Experiment 1: Determination of the strength of NaOH by using standard oxalic

acid solution
Principle: An acid-base titration is a neutralization reaction that is performed in the lab in order
to determine an unknown concentration of acid or base. The moles of acid will equal the moles
of base at the equivalence point. The neutralization method comprises volumetric determination
based on reactions of acids with alkalis, i.e. neutralization of acids and bases:

The neutralization method is used for determining the amount of acid (alkalimetry) or alkali
(acidimetry) in a given solution. At the equivalence point, neutralization is complete.

Moles of H+ = Moles of OH-

NaOH is a secondary standard substance. Thus oxalic acid can be used to prepare a standard
solution. Standard oxalic acid solution reacts with NaOH solution and produce sodium oxalate
and water.

Apparatus: Conical flask, pipette, burette, dropper, pipette pump.

Reagents: Standard oxalic acid, Sodium hydroxide, Phenolphthalein indicator.

Procedure:

(i) Take 10.0 mL of supplied oxalic acid (0.05M)solution by a pipette into a conical flask
(ii) Add approximately 25 mL distilled water and add 1-2 drops of Phenolphthalein
indicator in it.
(iii) Then titrate the acid solution with NaOH solution from a burette until the color of the
solution turn to pink.
(iv) Repeat the titration for at least three times and the agreement between the titrations
should be within 0.1 mL. record your titrations data in tabular form as follows
 Table: Determination of the strength of NaOH with standard oxalic acid solution
using phenolphthalein as an indicator

No of Volume of Burette reading Average

observation oxalic acid burette
(mL) Initial Final Difference reading
burette burette burette (mL)
reading reading reading
(mL) (mL) (mL)
1
2
3

(v) Calculate the strength of the alkali solution.

Calculation:

b.VaMa = a.VbMb

NB.

● NaOH readily absorbs CO2 and water vapor from the air and hence there is a change of
weight therefore, it is a secondary standard substance.
● Oxalic acid is a crystalline substance, stable at atmospheric conditions and corresponds
exactly to its formula, which can be obtained chemically pure.
● Phenolphthalein indicator’s color change pH range is 8.3 to 10.0 and produces red color
at basic solution whereas colorless at acidic or neutral solution.
Experiment 2: Determination of conductance titration curves of a strong acid and a weak
acid against a strong alkali.

Principale: A strong acid, hydrochloric acid, HCl for instance in which a solution of a strong
base, sodium hydroxide NaOH, is added. The reaction occurs. For each amount of NaOH added
equivalent amount of hydrogen ions is removed. Effectively, the faster moving H+ cation is
replaced by the slower moving Na+ ion, and the conductivity of the titrated solution as well as the
measured conductance of the cell fall. This continues until the equivalence point is reached, at
which we have a solution of sodium chloride, NaCl. If more base an increase in conductivity or
conductance is observed, since more ions are being added and the titration of a strong acid with a
strong base, the conductance has a minimum at the equivalence point. This minimum
equivalence point can be used instead of an indicator due to determine the endpoint of the
titration.
The conductance of a dil. acetic acid solution is due to the small amounts of H+ ions resulting
from the dissociation of the weak acid. When a small amount of alkali is added and the H+ ions
are neutralized an equal amount of H+ ions are not generated by further dissociation of the weak
acid because the CH3COO- ions suppress the dissociation due to common ion effect. Therefore
the conductance decreases.

Upon the further addition of alkali, the conductance increases because of the increases of Na+
ions and of CH3COO- ions. After the end point, the conductance increases at a sharper rate due to
increases of the last moving OH- ions, in addition to the Na+ ions.

Apparatus
Conductivity meter, Beaker (250mL), Burette, Pipette.

Procedure
i) Wash the conductance cell with hot distilled water.
ii) Take 10mL of the supplied acid solution in a beaker. Place conductance cell in
it and add sufficient water to keep the electrodes of the cell immersed.
iii) Get a graph paper ready for plotting conductance data.
iv) Measure the conductance before the addition of NaOH.
v) Charge the burette with the supplied 0.2M NaOH solution. Add 1 mL aliquot
portions of the alkali solution from the burette, stir the solution, and measure
the conductance after each addition.
vi) Record all the data in a tabular from.
 Table -1
Table for the recording of conductance against volume of NaOH vs HCl
Volume of
NaOH (mL)
Conductance
(µS)

Table -2
Table for the recording of conductance against volume of NaOH vs
CH3COOH

Volume of
NaOH (mL)
Conductance
(µS)

vii) Plot observed conductance vs. volume of alkali added.

viii) In the case of weak acid, measure the first few (2-3) points by adding
0.1mL aliquot to demonstrate the decreases in conductance. The selector
switch of the conductometer should be at 1-199 µS.
ix) After that the conductance increases with further addition. To make sure that
you measure at least 4-6 points before and after the end point, plot each point
before measuring the next point.
x) The point after the end point gives a steeper straight line.
xi) Find the end point and volumes of NaOH at the end point from the graph.
Calculate the concentration of strong acid and weak acid.
NB.
Conductance titration
Conductance is the movement of ions in solution. The conductivity of a solution is dependent on several
factors, including the concentration of the solute, the degree of dissociation of the solute, the valence of
the ion’s present in the solution, the temperature, and the mobility of the ions in the solution.
In conductometric titrations the variation of the electrical conductivity of a solution during the course of a
titration is followed. This technique is of wide applicability and good precision. Since the property
measured bears a direct (not Iogarithmic) relation to the concentration, the titration curves
(volume-corrected) consist of intersecting straight lines. The equivalence point is that at which the
conductivity undergoes a sudden change. Marked increases or decrease in conductance are associated
with the changing concentrations of the two most highly conducting ions- the hydrogen and hydroxyl
ions. The method is used for titrating colored solutions or homogeneous suspension (e.g.: wood pulp
suspension, which cannot be used with normal indicators. Acid base titration, redox titrations are known
to us where are known to us where indicators are used to locate the end point e.g. methyl orange,
phenolphthalein for acid base titrations and starch solution for iodemetry type redox process. However
electrical conductance measurement can be used as a tool to locate the end point.
Consider a solution of a strong acid, hydrochloric acid, HCl for instance in which a solution of a strong
base, sodium hydroxide NaOH, is added. The reaction occurs. For each amount of NaOH added
equivalent amount of hydrogen ions is removed. Effectively, the faster moving H+ cation is replaced by
the slower moving Na+ ion, and the conductivity of the titrated solution as well as the measured
conductance of the cell fall. This continues until the equivalence point is reached, at which we have a
solution of sodium chloride, NaCl. If more base is added an increase in conductivity or conductance is
observed, since more ions are being added and the neutralization reaction no longer removes an
appreciable number any of them. Consequently, in the titration of a strong acid with a strong base, the
conductance has a minimum at the equivalence point. This minimum equivalence point can be used
instead of an indicator bye to determine the endpoint of the titration.
Experiment 3: Determination of the neutralization curve of a strong acid, weak
acid by a strong alkali by measuring pH
Principle: A glass electrode is immersed in solution of the acid whose strength is to be
determined. This electrode is sensitive to hydrogen ion activity, and has a potential proportional
to pH. The glass electrode is coupled with a standard calomel electrode (watch it inside the glass
tube). The cell is thus formed is connected to the potentiometer or electronic voltammeter. With
the addition of alkali, pH of the solution changes accordingly. The e.m.f. of the cell also changes
with pH of the solution in accordance with the relation:

E = Eo + 0.0591 pH

We actually will get value of pH directly from the scale, because the instrument so designed to
convert e.m.f. value directly into pH value and show it on the scale. The standard alkali solution
is added from the burette in small volumes. Upon each addition, the pH is recorded. The pH is
then plotted against the volume of alkali added. The steepest portion of the curve indicates the
equivalence point.

When the solution is very dil.ute or weak acid or bases are involved, the steepness of the curve is
less marked and it is difficult to judge the end point. In such case plot of the curve ∆E/∆V
volume of is used. The maximum of the curve indicates the end point.

Apparatus

pH meter. Burette, pipette, beaker (250 mL).

Procedure

(i) Wash the pH electrode with sufficient distilled water.

(ii) Calibrate the pH meter using buffer solution of pH = 0.36

(iii) Again clean the electrode with sufficient distilled water.

(iv) Take 100 mL of supplied 0.01M HCl in a beaker and immerse the electrode of pH
meter carefully in the beaker so that it does not touch the bottom of the beaker.

(v) Add 0.5 mL 0.05 M NaOH each time from burette in to the beaker and measure the
pH of the solution as the function of volume of NaOH until steady pH is found
followed by sharp increase in pH. Record the data in a table as follows.
Table-1

Table for the recording of pH against volume of NaOH vs. HCl

Volume of
NaOH (mL)

pH

Table-2

Table for the recording of pH against volume of NaOH vs. CH3COOH

Volume of
NaOH (mL)

pH

(vi) Repeat the whole process for 0.01 M acetic acid. Record the data in a similar table
like Table-1.

(vii) Plot pH vs volume of NaOH for i) HCl and ii) acetic acid indicating point of
equivalence in separate graph paper.

Glass electrode (pH)

The glass electrode for measuring pH consists of a glass indicator electrode and a reference
saturated calomel electrode immersed into an unknown solution of PH. The PH indicator electrode
consist a thin PH sensitive thin glass membrane sealed onto end of a heavy-walled glass or plastic
tube. A small volume of dil.ute HCl acid saturated with AgCl is contained in the tube. This
electrode is sensitive to hydrogen ion activity, and has a potential proportional to PH. The
responsiveness of a glass electrode to the hydrogen ion activity is a result of complex process at
the interface between the glass membrane and the solutions either side of it. The cell is thus
formed is connected to the potentiometer or electronic voltammeter. With the addition of alkali,
PH of the solution changes accordingly. The emf of the cell also changes with PH of the solution
in accordance with the relation:
E = E0 + 0.0591 PH
We actually will get of PH directly from the scale, because the instrument so designed to convert
e.m.f. value directly into PH value and show it on the scale. The PH electrode is calibrated against
standard buffer solution before the any measurement of unknown PH.
Experiment 4: Determination of the amount of Fe(II) and Fe(III) in a given
sample using a standard dichromate solution
Principle: The aqueous solution of K2Cr2O7 of exactly known concentration can be prepared by
weighing and the solution thus prepared is stable indefinitely if protected from evaporation.
K2Cr2O7solution is used in the determination of Fe(II) and Fe(III) in ions ores.

Fe(III) must be reduced to Fe(II) before titrating with standard dichromate solution. The
reduction is carried out by the addition of a very small excess of SnCl2 solution to the hot HCl
solution of the Fe(III) sample followed by the removal of the excess SnCl2 with HgCl2. The
sequence of the reaction is as follows:

The titration is performed in presence of a mixture of H2SO4 – H3PO4 acids. Sulphuric acid
provides mainly the necessary H+ ions while H3PO4 converts Fe3+ ion into the colorless stable
[Fe(HPO4)]+ complex, thus rendering the end-point more visible. Removal of Fe3+ by complex
formation also lowers the reduction potential of the Fe (III) – Fe(II) couple and thus tend to
increase the reducing power of the Fe2+ ion.

The usual indicator in the dichromate titrations is diphenylamine, which is a redox indicator
gives a very sharp color change from colorless through green to red-violet color
(diphenylbenzidine violet – a system of conjugated double bond).

Apparatus:

Conical flask, pipette, burette, dropper, sprit lamp.

Procedure:

● Pipette out 10.0 mL of the given iron solution in a conical flask and add 10 mL of
dilute HCl solution in it. Now reduce Fe (III) of the solution be heating the content of
the conical flask at about 90oC.

● Add concentrate SnCl2 solution in hot condition drop wise till the yellow color of the
solution has nearly disappeared.
● Complete the reduction by adding dil. SnCl2 drop wise till the solution has a faint
green color. A slight excess of SnCl2 is necessary for complete reduction of Fe (III) to
Fe (II).

● The solution is then rapidly cooled under the tap water to about 20oC, with protection
from the air. Add 10 mL of the saturated HgCl2 solution to remove the slight of SnCl2.
A slight silky white precipitate will form. Formation of a heavy (gray or black)
precipitate indicates addition of too much SnCl2 during reduction. If no precipitate
forms on the reduction of HgCl2 reduction of Fe (III) is probably incomplete. Such a
determination should also be rejected.

● After the successful reduction of Fe (III) to Fe (II) allow the content of the conical
flask to stand for 5 minutes. Then dilute the solution with distilled water to about 50
mL and add about 20 mL H 2SO4-H3PO4 mixture..

● Add a few drops of diphenylamine indicator and titrate with standard potassium
dichromate solution. Titrate slowly, whilst stirring constantly with the standard
dichromate until the solution assumes a bluish-green tint near the end point.

● Continue the titration, adding the dichromate solution drop wise and maintaining an
interval of a few seconds between each drop, until the addition of 1 drop causes the
formation of an intense purple or violet-blue coloration, which remains permanent
after shaking and is unaffected on further addition of the dichromate.

● Repeat the process for at least three times.

Table: Estimation of Total Iron content

No of Volume of Burette reading Average

observation Iron (K2Cr2O7) burette
solution Initial Final Difference reading
(mL) burette burette burette (mL)
reading reading reading
(mL) (mL) (mL)
1
2
3
 ● Calculate the total iron (Fe2+ and Fe3+) content of the supplied solution.

N.B.

● If Sn2+ is too much, the second step will be replaced, at least partially, by the reaction

The occurrence of this process ruins the determination of iron. Thus the quantity of
Sn(II) used in the first step is critical. Fortunately, the solution of Fe(III) in HCl
media becomes bright yellow ( due to the formation of [FeCl4(H2O)2]- when heated,
this makes it easier to detect the point when reduction of Fe3+ by SnCl2 is complete
and this color just disappears. One or two drops more of the dilute SnCl2 solution is
then added to ensure that a slight excess of Sn (II) is present. If the procedure is
performed properly, a silky white precipitate Hg2Cl2 appears when HgCl2 is
introduced. If a heavy precipitate forms grey or black, too much SnCl2 has been
added and therefore, the reduction process must be repeated.
● The small amount of HgCl in suspension has no appreciable effect upon the
oxidizing agent used in the subsequent titration, but if a heavy precipitate forms or a
gray or black precipitate formed which indicate too much SnCl2 solution has been
used. The results are not accurate and the reduction must be repeated.
Experiment 5: Investigation of the kinetics of the reaction and the determination
of the order of the reaction with respect to thiosulphate ion.

Principle:

The reaction takes place at room temperature with measurable rates. Colloidal sulphur is
produced in the reaction and the solution becomes turbid. A measurement of the rate of
formation of sulphur allows the determination of the rate of the reaction.

It is not easy to measure the amount of Sulphur formed in any time interval. The purpose of the
present experiment is to investigate how the concentration of reactants influences the rates of the
reaction. Therefore, if the time to form a fixed amount of Sulphur is measured with various
concentration of one reactant, keeping the concentration of the other reactant constant, the
dependence of the rate of the reaction on the concentration of this reactant can be investigated.

If the reaction is carried out in a glass beaker, a black mark on white paper kept under the beaker
will become invisible after a certain amount of colloidal Sulphur is formed. If the volume of the
solution is kept constant in all experiments using various concentration of the chosen reactant,
the mark will become invisible after the same amount of Sulphur is formed. Let this amount of
Sulphur is x. The rate of the reaction is given by

v = x/t ------------(i)

The rate equation for the reaction may be written as

v = k [thio]α [acid]β-----(ii)

If the concentration of acid is kept constant, the above equation may be written as

v = k/ [thio]α--------------(iii)

Where k/ = k [acid]β

Putting the value of v from equation (i) in equation (iii) we obtain

x/t = k/ [thio]α----------(iv)

or, log t = log x – log k/ - α log [thio] -------(v)

A plot of log t vs. log[thio] should give a straight line with a slope of (-)α. Therefore α, the order
of the reaction with respect to thiosulphate ion can be determined by measuring the time in
which the fixed amount of sulphur ‘x’ is formed in several experiments with different
concentrations of thiosulphate.

Apparatus:

Stop watch, beakers, burette and stirrer.

Procedure

(i) Prepare solutions in a100 mL beaker by mixing 0.1 M Na2S2O3 solution with water
according to the Table-1.

Table-1

Table for the preparation of Na2S2O3 solution of different concentrations.

Exp. 1 2 3 4 5 6 7 8
No.
Solution 99 89 79 69 59 49 39 29
A (mL)
Water 0 10 20 30 40 50 60 70
(mL)

(ii) Make ready a white paper with cross mark with black ink.
(iii) Place the beaker with the solution on this black mark.
(iv) Be sure of sufficient light around the beaker.
(v) Add 1 mL HCl from the burette to the solution in the beaker. Start stopwatch
immediately, and stir the solution for 5 seconds.
(vi) Measure the time in which the black mark becomes invisible.
(vii) Present the results of measurements and the necessary calculations for the
determination of the order of the reaction with respect to thiosulphate in Table-2.
(viii) Plot log t vs. log[thio]
(ix) This should give a straight line with a slope of (-)α. Where α be the order of the
reaction.
Table-2

Table for the plot of log t vs. log[thio]

Time Cal. Conc. of

Exp. No. required for log t thiosulphate log[thio] α from graph
producing ‘x’ in the mixture
gram of S
1
2
3
4
5
6
7
8
Experiment 6: Determination the densities of different inorganic and organic
solution at room temperature and find out the concentration of unknown solutions.

Principle: Density is an intensive property, meaning that density that does not depend on how
much of the sample is being measured. The mass any block of lead divided by its volume will
yield the same ratio, regardless of the size of the block. The density of a liquid is usually directly
related to the solution concentration. Because the density of a liquid is easy to measure, this
provides a convenient method of analysis. For example, the state of change of an automobile
battery can be determined from the density of the aqueous sulphuric acid battery fluid. Density is
defined as: Density= Mass/Volume.

By measuring the mass of an unknown volume of liquid, the density may be calculated. Far a
liquid, the volume is readily determined using accurately graduate glassware such as pipettes,
burettes, or volumetric flasks. Since the volume of a substance varies with temperature, it is
important to record the temperature of density measurements, when comparing the density of
different samples the temperature should be held constant for all the density measurements.

If the density of solution varies linearly with the molar concentration of the solutions, then a
straight line will be obtained by plotting density vs concentration of the solutions. From the plot
the unknown concentration of a solution can be found out by measuring the corresponding
density.

Apparatus and Materials: Density bottle, balance, supplied Inorganic and Organic solutions.
Procedure
● Clean, dry and weigh the density bottle or pycnometer. Fill it with water and weigh it
again. From the weigh and density of water at experimental temperature (from table),
find out the density bottle or pycnometer.
Prepare 5 to 7, 0.1 M – 0.5 M organic or inorganic solution in water (100 mL each).
● Fill the density bottle/pycnometer with each solution and take weight each time.
● Divide the mass of each solution by the volume of the density bottle/pycnometer and get
density.
● Plot density vs concentration of solution and from the plot find out unknown
concentration.
 Table: Densities of different inorganic solution

Serial no Conc. Of Mass of Mass of Mass of Volume of Density of

solutions empty bottle Solution bottle solution, ρ
(M) bottle (g) +Mass of (g) (mL) (g/mL)
solution
(g)
1.
2.
3.
4.
5.
6.
7.

Experimental Temparature (0C) =

Mass of empty bottle (g) =
Mass of empty bottle + water (g) =
Volume of density bottle (mL) =

Calculations:

Volume of bottle = (mass of water/ ρ water)

Density of solution = mass of solution/volume of bottle.
Apparent molar volume, =1000(ρ0- ρ)/C ρ0 + Mw/ ρ0
Where, ρ0 = density, ρ= density solution, Mw = molecular mass of solute,
C= Concentration of solute in mol/L