SEMI AUTO MATIC BOMB CALORIMETER

BOMB CALORIMETER
INSTUCTION MANUAL

RBCMM

HOLY SCIENTIFIC

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BOMB CALORIMETER IS SUPPLIED COMPLATE WITH FOLLOWING
PARTS/COMPONENTS.
CONFIRMING TO IP 12/63 T & BS 1016
1. Bomb & closer ring. (01 nos.)
2. Calorimeter vessels with bomb support.(01 nos.)
3. Water jacket. (01 nos.)
4. Combined lid for calorimeter water jacket.(01 nos.)
5. Stirrer (01 no.)
6. Connecting lid (01 no.)
7. Connecting tube to connect pressure gauge & oxygen cylinder. (01 nos.)
8. Oxygen regulator
9. Spanner for oxygen cylinder (01 nos.)
10. Ignition wires (10 meter.)
11. Cotton reel. : 1 reel
12. Hook for lifting bomb (01 nos.)
13. Stainless steel crucible. (01 nos.)
14. Sheared valve (03 nos.)
15. Valve key. (01 nos.)
16. Microprocessor based control unit with automatic calculation facility: (01 nos.)
17. Pallet press. (01 nos.)
18. Bomb „o‟ ring. (01 nos.)
19. Stirrer belt (02 nos.)
20. Valve body O ring (02 nos.)
21. Benzoic acid of known calorific valves 6319 cal/ gram. (30 grams)

HOW TO OPERATE:
1. Connect the mains cord to 220 V, 1Ø
2. Switch on the unit.

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 3. Tack 1 gram (approx) combustible material.
4. Palletize the material with the help of pallet press.
5. Bound both the electrode of bomb lid with nicrom wire. (7 centimeter)
6. Tack the cotton reel (7centimeter)bound the one end to the nicrom wire & put the another end in
crucible which contain combustible material
7. Close the ring with hand. Full tighten the thread.
8. Connect the oxygen cylinder to & pressure gauge to the S.S bomb with connecting tube.
9. Fill the pressure inside the S.S bomb 26 kg/cm2.
10. Remove the connecting lines.
11. Tack 2 liter water in bucket.
12. Place the bomb opposite side of stirrer with lifting hook in bucket.
13. Connect the electrical connecting lid to bomb.
14. Close the vessel with combined lid.
15. Place the stirrer inside.
16. Place the sensor inside the bucket dip in water.
17. Connect the connecting lid, sensor connector, stirrer connector etc to control box.

Sensor
Main cable
connection Main switch
ON/OFF switch

Electrical lid
connection

Stirrer ON/OFF
stirrer
switch

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18. After connect the connection Switch on the unit.
19. Switch ON the stirrer
After switch ON the unit main display will show as below

20. Press set button. Than display ask “Enter password”

21. Enter 001 & press set.
22. In weight of sample enter actual weight of sample & press set
23. In set offset enter temperature offset. (if any)
24. In time to observe enter known time to complete the test if the time is unknown than enter 9.9 min &
than press enter key.
25. Wait till temperature become stable than press tare button than A. temp shows actual temp of water & I.
temp shows 0.00.
26. Press fire button. It will ignite the sample after few second temperature start rising.
27. After the sample burnt control box switch ON the buzzer for 10 sencond to intimate test complete &
display the calorific value in calorie per gram.
28. To start new test press enter button

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Note:

do not keep the sensor & stirrer in water, when the unit is not in use.

In emergency press enter button to stop the test in between.

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INSTRUCTION MANUAL FOR BOMB CALORIMETER

1. INTRODUCTION
A Bomb Calorimeter will measure the amount of heat generated when matter is burnt in a sealed
chamber (Bomb) in an atmosphere of pure oxygen gas.

The BOMB CALORIMETER provides a simple. Inexpensive yet accurate Method for determination
of heat of combustion, calorific value and the sulphar content of solid and . Liquid fuels. The outfit supplied
is complete for analysis as per methods recommended by the Indian Standards Institutions (IS-1350- 1960),
British Standards Institution ( BS 1016 Part 5 "1967) and: the institute of Petroleum (IP )2/63 T). Each Part
of the outfit has been finished and tested according to the specifications laid down by these institutions.

2. PRINCIPLE OF OPERATION
The known amount of the sample is burnt in a sealed chamber (latter on shall be refer to this chamber as
“Bomb”. The airs replaced by pure oxygen. The sample is ignited by electrically. As the sample burns heat
is produced. The rise in temperature is determined since, barring loss of heat; the amount of heat absorbed
by the burning the sample must be equal to the amount of heat absorbed by the calorimeter assembly, a
knowledge of the water equivalent of the
calorimeter assembly, and of the rise in temperature enables one to calculate the heat of combustion of the
sample. If

W = water equivalent of the calorimeter assembly in calories per degree Centigrade

T= Rise in temperature (registered by a sensitive thermometer) in degrees Centigrade.
H = Heat of sample burnt in grams.-
'H' is calculated easily since W, T and M are known.

3. Definition & units.

Calorimetric measurement involves the use of various temperature and energy units. In Order to
avoid errors .and confusion in the interpretation of these date. Their relationships should be well understood.

 Temperature: temperature is measured in degree centigrade.

 Mass: is expressed in grams.
 Heat energy: heat energy expressed in either calories or British thermal unit. The international stem table
calories is the basic unit in this system & equal to 4.1868 joules & is equivalent to heat energy required to
raise the temperature of one grams of water by one degree centigrade at 15.56hO c. The British Thermal
Unit equal 251.996 calories, or 1055.07 absolute joules, and is roughly equivalent to heat energy required
to rise the temperature of one pound of water-by one-degree Fahrenheit at 60h0F.

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 HEAT OF COMBUSTION; - As determined with the oxygen Bomb calorimeter is defined as the number
of heat units liberated by a unit-mass of the substance. When burnt in a sealed enclosure of constant
volume in an atmosphere of pure oxygen gas. In this reaction the substance and the oxygen are cooled 'to
within few degrees of the initial temperature also the water vapor formed by the combustion is condensed
to the liquid state. Therefore, a more exact definition would specify the temperature at which reaction
begins and ends, however, the change in the specific heat of water with the possible variations in the initial
Temperature is so small that this specification is not necessary
It is commonly expressed either in calorie per gram (cal/g) or British thermal unit per pound
One (cal / g) equals 108 Btu / lb

4. CHARACTERISTICS REQUIREMENTS
 Bomb:--When the sample burns, the pressure of gases increases rapidly. The Bomb walls, lid and joints
should e strong enough to withstand the maximum working pressures and there should be no leaks. Normal
working pressures are about 30 .atmospheres and overload pressures peak up to 100 atmospheres.
 The capacity of Bomb should be large enough to store enough oxygen to ensure complete burning of the
sample.
 During burning: the nitrogen & sulphur contents are oxidized to gases and then to nitric acid and sulphuric
acid. The bomb lining must therefore by resistant to acidic or basic ash & should be corrosion proof.

Ignition wire : it is recomonded that platinum wire to be used but

nicrom wire is also applicable

Standard sample:
 Benzoic acid: it is most commonly used as standard reagent.
 Nephalene is some time used as combustion standard. It is not hygroscopic but due to its volatility it
is necessary to use care to avoid error for sublimation. The crystalline material should be ground to
powder before using.
 Sucrose or cane also used as standard sample & as combustion aid. This material is neither volatile
nor strongly hygroscopic but is rather difficult to ignite. & some times it does not burnt completely

Standard alkali solution :

The washing form the oxygen bomb test must be titrated against standard alkali solution to
determine the acid correction. A 0.1 N sodium carbonate solution is recommended. This is prepared by
dissolving 5.2996 grams Na2 Co2 in water & diluting it in 1 liter water. Sodium hydroxide & potassium
hydroxide solution of the same normally are acceptable.

Methyl orange & methyl indicator:

This are usual indicator used for acid alkali titrtations.

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Allowable sample size:
Care should be taken to avoid over charging bomb. The mass of combustible charge (sample plus
combustion aid) should not more than 1.100 gram. When stating test with new or unfamiliar material it is
best to use the sample or less than 1 gram. Not more than 10,000 calories should be liberated in any test &
it is advisable to work with mass liberating less than 7000 calories.

Selection & preparation of solid sample.

It is necessary that solid sample be air dried & ground until all particle passes through 60 mesh screen. The
particle size is important because combustion reaction proceed s to completion within a few seconds. & if
any of the particle are to large they will not burnt completely. A sample is too finally divided is also
difficult to burnt. because extremely small particle can be swept out due to turbulence of the gasses. And if
they felt to bottom of the bomb without ignition it will give erroneous result. Pallet press offer the solution
to the problem of incomplete combustion in case of the finally divided samples.

Offset stirrer: it consists of a stirrer driven at a constants speed of 800 rpm by a motor though a heat
insulator rubber belt. The motor unit kept at sufficient distance from the vessel for eliminate the heating.
This arrangement does not raise the temperature of water by even 0.1 C in ten minutes. Thus easily meeting
requirement accepted by the Indian standards institution laid down by the British standard insulation, & the
institute of petroleum. The terminals provided in the electrical box firing unit.

Calorimeter vessel: is made of copper or S.S and is brightly polished out side.

Bomb firing unit & digital back men thermometer:

The unit is operated by A.C mains (230 V, 50Hz, single phase). It consists of two parts viz. the
electrical box & digital back man thermometer. The electric box provided with terminals for the stirrer unit
& firing the other parts used to measure the temp. Initial & temp. Rise.

Pressure gauge & stand:

An accurate pressure gauge is supplied for measurement of pressure of the oxygen is filled in the
bomb. The dial is graduated from 0 to 70 Kg/cm2 (0 to about 800 lb. /in2)

Pallet press:
The pallet press has 10 mm diameter punch & die. Coal or other powdered samples are compressed
into pallet before weighing and burning. This retards the burning rate and tends to retains the particles in
the crucible/capsules. There by reducing changes for incomplete combustion. The pallets are easier to
handle than loose sample. The pallet should not be made very hard as excessive hardness leads to bursting
upon ignition with consequent incomplete combustion.

Crucibles:
The stainless steel crucible is offered as standard with instrument. Platinum quartz & nickel crucible
are being offered as accessories extra cost.

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 Anthracites and cock:
While testing anthracite coals, cock, or other material of slow burning characteristics. It may be
difficult to secure ignition and complete combustion of the entire sample. In these eases the sample is
ground fine enough to pass through IS sieves 20 (211 microns)

Food stuffs and cellulosic materials:

The high moisture content of most food stuffs will usually require that they are dried before making
calorific test the operator will have to select the method for preparing the sample that will not destroy or
remove any of the combustible constituents. It may be necessary to make several preliminary tests to
determine the approximate ignited in the bomb without difficulty.

Gelatin capsules:
Volatile liquid samples to be burnt in oxygen bomb can be weighed and handled in gelatin capsules.
The capsules consists of two caps which telescope together with a friction fit educate retain most liquids
correction must be made for heat combustion of the gelatin. When used in calorimeter.

Explosive & high energy fuels

Special precaution must be observed when testing materials which release large volumes of gas upon
ignition or which denote with explosive force, it is possible to test many slow burning gun powders &
rocket propellant in conventional bombs. But the user must understand that the user must understand that
this bomb are not design to withstand the shock pressure produced by certain premiers and other mixture
which denote with explosive force it is most safer to test this in special high pressure oxygen bomb.
Each new explosive & sample or high energy fuels introduces special problems which can be solved
only by carefully experimentation usually it will be well to observe the burning of a small amount of
sample over an open flame to determine the explosive behavior and than proceed to bomb combustion
combustion using only one tenth or one fifth amount of the sample. Further incrace up to 7000 calories.
Permissible maximum should be made gradually & only after all evidence indicates the absence of violent
behavior

6. Setting up and assembly:

General arrangement:
The laboratory in which the calorimeter is to be operated should be equipped with many or the
facilities commonly used for chemical analysis these include desk space funning water an analytical
balance, apparatus for volumetric titration & misalliances items of laboratory ware. The calorimeter should
be used in a room where fluctuation in temperature can be avoided in particular the instrument should not be
taken from one chamber to another chamber maintained at different temperature through out the chamber
before starting the use of calorimeter. All part of the calorimeter should be kept clean to remove any
moisture. Which may have condensed on the wall, before starting the use of new calorimeter it is advisable
to assemble all parts or the apparatus without a charge in the bomb and without water in bucket. To be sure
that everything is in perfect working order.

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Assembly of calorimeter parts :
Piece of triangular/ star of calorimeter vessel support at the bottom of the jacket and set it so that the
„U‟ shape strip welded inside the jacket do not allow it to be displaced place the bucket on the star support
fit the support strip in the groove lift the bomb on its stand by hook and place it inside the bucket. Attach the
supply to the electrodes provided on the lid bomb place the combined lid of the bucket & water jacket in
such a way that a pin provided on the lid of bomb. Place the combined lid of bucket and water jacket in such
away that a pin provided on the cover plate of jacket fits in to the seller grooves provided on the lid.
Mount the stirrer assembly on the stirrer rod provide on the cover plate of the calorimeter jacket
passing the stirrer pipe through the opening provided on cover of the calorimeter jacket. The connection are
then further taken firing box terminals market “BOMB” insert the sensor of digital back man thermometer
in the water of bucket/calorimeter vessel through the combined lid. So that it remained dipped in water of
calorimeter vessel.

Attaching the fuse :

All manipulation prior to closing the bomb can be performing by holding the bomb head in bomb
support stand. Cut a single length of fuse wire 7 cms. Of fuse wire attach it to electrodes.
It is not necessary to submitter the wire in powder sample in fact better combustion usually be
obtained if the loop of the fuse is set slightly above when using pelleted samples, bend the wire so that the
loop bear against side of the pallet firmly enough to held it against the side or the capsule. It is also a good
practical to till the capsule slightly to one side so that the flame amercing from it will not impinge directly
on the loop of the straight electrodes.

Nicrom arrangement:
Nicrom wire can be attached to the electrode in the manner described above but most nicrome wire
ignition procedure required cotton or nylon thread to carry on ignition flame the sample. A coil is formed by
winding out few turns of wire around 2 mm diameter rod removing electrode. The resulting coil is axis of
the coil pointing toward the sample. A short length is them inserted through the coil end in to the crucible.

Water in to the bomb:

Place 2.0 ml of distilled water in the bomb from pippet.

Filling the bomb with oxygen

While closing the bomb always make certain that the head gasket or sealing ring in good condition
& care must be taken not to disturb the sample. Commercial oxygen produced by rectification of liquid air
can be used directly from the supple cylinder.
To attaché the filing connection place the bomb on its stand. Put the high pressure valve on oxygen
cylinder outlet and connect flexible tube to valve outlet. Draw up the union joint tightly connect the other
end to the pressure gauge cum safety device. & pressure gauge to bomb. Open the cylinder with cylinder
key. Than open the high pressure valve slowly. Observe the gauge & allow the pressure in to the bomb until
25Kg/cm2. Close the valve. to release the pressure push the pin valve with soft hand or pressure release
valve.

Precaution: the operator must follow the following basic points in order to operate this oxygen bomb
safety.

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1. Do not use too much sample. The bomb can be withstanding the effects of combustible charges which
librated more than 10000 calories. This generally limits total weight of combustible material (sample gas
gelatin, firing oil or any combustible aid) do not more than 1.10gram. Do not charge with more oxygen
than is necessary and do not fire the bomb if an overcharging the oxygen should accidently be admitted.
2. Keep all parts of the bomb especially electrodes in good repairs in all times do not fire if gas bubbles are
leaking from the bomb when it is sub merged in water.
3. Proceed with caution & use only fraction of the allowable maximum sample when testing new materials,
which burn rapidly, or have explosive characteristics.

Standardization of the calorimeter:

Definition: the water equivalent is the weight of water which is equivalent in effective heat capacity of the
entire system. (calorimeter vessel containing a specific weight or the weight of water calorimeter bomb
charge with oxygen fuel & water calorimeter and stirrer) since the specific heat of water is 1.000.

Principle:
The effective heat capacity of the system is determined by burning pure & dry benzoic acid weighed
not less than 0.9 & more than 1.1 gram. Determine the corrected temperature rise T from the observed test
data also titrate the bomb washing to determine the nitric acid correction & measure the un burnt fuse wire
compute the equivalent by substitution in the following question.

W = HM + E1 +E2
-------------------
T

Where: -

W: energy equivalent of the calorimeter in calories per degree centigrade.

H: calorific value of standard benzoic acid/sample in calories per gram.
M: mass of standard benzoic acid/ sample in grams.
T: corrected temperature raise in degree 0C
E1: correction of heat formation of nitric acid in calories and
E2 : correction for heat of combustion of firing wire in calories.

HOLY SCIENTIFIC
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