(Part B: Engineering Exercises)

Contents
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Experiment -1 Determination of flash point of oils by Able’s apparatus
Experiment -2 Determination of flash point of lubricating oil by Pensky Martin’s
‘closed’ tester
Experiment -3 To study the viscosity of the given sample of lubricating oil with a
Redwood viscometer and to study the viscosity at various
temperatures
Experiment -4 To find out the aniline point of the given sample of fuel
Experiment -5 Determination of Steam Emulsification Number (SEN) of a given
lubricating oil

Experiment -6 Determination of viscosity average molecular weight of a polymer

sample by Viscometer

Experiment -7 Determination of the calorific value of a given sample of fuel (liquid

and solid) by bomb calorimeter

Experiment -8 To carry out the % of moisture content only of a given sample of

coal as a part of proximate analysis

Experiment -9 To study the adsorption of acetic acid by activated charcoal from an

aqueous solution

Experiment -10 Determination of Total Dissolve Solids (TDS) of given samples by

Digital TDS meter & conventional method

Experiment -11 Determination of Turbidity of given samples by Digital Turbidity

meter/Nephelometer

Experiment -12 Determination of Dissolved Oxygen in water by Dissolved Oxygen

Meter method
 Experiment – 1
Determination of flash point of oils by Able’s apparatus.

Definition and Object

The flash point of oil may be defined as the minimum temperature to which it must be
heated to give off sufficient vapour to form an inflammable mixture with air. This is deducted
by the appearance of momentary flash upon the application of small flame over the surface of
oil. The flash point is defined as closed or opens accordingly as the apparatus is provided
with a cover over the oil cup or not.

This test is of immense importance for illuminating and lubricating oils. This helps in
detecting the highly volatile at ordinary temperatures, the issuing vapours may cause the fire
hazardous. So to ensure safety, certain minimum temperatures are laid down for fuels and
lubricating oils below which they should not give off adequate vapours to make them burn.

Outline of the method

This method applies to oils having a flash point less than 490C.

The sample is placed in the oil cup of the apparatus and heated at a slow uniform rate.
A small test flame is directed into the cup at regular intervals, and the lowest temperature at
which application of the test flame causes the vapour above the sample to ignite, with a
distinct flash inside the cup, is recorded as Able’s flash point.

Description of the apparatus

The Able’s apparatus is depicted in the sectional diagram; it consists of the following
essential parts:

Oil cup (A): This is a cylindrical vessel open at the top and fitted on the outside with
a flat circular flange projecting at right angles. It is made of brass or gunmetal and within the
cup, near the top, there is a level mark (L).

Cover (B): The cup is provided with a close fitting cover. The cover is provided with
a thermometer socket (C), turn ions to support an oil test lamp (D), a pair of guides in which
a slide (E) moves, and a white bead (F). The top of the cover is pierced by three rectangular
holes which are covered or uncovered by moving the slide which has two perforations allow
air to enter the oil cup and bring contact between vapours of the oil and flame of the test-
lamp when in ‘open’ position.

A white bead, the dimensions of which represent the size of test flame, is mounted in
a visible position on the cover. In a modified apparatus the cover is also provided with a
stirrer (G) consisting of a round stem having four blades at one end and projects into the oil
cup.
 Heating vessel: The heating vessel consists of two flat bottomed cylindrical copper
vessels (H) and (I) placed coaxially, one inside the other, and soldiers at their tops. The space
between the two vessels is thus enclosed and is used as a water jacket. When the oil cup is
placed into the hole at the top of the vessel, it fits into it and leaves an air bath (J) and
provides proper heating of the oil.

The vessel rests upon a tripod stand (K) and can be heated electrically or with a
burner or spirit lamp. Two thermometers are provided with the apparatus, the one (T1) for
measuring the temperature of the bath, the other (T2) for determining the flash point. The
heating vessel is provided with a funnel (M) for introducing water outlet (N) tube.

Procedure: Following two methods may be used for the closed flash point of oils by Able’s
apparatus method A is for oils flashing below 320C, and method B for oils which flash
between 320C and 490C inclusive.

Method A

The heating vessel is filled to overflowing with warm water and its temperature is
adjusted to 550C at the beginning of the test. The test flame is adjusted to a bead
approximately four mm in diameter and compared with the projecting white bead mounted on
the cover, to maintain its size constant.

The temperature of the sample is adjusted to approximately 150C and filled in the
already washed and dried oil cup until the liquid just reaches the level mark. The oil cup is
fitted with the cover, with the slide closed, and placed in the heating vessel. The
thermometers are so inserted that if cup is properly placed the thermometers scale faces the
operator.

The test flame is set up and when the temperature of oil reaches 200C test-flame is
applied, by slowly opening the slide after every 0.50C rise in temperature and closed
immediately, until a distinct flash occurs in the interior of the cup. This temperature is
recorded as flash point. The vessel is not heated during the test.

Method B

The method is same as described above expect that in this case the air chamber is
filled, to a depth of four cm with cold water and the heating vessel is filled with cold water.
The vessel is heated at a rate which gives a temperature rise of 10C per minute. The testing in
this case is started when the temperature has risen to 250C.

Observation: (Illustration)

Barometric pressure......mm Hg

S. No. Temperature 0C Interferences

1 38 No flash
2 39 ””
3 ...... ””
4 45 Flash observed

Results: The ‘closed’ Able’s flash point of the oil is found to be 450C at barometric
pressure............ mm Hg.
 Experiment – 2
Determination of flash point of lubricating oil by Pensky Martin’s ‘closed’ tester.

Definition and Object

Same as described for the preceding experiment.

Description of the apparatus

This apparatus is used for the oil flashing between 490C and 3700C.

A Pensky Martin apparatus consists of the following major parts:

Oil cup (A): It is a cylindrical vessel, made of brass, with a filling mark grooved
inside near the top. The inside of the cup is of slightly larger diameter above the filing mark
and is covered with a lid.

Lid (B): It is equipped with the following parts:

(I) Stirrer: The stirring device consists of a vertical steel shaft (C) mounted in the
centre of the cup and carrying two two-bladed brass propellers.
(II) Cover proper: It is made up of brass having a rime projecting downward and
fitting the outside of the cup closely. It has four openings: one for thermometer (T); and the
rest for the oxygen entry and exposure of vapours to the test flame.
(III) Shutter: The lid is equipped with a brass shutter (D) operating on the plane of
the upper surface of the cover proper. The shutter is so shaped and mounted on the lid that
when in one position, the holes are completely closed when in the other, these orifices are
completely opened.
(IV) The flame exposure device: The lid is equipped with a pilot-lamp (L) with
such a mechanism that its flame operates simultaneously with the shutter. When the shutter is
in the ‘open’ position, the tip is lowered down in the centre of the central orifice.

Stove: The cup is heated by means of a properly stove (C) which consists of an ‘air
bath’ (E) and a top-plate (F). The air-bath has cylindrical interior about 4 cm deep and can be
heated by a direct flame or an electric resistance element. The top-plate is also made of metal
and mounted with an air gap between it and air bath.

Procedure:
The cup and its accessories are well cleaned and dried before the test is started. Now
the cup is filled with the oil to be tested up to the level indicated by the filling mark and
covered with the lid. The cup is now set in the stove properly and the thermometer inserted,
the test flame is lit and the heating rate is maintained, with the help of rheostat, at 5-60C per
minute and stirring rate at 1 to 2 rps.
Once the heating is started, the test flame is applied after each 20C rise of temperature
up to a temperature of 1050C. After that the test flame is applied after each 50C rise of
temperature. The first application of the test flame is made at least 100C below the actual
flash point, which can be determined in a rough experiment. The application of the test is
made by operating the device controlling the shutters and test-flame burner so that the flame
is lowered in 0.5 second, left in its lowered positions for one second, and quickly raised to its
position.

The temperature at which the flame application causes a distinct flash in the interior of
the cup is recorded as the flash point.

Observation: (Illustration)
Barometric pressure......cm Hg

S. No. Temperature 0C Observations

1 90 No flash
2 91 ””
3 92 ””
4 93 ””
5 94 ””
6 95 ””
7 96 Flash observed

Results: The Pensky Martin’s ‘closed’ flash point of the given sample of oil comes out to be
960C at a pressure of............cm Hg.
 Experiment – 3
To study the viscosity of the given sample of lubricating oil with a Redwood
viscometer and to study the viscosity at various temperatures.

Object of determination

Viscosity is one of the most important properties of a lubricant which tells about its
suitability for lubricating purpose. A lubricant reduces friction between different moving
parts of a machine by avoiding direct metal to metal contact. The thin film of the oil, formed
between the moving surfaces, keeps the apart and thus the frictional resistance is entirely on
account of the shearing of the liquid. The viscosity of the fluid measures the amount of this
internal friction.

The object of this determination, therefore, is to ascertain whether the oil is

sufficiently viscous, under the higher pressure and temperature of the machine, to adhere to
the bearing. The variation of viscosity with temperature is of great importance to the engineer
in all problems of fluid low and fluid friction and also in pumps, fans and all types of
bearings.

Theory and general discussion

Viscosity is the property of a homogeneous fluid which causes it to offer frictional

resistance to motion. The property may be measured in several ways, one of which is
determining the time required for the liquid to flow through a capillary. Such method
includes the use Saybolt, Engler and Redwood viscometer.

The viscosity may be expressed as dynamic (or absolute) viscosity, kinematic

viscosity or the viscosity called after the name of the apparatus used for its determination.

Dynamic viscosity

Dynamic viscosity is the tangential force on unit area of either of the two parallel
planes, at unit distance apart, when the space between the planes is filled with the fluid and
one of the planes moves relatively to the other with unit velocity in its own plane. It is
defined as the ratio of the shearing stress to the rate of shearing stress to the rate of shearing
strain. If F is the force required to keep moving an article, of surface area A in contact with
the fluid, separated from stationary surface by a thickness d, with a velocity V, then,

Shearing stress = F/A; Rate of shearing strain = V/d

Fd
Therefore, absolute viscosity µ = ........ (1)
AV

The numerical value of the µ depends upon the units used in Eq. (1). In metric system
the unit is poise (F = 1 dyne, A = 1 sq. cm, V = 1 cm per second). A smaller unit, centipoises
is more often used. Absolute viscosity is also referred to as “coefficient of viscosity”.
 Kinematic viscosity

This is absolute viscosity divided by the density of the fluid. The metric units are
stoke and centistokes. Thus, if ρ is the density then,


Kinematic viscosity ν = Stokes


Since the rate, at which a fluid will flow through an aperture, increases as the internal
friction of the fluid decreases, the rate of flow through an orifice or short tube may be used as
a means for measuring viscosity. This is the principle involved in the Redwood viscometer
which is an English standard and is one of the several short tube viscometers used for oils.

The time in seconds required for 50 ml of oil to gravitate through the Redwood
viscometer at a given temperature is expressed as its viscosity in Redwood seconds at the
temperature.

Absolute and Kinematic viscosities can also be determined from the Redwood values
by means of following formula:

Absolute viscosity = ( At − B / t ) × ρ

Kinematic viscosities = = At − B / t


Where A and B are constants known as instrument factors, t is Redwood viscosity,

and ρ is the density of fluid. The values of A and B for Redwood viscometer No. 1 are as
follows:

Viscosity range in R.I. second A B

34-100 1.79 0.00260
Above 100 0.59 0.00247

Description of apparatus:

The Redwood viscometer is available in two types, no. I and II. Both are suitable
for use with oils having flow time, at the temperature of the test, of not less than 30 seconds.
When the flow time with no. I apparatus exceed 2000 seconds the use is made of no. II
viscometer. The only main difference between the two viscometers is in the diameter of
the discharge jets, the no. I jet having a diameter of 1062 mm and length of 10 mm,
while the no. II jet is 3.88 mm in diameter and 50 mm in length.

A general description of the two viscometers is as follows:

The viscometer consists of an oil cup (A) which is a cylindrical vessel made of brass.
The upper end of the cup is open while the bottom of the cup is concave internally, to allow
complete drainage of the liquid with which it may be fitted. The base of the cup has a
tapering central hole in which the jet (J) is fitted. A stout wire, turned upwards at right angles,
is fixed into the side of the oil cup to indicate the level (B) to which the oil is to be filled.
 The jet, constructed of agate, is provided with a concave depression which can be
covered with a ball value (C) for starting or stopping the flow of oil.

The cup is surrounded with a cylindrical heating bath, the contents of which can be
heated by an electrically heated coil (E) placed in it. The bath is provided with a tap (F) for
emptying. Stirring of the bath is affected by means of a cylinder surrounding the oil cup,
provided with four vanes (G) the upper and lower portions of which are turned in opposite
directions.

The apparatus is elevated on legs or tripod stands so that a receiving flask (H) can be
placed beneath the jet to catch and measure the oil flowing from the tube. The flask is of
special type, graduated with a 50 ml mark at the neck and with a flaring mouth. The tripod
stand has levelling screws at the bottom and the thermometer (T1) is suspended in the oil by
means of a spring clip (l) sliding on the vertical rod fixed on the top of the cup. The cover of
the in cup has provisions for the insertion of thermometer and the ball-valve projects outside
the cover through a hole. Another thermometer (T2) measures the temperature of the bath.

Procedure: The apparatus is prepared first by cleaning it and then levelling by the
screws provided for this purpose.

When marking the viscosity determinations, the bath is heated to a few degree above
the desired test temperature. The test sample is adjusted until the sample in the cup is at the
test temperature, stirring the contents of the bath the cup during this process. When the
temperature of the sample has become quite steady at the desired value, the liquid level is
adjusted by allowing the sample to flow, until the surface of the sample touches the filling
mark. The oil cup is covered and the thermometers inserted. The clean, dry, standard 50 ml
flask is placed centrally below the jet properly. The ball value is lifted and the stopwatch is
started simultaneously. The valve is not removed completely, but kept immersed in the oil by
supporting it by the hook provided for the purpose. The receiving flask is positioned so that
the oil strikes the flared mouth and does not drop directly into the opening which would cause
foaming. The stopwatch is stopped when the level of the oil reaches 50 ml mark in the neck
of the flask.

The time elapsed in seconds is recorded as Redwood viscosity at the test temperature,
observed before the flow was started.

Following this procedure the viscosities are determined at one or more of the
following temperatures: 700F (21.10C); 100 (37.8); 122 (50); 140 (60); 200 (121); 300 (149);
and 400 (204).
 Experiment – 4
To find out the aniline point of the given sample of fuel
fuel.

Object of determination

The approximate method of testing the ignition quality of oils is based on

measuring the proportion of paraffin hydrocarbons in the fuel. In the case of petroleum fuel
oils the high paraffin content to better ignition quality.

The aromatic hydrocarbons mix readily with aniline at room temperature but paraffins
mix only at relatively
tively higher temperatures. A high aniline point indicates a high paraffin
content and higher ignition quality.

Moreover aromatic hydrocarbons dissolve natural rubber and some synthetic rubbers
also. This means a higher aromatic content in a lubricating oi
oill may not be desirable as
otherwise it may damage the oil sealing or packing which are usually made of rubber and
used in the machines.

Definition: The aniline point of an oil is the lowest temperature at which the oil is
completely miscible with an equal volume of aniline.

Procedure: Equal volume of aniline and on are heated to effect complete dissolution
and the cooled under controlled conditions. The temperature at which the entire mixture
becomes cloudy throughout is reported as the aniline
aniline-point of the lubricating oil.

The apparatus used for the determination of aniline

aniline-point
point of a lubricating oil is shown
in given fig.

The apparatus is thoroughly cleaned and dried at 1100C before starting the
experiment. About 10 ml of pure and dry aniline (dried over pure KOH pellets, pellets filtered and
freshly distilled) are taken in a heat resistant pyrex or corning test tube (2.5 cm – 15 cm) and
an equal volume of the lubricating oil is added. The tube is fitted with a cork which also
holds an electrically operated stirrer and a thermometer in such a way that the bulb of the
thermometer is about 5 mm above the bottom of the test tube. The tube is inserted into an
outer jacket (4 cm-17.5 cm). The stirrer is started and the aniline-oil mixture is observed to
find whether the miscibility is complete at room temperature itself. If so, the jacket holding
the tube is immersed in an non-aqueous cooling bath. Cooling is continued slowly at a rate of
0.5 to 10C per minute, until the entire aniline-oil mixture suddenly becomes cloudy
throughout. This temperature is recorded as the aniline-point of the lubricating oil.

If the aniline-lubricating oil mixture is not completely miscible in the tube at the room
temperature, then slowly and carefully heat the jacket, holding the tube either directly or by
immersing in a hot bath. Stirring is continued while slowly raising the temperature, until the
aniline-oil mixture is completely miscible. Then the jacket holding the tube is withdrawn
from the burner or the hot bath, as the case may be. Now, while the stirring is continued, the
temperature is allowed to fall at a rate of 10C per minute. A cold bath may be used for this
purpose, if necessary. The temperature at which the entire aniline-oil mixture becomes cloudy
or hazy throughout and the outline of the thermometer bulb is observed is taken as the
aniline-point of the oil sample.

Results: .......................................................................................................

Precautions

1. The whole apparatus should be perfectly dry, because even traces of moisture may
give erroneously high results.
2. Aniline used should be perfectly pure and dry.
3. Aniline is hygroscopic and hence water should not be used even in cold and hot
baths. Non-aqueous, non-volatile and transparent liquids should be used for the cold
and hot baths.
4. Aniline is highly toxic and hence it should not be sucked into the pipette by mouth.
Pipette provided with a rubber suction bulb or an aspirator should be used for this
purpose.
5. Stirring should be done at such a rate that undue splashing of the liquid or formations
of air bubbles are avoided.
6. If the expected aniline-point is below the dew point at the atmosphere, the space
above the aniline-oil mixture in the tube should be filled with dry N2.
7. The true aniline point is characterised by a turbidity which increases sharply as the
temperature is lowered. The minimum equilibrium solution temperature, i.e. the
temperature at which the entire aniline-oil mixture suddenly becomes cloudy
throughout is taken as the aniline-point.
 Experiment – 5
Determination of Steam Emulsification Number (SEN) of a given lubricating oil.

Object of determination

Certain lubricating oil mix intimately with water and form emulsion which has a
tendency to collect dirt, grit particles and other foreign matter. Thus the solid particles are
wearing out of the machinery.

The tendency of an oil to emulsify increases with the time, it is used as a lubricant. A
good lubricating oil is one which does not form emulsion under lubricating conditions and
even if it forms an emulsion, it should break off very quickly.

Outline of method: The tendency of emulsification is determined by ASTM emulsion test.

An emulsion of oil and water is made under standard conditions and then allowed to break.
The time, in seconds, required for the complete separation of water from oil is reported as
steam emulsification number.

Description of the apparatus: The construction of the apparatus is very simple. It consists
of a steam generator G, which is a litre round bottomed flask heated from below with a
burner. D is a 2.5 by 20 cm test tube used as sample tube, graduated from 0 to 50 ml. The
tube is suspended in an emulsifying bath E, which is a glass battery jar of three litre capacity.
A similar jar H is used as separating bath. Steam from G is led into the sample by means of a
delivery tube, the other end of which is cut-off at an angle of 30 degree.

Procedure: The flask G heated to generate steam and maintained at a temperature of 93-950C
by passing steam. Jar E is filled with water and the temperature is adjusted to 20-250C at the
start and then it is not controlled during the test. 20 ml of the sample oil are poured into the
test tube at room temperature and the tube is placed in the holder M of the bath E and the
cork stopper containing a thermometer T is put in place.

The steam delivery tube, which should first be steamed out until all condensation
disappears, is then inserted through a loose hole in the cork so that the point touches the
centre of the bottom of the test tube. Steam is then admitted at a rate which will maintain the
temperature of oil between 77-800C, which is affected by controlling the value L. The
steaming is continued until the total volume of the contents of the test tube becomes 37-43
ml. The process of steaming should not take less than 4 minutes.

When the emulsification is complete, the cork and attachments are quickly removed
from the test tube and the same is transferred rapidly to the separating bath, maintained at 93
-950C and a stop watch is starred at the instant of immersion. The contents of the test tube are
examined every 30 seconds and the volume of separated oil is recorded until 20 ml of the oil
is separated.

The time in seconds elapsed during the separation of 20 ml of oil is reported as SEN.

Results: .......................................................................................................
 Experiment – 6
Determination of viscosity average molecular weight of a polymer sample by
Viscometer.

Theory: Addition of even a very small amount of a polymer to a solvent of low viscosity
causes a sharp increase in its viscosity. The magnitude of increase in viscosity depends in
addition, to other factors such as concentration, shape and size of the solute molecules, on the
molecular weight of the polymers.

The ratio of the coefficient of viscosity of the solution (ηs) to the coefficient of
viscosity of the pure solvent (ηo) at the same temperature is known as viscosity ratio or
relative viscosity (ηr) which can be written as:

ηs ρs t s
ηr = =
ηo ρ 0 t o

Where, ρs and ρo are respective densities of polymer solution and pure solvent; ts
and t0 are the corresponding efflux time. For a dilute polymer solution (≈ 0.5 g/ 100 ml) the
two densities can be taken as equal. Then the equation becomes:

ts
ηr =
to

η s − η0 η s t
η sp (specific) = = − 1 = ηr − 1 = s − 1
ηo ηo to

The ratio of the specific viscosity of the solution to its concentration C, is called
viscosity number or reduced specific viscosity.
η sp
η red =
C

C = concentration in g/ 100 ml
The plot of ηred versus C is a straight line is extrapolated to zero conc. (i.e., cut into
the Y-axis, ηred). The intercept on the ordinate is the viscosity at zero conc. or the limiting
viscosity and termed as limiting viscosity number or intrinsic viscosity, [η], which is related
, by an empirical equation.
to molecular weight M

 α
[η] = K M

Where ‘K’ and ‘α’ are constants for a particular polymer/ solvent/ temperature system
and can be obtained from the books.
Procedure:

(A) Preparation of polymer solution: Weigh accurately 500 to 100 mg of the well
dried powdered polymer (whatever concentration you need to prepare) and transfer to a 100
ml volumetric flask. Add 80-90 ml of the solvent (in which polymer is soluble) stopper the
flask and suspend in a thermostatic water bath at 250C, shake occasionally to dissolve the
sample and then fill the solvent up to the mark.
(B) Measurement of flow time with Ostwald Viscometer: Wash the viscometer with
chromic-sulphuric acid mixture and keep for drying in air oven. Pipette 20 ml of the solvent
into the wide arm (reservoir R) and affix in a thermostatic water bath. Allow 5-10 minutes for
attainment of temperature. Using a rubber ball, force air into the wide arm so as to raise the
level of liquid into the capillary arm above the higher mark M1. Then release the pressure and
with a timer measure the time in which the liquid meniscus moves from the upper mark M1 to
the lower mark M2 and use the flow time as t0.

Pour out the liquid from the wide arm as completely as possible. Clean the viscometer,
dry it and fill it with 20-25 ml of the polymer solution and determine the flow time in the
similar condition (ts). Similarly determine the flow times for solutions of minimum three
different concentrations.

Observation and Calculation:

Temperature of the experiment =

Solvent used =
Values of constant for
Polymer / solvent / 250C K =

α =

Volume of liquid used for the experiment =

 Polymer solution Flow time in Relative viscosity Specific Reduced
Concentration seconds ts viscosity viscosity
ηr = η
to η red = sp
ηsp = ηr - 1 C
Pure solvent t0
0.1 t1
0.2 t2
0.3 t3
0.4 t4
0.5 t5

Plot the graph between ηsp/C versus Concentration and get the value of [η] limiting viscosity.

Calculation of molecular weight:

α
[η] = K 
M
α
log [η] = log K + log 
M

 log [η ] − log K

log M =
α


 log[η] − logK 
M = antilog  
 α 

Result: The viscosity average molecular weight of the polymer is.............

(K and α values will be taken from the teacher)

 Experiment – 7
Determination of the calorific value of a given sample of fuel (liquid and solid) by
bomb calorimeter.

Object and determination

Calorific value of any fuel tells about its heating value which is the most important
property of a fuel. Thus to know about a fuel it is necessary to know its Calorific value.

Definition and general discussion

Calorific value of a fuel is defined as the quality of heat energy given out upon the
complete combustion of a unit quality of the.

The quality of heat is commonly expressed either in the British thermal unit (Btu) or
in metric system as Calorie. A Btu is defined as the quality of required to raise the
temperature of one lb. of water by 10F (from 62 to 630F), while a Calorie is the quantity of
heat which raises the temperature of one kg of water through 10C (i.e. from 15 to 160C). The
relation between these two units is as under:


1 Calorie = × 2.2046 = 3.9683 Btu

There is still a smaller unit written as ‘calorie’ which is one thousandth of a calorie and is the
heat which raises the temperature of 1 g of water through 10C.

Since however the calorific value is expressed as Btu per lb or calories per kg, the
relation becomes:

.

Calorie/kg = = 1.8 Btu

.

‘ Thus if all the determinations are carried out in metric unit, the value in Btu can be
obtained by multiplying the result by a factor 1.8.

Furthermore, the calorific value is expressed as gross net calorific value.

Glass or higher calorific value

This is defined as the calorific value at constant volume, determined by burning the
fuel in the oxygen, saturated with water vapour, the original and final materials being at 150C.
The residual products being CO2, SO2, N2 and H2O, the H2O other than that originally present
as vapour being in the liquid state.

Net or lower calorific value

It is the calorific value determined by burning the fuel in O2, saturated with H2O
vapour, the original and final materials being at 150C and the residual products being CO2,
SO2, N2 and H2O vapour.
 The higher calorific value includes the amount of heat given out by burning the coal
plus the heat given out due to the condensation of steam at 1000C and sensible heat of water
when it cools from 1000C to 1500C. This stream is formed during the combustion of coal. In
actual practice this heat is lost with the combustion product and thus the net heating value can
be obtained by subtracting this heat from the gross calorific value.

Description of the apparatus

The actual construction of the apparatus is somewhat complicated and varies with the
make. It however contains certain essential parts which are always present irrespective of the
make so a general description of such parts follows:

1. Combustion bomb: This is the most important part of the apparatus in which the test
material is subjected to rapid combustion under high oxygen pressure. This is a cylindrical
vessel of ml capacity made of strong acid and alkali proof steel. The inner fixtures of the
bomb are similarly made of heat and acid resistant stainless steel. It is equipped with a cover,
usually made of the some material, sealed tightly by means of a recessed gasket, designed to
withstand a pressure of 4000 psi without developing leaks. The cover has provisions for inlet
and outlet of oxygen, electrical connections and bearing the crucible containing the sample.
2. Calorimeter vessel: The bomb assembly (A) is placed in the calorimeter vessel (B)
which is cylindrical in form and made of brightly electroplated and polished brass-sheet
having a capacity of about 3-5 litres. This contains a known volume of water the rise in
temperature of which permits the calculation of the heat produced, from which the calorific
value of the test material can be computed.
3. Calorimeter jacket or thermostat: The calorimeter vessel along with the bomb is placed
in what is called as calorimeter jacket (C). This is actually a double-walled asbestos-insulated
cylindrical vessel. The space between the walls is filled with water at a temperature 2-30C
below the room temperature in order to increase the heat capacity of the calorimeter. The
cover of the thermostat is made of heat insulating material and posses holes for insertion of
electric wire, thermometer (T) and stirrer (S). The thermostat protects the calorimeter from
heat loss and from the influence of external the entire course of the test.
4. Thermometer: The temperature of the calorimeter water is recorded with a thermometer
(T) graduated to at least 0.010C. Usually a magnifying glass (G) is used to read the
temperature accurately.
5. Stirrer: The water of the calorimeter is stirred with the help of an electric motor driven
stirrer (S) which is operated with the help of a transformer.

The transformer, a thermostat, a ratio switch and a push button are usually assembled in
a control box (D) and also give necessary voltage to ignite the fuel sample placed in the
bomb.

Oxygen necessary for combustion is added to the calorimeter bomb through a feed
device, consisting of a pressure regulator, a pressure gauge and a feel tube. From the gas
cylinder oxygen is made to pass, through the pressure regulator, to the pressure gauge and
through a piping to the bomb (not shown in the figure).

The calorific value of some coal grades may be tested only on pallets. Material of high
ash content cannot be burnt completely in pulverised condition. A tablet press is usually
provided to permit their transforming into pellets.

Procedure

a) Weighing the sample:

(I) Solid fuel: If the sample is now in ash content and high in volatile matter it is taken
in the pulverised from in an already weighed silica or platinum crucible. If the sample is of
high ash content, a pallet is preferred and if the ash content exceeds 50% the pallet of the
sample is wrapped in tissue paper, blended with some other material of known calorific
value. When calculating the combustion heat, the amount of heat produced by the auxiliary
material is subtracted from the result. Thus after taking about 1.0-1.5 g of the material, the
crucibles reweighed to the nearest 0.1 mg. The weight of the sample taken should be
sufficient to give a temperature rise of about 2-30C.
(II) Liquid fuel: In case of liquid fuel the sample is taken and weighed in a specially
made glass or gelatine capsules. The empty as well as filled capsules are weighed to the
nearest 0.1 mg. The capsule is then placed into the silica or platinum crucible already
containing the exactly weighed 0.2-0.3 g of firing oil. The firing oil capsules both have
saturated heat values.
b) Assembling the bomb: The crucible containing the sample is placed on the holding ring
protruding at the bottom of the bomb cover and the two poles are connected by a piece of
ignition wire of known weight. The wire has a loop of cotton wicking of known weight, to
make contact with the sample to be burnt. While calculating the calorific value, the amount of
heat released by the cotton wicking and the ignition wire is taken into account.

After introducing the sample, 10 ml of distilled water plus 10 ml of 3% H2O2 are

introduced in the bomb and the cover is made tight using spencer. The oxygen inlet opening
is connected to the charging equipment and the bomb is filled with oxygen until a pressure of
30 kg/sq. is reached. (Care is being taken while introducing oxygen into the bomb lest to
powerful gas stream should blow out the sample from the crucible.) After charging, the bomb
is disconnected from the charging equipment and the inlet opening is closed.

c) Assembling and calorimeter: The calorimeter vessel is filled with water of a temperature
lower by 2-30C than room temperature and the assembled bomb is immersed in it. The quality
of the water used in all tests should be same and so selected that it covers two-third parts of
the values on the bomb. The water is weighed directly in the vessel to the nearest 0.5 g. The
terminals on the calorimeter bomb are connected to a power supply unit through an insulated
wire. The calorimeter vessel is then placed in the thermostat properly and the latter is
covered. The Beckmann thermometer is now introduced and immersed in the calorimeter
water in such a way that the mercury container is at the half of the height of the bomb,
without the thermometer touching the vessel, bomb or stirrer. The stirrer is started with a
regulated speed. The apparatus is now ready for igniting the fuel.
d) Igniting the fuel and recording the temperature: In order to make correction for
radiation, Dickinson method of taking observation and calculating the results has been
approved by ASTM which enables us to determine the corrected initial and final
temperatures. The method is as follows:
1) In order to find out the rate of temperature change, before firing, in 0C/min, the
thermometer is read every minute, to the nearest thousandth parts of a centigrade, six times in
succession. Simultaneously with the sixth minute the sample is ignited and this time is
designated as time A.
2) Soon after firing the sample the main test starts and the thermometer is read to the
nearest of 0.0010C after every half a minute until the temperature rise ceases. This is
designated as time C.
3) In an after test the rate of cooling is recorded. Soon after the temperature has reached
to its maximum at time C. Cooling starts and again the thermometer is ready for another five
minutes recording the temperature every minute.

When the test has been concluded the calorimeter is dismantled. The bomb is opened and
examined for any unburnt sample and if found to be so, the determination is repeated.

In order to dismantle, the bomb is taken out of the calorimeter and the pressure released
gradually by opening the needle point valve and then only the lid or cover is unscrewed.

Note: (1) When extreme accuracy is required, the heat evolved due to formation of
HNO3 and H2SO4 should be accounted for. This is done by following the ASTM test
procedure the details of which are omitted here.

(2) The contents of the bomb after test may be used for sulphur determination.

e) Water equivalent: For all determinations a bomb calorimeter is first standardised by

finding out its water equivalent. For this a known weight of standard fuel of known calorific
value is burnt under exactly the same condition as in the determination with coal. A weighed
pill of any of the following substances is placed in the bomb and experimented upon.
Naphthalene Calorific value = 9622 Calories/kg
Benzoic acid Calorific value = 6322 Calories/kg
Then, if a = weight of material × calorific value
b = heating value of the fusion wire in calories
c = heating value of the titre
d = corrected rise in temperature
e = weight of calorimeter water in gram
and g = water equivalent of apparatus in gram
a+b+c
Then, g= -e
d

Thus the water equivalent is calculated.

Calculations

The following method for calculating radiation correction has been recommended by
ASTM.

R1 = rate of rise of calorimeter temperature in 0C/min before ignition.

A = the time at which the sample is fired.

B = the time B is defined as the time at which 60% of the total expected rise of
temperature has occurred. This is found out by calculating this temperature and finding out
the corresponding time from the observation table.

C = the time at which the temperature has reached its maximum.

R2 = the final rate of cooling in 0C/min

Corrected initial temperature: Multiply R by the time (B-A) nearest to 0.1 minute
and add this product (subtracted if the temperature was falling at time A) to the temperature
at A.

Corrected final temperature: R2 is multiplied by (C-B) and add this product

(subtracted it if the temperature at C) to the temperature at time C.

Result: The gross calorific value of the given fuel sample by bomb calorimeter is
found to be ............... calories/g.
 Experiment – 8
To carry out the % of moisture content only of a given sample of coal as a part of
proximate analysis.

Object of determination

The commercial value of coal is guided by proximate analysis which furnishes the
necessary data for its characterisation and evaluating its utility. In the course of a proximate
analysis the determination of the following constituents of coal is made:

1. Moisture
2. Volatile matter (V.M.)
3. Ash
4. Fixed carbon (F.C.)

Coal sample received from coal-beds contain considerable amount of moisture which
entails loss of heat energy, lowering thereby the calorific value of the coal. It is essential,
therefore, to estimate the percentage of moisture in the coal sample.

The residue left after burning coal sample is called ash. Ash is considered as impurity
consisting of inorganic matters which are intimately mixed with coal. It lowers the calorific
value of coal and hence greater the percentage of ash the poorer is the quality of coal.

On the basis of moisture and ash content the result of the proximate analysis of coal is
usually reported in the following manner:

a) As received basis (coal received from collieries)

b) Air dry basis (A.D. basis)
c) Moisture free basis (oven dry basis)
d) Moisture and ash free basis

In practice the air dry powdered coal sample is analysed in the laboratory. Fixed
carbon is obtained by subtracting from the quality from the quantity of coal, the percentage of
moisture, V.M. and ash. Carbon contributes much towards the heating value of a fuel. Thus a
higher percentage of ‘fixed carbon’ ascertains a higher calorific value.

Procedure

(1) Moisture: A well cleaned china crucible, ignited for constant weight, is weighed while
empty. About 1 g of air dried powdered coal sample is taken in the crucible from the sample
bottle and weighed quickly. It is then placed in an electric oven or over a low Bunsen flame.
The temperature in any case is restricted to 1100C for about 30-40 minutes. Now it is allowed
to cool down to room temperature in a desiccator for about 10 minutes and then weighed to
the constant weight.
(2) Volatile matter: About 1 g of the air dried sample is taken into a clean platinum or silica
crucible and weighed. The crucible is provided with a close fitting capsule cover and is of
known weight. It is then heated by placing in an electric furnace at 9500C, for exactly 7
minutes. Special furnaces are available for this purpose but otherwise the routine work can be
carried out by using a ‘Meker burner’ with artificial gas, placing the crucible 1 cm from the
top of burner. The lid of the crucible must fit snugly.

After heating it exactly for 7 minutes the crucible is removed from the furnaces and
cooled in a desiccator to room temperature and weighed.

Coals particularly high in volatile matter or moisture may cause the cover to pop out of
the crucible when treated as above. In such cases, the crucible containing the sample is heated
slowly over a low flame for not less than 5 minutes and not more than 10 minutes, thus
subjecting it to preliminary heating which causes the discharge of the volatile matter at a rate
not sufficient to cause sparking. After this the crucible is transferred to the furnace and heated
for 6 minutes at 9500C and weighed as in the regular cases.

(3) Ash: A well cleaned platinum or silica crucible is ignited for constant weighed. About 1
g of the air dried sample is taken in the crucible and weighed again. Sample is then placed in
a muffle furnace maintained at 7500C and heated for 40 minutes. Then it is taken out and
allowed to cool first outside and then in a desiccators to room temperature. The crucible is
weighed. It is heated again with ash in for further 10 minutes and weighed after cooling till a
constant weighed is obtained.
(4) Fixed carbon: This is determined by the method of difference i.e. by subtracting from
100, the sum of the percentage of moisture, V.M. and ash.

Observations: (Illustration)

(1) Moisture:
Weight of crucible =Wg
Weight of crucible + coal = (W + 1.0) g
Weight of coal sample = 1.0 g
Weight of crucible + coal (after heating) = W + 0.99 g
Therefore, weight of moisture = 0.01 g
(2) Volumetric matter:
Weight of coal sample = 1.0 g
Weight of sample (after heating) = 0.94 g
Therefore, weight of moisture + V.M. = 0.06 g
Therefore, weight of V.M. (0.06 – 0.01) g = 0.05 g
(3) Ash:

Weight of coal sample = 1.0 g

Weight of sample after ignition = 0.10 g
Therefore, weight of Ash = 0.10 g
Calculations

(A) Air dry basis:

0.01× 100
I. Moisture = = 1.0 %
1.0
0.05 × 100
II. V.M. = = 5.0 %
1.0
0.10 × 100
III. Ash = = 10.0 %
1.0
IV. F.C. = [100 – (1 + 5 +10)] = 84%
(B) Oven- dry basis:
I. Moisture = Nil
0.05 × 100
II. V.M. = = 5.05 %
(1 − 0.01)
0.10 × 100
III. Ash = = 10.1 %
(1 − 0.01)
IV. F.C. = [100 – (10.1 + 5.05 +10)] = 84.85%
(C) Moisture and ash free basis:
I. Moisture = Nil
0.05 × 100
II. V.M. = = 5.6%
1 − (0.01 + 0.10)
III. Ash = Nil
IV. F.C. = (100 – 5.5) = 94.4S%

Results: However, in the laboratory, for practical classes we find out the result on oven dry
basis and the result is reported as follows:

% of Moisture =..................................................
 Experiment – 9
To study the adsorption of acetic acid by activated charcoal from an aqueous
solution.

Apparatus required: Conical flasks, funnel, well cleaned and stoppered bottles (4
numbers), 25 ml pipette, 50 ml burette, two volumetric flasks (250 ml), and 100 ml
measuring cylinder.

Chemical required: Acetic acid (approx. 0.1N), NaOH (approx. 0.1N),

phenolphthalein indicator, activated charcoal.

Principle: Adsorption is a surface phenomenon. When charcoal powder is added to a

dilute solution of acetic acid, it is adsorbed on the surface of charcoal particles. Generally, the
adsorption increases with increase in the surface area on adsorbent (charcoal). Freundlich
gave the following relationship which is known as Freundlich isotherm.

x/m = KCn .......... (1)

Where, x is the mass of substance adsorbed (adsorbate), m is mass of adsorbent, C is

the equilibrium concentration of the substance (adsorbate), K and n are constants which
depends on the nature of the adsorbent and adsorbate and on the temperature.

Taking logarithm of eq. 1,

log (x/m) = log K + n log C .............. (2)

A plot of ‘log (x/m)’ against ‘log C’ is a straight line with slope equal to ‘n’ and
intercept to ‘log K’.

Procedure

1. Weigh 1.575 g (W) oxalic acid (eq. Wt. = 63) and dissolve in 250 ml.
2. Prepare 250 ml NaOH solution by dissolving 8-10 pallets of NaOH. Take 25 ml
oxalic acid solution by pipette in a conical flask, add 1 drop phenolphthalein indicator
in it and titrate with NaOH (from burette) till colourless to pink colour change occurs.
3. Take 25 ml supplied acetic acid solution by pipette in a conical flask, add 1 drop
phenolphthalein indicator in it and titrate with NaOH (from burette) till colourless to
pink colour change occurs.
4. Take 0.5 g of activated charcoal in each Stoppard bottle marked as ‘1’, ‘2’, ‘3’, and
‘4’ (use balance for weighing). Then, add acetic acid and distilled water in the bottles
as per following ratio; bottle 1-100 ml acetic acid and 0 ml distilled water, bottle 2-75
ml acetic acid and 25 ml distilled water, bottle 3-50 ml acetic acid and 50 ml distilled
water, bottle 4-25 ml acetic acid and 75 ml distilled water. Keep the bottles on a
mechanical shaker and shake it for 45 min.
5. After 45 min of shaking, filter the solution in the bottles and collect the filtrate in four
different conical flasks.
6. Take 25 ml of filtrate, obtained from bottle 1 filtration, by pipette in a cleaned conical
flask, add 1 drop phenolphthalein indicator in it and titrate with NaOH (from burette)
till colourless to pink colour change occurs. Follow the same procedure for the filtrate
of bottle 2, bottle 3 and bottle 4. Volume of NaOH consumed are V1 ml, V2 ml, V3 ml
and V4 ml, respectively.

Results and calculations:

1. Preparation of oxalic acid solution:

Weight of empty tube = W1 g

Weight of empty tube + oxalic acid = W2 g

Weight of empty tube after transferring oxalic acid = W3 g

Weight of oxalic acid taken (W2 - W3) = W g (say)

Strength of 250 ml oxalic acid solution = W / (63 × 0.250) = ‘p’ N (say)

2. Standardisation of NaOH with oxalic acid

Volume of oxalic acid used, Volume of NaOH used, ml Concordant reading,

ml ml
25 V5 V6 (say)
25 .......
Strength of NaOH = (25 × p) / V5 = ‘q’ N (say).

3. Strength of supplied acetic acid

Volume of acetic acid used, ml Volume of NaOH used, ml Concordant reading,

ml
25 V5 V6 (say)
25 .......
Strength of supplied acetic acid = (V6 × p) / 25 = ‘r’ N (say).

4. Calculation of adsorbed acetic acid an charcoal

Temperature = ..........0C
 Bottle Weight Strength of Strength of Change in Amount of log log
no. of CH3COOH CH3COOH strength of CH3COOH (x/m C
charcoal before after CH3COOH adsorbed )
(mg) adsorption adsorption due to (‘x’ g)
(mole L-1) (‘C’ mole adsorption [100 ml
L-1) (mole L-1) solution]
1 r (V1 × q)/25 s1 - t 1 [60(s1 - t1)]
= ‘S1’ (say) = ‘t1’ (say) / 10
2 (75 × r) / (V2 × q)/25 s2 - t 2 [60(s2 - t2)]
100 = ‘t2’ (say) / 10
= ‘S2’ (say)
3 (50 × r) / (V3 × q)/25 s3 - t 3 [60(s3 - t3)]
100 = ‘t3’ (say) / 10
= ‘S3’ (say)
4 (25 × r) / (V4 × q)/25 s4 - t 4 [60(s4 - t4)]
100 = ‘t4’ (say) / 10
= ‘S4’ (say)

5. Plot a graph of log (x/m) against log C on a graph paper.

From the plot, log K = intercept and n = slope
 Experiment – 10
Determination of Total Dissolve Solids (TDS) of given samples by Digital TDS
meter & conventional method.

Introduction

Digital TDS meter is a solid state instrument designed to provide the precise
conductivity measurement. The instrument is ideal for monitoring salt contents a natural
water, drinking water, treated water, brine solution, sea water and soluble salt in soils. A
multi position selector switches quickly sets the digital display to the desired test range. The
LED display is easy to read even in the dark. The use of the solid state I.C. circuitry makes
the model versatile and reliable. The instrument is extremely useful for agriculture and soil
analysis laboratories, swimming pools, water quality control in boiler feed water, water
works departments, fertilizer plants, petroleum refineries, transport undertakings, breweries,
textiles plants, rayon and silk mills etc. The conventional method is used on dry weight basis
as deposited after evaporation of liquid.

Object of determination

A TDS cell dipped in a measuring solution is placed in the inverting input path of a
operational amplifier when AC voltage of constant amplitude and suitable frequency is
applied to the system then for a given feedback resistance Rf., the account is linearly
proportional to the conductance of the solution. The conductance value is normally required
to be multiplied by the cell constant to convert into conductance (as per the provision already
exists in the instrument to displayed on 3.5 digit display). This indicates directly, the TDS of
the solution under measurement referred to the reference measurement i.e. 250C. The utility
of the conventional method is verify the result as obtained from Digital TDS meter.

Description of Apparatus

Digital display: A 3.5 digit LED display that reads TDS value of any aqueous solution.

Function switch: This is a 3 position switch.

1. In the TDS position it measures total TDS.

2. In the CHECK position the display will read 1.000.
3. In CELL CONST. Position, display reads cell constant value.

Cell constant: This control is used for cell constant compensation.

Back panel controls

ON/OFF: This switch is used to make the instrument.

CAL Control: When function switch is at CHECK, position adjusts 1.000 on display by
CAL control.

Input Connections: Two banana sockets at the back are the input of the instrument. The
TDS cell leads fitted with banana plugs is connected to these banana sockets.

Fuse: 100 mA fuse is over current protection.

1. Wash the conductance cell thoroughly with distilled water (before use the cell should
be kept in distilled water for 24 hrs)
2. Fit the electrode leads to the input sockets at the rear of the instrument.

Calibration of the Instrument

The following procedure is to be adapted to CALIBERATE the instrument with

measuring cell:

1. Take a standard solution of known TDS at 250C in a beaker and dip the cell into the
solution.
2. Set the ‘Range’ switch within range of the standard solution.
3. Switch the ‘FUNCTION SWITCH’ to the CHECK position and see that the display
reads 1.000 if not, set it with (CAL) which at the back of the instrument.
4. Set the function switch TDS position and bring the display to the reading corresponding
to the known TDS by means of the CELL CONSTANT check the cell constant value. If
it does not match the value marked on the cell.

Please mark new CELL CONST. value on the TDS cell. The instrument is
calibrated and can be used to determine the TDS of unknown solution.

TDS MEASUREMENTS

To measure the TDS of any solution proceed as follows:

(A) Rinse the cell with solution whose TDS is to be measure.

(B) Dip the TDS cell in the solution under test.
(C) Set the FUNCTION SWITCH to CHECK position.
(D) Display must read 1.000, if not set it with CAL control at the back panel.
(E) Set the CELL CONSTANT control to the cell constant value of the TDS cell.
(F) Set the FUNCTION switch to TDS position.
(G) Connect the TDS cell at the rear of the instrument.
(H) Set the temperature control to the actual temperature of the solution under set.
(I) Bring the RANGE switch at a position where maximum resolution is obtained.
(J) Read the display, this will be the exact TDS at 250C.
Standard TDS reagents
Dissolve 0.5232 g KCl dried at 1800C for 1 hour in distilled water and dilute to 1000
ml. The distilled water used for preparing standard solutions should have a very low
conductivity. The specific conductance if this solution at 250C is 140 µs/cm.

The TDS value of 1000 µMhos/cm solution is approx. 650 ppm (mg/1).

Cell constant verification

Checking the cell constant as per the following pressure is recommend before any
measurement:

A. Set the ‘FUNCTION’ switch to CHECK position and adjust the display 1.000.
B. Dip the cond. cell in a solution of known value and adjust the temperature control into
the actual temperature of the solution.
C. Move the FUNCTION switch to TDS. Position and range switch appropriate value of
the solution.
D. Adjust the cell constant knob so that the display reads the known value the solution.
E. Bring the FUNCTION switch to CELL CONSTANT position.
F. The display shows the cell constant of the TDSA cell.

Care of TDS cell

After the use the cond. cell must be thoroughly washed or immersed in distilled water.
The cell may be washed by cleaning it in 90% detergent solution and scrubbing it with very
fine brush. For more tenacious deposits, 2% solution of HCl may be used. Utmost care must
be kept so that ‘Platinization’ of the electrode is not damaged.

Observation Table & Results:

S. No Sample TDS Result

Convetional Method

Measurement:

Weight of empty crucible = W1 g

(After that put 15-20 ml liquid in the crucible whose Total Dissolved Solid needs to
be measured)
Weight of empty crucible + deposited solids = W2 g
(After evaporated to dryness & cooled in room temperature)

Weight of Total Dissolved Solid (W2 – W1) =Wg

Calculations:

Say, in 15 ml liquid contains Total Dissolved Solid = W g


∴ 1000 ml liquid contains Total Dissolved Solid = × 1000 g


Result: ............................................. mg/L or ........................ppm.

 Experiment – 11
Determination of Turbidity of given samples by Digital Turbidity
meter/Nephelometer.

Introduction

Clarity of water is important in producing products destined for human consumption

in may manufacturing uses, brewer age production, food processors and treatment plants.
Drawings of the surface water supply commonly rely on coagulation, setting and filtration to
ensure an acceptable product. The clarity of a natural body of water is a major determinant of
the condition and productivity of that system.

Turbidity in water is caused by suspended matter such clay, slit finely divided organic
compounds and plankton and other microscopic organisms. Turbidity is an expression of
suspension in the sample. Optically black particles such as those of activated carbon may
absorb light and effectively increases turbidity measurements.

The Digital Turbidity Meter is a very accurate and stable instrument for measurement
of turbidity up to 1000 NTU and 200.

CONTROLS AND SERVICES

DISPLAY: 3.5 digit, bright red LED display for accurate reading of turbidity.
TEST TUBE HOLDER: The test tube holder keeps the test tube containing solutions to be
tested.
RANGE SWITCH: It is a two position selector switch with 200 and 1000 NTU range. The
resolution of the instrument is 1 NTU and 20 - 200 NTU range.
SET ZERO: This control is used to set Zero of the instrument when a black solution (say
distilled water) in the test tube is kept in the test tube holder.
CALIBRATE: This control is a 10 turn pot for calibration of the instrument to adjust
standard value.
ON/OF SWITCH: This is a two position toggle Switch used to Switch ON the power to the
instrument at the time of its use. The instrument must be switched OFF when not in use.
TEST TUBE HOLDER COVER: The cover of the test tube holder prevents external
COVER light to enter the solution under test.

OPERATING INSTRUCTION
Instructions

a) Take out your Digital Turbidity Meter and accessories from the card board box.
b) Check all the accessories and if there is any discrepancy, kindly report to the concerned
dealer or the company immediately.
CALIBRATION

Reagent preparation

Turbidity free water: Turbidity free water is difficult to obtain. The following method is
satisfactory for obtaining turbidity as low as 0.02 NTU. Pass distilled water through a
membrane filter having precision-size holes of 0.2 mm, the usual membrane filter used for
bacteriological examinations is not satisfactory. Rinse collecting flask at least twice with
filtered water and discard the next 200 ml, filtered water. Some commercial bottled
demineralised waters are nearly particle-free. These may be used their turbidity is lower
than that can be achieved in the laboratory.

Stock turbidity suspension:

1. Solution-I: Dissolve 1.000 g hydrazine sulphate (caution: carcinogen; avoid inhalation,

ingestion and skin contact) (NH2)2 H2SO4 in distilled water and dilute to 100 ml in a
volumetric flask.
2. Solution-II: Dissolve 10.00 g hexamethylenetetramine, (CH2)6N4 in distilled water
and dilute to 100 ml in a volumetric flask.
3. In 100 ml volumetric flask mix 5 ml solution I and 5 ml solution II. Let them stand for
24 hrs at 25 ± 30C dilute to mark with distilled water to 100 ml and mix. The turbidity
of suspension is 400 NTU.
4. Prepare the solutions and suspension weekly.

STANDARD TURBIDITY SUSPENSION

Dilutions of other values can be prepared from this 400 NTU solution by the
following successive dilution method:

Solution Suspension, ml Distilled H2O, ml

200 NTU 50 50
100 NTU 25 75
CALIBRATION
1. Switch ON the instrument and keep it ON for some time.
2. Select appropriate range depending upon the expected turbidity of the sample.
3. Set zero of the instrument with turbidity free water using a blank solution adjust 000
with the “set zero” knob.
4. Now in another test tube take standard suspension just prepared as described given
above table. For 0-200 NTU range use 100 NTU solution and for higher range use 400
NTU solutions as standard.
5. Take its measurement and set the display to the value of the standard suspension with
the calibrate knob.
6. Now the instrument is steady to take measurement of any solution of unknown
concentration.

INTERFERENCES
1. Turbidity can be determined for any water sample that is free of debris and rapidly
settling coarse sediments.
2. Dirty glassware or the presence of air bubbles disturb the surface visibility of the
sample and will give false results.
3. “True colour” i.e. water colour due to dissolved substance that absorb light causes
measured tepidities to be lowest.
4. This effect usually is not significant in the case of treated water.

OPERATION
1. Allow sufficient warm up period after switching ON the instrument.
2. Take the test tube containing distilled water or blank solution in the test tube holder and
close the test tube holder cover. Make sure that the mark on test tube coincides with the
mark on the panel.
3. Select the required range for measurement.
4. Adjust the display to 000 by adjusting ‘set zero’ knob.
5. Remove the test tube containing distilled water and fill another test tube containing
standard solution say 400 NTU as per the expected range of unknown solution. Place it
in the test tube holder.
6. Take the measurement of the solution suspension and adjust the ‘calibrate’ knob so that
the display reads the selected standard solution value.
7. Again check the display zero with the test tube containing distilled water.
8. Now the instrument is ready measurement of any unknown suspension.

Note: Please ensure that the appropriate range is selected.

Observation Table & Results

S. No Sample Nephelometer Result

PRECAUTIONS

1. Sample test tube must be thoroughly cleaned both inside and outside. In case the test
tube gets scratched or etched, discard it.
2. Do not touch the test tube where the light strikes i.e. at the sides of the test tube. So
hold test tube only at the top end.
3. Fill the test tube with samples or standards which have been thoroughly agitated.
4. Please ensure that the mark on the test tube coincides with the mark on the instrument
panel while taking the readings.
 Experiment – 12
Determination of Dissolve
Dissolved Oxygen in water by Dissolved Oxygen Meter
M
method.

Introduction

Dissolved Oxygen (DO) in water is an index of physical and biological processes

going on; non-polluted
polluted surface waters are generally saturated with dissolved oxygen.
oxygen There
are two main sources of dissolved oxygen in water:
1. Diffusion from air/absorption from air
2. Photosynthetic activity within water by vegetation etc.

Diffusion of air from air water is a physical phenomenon and is influenced by factors
which affect the oxygen solubility, like temperature, water movement and salinity etc.
Photosynthetic activity
y within water is a biological phenomenon carried out by autotrops
(mainly phytoplanktons in water) and depends upon autotroph population, light conditions
and available gases etc.

Oxygen is considered to be a limiting factor, especially in lakes and in waters with a

heavy load of organic material. Organisms have specific oxygen requirements. Low
dissolved oxygen may prove fatal for many organisms for their survival.

Oxygen meter method: This method is convenient, quick and reasonably accurate.

Measuring Dissolved Oxygen (DO)

The concentration of dissolved oxygen in water can be measured by dissolved oxygen

meter method, which requires no calculations, is using a dissolved oxygen meter and the
working function is shown in the figure.

Figure 1: Working function of Dissolved Oxygen Meter

 Figure 2: Dissolved Oxygen Meter

A Dissolved Oxygen meter consists of a probe filled with potassium chloride and
covered with a semi-permeable membrane, a wire carrying electricity and two electrodes.
When the probe is placed in the water, the potassium chloride attracts oxygen, just as
haemoglobin does in our blood and pulls the oxygen out of the water and into the probe. The
semi-permeable membrane allows oxygen to pass into the probe but does not allow water in.

The probe is connected to a wire through which DC electricity flows (the red dashes in
the drawing above). There is a gold and a silver electrode on the wire, one on either side of
the probe. These electrodes as devices which measure the amount of electricity passing
through the wire at that point.

Where the probe joins the wire, oxygen mingles with the electricity. Oxygen is not
very ionized, meaning that it does not have a negative charge as electricity does, so the
oxygen dilutes the current at the electrode beyond the probe. The meter measures the
difference in current between the two electrodes and uses that difference to determine the
amount of oxygen in the water.

When using a DO meter, the meter must be properly cared for. The membrane must be
kept wet and have potassium chloride solution within it at all times. The electrode should
also be maintained. The electrode assembly can be cleaned by dipping the electrode tip into
ammonium hydroxide.

The meter must also be calibrated before use to ensure that the reading is accurate. The
meter can be calibrated using water with a known concentration of DO at set temperature.
This can be done by filling a biological oxygen demand (BOD) bottle halfway full of
distilled water. The water is shaken vigorously to saturate the water with air. Then the probe
is placed in the bottle and the reading is adjusted to the known concentration of DO in the
bottle.

Result: ..............................................................