use of a Gelatine Capsule (CAL2K-4-GC) or Crucible Cover Disc (CAL2K-FLDS) needs to be
used with a solid sample or a volatile liquid sample respectively. When using these items, you will first need to
determine the energy value of the item in question. You will need to use Benzoic Acid as the substance for spiking,
as the Gelatine Capsule of Cover Disc becomes the “sample”. Once you have determined this value, you will then
have the “Spike Value” for your determination.
SPIKE MASS
This is the mass of the substance to be used for spiking. The procedure to follow, is to place the crucible on the
balance and press TARE. Then add the substance to be used for spiking to the crucible. This Mass value is the “Spike
Mass” and must be entered manually into the Calorimeter. Then add the sample. This mass is the spike item’s mass
plus the sample’s mass and must be entered in as the Mass. This can be read directly from the balance if a balance is
connected.
SPIKING ON/OFF
1 Spiking is ON
0 Spiking is OFF
NOTE: Unlike some of the other features, Spiking will stay ON until it is turned OFF.
Enter a new time in the format HHMM and then press . The new time will be displayed.
DATE IN DDMMYY
This is the same as time but displays the date in DDMMYY format.
CLEAR HEAP
HEAP is the term given for the combination of MASS and SID. To clear these entries, select the relevant Menu Option
To change the value, select the relevant Menu Option. Enter the new value, then press . The new value will
now be displayed.
CALIBRATION DEVIATION
This is the Calorimeter factor and is usually set at a factor of 1,0000. All results are multiplied by this factor. It allows
an entire Calorimeter to be adjusted up or down. To calculate a new factor:
For example, enter 1.1 to save in C1. The new calibration curve will now be saved.
RECALL CALIBRATION
This will show which calibration curve is being used.
Vessel No.
NOTE: If “AV” appears in the curve number place and “?” in time or date, then there is no date for
that particular curve number.
Menu Option. Enter new value e.g.: 0.0030, then press . The new value will now be displayed.
To change this time, select this Menu Option and then enter a new value e.g. 1.5. Now press , and the new
value will be displayed.
this value, select this Menu Option. Enter a new value e.g. 1.0, then press . The new value will now be
displayed.
CORRECTION #1 (SULPHUR)
This is the correction for sulphur (mass related). To change the value, select this Menu option. Enter the new value,
CORRECTION #2 (COTTON)
This is the correction for cotton and firing wire (not mass related). Change the value the same way as for Correction
# 1.
ID 2 enter 2.2. Then press , and the new number is now displayed.
recommended value). Now press . The new value will now be displayed.
1 is ON
0 is OFF
This feature is not operational, however the Menu option has been retained. This Menu option can be ignored.
option. The existing value will be displayed. Enter a new value, then press . The new value will now be
displayed.
0 is Off
1 is ON
Setting this Menu Option to “OFF” allows for Tray ID entries. This option should normally be left “ON”.
1 = BTU/lb
2 = CAL/g
3 = MJ/Kg
To change the unit of Measurement setting, select this Menu Option. The existing units will be displayed. Enter the
new number e.g.: 3, then press . The new unit of measure of the display will now be reflected.
0 is OFF
1 is ON
1 is ON
0 is OFF
This function is used when the temperature rise of the sample is less than 4 degrees C. When the temp. rise is low
then calibration curve C1 is used instead of C0 and the error “Misfire” is ignored.
0 is OFF
1 is ON.
SPIKE MASS
This is the mass of the substance to be used for spiking. The procedure to follow, is to place the crucible on the
balance and press TARE. Then add the substance to be used for spiking to the crucible. This Mass value is the “Spike
Mass” and must be entered manually into the Calorimeter. Then add the sample. This mass is the spike item’s mass
plus the sample’s mass and must be entered in as the Mass. This can be read directly from the Balance if a Balance is
connected.
Once the determination is complete, the result will display the calculated calorific value of the sample. The
calorimeter will automatically take the end result, minus the spike energy and present your final result of your
sample.
The minimum system requirements for the CAL2k software are as follows:
• 100Mz Processor
• 128MB RAM
• Microsoft® Windows® 98/2000/XP/NT4.0 ENGLISH VERSION ONLY
• 100MB Hard disk space
NOTE: Before you begin please make sure your screen layout settings on the PC are set correctly.
The DPI setting must be set to 96dpi and not 120dpi.
NOTE: If you are using a laptop which has this software loaded, please make sure you have the
correct USB adaptor which allows you to connect to an RS232 port. Not all USB adaptors/converters
work the same way.
The Microsoft. NET Framework package will need to be installed. Select “Yes”.
The Microsoft. NET Framework license agreement screen will appear, select “I Agree” and click on “ Install”. The
package will begin to install.
Once the package is finished installing the following screen will appear:
Click on “OK”
The CAL2k Management Tool Setup Wizard will begin immediately afterwards. Click on “Next”:
You can select whether you are loading the software for yourself or everyone who is using the computer by selecting
the appropriate radio button, shown below. You can also change the folder where the software will be saved. It is
recommended that you keep to the default settings. Always save software programs under “Program Files” when
using Microsoft Windows.
Click on “Next” once you have made your selection/changes (It is recommended to leave these options on their
Default choices):
The Installer will request that you confirm the installation, click “Next” to continue:
Once the CAL2k software has been completely installed, you will see the following screen and you can now click on
“Close”.
The CAL2k software has been successfully installed. You can double click on the icon to run the software. Before you
run the software make sure your display settings on your PC are set to Windows Standard. To change the settings go
to Windows “Control Panel”, click on “Display”. This will bring up your Display properties. Click on the Appearance
Tab, under “Schemes” select Windows Standard, then click Apply.
The login screen will now appear. Click OK to access the software. IT IS NOT NECESSARY TO ENTER A USERNAME
AND PASSWORD. THIS OPTION IS NOT ACTIVATED, CLICK ON OK TO GO TO NEXT SCREEN. NO USERNAME AND
PASSWORD IS REQUIRED.
Once you have accessed the software you will see the following status screen:
In order to setup your security feature you will need to access the User Security Manager. Click on .
The following screen will appear:
Username: LabMan3
Password: cal2kAdminUser
You will now return to the Main Screen however you will now have access to the User Security Manager by clicking
on the button.
After clicking on the Admin button you will see the following screen:
ADMINISTRATE USERS
There are four (4) options available. The Lab Manager or Agent will need to select the one which is most suitable:
• None – this simply means the software is not locked or secured and anyone can use the software
• Edit and Existing User – if the Lab Manager or Agent has already set up a user this can be edited
• Create a New User – the Lab Manager or Agent can create a new user
• Delete a User – the Lab Manager or Agent can delete an existing user
You will note that for creating a new user, there is a block called “User Info”. This is where details for the new user
must be entered.
After each selection, you must select “Saves User Changes” to activate the changes made.
Remember once changes have been made, click on “Save Changes” to effect those changes.
FILE MANAGEMENT
Here you can select your operating director and file name. Please note that the file will be saved with a CSV
extension. You also have the option of formatting the CSV file which will affect the data sequence and contents.
Select “Format file contents”.
Once you have selected the contents and sequence of the data you want, select “OK”.
Remember before closing to save any changes that have been made to the Security Manager, once you select
“close” you will return to the main status screen:
A destination number must be displayed, i.e. a number between 1 and 7, as there can be only 7 systems networked
together. If the destination number is 0 then there is a problem (your Calorimeter is not being picked up) and you
must check the connection between the PC and Calorimeter.
Click on the “Status” button to acquire the latest data from the network. While the PC loads the connected
Calorimeter, the following dialog box will appear:
All Menu Items, Displayed Information and Buttons will now be described.
MENU ITEMS
The Menu Items can now be located under the main screen under “Tools”:
DECIMAL SEPARATOR
Please note the Decimal separator must be set prior to printing or downloading results. The decimal separator
applies to the entire setup of the Calorimeter, as well as the results. In Europe they use the comma to separate the
Decimal, in South Africa we use the decimal point (period), so therefore please make sure you set the decimal
separator according to your requirements.
TOOLS
ITEM DESCRIPTION SOFTWARE IMAGE
Set Time Click on “Set Time” if you want the
time of the Calorimeter to be the
same as that on your PC.
Display Data in You can select the unit of
measurement that you would like
your results or parameters to be
displayed in, by selecting the
relevant unit of measurement under
“Display Data in”. You have the
option of selecting: BTU/MJ/CAL.
Clear Memory Click on “Clear Memory” to clear the
result memory of the CAL2k.
Reset Calorimeter Click on “Reset Calorimeter” to reset
(clear) the station you have selected.
This destroys all HEAP information.
This function is helpful if a “fresh
starting point” is required.
The following screen will appear after selecting to Reset the Calorimeter. Select “Yes”, if you are completely certain
you are happy to lose all data in memory.
STATUS
SETUP CALORIMETER
When you initially select this button, four options will be available: ”Upload from file”, “Upload from CAL2k”,
“Download to CAL2k” and “Download to Default”. In order to have all the items available, you will need to click on
“Upload from CAL2k”. Please read the details in the section “Setting up a Calorimeter” before clicking on this option.
HELP
BUTTON ITEMS
There are Buttons on the Main Screen, which are described as follows:
To set up the Calorimeter, click on the button. The following screen will appear:
The parameters for the destination Calorimeter are immediately displayed. Any of the parameters in the boxes can
now be changed. Once changes have been made, you can save the new parameters. To save a set of parameters
onto a file, click the button and select another folder on your C Drive or Network Drive or create a new
folder. Re-name your file and then click on “Save”.
Change folder
or directory
Change
filename
LOADING A FILE
To load a file, click the button, then select . All previously saved set up
files will be displayed, as indicated in the screen print below:
Select the required file by clicking inside the check box under “File Name” so that a tick mark appears, as shown
above.
Once you have selected a file, click on the button. The loaded file will now be displayed on the screen.
To download a parameter file to the Calorimeter, ensure that the required file is displayed on the screen. Then click
on “Download to CAL2k”. The file will now be downloaded onto the Calorimeter. The displayed file can also be
downloaded to the default values in the Calorimeter in a similar way by clicking on “Download to Default”.
Download to
CAL2k
Download to
Default
To delete a saved file from the list of saved setup files, select the file by ticking the box next to the file name. Then
click on the “Delete” button. A window will appear which will read “Are you sure you want to delete”. If you want to
delete click on “Yes”. That file will now be deleted. Only one file can be deleted at a time.
Delete button
To view the uploaded results click on the button. The following dialog box will be displayed:
Click the “Start Upload” button to upload the data. The records will now be sorted into new “duplicates” as well as
results, parameter changes and errors (as above). “Duplicates” in this case are records that have been previously
uploaded.
Click on the button. The result history database will now be displayed:
Get the data by selecting the relevant date and then click on the button. This will customise your view
and will display the five columns as indicated below:
The “Indicators Name” is a fixed column and cannot by changed. It indicates the parameters that are stored in a
result.
Under the column called “Header”, the indicator’s name can be changed.
In the column called “Screen Display”, this is the sequence in which the parameters will be displayed on the screen
and can be changed. “POSI” indicates in which column the parameter will appear. For example,
0 = will not be displayed at all
1 = will appear in column one, etc.
Clicking on the “POSI” drop down arrow, will indicate which columns can still be used (i.e. are still available). The
“Field Size” indicates the width of the column.
The “Print Position” and “Export Format” columns set the format for printing and exporting data respectively.
Once the columns have been set up, click then click on to exit the “Format View”
screen. Then click on the “Result Display” screen and click on . The
results will now be displayed in the new format. While in the Result History screen you can also Print Data and
Export Data.
To print data click the button and then follow the prompts in your print dialog screen.
To export data click the button. Select where the data must be exported to and the file name, then
click “Save”. The exported data will be in Microsoft Excel format and can then be changed, plotted or manipulated.
VIEW VESSEL
Click on the button, and a screen with general/default data will be displayed. Ensure that the Vessel is
inserted into the Calorimeter. To load the data click on the button. The actual data from the
Vessel will now be displayed against a grey background, indicating that the data can only be viewed and not
changed.
TEMPERATURE GRAPH
Click on the button, to display the temperature curves during a determination. This is opened as
a separate screen.
Temperature curve is the default screen. There are two options: a) Show all 8 Sensors or b) Show the average temp.
Ticking the box as shown in the diagram above can activate both or either of these options.
GRAPH EXPLANATION
The temperature scale is auto ranging and the firing point is fixed. Only the last two minutes of the initial period are
shown. The graph is refreshed automatically every 6 seconds.
At the end of a determination a window will appear on the screen indicated as “Temperature Curve”, and it will
need a description. Enter a description for this determination e.g.: sample ID number and press enter. The data is
now stored and can be recalled later for comparison purposes. The graph stays on the screen until the next
determination is started. Clicking on the “Refresh” button will clear the screen. You are able to recall the saved
curves by selecting the button. The following screen will then appear:
Select the curve you wish to load and click on the “Load >>” button.
DRIFT CURVE
To show the Drift Curve click on the button. This curve shows the difference between two
consecutive average temperature readings. I.e. how the average temperature of the Vessel is drifting.
CALORIFIC CURVE
To show the calorific value curve click on the button. This curve shows the calorific value of the
sample after firing. Before firing the value is zero.
LOAD CURVES
This same procedure applies to “Temperature Curve”, “Drift Curve” and “Calorific Curve”.
To load a saved curve click on the button. A list of saved temperature curves will then be
displayed. Tick the box next to the file you wish to select; you can load up to 4 curves at one time. Once all the
curves have been selected click on “Load>>”.
All loaded curves are displayed in pink to highlight a curve. Click on the relevant curve from the list displayed on the
left side of the screen.
List on left
hand side
A real time determination can be displayed at the same time as a loaded curve. This allows for comparisons between
determinations and also for comparisons between different Vessels.
To exit the “Temperature Curves” click on the exit button on the Windows bar.
HEAP MANAGEMENT
To view the HEAP records click on . The HEAP consists of a mass attached to a sample ID (SID) that has
been entered into the Calorimeter but has not yet been analysed. Click on to upload the contents
of the HEAP. The contents are now displayed on the screen.
To delete records, select the record by ticking the box next to the HEAP in the Status column. Multiple records can
be selected. Click on “Delete Items from Heap” a window will appear “Are you sure you want to delete”. Click “Yes”
to continue or “No” to abort.
ADVANCED CALIBRATION
To enter this option, click on the button. A screen without any data will be displayed.
To load the calibration curves from a Vessel, insert the Vessel into the Calorimeter and click on
. The curves are then uploaded and displayed on the screen. The curves can now be
manipulated, copied and saved.
CURVES
The value stored in the calibration curve can be displayed at anytime by clicking on the pointer next to the “Final
time” text and holding the mouse button down and then dragging the pointer to the left or right as desired. The
value at a specific time is now displayed in the column.
Drag Pointer
The Deviation, Average, Standard Deviation and Mean of any selected curve are displayed for the selected time, at
the bottom right of the screen.
SAVING OPTIONS
Average Takes the average of the selected curves (more than one curve must be selected).
Mean Takes the mean of the selected curves (more than one curve must be selected).
Copy Allows the selected curve to be copied to another destination (curve position) (only one curve
can be selected).
Change factor Allows the entire curve to multiply by a factor (only one curve can be selected).
Save to File Allows a curve to be saved as a file, which can be recalled later (only one curve can be selected).
NOTE: The saved curve will not be displayed until “Load from Vessel” is selected. Once “Load from
Vessel” has been selected you will see the saved curve displayed.
• Click on the button. A list of saved calibration curves will now be displayed.
• Select the file to be loaded (only one), by ticking the box next to the file name.
• Select the destination curve (only one) (far right hand column C0-C9).
• Click on the “Load>>” button.
• The loaded curve will not be displayed until “Load from Vessel” has been selected.
STATUS
Whenever a calibration curve has been manipulated then the status is changed.
The symbols in brackets are the codes displayed on the screen of the Calorimeter when the “Vessel Data” is
displayed.
NETWORK OPERATIONS
The PC software supports CAL2k Network Operations. The only difference is that when the status is acquired then
multiple units are displayed on the screen.
NOTE: Each unit connected to the networked system must have a different Calorimeter number
from 1 to 7, as only a maximum of 7 systems can be networked.
The units that have not been integrated will have a “talk to me” button. To change the Calorimeter that is being
integrated press “STATUS” and then “Talk to me” of the required unit. The procedure is now the same as for a single
unit. This is only applicable if 1 or more systems are connected (networked).
OPERATION
Operation is designed so that the Calorimeter can still be operated via the PC even if a display or Keyboard fault
occurs on the Calorimeter unit itself.
NOTE: The “Operation” feature will only work on the host Calorimeter. That means the PC must be
connected directly to the CAL2k Calorimeter, which is to be used via the Operation Software.
1. where the CAL2k is still operational and the PC screen displays the status of the Calorimeter.
2. where the Calorimeter is controlled from the PC screen.
In order to switch between the two methods of operation, simply click on either “User Controlled” or “PC
Controlled” button once.
NOTE: Once in PC Control the Calorimeter is LOCKED OUT and can only be returned to User Control
by clicking on PC Control – escaping out of the screen or closing the program or switching off the PC
will leave the Calorimeter in PC Control. EXPLANATION OF SCREEN
SETUP
A C
B D
F
E
A These five fields on the left indicate the status of the Calorimeter.
In the above Setup screen you need to enter the information in the area indicated by B.
B This section displays the Mass and SID setup for the Calorimeter.
B Mass: Displays the mass transmitted from the balance (if a balance is connected to the Calorimeter). To
accept this mass click on Once the balance Mass is accepted, the Balance
Mass is transferred to the Mass field. The accepted mass is already transferred to the CAL2k.
Mass: Allows for manual mass entry. Enter the mass and then press “enter”. Mass block will turn red if the
mass is outside of the preset limits.
SID: Sample ID. First 4 characters are alpha numeric, last 4 are numeric only. This automatically
increments in PC controlled mode.
GID: Group ID. Can be alpha numeric. This is not a required field
C This section displays the calibration information presently used by the Vessel.
Run a Calibration Click this box to perform a calibration. A Check mark (√) will appear in the box (this is
automatically reset once the calibration is complete i.e. only stays on for one
determination).
Calibration #: Displays the present calibration curve being used. It will always be curve “0”.
Cali Details: Displays the manipulated status of the calibration curve in position “0”.
Date: Displays the date and time of when the calibration curve “0” was
done.
D This section displays the Temp, Drift and Time of the determination. The only two fields with numbers in at
the Setup stage are Temp and Drift Limit.
Temp: Continuously displays the temperature of the Vessel when it is in the Calorimeter’s Well.
Drift Limit: This is the drift limit during the initial phase, which is preset via the setup menu.
Below is the list of messages which could appear in the message box:
The above messages will be appended to one another should there be more than one fault. The message display will
show the state of the CAL2k, regardless in which Operational mode the screen is being used.
INITIAL
In the “User Controlled” mode, this field automatically changes to “Lid Closed” when you close the lid of the
Calorimeter.
In “PC Controlled” mode, “Lid Open” needs to be clicked once to change it to “Lid Closed”. The physical lid of the
Calorimeter also needs to be closed for the Initial phase to start.
Once in the Initial phase, the numbers in Temp, Drift and Initial Time start to change.
Drift Displays the actual temperature drift of the Vessel during the Initial phase. The Drift needs to be
lower than the Drift Limit for a certain time before the Vessel can be fired.
Initial Time This displays the time of the initial phase. This time continuously increments until firing when the
counter stops and the total initial time is displayed. The Initial Time is displayed in 6 second
intervals e.g. 1.5 = 1 minute 30 seconds.
FIRE
This mode cannot be changed. The Fire mode is automated and will sometimes not even be seen by the operator of
the CAL2k.
The Calorimeter then fires the Vessel. The screen above appears only for a short moment. The “Temp Fire” now
reflects the temperature at which the Vessel has been fired. .
At the Fire phase, the sample mass and the SID are used and removed from the HEAP. Also, the “PC Controlled/User
Controlled” button is disabled so that the determination can complete its course. Should a misfire occur, the button
will be enabled again.
MAIN
Once in the Main phase, the numbers in Temp Rise, Temp, Drift and Final Time change.
Temp Rise: Displays the temperature rise of the Vessel from the firing during the final phase (no temperature
deployed during calibration).
Final Time: Displays the time taken for the final CV value to be allocated. The Final Time can be changed in the
Setup window. The Final Time is displayed in 6 second intervals. E.g. 3.1 is 3 minutes and 6 seconds.
G Amount now starts reflecting in the CV field. The value in the CV field is a pre calculated value based on the
present temperature rise in the calibration curve.
DETERMINATION DONE
Once the “Final Time” has been completed, the screen moves to the “Determination Done” phase. The screen now
changes to the final “Determination Done” screen, as indicated above.
The CV button now turns to green and the result is reflected in the units of measurement as selected.
The determination of this sample is now fully complete. The lid can now be opened.
In the “User Controlled” mode, the field automatically changes to , when the lid of the
Calorimeter is opened. Once the lid is opened, the Done phase is complete and the screen will indicate Setup phase;
the beginning of the next determination.
In the “PC Controlled” mode, the physical lid of the Calorimeter needs to be opened and in the software select
to open the Lid on the Done screen. will now reflect and the screen now changes back
to Setup and you can commence with your next determination.
MAINTENANCE
CALORIMETER
The Calorimeter needs very little maintenance. The Calorimeter should never be opened, as there are no serviceable
parts inside.
• Ensure that the Vessel Well is clean – blow out any dirt with compressed air if necessary.
• Ensure that both connections to the Vessel (one in the lid and one in the base) are clean and that they do
not stick down when depressed.
• If the Vessel Well or Lid Polystyrene is damaged, call a service technician or your local Agent to replace them.
• If the Keyboard or the display fails, call a service technician or your local Agent.
• Always ensure that the Door Knob of the Lid latches correctly, as this incorporates the lid microswitch and is
also a safety device to prevent the Lid from lifting in case of a Vessel failure.
COOLER
WEEKLY MAINTENANCE
• Clean Vessel base to ensure that the Vessel sits neatly and central and that the contacts meet successfully
with the base of the Vessel and its contact rings.
• Ensure the base contact operates freely.
• The contacts are spring loaded and when pressed down and released they should return to their original
position.
FILLING STATION
Arm
Knob
Holder
Ex Centre
Shaft
Piston O-ring
Piston
Spring
Nipple O-Ring
Nozzle O-ring
Knurled Nut
O-RING REPLACEMENT
It is strongly suggested the following checks be made every 3 months or sooner depending on the number of firings
you perform per day, as well as the type of sample you are analyzing (for the Vessel). A sample which ignites easily
(highly combustible) will cause the Vessel o-rings to perish a lot faster than a substance which is less combustible.
• Verify the oxygen flow rate and re-adjust the Flow Adjustor if necessary. The rate of flow should be adjusted
to fill a Vessel in approx.45 seconds. Replace the O-ring if necessary.
WARNING: DO NOT over tighten the Flow Adjustor – it should be tightened by hand and as soon as
any resistance is felt stop tightening!
WARNING: Please DO NOT apply any OIL in any form to any o-rings on the Vessel. You may apply a
light film of silicon grease on the nozzle o-ring of the Filling Station ONLY, however it is advised not
to apply grease to any other o-rings.
Before an O-ring is replaced, turn the oxygen supply OFF at the bottle and release the pressure in the pipes by filling
a Vessel until both gauges on the Filling Station read zero.
NOZZLE
The O-ring in the Nozzle, which seals onto the Vessel’s lid valve, is replaced by unscrewing the cover (knurled nut)at
the end of the Nozzle. (A pair of round jaw pliers may be required to grip the nut, but generally it should be hand
tight and can be opened by hand). Once the knurled nut has been removed the o-ring can be replaced. Lubricate the
new o-ring with a very SMALL amount of silicon grease before use. The knurled nut can now be replaced onto the
nozzle.
PISTON
There is an O-ring between the Nozzle and the Piston. To replace this O-ring the two pressure pipe connections to
the Nozzle must be removed FIRST. The Nozzle can now be unscrewed from the Piston. To stop the Piston from
turning when the Nozzle is unscrewed, we suggest that the arm be put down in the latched position. The O-ring can
now be changed. The O-ring on the Piston is the same as the Nozzle O-ring. Before re-assembly, ensure that the
nipple inside the Nozzle is in place. Screw the Nozzle back onto the Piston and then re-attach the two pressure pipe
connections.
FLOW ADJUSTOR
To replace the O-ring on the screw Flow Adjustor, unscrew the adjustor completely and remove it. The O-ring must
now be cut off the Adjustor and a new one put on. The Adjustor can now be screwed back in completely using your
hand to tighten.
WARNING: DO NOT over tighten as this can damage the plastic seal (Nipple).
Now un-screw the Adjustor about 1/4 to 1/2 a turn outwards. The filling flow must now be adjusted by trial error as
explained in the section about Adjustments for the Filling Station above.
VESSEL
RECONDITIONING
Every 6 months a service engineer or your Agent, must inspect the threads of the Vessel for excessive wear and tear.
If the wear is excessive the Vessel must be returned to dds for reconditioning. Irrespective of time, the Vessel must
be returned to dds for inspection and possible reconditioning after 5000 firings. The built in counter will prevent the
Vessel from operating after 5000 firings.
MAINTENANCE SCHEDULE
The Vessel design incorporates several O-rings and other consumable items and parts, which require checking,
cleaning and/or replacing on a regular basis. Please remember that the frequency of replacement of consumables is
a function of usage, quality and type of sample and Vessel cleaning techniques. The following Vessel maintenance
schedule provides a guideline.
NOTE: This is A GENERAL GUIDELINE and depending on the quality of the sample, the maintenance
schedule may need to be followed more regularly. i.e. With a substance which ignites easily (highly
flammable) the o-rings may only last 5-10 firings (sometimes less) and therefore it may be necessary
to change the o-rings more often. Please do take note of this and use this maintenance schedule as a
GUIDELINE only.
After every determination clean the inside of the Vessel with a paper towel to remove any residue or moisture.
Clean the threads on both the Vessel body and Vessel Cap using the Wire Brush.
• For additional accuracy, place the sample on the bottom of the crucible in a spread out form. This prevents
clogging and oxygen starvation.
• Spiking. In certain cases it is necessary to know the calorific value of a substances whose combustibility is too
low for self-ignition. In such cases the technique of “spiking” is used. A known amount of a more
combustible substance of known calorific value is mixed with the sample, thus allowing the composite
material to ignite. Provided the total calorific value of the “spike” is entered in the CAL2K-1 Calorimeter,
automatic compensation is made, and the true Calorific value of the sample is displayed.
• Sample preparation: a 200-mesh sample size is sufficient. Please note this refers to coal samples only.
• An easy way to check for leaking Vessel lid o-rings, is to fill the top of the Vessel cap with water (lid assembly
must be inside the Vessel, the Vessel cap screwed down and the Vessel filled with oxygen (under pressure)).
If bubbles are seen in the water then it is clear that one or more of the o-rings are leaking and should be
replaced. Remember only to fill the lid cap (lid assembly inside Vessel) with a little water – DO NOT immerse
the entire Vessel in water!
OPERATING HINTS
• Remember to use the correct firing wire and firing cotton when running a normal determination with
oxygen. DO NOT use the demo firing wire when running a normal determination with oxygen.
• Fill the Vessel with oxygen to 3000Kpa to avoid a misfire. Please note it is important to fill the Vessel to this
pressure, however with some samples (highly combustible, easily ignitable samples) the pressure can be
less. Please note the Vessel pressure must NEVER be more than 3000Kpa.
DO NOT COOL VESSEL IN WATER, RATHER USE CAL2K-2 COOLER TO COOL THE VESSEL.
DO NOT SUBMERGE THE VESSEL IN WATER FOR CHECKING FOR LEAKS, CLEANING OR COOLING.
DO NOT APPLY GREASE OR ANY OTHER FORM OF LUBRICANT TO THE O-RINGS ON THE LID
ASSEMBLY OR VESSEL.
“NOT IN CALIBRATION”
You have tried to save a calibration curve, but the CAL2K-1 is not in calibration mode.
The entry required is the "security" type, which requires a double entry, separated by a decimal point.
"ENTRY REQUIRED"
The RECALL CALIBRATION requires a Keyboard entry. The purpose of the RECALL... command is to take a calibration
curve from 1-9 to slot 0, which is the slot used for all determinations.
• Vessel was not filled with oxygen or not filled to 3000KPA. Filling the Vessel with less than 3000KPa may
cause a misfire. Bear in mind that some sample types require less oxygen pressure.
• Firing voltage is set too low. Must be set to 25.0
• Firing Cotton was not attached correctly to the firing wire
• Sample too low in calories: use SPIKING. This is useful when the sample does not ignite easily however it is
important to follow the steps and understand the steps of spiking.
• Maybe using the incorrect firing wire, make sure you are not using the demo firing wire.
"TERMINATED AT 5 MINUTES"
For some unknown reasons the FINAL drift is wrong. The CAL2K-1 Calorimeter has terminated the determination.
"TEST STARTED"
This message informs that the test function was activated from the Calorimeter Keyboard.
"SPIKING ENABLED"
This indicates that SPIKING has been enabled. The calorific calculation will use the spike mass and spike value.
"SPIKING DISABLED"
Spiking is disabled. Spike mass and Spike value are ignored.
SPECIAL DISPLAYS
Some display functions are special, and the details are explained below.
BOMB DETAILS
Details of the Vessel in the well can be displayed by typing a SUBMENU entry from 0-14, to identify specific
information.
CAL.No: N_C_DDMMYY_HHMM_AAAAiiii_VVVVVVV
Where: N = Calibration curve 0-9
C = Calorimeter number 1-7 which was used
DD = Day
MM = Month
YY = Last two digits of year
HH = Hour
MM = Minute
AAAAiiii = Sample identification
VVVVVVV = Standard value
CUST: AAAAAAAAAAAAAAAAAAAAAAAAAAAAAAAA
Where: AAA = Customer related text.
RESULT DISPLAY
The last result can be displayed by pressing the {R} Key in the form:
ddmmyyhhmm_Bnn_S_M.MMMM_IIIIIIII_RR.RRRR
Where: dd = Day
mm = Month
yy = Last two digits of year
hh = Hours
mm = Minutes
Bnn = Bomb number
S = Status
M.MM = Mass
IIII = Sample identification SID
RR.R = Result in chosen unit of measure.
A description of the (BRACKETED) words can be found after the table of LCD readings below.
RETURNS TO STEP 3.
(Drift) – Drift in degrees Celsius per 6 seconds.
(Mass) – Mass in grams.
(Result) – Calorific Value as it develops.
(SID) – Sample ID.
(Temperature) – Temperature of Vessel.
(Time) – Time in decimal minutes.
(T rise) – At firing, the temperature is set to zero and the ‘Temperature rise’ is displayed.
SUPPLY VOLT: S.S = Supply Voltage (this should be 9.0 +/- 0.1 Volts
Open the Calorimeter’s Lid, insert the Vessel with Firing Wire and Close the Lid:
Display will now be: CLOSED CLOSED
COOLER
This section is intended to coincide with the section “Cooler : Performance Testing”. If any problems are
encountered, please return to the section “Getting Started” and see the subsection “The CAL2K-2 Cooler –
Performance Testing”, to refer to the following diagnoses:
FILLING STATION
a) Bottle pressure gauge does not indicate – check the regulator on the oxygen bottle. Check the connection
between regulator and Filling Station.
b) Vessel does not fill – check the setting of the Flow Adjustor, check Lid Assembly of the Vessel.
c) Nozzle leaks while Vessel is filling – replace the Nozzle O-ring.
d) Nozzle leaks even with no Vessel inserted – replace Valve O-ring (Nipple) inside Nozzle assembly.
VESSEL
a) “No Wire” – check that the Firing Wire is present and securely clamped by the sleeves. Make sure you are
using the correct Firing Wire and not “Demo” Firing Wire.
b) Oxygen leaks – replace all Lid Assembly O-rings. Make sure the Vessel is filled to 3000Kpa. If under filled it
could cause leaking. Remember however, that high combustion samples require less oxygen.
c) Cap is difficult to turn – clean threads on both the Vessel Cap and Vessel Body with a wire brush.
d) Display shows “No Bomb” when Vessel is in the Well – clean the base of the Vessel and contacts in the
Well. Give the Vessel a twist to ensure a better contact. Make sure that the Vessel’s base is NOT wet!
e) Centre elEctrode does not move freely – strip and clean the Lid Assembly.
• Sample mass
• Sample identification
• Sample group identification (tray)
• Other
WARNING: The GID can ONLY be in alpha (letters of the alphabet) or numerical (numbers/digits)
format. NO special characters can be interpreted (e.g. dash, slash, full stop, bracket, etc.). The SID
can ONLY be in numerical format (NO Special Characters) as it is a number which gets incremented.
From the Docking Station, the prepared Vessel can then be inserted into any Calorimeter without further action. For
this to happen automatically, two conditions must be met:
A. A MASS and SID must be present in the Vessel. Only a Docking Station can perform this task.
B. The “BOMB MASS” operation must be enabled in the CAL2k via the Keyboard commands or via the PC
Interface. This operation needs to be performed once only.
Calorimeter (CAL2K-1)
Operation:
Balance
Vessel Mass Enabled
Docking Station
(CAL2K-5)
Vessel
Barcode (CAL2K-4)
Scanner 0-9 Normal
numerical value
Return (Back Space)
Enter
Optional External
Keyboard
Result includes: Group ID, Sample ID,
MASS from Vessel
The barcode scanner port is shared with the external Keyboard. Either or both can be used. The Docking Station has
some of its own pushbutton Keys as follows:
Keypad (Keyboard):
Numerical Keys 1
to 0
Enter Key
Confirms entry
2) Enter (as an example) – No: = 1 Use: = 83 – where “No: “ is the Vessel number e.g.: 1 and “Use:” is the
firing count of the Vessel e.g.: 83. Then enter the Sample ID. The Sample ID needs to be numerical ONLY
as it is incremented automatically.
3) Scan the barcode or enter the Sample ID from the Keypad. The sample ID will be indicated on the
display. If a change (edit) or a re-scan is required, then this can be done at this time.
4) Weigh the sample. Once the weight is indicated press the ENTER Key on the Keypad. An error message
may be displayed (see errors), otherwise the confirmed message “DONE REMOVE VESSEL” will be
displayed. This concludes the operation and the MASS, SID and GIDhave now been entered in the Vessel.
5) Remove the Vessel from the Docking Station and place the Crucible into the Vessel.
6) Fill the Vessel with oxygen.
7) The Vessel is now ready to be inserted (after a 1 minute stabilization period) into any CAL2k Calorimeter.
8) The CAL2k will recognize the charged (loaded) MASS, SID and GID if: “ENABLE BOMB MASS ENTRY/ON” is
set on the CAL2k. This can be confirmed through the CAL2k Keyboard MENU function. The “ENABLE
BOMB MASS ENTRY” needs to be set once only.
Bomb full - Vessel already has SID and MASS in its memory – to overwrite this, press Enter.
Done Remove Vessel - SID and MASS successfully entered into Vessel
Bomb FLT (Bomb Faulty) - Vessel is in Holder but it is not communicating with the Docking Station.
Remove the Vessel and re-insert it. If it is still faulty, try another Vessel.
S = SID
M = MASS
NO = Vessel Number
VSE = Firing Count
E.g.: F541
So 5531210628
55312 = GID
1062 = SID
8 = IGN
E.g.: F260
Note the missing letter “G”. If the missing letter(s) are important in the case that the numerical content is LESS than
4 digits, then the Fxxx (Format) must be changed to shift the missing digits to the GID, as follows:
E.g. F710
NOTE: The SID display shows the “formatted” SID BEFORE conversion to the CAL2k format.
RULE: The numerical portion of the SID must be more than 4 digits without any character other than
numbers! If this is not possible, then the Docking Station will ignore the “non-numerical” characters,
unless they are shifted to the GID with the format setup (Fxxx) as shown above.
NOTE: In manual SID entry if the SID is set to 4 characters then 4 characters must be entered e.g.: a
SID of 10 must be entered as 0010 (leading zeros must be entered). NO Special Characters are to be
entered, only numerical characters.
To clear the screen and start again during an entry type “x”.
CALIBRATION
A sample can be set as a calibration sample at the Docking Station as follows:
CERTIFICATIONS
APPENDIX 1
PRESSURE CONVERSIONS
3000KPa = 3 MPa
= 30 Bar
= 30 Atmospheres
= 435 PSI
APPENDIX 2
MJ / CAL / BTU ENERGY CONVERSIONS
1 MJ/Kg = 429.9 BTU/Lb
1 MJ/Kg = 238.85 Calories/gm
APPENDIX 3
BALANCE SETTINGS FOR CAL2K BOMB CALORIMETER
Data Output: Automatic output synchronous readout at stability
Characters: 7 Bit
Baud Rate: 2400
Synchronisation: 1 start bit, 1 stop bit
Parity Bit: Odd
DB25 CONNECTOR
Pin 1: Ground
Pin 2: Balance transmit (output)/input to CAL2k or ECO