Indian Institute of Technology Ropar

Department of Chemistry

Laboratory Manual
CY101 Chemistry for Engineers (3-1-2-4)
B. Tech First Year

1
Introductory remarks
All students are required to attend all laboratory sessions. Students must come on time to avoid
missing the introduction to the experiment (around 15 to20 min) given by the instructor. Zero
marks will be recorded for each missed Class. One turn will be given at the end of the scheduled
experiments to make up for one missed experiment in case of sickness or similar reasons with the
approval of the instructor/coordinator.

The 14 weeks in the semester will be used as follows:

1st week: general instructions to be given by the teacher regarding the course, laboratory manual,
lab reports, safety in the laboratory and distribution of marks.
2nd to 12th week: experiments 1-11
13th week: repeat turn for sick leave cases
14th week: lab test

There will also be a common quiz at the end of the semester

There will be a laboratory handout of each instructor. Students must come with a lab note book in
which experimental observation and readings are to be note down and readings should be counter
signed by the instructor / tutor on the day of experiments. Calculation / graphs and final results
should be shown to the instructor during the next laboratory class.
Instructors are advised to bring to the attention of the coordinator the names of students who do
not comply with these instructions or miss lab classes without valid reasons

Safety in the Chemistry Laboratory

It is very important that you are completely familiar with the experiment. Before beginning, the
experimental details should be carefully read and use the correct techniques demonstrated and
discussed by the instructor / lab staff. The best precaution against accident is a well-prepared
experiment and a neat and well organized laboratory bench. Planning your experiments in
advance not only minimizes accidents but also makes your work proceed more rapidly and
smoothly. Safety rules should be followed strictly. The excuse that someone else is responsible
for mistake / accidents is never acceptable in a scientific laboratory. The following regulations are
an absolute necessity for a safe laboratory. Please read them carefully. Since there are personal
hazard risks associated with non – compliance (fire explosions, burns etc.), you may be asked to
leave the laboratory immediately if you don’t follow these rules.

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1. Report any accidents immediately to your instructor or laboratory staffs
2. No eating or drinking in the laboratory.
3. Do not sit on the bench tops.
4. It is mandatory to wear a protective lab coat to prevent damage to your clothing or skin from corrosive
chemicals (Avoid wearing flowing and costly clothes in the laboratory). Use covered footwear (shoes, sneakers
etc.) in the laboratory. No sandals, high heeled shoes or bare feet will be permitted. Students are strongly
advised to use a good quality safety goggle while at work. In majority of cases the best emergency
treatment for chemicals that enter the eye is to wash the injured eye with copious quantities of water.
5. Long hair must be tied back. It is advisable to minimize the use of hair sprays and other hair products,
because they are highly flammable.
6. Contact lenses should never be worn in the laboratory.
7. Be aware of the location of the safety shower, eyewash station, fire extinguisher, first aid equipment, and
the exits.
8. Know the hazardous properties of the chemicals you are using. Specific instruction for dealing with
hazardous materials will be given by the instructor to their use. When in doubt ask!
9. Use only those chemicals which are required in your experiment. Make sure that you know what chemicals
you are looking for. Many chemicals have similar names or formulas, treat all chemicals as hazardous.
10. Flammable liquids and toxic chemicals should be disposed off in the waste disposal container provided.
11. All chemicals should be considered potentially toxic therefore never taste a chemical or solution or bring
eatables into the laboratory. If you are asked to smell a chemical, gently fan the vapours towards your nose.
Wash thoroughly your hands with soap after every lab session before touching any food stuff. If any chemical
stain remains on your hand, use spoon to eat till the stain goes off.
12. Do not keep any organic solvents near a Bunsen burner. If there is a fire of any sort, report to your
tutor/instructor immediately and follow his /her directions.
13. Do not lean on the workbench while working. While using ammonia, remember to keep the exhaust fans
on. The same is applicable if any noxious fumes are evolved during a reaction. If you have accidentally taken
inside your mouth any solution, wash your mouth immediately with lots of water and contact immediately your
instructor or tutor for further help.
14. If any acid or base fall on your hand, immediately wash with lots of water and contact your tutor if there is
any uneasiness. While heating solutions over the flame make sure that the mouth of the vessel is not directed
towards you or others working nearby.

No cellular phones allowed. These are strictly forbidden and no exceptions to this rule

Be fully alert on what you are doing and what is going on around you while working in the laboratory.

In all cases of accident or injury, no matter how slight, report to the instructor or lab staff immediately. While
the emphasis should be on the prevention of accidents, a high priority is placed on personal safety in the event
of an accident.
3
 General introduction
How to use a burette: The burette should be washed thoroughly before use. When mounting the
burette, make sure that it is clamped vertically and the tap is on your right side. It is then filled up to
the zero mark and the nozzle is filled by opening the tap for two or three seconds. The reading of the
bottom level of the meniscus is taken. The tap is held by left hand (Thumb and forefinger). The flask
containing the solution is held in the right hand. During the titration, the solution is added slowly
from the burette and the flask is whirled with right hand. The burette after use should be emptied and
washed thoroughly with water before leaving the lab.
How to use a pipette: The pipette should be thoroughly washed before use. Hold the pipette in the
right hand and keep your fore – finger free. Suck the liquid, till the liquid level reaches a little above
the mark. Take it from your mouth and close the top with your fore- finger. The Pipette is then raised
at our eye-level and by controlled release of the fore-finger: the liquid level is adjusted to the mark.
The lower end of the pipette is then introduced into a conical flask and by removing the fore- finger;
the liquid can be drained off. A little liquid will remain there in the tip and no attempt should be made
to remove because the required volume has already delivered in the flask.
How to use a standard measuring flask: Standard flask is a narrow necked flask fitted with a glass
stopper. A weighed amount of the substance is usually transferred to it by using a funnel. The funnel
and its stems are washed down into the flask. The funnel is removed and the substance is then
dissolved by giving a rotating motion to the flask. Water is then added to it till the lower water
meniscus coincides with the mark on the standard flask. The flask is then closed and shaken well till
the solution gets a uniform concentration.
End point: The end point of a titration is the point at which complete reaction takes place between
two solutions. The end point is usually determined by using an indicator which shows a marked color
change at the point completion of the reaction.
Indicator pH range Color in acid solution Color in alkaline
solution
Methyl orange 3.1 to 4.4 Red Orange
Phenolphthalein 8.3 to 10 Colorless Pink

1. All apparatus should be extremely clean to start with. Test tube, beakers can be cleaned with soap
powder with a semi micro brush. At the end of the day’s work, you must clean all the apparatus and
return to the lab staff.
2. Dropper containing the reagents should not be allowed to touch on the sides of the test tube during
addition. Reagent drops should be allowed to fall directly into test tube without touching the sides;
otherwise the reagent bottle will get contaminated.

4
 PART-I
List of Experiments
1. Chemical Kinetics – Acid hydrolysis of ethyl acetate

2. Potentiometric titration using a pH meter

3. Conductometric titration

4. Partition coefficient

5
 Experiment 1

Chemical Kinetics – Acid hydrolysis of ethyl acetate

Kinetics and thermodynamics are two topics associated with all chemical reactions. Kinetics is the
study of the rate at which (and the path by which) a chemical reaction occurs while thermodynamics
deals with the extent to which the reaction occurs. There is no necessary connection between the rate
measured by a rate constant k, and the extent, measured by an equilibrium constant Keq.

Rate of reaction

The reaction rate defines how the concentration of a reactant or product changes with time. The
rate is defined to be a positive number. If we consider a reaction such as

A+ B C+D

We can find out how the concentration of A, B, C and D, change over time. The average reaction rate
is therefore given by the simple expression

Average reaction rate = change in concentration/ change in time [rate = ∆[C] /∆T]

Since the rate of production of C is the same as the rate of production of D (One molecular of D is
produced when one molecule of C is produced), and is the negative of the change in A and B(for each
molecule of C, one A and one B get used up), we also have

Rate = ∆[C] /∆T = ∆ [D] /∆T = -∆ [A] /∆T = -∆ [B] /∆T

Rate constants and order of a reaction

The rate of a reaction can be expressed in terms of the concentrations of the various species. In
general, the higher the concentration of the reactants, the faster is the reaction.

For a general chemical reaction of the type

aA +bB products

The rate expression has the form

Rate = k [A]m [B]n

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k is the rate constant for the reaction, [A] is the concentration of A, [B] the concentration of B, m is
the order of the reaction with respect to A and n is the order of the reaction with respect to B. The
overall order of the reaction is the sum of m and n. If the power m or n is zero, then the reaction is 0
th order in that species; m or n = 1 means the reaction is first order and 2 means 2nd order, and so on.
For example, if a reaction has the rate expression rate = k[A]²[B]¹. The reaction is 2nd order in A, 1st
order in B and overall the reaction is third order. Thus if a reaction between two reagents display
second order kinetics, it means that both species are involved in the rate determining step of the
reaction. In other words, the structure of the transition state must contain both reactants.

One method for determining the order of a reaction is to plot the rate of the reaction versus
concentration and observe the nature of the plot obtained. For a zero order reaction, one will observe
a line parallel to the x axis, while for a first order it will be a straight line passing through the origin
and for the second higher orders, a curve. One can also plot log of rate against log of concentration
and obtain a line whose slope will correspond to the order of the reaction [log-log plot].

First order reactions:

Consider the reaction

A products

Let the initial concentration of the reactant A for this reaction be ‘a’ gram moles/liter, out of which
‘x’ gram – moles/liter is converted into products in time ‘t’ seconds. Thus after time ‘t’ from the
beginning of the reaction, the concentration of the reactant will be (a-x) gram- moles/liter. The rate of
the reaction at this instant will be given by

dx/dt = k (a-x)

Integrating this equation within the time limits t = 0 and t = t and using the fact that when

t = 0, x = 0. We get

This the equation which gives the rate constant for a first order reaction

Unit of k is reciprocal of unit of time [secˉ¹, minˉ¹) and k is independent of the units of the
concentration.

The hydrolysis of ethyl acetate can be catalyzed either by acid (for e.g. dil HCl) or base (e.g. NaOH).
The acid catalyzed reaction can be represented as follows

7
This reaction is of first order as the concentration of water is in large excess and does not change
significantly during the progress of the reaction. It is thus a pseudo unimolecular reaction.

The base catalyzed reaction can be best represented as follows

This reaction is best investigated by mixing ester and sodium hydroxide in equivalent amount
(which means that the initial concentrations of both reactants are the same) at constant
temperature. Hence this reaction follows second order kinetics.

In this experiment you will determine the rate constant k for the acid catalyzed reaction

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Procedure:

Apparatus and chemicals: 2 flasks with corks, beakers, 0.5N HCl ethyl acetate, standard NaOH
solution, crushed ice

1. Measure 100 ml of 0.5 N HCl using a volumetric flask and transfer in to a clean and dry 250 ml conical
flask.

2. Keep a burette filled with standard NaOH (1N) ready for titration.

3. Keep a 250 ml conical flask ready containing 25 ml of distilled water and a few pieces of
crushed ice in order to arrest the reaction.

4. Add 7.5 ml of ethyl acetate using a burette to the flask, shake well and immediately withdraw
10 ml of the solution using a pipette.

5. This is immediately allowed to run into to the conical flask with crushed ice to arrest the
hydrolysis reaction. (Note the time t to the nearest second as the initial time to)

6. Add indicator (phenolphthalein, 1-2 drops), and titrate the acid solution as fast as possible
against standard NaOH solution taken in a burette. This volume corresponds to Vo.

7. Withdraw 10 ml of the solution from the reaction mixture after 10, 20, 30 and 40 min after to,
arrest the reaction with the crushed ice as given in step 5, add indicator, and titrate the acid
solution against standard NaOH. This will provide volumes V10, V20, V30, and V40.

8. The reading corresponding to V∞ is take as follows

25 ml of the reaction mixture is taken in a conical flask and suspended in a water bath at about
70 °C and left there for about 20 minutes so that the hydrolysis is complete. After the hydrolysis
is complete, the flask is cooled to room temperature and 10 ml of the solution from the flask is
withdrawn and titrated against standard NaOH solution using phenolphthalein indicator.

Confirm the V∞ volume cone again by keeping the flask at 70 °C for another 20 minutes

and repeating step 8. This is to ensure that the reaction was complete.

Calculations:

If Vo, Vt and V∞ are the titer values at initial time, at time t and at infinite time (indicating
completion of reaction), then the rate equation can be written as

k = 2.303 log (V∞ - V0)

t (V∞ - Vt )

Knowing the values of V0, Vt and V∞ calculate the rate constant k at various values of ‘t’. It will
be observed that the value of k remains almost constant indicating thereby that the reaction under
investigation is of the first order.

9
Graphical method can also be employed for calculating the k.

A plot of log (V∞ - Vt ) (y axis) against ‘t’ (x axis) will be a straight line whose slope will be equal
to –k/2.303. Therefore from the slope of the line, the value of k can be determined. Compare this
with the calculated values of k.

Note: Towards the end point of the titration, NaOH start to react with free ester and causes the
disappearance of the pink color obtained when excess of alkali has been added.

For further reading

1. A text book of practical physical chemistry, J Rose, Khosla publishing house, New Delhi1993

2. Senior practical physical chemistry, B.D. Khosla, V.C. Garg, A. Gulati, R. Chand and Co, New
Delhi

10
 Experiment 2

Potentiometric titrations using the pH meter

Analytical methods that are based on electrode potential measurements are termed as
potentiometric methods. In this experiment the pH meter will be utilized to measure potentials
and pH to carry out potentiometric titrations.

pH and its measurement

The pH of a substance is a measure of its acidity just as a degree is a measure of temperature. The
term pH means hydrogen ion exponent and is defined in terms of hydrogen ion activity ‘a’. When
we measure pH with a pH meter, we are measuring the negative logarithm of the hydrogen ion
activity, not its concentration.

pH = -log10 aH+ or 10-pH = aH+

The activity is the effective concentration of the hydrogen ions in that solution. It is to be noted
that for every decimal change in activity the pH changes by one unit. [Chemists use the term
activity to describe quantitatively the effective concentration of participants in equilibrium at any
given ionic strength. Activity is almost the same as concentration in very dilute solutions]

Electrodes

To measure potential one requires electrodes and absolute electrode potential of a single electrode
can be determined only with respect to a standard reference electrode. The electrode, which
responds to the species being analyzed, is normally called the indicator electrode. The reference
electrode has a fixed composition and a constant potential. There are two main types of standard
reference electrodes.

a) Primary reference electrode: The standard hydrogen electrode is the primary reference
electrode and its potential is taken as 0 volts. It consists of a 1 M solution of HCl with a Pt
wire having a platinized foil immersed in it. Through the solution, pure and dry H2 is passed
at 1 atm. However, this electrode is inconvenient to prepare and handle under normal
conditions and so secondary reference electrodes are often used in its place.

b) Secondary reference electrodes: There are many secondary electrodes such as Calomel
electrode (Hg/Hg2Cl2/KCl) and the Silver-Silver chloride electrode. The calomel electrode is
based on the reaction.

½ Hg2Cl2 (s) + e- Hg(l) + Cl-

The standard potential of this reaction is +0.268 V. However, if the cell is saturated with KCl at
25oC, the potential is + 0.241 V (This is because the activity of Cl- is not unity in a saturated
solution of KCl. The solution of saturated not only with KCl but also with Hg2Cl2 and the
saturation concentration of highly soluble KCl is well above 1.0 M and hence the potential is only
0.241 V). A calomel electrode saturated with KCl is called a saturated calomel electrode (S.C.E).

11
The advantage of using saturated KCl is that the concentration of Cl- does not change if some
liquid evaporates. Although calomel reference electrodes were popular, these days due to the
mercury toxicity, they are replaced by safer electrodes such as the Silver – silver chloride
electrode. The Silver – silver chloride is based on the reaction.

AgCl(s) + e- Ag(s) + Cl-

The standard reduction potential for AgCl | Ag couple is + 0.222V at 25oC. But as it is kept in a
saturated KCl solution, due to reasons mentioned above, the potential of the electrode is + 0.197
V with respect to standard hydrogen electrode.

The Glass electrode

To determine the pH value or [H+] for a solution, we shall need an electrode reversible to H+
ions. In pH meters glass electrode as an indicator electrode is employed for this purpose. A glass
electrode has an electrode membrane made of special glass that responds to pH. The property one
seeks for this glass material is that it must generate a potential that accurately corresponds to the
pH of the solution and even though it must be accurately corresponds to the pH of solution and
even though it must be accurately sensitive to acidity and alkalinity, it must not be damaged by
them. The glass membrane is normally made of special glass with an approximate composition of
72% SiO2, 22% Na2O and 6% CaO. This type of glass has the desirable properties of low melting
point, relatively high electrical conductivity and a hygroscopic nature. This material is good for
the pH range 1-9. However in solutions of high alkalinity this electrode gets subjected to an
‘alkaline error’. Nowadays lithium based glasses are exclusively used for hydrogen response glass
electrodes required for use at high pH values.

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Glass electrode may be used in solutions containing oxidizing or reducing substances, colloids or
biological fluids. The determination of hydrogen ion concentration depends upon the fact that
when a thin glass membrane is in contact with solutions having different hydrogen ion
concentration on its two sides, a difference of potential is developed across the membrane. The
magnitude of the potential difference depends on the difference in the concentrations of the
hydrogen ions in the two solutions.

Glass electrodes are now available as combination electrodes which contain the indicator
electrode (a thin glass bulb) and a reference electrode (silver-silver chloride) combined in a single
unit as shown in the figure. The thin glass bulb and the narrow tube to which it is attached are
filled with hydrochloric acid (normally 0.1 M) and carry a silver-silver chloride electrode. The
wide tube is fused to the lower end of tube B and contains saturated KCl solution which is also
saturated with silver chloride. It carries a silver-silver chloride electrode E. The assembly is sealed
in an insulation cap through which the two leads from the electrodes are taken. The line diagram
of this cell can be written as follows.

Provided that internal hydrochloric acid solution is maintained at constant concentration, the
potential of the silver- silver chloride electrode inserted into it will be constant and so too will be
the potential between the hydrochloric acid solution and the inner surface of the glass bulb. Hence
the only potential which can vary is that existing between the outer surface of the glass bulb and
the test solution in which it is immersed. Therefore the overall potential of the electrode will be
decided by the hydrogen ion concentration of the test solution.

Potentiometric titrations

The determination of the equivalence point of titrations based on potential measurements is called
potentiometric titrations. The electrode potential of an electrode depends upon the concentration
of its ions in the solution. Hence, the potential of an indicator electrode goes on changing with
respect to a standard reference electrode by the change of the concentration of the ions during
titration. In other words, finding the difference in potential of the indicator electrode can be used
an indicator in volumetric titration. The equivalence point is indicated by a fairly large change in
potential. A good potentiometric titration requires a suitably selected indicator electrode and a
standard reference electrode. Since this is there with the pH meter, one can use the same for
potentiometric titrations.

The advantages of potentiometric titration over conventional methods are that these titrations are
applicable even to colored that turbid solutions, they are rapid and can be carried out in

13
microscale, the results are highly accurate and one also use the method for even weak acid- weak
base titrations.

Part A: Determination of hydrogen ion concentration and pH of a given solution

Procedure

1. Switch on the pH meter and allow the instrument to warm up for 10 min (this will be done by
the staff)
2. Set the temperature control to room temperature.
3. Insert the electrode assembly into the buffer solution.
4. Set the selector switch of the instrument to read pH.
5. Remove the electrode assembly, rinse in distilled water and place it back into the beaker
containing distilled water.
6. Measure pH of different solutions given to you and determine their hydrogen ion concentration.

Part B: To titrate a polybasic acid (H₃PO₄) against a base

Procedure

1. Take 25 ml of the given phosphoric acid in a beaker and measure pH as given in part A. Also
measure its potential.
2. Add known volumes of NaOH (from a burette) to it. Shake the mixture and measure its pH as
well as potential.
3. Continue the addition and measurement of pH (and potential) a little over the end point.
4. Plot pH (y- axis) versus volume of NaOH added (x-axis) and obtains the endpoint from the
graph. Also plot voltage (mV) versus volume and obtain the end point from the graph.
5. Explain the nature of the pH versus volume curve
6. How will you obtain the three dissociation constants from the titration plot? (hint : use the
Henderson Hasselbach equation, pH= pKa-log[acid]/[base].

For further reading

1. Quantitative chemical Analysis Daniel C. Harris 6th ed, 2003 W.H. freeman NY

2. Analysis using glass electrode P.W. Linder, R.G. Torrington, D.R. Williams, Open University
Press 1984, Universities Press (Belfast) Ltd.

3. pH measurements : C Clark Westcott, 1978 Academic Press NY

4. A text book of practical physical chemistry, J. Rose, Khosla publishing house, New Delhi
1993.

14
 Experiment-3
Conductometry
Determination of dissociation constants and titration using conductance of electrolytic
solutions

Many compounds wholly or partially dissociate into ions when dissolved in water. Although
water is itself a very poor conductor of electricity, the presence of ionic species in solution
increase the conductance considerably. The conductance of such electrolyte solution depends on
the concentration of the ions and also the nature of the ions present (through their charges and
mobilities). The electrolyte conductance of an electrolyte is measured using specially designed
conductivity cell (see figure) in which two plates of an inter material such as platinum or gold are
provided for the flow in and flow out of electrons. The resistance or conductance of an electrolyte
solution can be measured by immersing a conductivity cell in it. A simple commercial
conductivity cell comprises of two platinum electrodes mounted inside an open glass tube.

In this experiment you will use a conductivity cell to determine the dissociation constant of weak
electrolytes (e.g. acetic acid) and also determine the end points of reactions between electrolyte
solutions (e.g. neutralization of acids and alkalis)

Conductivity experiments:-

Electrolyte solutions obey Ohm’s law just as metallic conductors do. The resistance of any
conductor at a definite temperature varies directly as its length (l cm) and inversely as it cross
sectional area (a, cm2)

R =ρ(l/a)

Here ρ is a constant which depends on the nature of the material and is known as
specific resistance or resistivity of the material. The conductance G is defined as the
reciprocal of resistance and is expressed in Siemen (S), that is in Ohmˉ¹ or mho. The
conductance of a homogenous body of uniform cross section is proportional to the
cross section a and inversely proportional to the length l.

G= k(a/l)

Where k (kappa) is the reciprocal of resistivity and is called specific conductance or

conductivity. k=1/ρ and its units are S cmˉ¹. In other words one can say that specific
conductance is the conductance of one cm³ of the material.

k = l/a .Conductance. Or in order to obtain the value of specific conductance, the

measured conductance has to be multiplied by a certain factor known as the cell
constant.

k = cell constant x measured conductance.

15
The cell constant which is the effective value of l/a can be determined by measuring the resistance
of a cell filled with a solution of known conductivity. Often a 0.02 M solution of KCl is used for
this purpose which has a specific conductance equal to 0.002768 S cmˉ¹ at 25°C. One can also use
KCl solutions of comparable concentrations for the same.

Two other useful quantities which are handy when dealing with electrolyte solutions are the
molar conductance and the equivalent conductance since the conductivity of a solution
depends on the concentration and mobilities of the ions present.

The molar conductance Λ, is given by

Λ= 1000. k/C

Where C is the molar concentration of the electrolyte that is expressed in mol. dmˉ³.

1000 is the factor arising from the fact that 1 dmˉ³ =1000cmˉ³. Thus the molar conductance is
expressed in S.cm².molˉ¹. The molar conductance is described as the actual conductance of that
volume of solution which contains one mol of the solute when placed between parallel electrodes
1 cm apart with a uniform electric field between them.

In order to compare the conductances of electrolytes differing in its ionic composition or to

compare the conductivities of equivalent number of ions under similar circumstances the term
equivalent conductivity Λeq is used and is expressed in units of S.cm². eqˉ¹. For univalent ions it
is the same as S.cm². molˉ¹. The equivalent conductivity, Λeq is defined as the conductivity per
gram equivalent of the electrolyte. That is

Λeq = 1000. k/Ceq

Where Ceq is the equivalent concentration of the electrolyte (gram equivalent. dmˉ³).

Conductivity of strong and weak electrolytes

The variation of equivalent conductivity with concentration

shows different trends for weak and strong electrolytes. Strong
electrolytes like KCl dissociate completely into ions when
dissolved in water and therefore have relatively high equivalent
conductivities. At low concentrations, the equivalent
conductivity has been found to obey the following expression.

Λeq = Λ−A'∙ √C

[Λeq is Λo when C tends to zero]

Here Λo is the equivalent conductivity at infinite dilution and A' is a constant which depends on
the solvent, the temperature and the nature of the electrolyte (where it dissociates into singly and
multiply charged ions) and the value of Λo. The variation of Λeq with concentration is caused by
the interactions between the ions. A theoretical expression for A' was developed by Debye,
16
Huckel and onsager which agreed well with the experiments at low concentrations. The
significance of this equation is that it allows one to calculate Λo for strong electrolyte from
measurements of Λ at a series of concentrations. Kohlrausch demonstrated another important
property of the conductivities of strong electrolytes namely that at infinite dilutions the equivalent
conductivity of any electrolyte can be expressed as the sum of the contributions from individual
ions. This results from the independent migration of ions (as at infinite dilution they cannot
interact) and for an electrolyte this may be expressed as

Λo = Λ⁺+ Λˉ

Where Λ⁺ and Λˉ are the ionic conductivities of the individual ions.

Table: molar conductance of a few selected ions at infinite dilution (25°C)

Cation In S cm²molˉ¹ Anion In S cm²molˉ¹

H⁺ 349.8 OHˉ 197.8

Li⁺ 38.7 Clˉ 76.4

Na⁺ 50.1 Brˉ 78.2

K⁺ 73.5 Iˉ 76.8

NH4⁺ 73.4 CH₃COOˉ 41.0

This behavior may be explained by the dominant effect of the degree of dissociation (α) of the
electrolyte on its equivalent conductivity. α is related to the observed equivalent conductivity by
the Arrhenius expression

α = Λeq/ Λo

where Λeq is the equivalent conductivity of the electrolyte at any concentration and Λo is the
equivalent conductivity at infinite dilution.

The method employs a simple equilibrium expression, often referred to as Ostwald’s dilution law.
Consider the ionization of a weak acid such as acetic acid

H₂O+ CH₃COOH H₃O⁺+CH₃COOˉ

C(1-α) Cα Cα

By measuring Λ for a known concentration, one can evaluate Ka for an electrolyte since Ka =
(Cα)² / C(1-α) ; Ka = Cα² / (1-α) and hence 1/α = 1 + Cα/Ka

17
Conductometric Titrations

Since a measurement of conductivity with alternating current generally causes little electrolysis
and decomposition of the sample, it is an excellent means of speedy analysis and estimation.

Conductivity measurements are normally employed in monitoring rates of chemical reactions, in

estimating hardness of water and in soil and milk analysis etc. The equivalence point of a
chemical reaction in solution can be determined conductometrically, if there is a measurable
change in the conductivity at the equivalence point (note that you measure only conductance and
not conductivity). Acid base titrations in aqueous solutions are easily performed as the number of
speedy H⁺ and OHˉ ions are few at the equivalence point (see table). Even though the salt
produced by neutralization is present, the conductivity is a minimum when chemically equivalent
amount of acid and base are reacted. To minimize dilution effects, the added reagents (e.g. NaOH
in our reaction) are invariably concentrated.

When a weak acid or base is titrated, a sharp change (change of slope as shown in the figure), but
not a minimum in conductivity is produced at the equivalence point. The end point is deduced
graphically. The graphs below show the nature of some of the plots one observes from
conductometric titrations.

Part A: Determination of Cell constant

1. Set up the conductivity cell and make all electrical connections.

2. Take 25 ml of the given KCl solution in a 50 ml beaker and measure its resistance (or
conductance). Repeat the measurements two or three times and obtain the average reading.
18
Cell constant = specific conductance of KCl x resistance

Specific conductance of KCl solution at 25°C

Concentration Specific conductance [S or ohmˉ¹ cmˉ¹]

0.01M 0.001411

0.10M 0.012856

1.00M 0.111342

Part B: Determination of equivalent conductance, degree of dissociation and the

dissociation constant of a weak acid.

Prepare different concentrations of acetic acid such as 0.10M, 0.05M, 0.025M and 0.0125M and
measure the conductance using the conductivity cell.

Calculations:

(a) Calculate specific conductance for different concentrations.

(b) Calculate equivalent conductance for various concentrations.
(c) Calculate α for different concentrations of the acid and then Ka.
(d) Obtain Ka by plotting 1/α against c α and obtain Ka from the graph.

Since Ka = (Cα)² / C(1-α) ; Ka = Cα² / (1-α) and hence 1/α = 1 + Cα/Ka

Calculations

(a) Plot a graph between the conductance and the volume of titrant added for (i) strong acid
versus alkali (ii) weak acid versus alkali and (iii) BaCl₂ x MgSO₄.

(b) Determine the volume of alkali required for neutralization from the graph.

(c) Calculate the strengths of the acids and explain the shape of the different titration curves.

Plot 1/α against (Cα) and obtain Ka from the slope.

For further reading

1. Laboratory Techniques in electro analytical chemistry, P.T. Kissinger, W.R Heineman,

Marcel Dekker Inc, NY.1996
2. A text book of practical physical chemistry, J Rose, Khosla publishing house, New Delhi
1993 and Instrumental Methods of Analysis H.H. Willard L.L. Merritt, J.A. Dean, 4th ed,
Affiliated East West Press New Delhi.
19
 EXPERIMENT 4

Determination of partition coefficient of acetic acid in water and butanol.

Materials required : n-Butanol

Acetic acid 2N
Standardized NaOH 0.5N

Equipment and : Flat-bottomed bottle with ground stopper- 250ml

Special Glassware : Burettes and pipettes.

Partition Coefficient

If a solute is added to a system of two immiscible liquids such as oil and water, part of it will
dissolve in the oil and the rest in water. Provided that neither phase becomes saturated with the
solute, the ratio of concentrations in the two phases is approximately a constant at a given
temperature. The ratio may vary with concentration because of a number of factors, such as self-
association and partial mutual solubility of the two liquids. The partition coefficient
determinations are usually made at low solute concentrations. The ratio of concentrations of the
solute in the two phases is called the partition coefficient or distribution coefficient, K.

Most partition coefficients are determined between a non-aqueous (C1) and an aqueous phase
(C2), and by convention, the partition coefficient is expressed with the concentration in the non-
aqueous or lipophilic phase as the numerator. If a particular solute is in contact with the two
layers of a solvent so that when equilibrium is attained, both the liquid layers are saturated with
the solid substance, then the distribution law gives

K = C1 = S 1
C2 S2
where S1 and S2 are the saturation solubilities of the two substances in the two liquids.

20
An important point to remember is that the partition coefficient relates to the same

molecular species in each phase. For example, some carboxylic acids such as benzoic acid can
associate, through hydrogen bonding, in the non-aqueous phase, and can partially dissociate to the
ionized species in aqueous solution. Clearly, the absolute concentrations of RCOOH in the two
phases vary with the extent of association and dissociation, but the true partition coefficient is
independent of these factors.

The concept of the partition coefficient is applied in pharmaceutical and health care
industries in a variety of ways, including solvent extraction of drugs and dosage forms. Perhaps
thy greatest significance of partitions to pharmacy is the drugs are absorbs by partition. The lining
of the stomach, for example, is a lipid -protein membrane, and can be regarded as a non aqueous
phase in contact with the aqueous stomach contents. Hence, partitioning into and through the
stomach lining absorbs a drugs in the stomach.
In this experiment, acetic acid will be partitioned between an organic and aqueous phase. The
concentration of the acid in both the phase will be determined by taking out aliquots and titrating
against standardized alkali using an acid base indicator such as phenolphthalein. One can either
use a separating funnel to separating funnel to separate the two phases or carefully pipette out a
specific quantity from both the layers of solvents. The concentration of the solvents is varied by
adding additional equal quantities of fresh butanol and water and re- determining the distribution
coefficient

If C1 and C2 are the concentrations of the acetic acid in the butanol layer and aqueous layer
respectively, then C1/C2 = k, is the partition or distribution coefficient. This is independent of the
total amounts of substances presents.

21
 PROCEDURE

1. Take 40ml of 2 N acetic acid and 40 ml of n-butyl alcohol in a 250 ml capacity glass bottle
having a good ground glass stopper.
2. Stoppering the bottle, shake without spilling for 2 minutes and then allow the liquid to form two
separate layers. The upper layer will be the alcohol layer.
3. Carefully pipette out 5ml of the liquid from the upper alcohol layer into a conical flasks.
4. Add approximately 5ml of distilled water to the conical flask.
5. Titrate with a standard NaOH solution of 0.5 N strength taken in the burette after adding a few
drops of phenolphthalein indicator.
6. Repeat the titration with 5 ml of solution pipetted out from the lower aqueous layers. (Make sure
that the other end of the pipette is closed while the pipette nozzle is inserted to avoid solution
from the top layer entering the pipette).
7. At this stage, add 15 ml of n- butanol and 15 ml of distilled water to the bottle and shake the
bottle.
8. Repeat similar measurements with the B set and after adding fresh quantities of butanol and water
(15ml) with C set.

The concentration in normality of the acetic acid can be determined by using the V1N1= V2N2
relationship. The concentration in the butanol medium (Cb) and the concentration in the water
medium (Cw) are thus calculated. Calculated Cb/Cw. (by convention, the partition coefficient is
expressed with the concentration in the non- aqueous phase as the numerator). For A, B and C
sets, it should be the same within experimental errors. If there is dimerisation in the non aqueous
phase, like what has been shown for benzoic acid, then one would find that Cb/[Cw]2 will be a
constant instead of Cb/Cw.

22
 Layer volume Cb or Cw Cb/Cw Cb/[CW]2
of alkali
used
A Butanol
Water
B Butanol
Water
C Butanol
Water

Make sure that the burette is washed immediately after use as alkali can spoil glass stopcocks.
The same experiment can be carried out to find the partition coefficient of a variety of system
(e.g. partition of iodine in CCl4 and water and using iodometric titrations of partition of benzoic
acid in water and toluene and using acid base titrations).

23
 EXPERIMENT 5

AIM: TO PERFORM THE ALDOL CONDENSATION

Apparatus: Erlenmeyer flask, Buchner funnel, glass funnel, melting point apparatus
Materials: Benzaladehyde, acetone, sodium hydroxide, 95% ethanol, ethyl acetate, ice
Procedure:
1. 5g of NaOH was added to 25ml of H2O in an Erlenmeyer flask and the solution was swirled.
2. 25ml of 95% ethanol was added and the solution was allowed to come nearly to room temperature.
3. 2.9g of acetone and 10.5ml of benzaladehyde were added.
4. After 15 minutes of occasional swirling, the products were filtered on a Buchner funnel.
5. The product was washed with cold ethanol and was allowed to suck dry.
6. The yellowish product was recrystallized from ethyl acetate.
7. After recrystallization, a yellow crystalline was obtained.
8. The weight, yield, and melting point of the product were determined.

Note:
When precipitation appears to be complete, cool the mixture and isolate the solid. Rinse the product with about 5 ml of
each of the following pre chilled solvents: 95% EtOH.

Now recrystallize your product. You will need to find a suitable solvent or a solvent mixture. You may want to try 95%
aq EtOH and toluene (separately) to start. Use about 20 mg of crude product and about 1/4 ml of solvent in a dispo test
tube for each test. Remember, the point of recrystallization is to purify the solid by getting it to go into solution, then
come back out of solution in a way that creates clean sparkling, beautiful crystals without all the dirt from the reaction.
If your product is very soluble in a solvent at room temp, is that a good recrystallization solvent? How about if it
doesn’t dissolve at room temp, but does dissolve on heating?
(if neither of these solvents works , rumor has it that the next one to try might be 9:1 EtOH/acetone)

Once you’ve identified a viable solvent, recrystallize your entire batch of crude solid. Isolate and rinse the crystals in
the usual way, press them between two pieces of filter paper to draw most of the residual solvent, then put them
on a watch glass and pop them into the oven (100oC) for 14 min to drive off the remaining traces of solvent.

Your report for this experiment include the actual procedure you followed (eg; volume(s) of solvents you used
for crystallization, the appearance of the product, etc;), as well as a discussion that includes a clear explanation of
your structure determination based on the NMR.

REACTION:

24
 EXPERIMENT 6

Thin Layer Chromatography: Calculation of Rf Values

Aim: To calculate the Rf Values of ortho- and para-nitro phenols by using thin layer chromatography.

Chemicals: ortho-Nitro phenol, para-Nitro phenol, ethyl acetate, dichloromethane

Apparatus: TLC plate, capillary tubes, Iodine chamber.

Principle:
Most reactions produce more than one product. Naturally occurring materials are only rarely 100% pure. It
is therefore desirable to have a simple, fast and efficient way to determine the purity of organic mixtures.
The separation of a mixture by passing it, in solution, over an adsorbent (such as alumina or silica gel) is
the basic idea of chromatography. It involves the passage of a mobile phase across a stationary phase in a
column. Usually a mixture of compounds is present in the mobile phase. As soon as the mixture comes in
contact with the stationary phase, some or all of the components of the mixture are adsorbed on it. As
additional mobile phase comes along, some or all of the mixture will dissolve and continue moving. This
adsorption/solution process continues along the length of the column. If a proper choice of mobile phase,
stationary phase, solvent and other operating parameters was made, the mixture will be separated in the
column and its various components will emerge at different times. In Thin Layer Chromatography, a liquid
solution is directly applied to a solid adsorbent. Capillary action draws a developing solvent up the TLC
plate. As this solvent passes through the spot, the mixture will be dissolved and will begin to move with
the solvent front. However, the adsorbent will also reabsorb part or all of the mixture. As more solvent
comes by, the mixture will again go into solution, move further and be reabsorbed. Since different
materials will be dissolved and reabsorbed at different rates, separation will take place. This passage of the
solvent front through the adsorbent is known as developing the plate. The extent of separation, measured
by retention factor ("Rf ") value differences, will depend on the relative solubilities and relative strengths
of adsorption of the components of the mixture.
Organic compounds interact with absorbents by a variety of interactions. If the compound is non-polar,
it can only have weak 'Van der Waals' attractions for the absorbent. However, more polar molecules may
interact more strongly by a variety of mechanisms including dipole-dipole interactions, coordination, and
hydrogen bonding. The most important rule of chromatography is that the more polar compounds will be
absorbed most strongly on absorbents (stationary phases), while non-polar compounds will be only very
weakly absorbed. In a typical chromatography experiment, the non-polar compounds, since they are poorly
absorbed, will be held least strongly and will move quickly through the plate. Polar compounds, on the
other hand, will be slowed on their process through the plate by their strong interactions with the solid
phase. This separation based on polarity will explain most of the chromatography encountered in this
course.

Types of Adsorbents used in Chromatography

Listed in decreasing power of adsorption:
Alumina > Activated Charcoal > Magnesium Silicate > Silica > Starch

Solvents Commonly Used in Chromatography

Listed in decreasing polarity:
Acetic Acid > Water > Methanol > Acetone > Ethtyl acetate > Diethyl ether > Chloroform >
Dichloromethane > Toluene > Cyclohexane > Petroleum ether

For a typical separation, a variety of different combinations of solvent and adsorbent may be effective.
Once you have developed your plate, it must be visualized. This visualization may be accomplished by
reacting the developed plate with a chemical reagent. Iodine (I2) is one of the easiest to use of the several
common chemical visualizing agents. The developed slide is simply exposed to I2 vapors in a chamber
similar to the developing chamber for a few minutes. Almost all compounds will form a weak colored

25
complex with the I2. This complex will appear as a darker area on the slide. The 'spots' are characterized by
their Rf value, a measure of how far the spot traveled with that combination of adsorbent and solvent.

Procedure:
 Take 1 TLC plate handle it only on the edges, as fingerprints
contain UV-active materials.
 Using a pencil draw a very light line across the sheet (short
dimension) about 1 cm from one end.
 Then make 3 small light marks at even intervals along the line for
spotting the samples. Mark them as A, B, C
 Draw another light line about 1 cm from another end of the plate
for the solvent front.
 Obtain a TLC chamber and place solvent, a 5% ethyl acetate in
dichloromethane to 0.5 cm height.
 Place a piece of filter paper around the inside surface of the container and extend into the
solvent.
 A glass jar with a lid or a beaker with a watch glass or a cover of a Petri dish can be used as a TLC
chamber
 Using clean capillary tubes carefully spot two samples at two pencil marks
A: o-Nitrophenol, B: p-Nitrophenol, and C: Co-spot (mix spots of A and B)
 The spots should be as small as possible in order to minimize tailing and overlapping when the TLC
plate is developed. If a more intense spot is desired, let the spot dry and re-spot in the same location.
 When the spots are dry, place the TLC plate in the developing chamber. Then gently close the
chamber.

Running a TLC:
 Be sure that the bottom edge of the TLC plate is in the solvent but the spots are above the
solvent, and the filter paper does not touch the chromatographic sheet.
 When the solvent has moved to the front line (top line), remove the plate. Lay it on a clean surface in
well ventilated area and allow the solvent to evaporate until the plate appears dry.
 Visualize the plate under iodine chamber Measure all the distances traveled by the compounds and
solvent.

Calculate the retention factor (Rf) for each compound. and immediately draw a light pencil line around
each spot.

Calculation of retention factor:

Rf = Distance travelled by the compound / Distance travelled by the solvent system

Retention factor of o- =

Retention factor of p- =

26
 EXPERIMENT 7

DETERMINATION OF THE AMOUNT OF CALCIUM IN MILK POWDER BY

EDTACOMPLEXOMETRY

Materials required: Milk powder such as nestle/amulya, magnesium sulphate 0.01M, pH 10 buffer, EDTA,
EDTA 0.01M, NaOH 0.01M, Eriochrome Black-T.

Glassware: Standard Flasks, Burette, pipettes, droppers etc….

Key reference: McCommick, P. G., J. Chem. Educ., 50, 136, 1973.

Principles

In one cup (approx) Whole milk Non fat milk Low fat milk 1%
kilocalories 150 86 102
Protein (g) 7.5 7.5 7.5
Carbohydrate (g) 11.4 11.0 11.7
Fat (g) 8.2 0.4 2.6
Saturated fat (g) 5.1 0.3 1.6
Cholesterol (mg) 33 4 10
Sodium (mg) 120 126 123
Vitamin A (RE) 76 149 145

Vitamin C (mg) 2 2 2
Folate (mg) 12 13 12
Calcium (mg) 261 261 261
Magnesium (mg) 33 28 34
Zinc (mg) 0.93 0.98 0.95
Phosphorus (mg) 228 247 235
Iron (mg) 0.12 0.1 0.12

Calcium comprises 1.5-2.0 % of our body weight. It is required by the body to produce strong bones and teeth
and 99% of the calcium of our body is present in bones and teeth. Bones are mainly deposits of calcium
phosphate, Ca3(PO4)3 and hydroxyapatite, Ca5(PO 4)3OH in a collagen protein matrix. The teeth enamel is made
of hydroxyapatitewhose hydroxyl groups are susceptible to reaction with acids such as lactic acid produces in
mouth. Fluoride containing toothpaste replace these hydroxyl groups with fluoride and produce acid resistant
fluorapatiteCa5(PO4)3F. Calcium is always in great demand by the cells of the body including those of the heart,
nerves and muscles. Calcium is used for blood clotting, hormone release, regulation of amy enzymes and cell
division. The recommended daily allowance (RDA) for calcium is around 900-1000 mg/day. Teenagers
developing bones and teeth as well as women above 45 who are prone to osteoporosis (the depletion of bone
mass) have a higher RDA of 1300-1500 mg/day. Milk is a heterogeneous mixture of proteins, sugar, fat,
vitamins and minerals. Milk and milk products are some of the natural sources of calcium. About 250-300 mg
of calcium is present per 8-ounce cup of milk, which is about 1/3 rd of the RDA.

27
There are basically two ways of estimating the amount of calcium in milk: by conventional complexometric
titration or by using a calcium specific electrode. In this experiment, we will estimate the amount of calcium
present in milk by complexometric titration using the well known chelating ligand EDTA. Edta reacts with
calcium and many other metal ions to form very stable complexes. Milk will be analyzed for calcium content
using EDTA, which reacts to form CaEDTA. The calcium and magnesium in the milk react quantitatively with
EDTA at pH 10 to form very stable complexes. Since it is relatively inexpensive, this property of EDTA is
utilized in many commercial and medical applications. The well known and important use of EDTA is its use as
a chelate in chelation therapy. EDTA is a FDA (food and drug administration of USA) approved drug in
chelation therapy for lead and heavy metal poisoning. One of the recent findings has been its effect in removing
calcium deposits from arteries in arteriosclerosis. Na2MgEDTA is administered which removes all the free
calcium in blood. The blood re-equilibrates with plasma and the changed equilibrium with the low calcium
blood and calcified plaque in the blood vessels forces the calcium deposits to dissolve. The FDA has not yet
approved EDTA chelation therapy as an alternative to bypass surgery. However, reports say that more than
5,00,000 heart patients have been treated safely with EDTA chelation therapy. EDTA is also an antioxidant; it
reduces blood pressure and is quite cheap. EDTA is also added to blood samples to prevent clotting before
testing as it removes calcium which helps in clotting. In many complexes EDTA completely engulfs the metal
ion, forming a six coordinated species as shown above. Two nitrogen atoms occupy adjacent positions of the
octahedrally coordinated metal ion.

EDTA titration involves the use of an indicator such as Eriochrome black T or Murexide. These are metal ion
Indicators which are compounds whose color changes when it binds to a metal ion. For an indicator to be useful
it must bind metal less strongly than it binds to a metal ion. A small amout of Mg2+ is added to the indicator (In)
to form a magenta colored complex. As EDTA is added, it reacts with free calcium and then with the small
amount of MgIn complex. As the traces of calcium in milk are being complexed, the slight excess of EDTA
converts the magenta-colored magnesium complexed indicator into the free blue anion.The titration is to be
carried out at pH 10. This is because it results in increased EDTA4 concentration which favors complex
formation. The indicator used in this complexometric titration is Eriochrome Black-T.

28
 Eriochrome black T

The color change of the indicator from magenta to blue occurs at a pH above 7 and at this pH, precipitation of
hydroxides does not occur. A pH of 10 is maintained by adding a buffer composed of ammonia and ammonium
chloride. Ammonia a weak base raises the pH by forming hydroxide ions. It also neutralises added acids,
preventing the lowering of pH while the ammonium ion can react with any added hydroxide to form ammonia
and water thus preventing variations in the pH.

Ca2+ + EDTA4- CaEDTA2-

MgIn (magenta) + CaEDTA2- MgEDTA2- + In2- ( blue)

The color change occurs over the range of 2 drops of EDTA and happens from magenta to purple and to sky-
blue. The color change is slow with changes taking 2 to 3 seconds sometimes and takes place at a pH of 10 but
not pH 7.

PROCEDURE

In this experiment we will determine the combined amount of calcium and magnesium present is a
commercially available milk powder. A standard EDTA solution of 0.01M is prepared by using disodium
dehydrate of EDTA in a 250 ml standard flask. Prepare also a 0.1M solution in a 50 ml flask. Prepare a pH 10
buffer solution using ammonia and ammonium chloride.

Preparation of Mg-EDTA complex indicator

1. Mix 0.74 gm of the dry EDTA with 0.49 gm of MgSO4 in 100 ml of distilled water.

2. Divide the solution into two 50 ml portion.

3. To one portion, add a few drops of phenolphthalein. Dropwise, counting the drops, add sufficient 0.1 M
NaOH solution to make the solution turn faintly pink.

4. Once the number of drops of NaOH required for this color change has been found out, this 50 ml solution
can be discarded.

5. The the second 50 ml portion, add the same number of ml of 0.1 M NaOH solution as were added to the
first portion, then dilute to about 95 ml with distilled water.

6. Add 2 ml of pH 10 buffer solution (ammonia/ammonium chloride) and add 8-10 drops of Erichrome Black-
T indicator solution. At this stage there are two possibilities, the solution is either red or blue.
7. If the solution is red, Mg2+ is in excess. In that case add 0.01M EDTA solution dropwise until the solution
just turns blue.
8. If the solution is originally blue, then EDTA is in excess. In that case, add 0.01M MgSO4 solution dropwise
until the solution just turns red, then add 0.01M EDTA dropwise to make the solution turn blue again.
Preparation of milk power solution

1. Accurately weigh about three gm of dry milk powder (Amulya for eg.) into a 250 ml of beaker and add
approximately 100 ml of moderately warm distilled water. Stir to dissolve.

2. Transfer quantitatively by repeated washings with distilled water into a 250 ml volumetric flask. Let it
stand for a sufficient time, so that all bubbles disperse. If foamimg occurs it may be suppressed by the
addition of 1 or 2 drops of n-octanol.

29
3. Make up the solution to the calibration mark with distilled water. Mix well after stopping by inverting
shaking it repeatedly.
4.
Titration of Milk Solution for Combined Calcium and Magnesium

1. Pipette out exactly 50 ml of the milk solution into a 250 ml Erlenmeyer flask.

2. Add about 2 ml of pH 10 buffer, 10 ml of Mg-EDTA indicator solution and 3 drops of Eriochrome Black-T
indicator.

3. Titrate with the standard 0.01 M EDTA solution to a color change from pinkish red to blue through an
intermediate violet color.

4. Titrate at least two more milk samples using the same procedure.

5. From your experimental data calculate the percentage of Ca in the powdered milk for each aliquot that you
titrated. Calculate an average percentage.

6. This will give the combined Calcium-Magnesium amount in the milk powder.

The moisture content of the milk powder varies. Attempts to dry it in the oven around 80 oC can result in
yellowing of the powder which may result in precipitation. One can keep 3 gm of milk powder separately in the
oven at 80 oC, determine the weight loss and apply the required correction to the weights.

SAFETY NOTES: Do not smell or pipette out ammonia. The ammonia bottle should be opened and kept
in the fume-hood.

References:

1. A collection of Interesting General Chemistry Experiments, Anil J. Elias, 2002, Universities Press
(Hyderabad), India.
2. Analytical Chemistry: An Introduction, D. A. Skoog, D. M. West, F. J. Holler, 6th ed. 1994, Saunders
College Publishing, Florida.

3. Text Book of Polymer Science; F.W. Billmeyer, 3rd ed. 2007, John Wiely& Sons.

30