lab manual
lab manual
Principle:
The hardness of water is generally dåe to
Hardness is expressed as parts of CaCO3 dissolved salts of calcium and magnesium.
million parts of water. I mg of equivalent cquivalent
to the hardness causing ions
present per
hardness per litre is 1 ppm. Disodium salt of EDTA
(ethylene diamine tetraacetic acid) areagent, when
treated with hard water it reacts with and
consumes all the hardness forming cations in alkaline
medium (pH 8-10). The excess of this
reagent is indicated by the reaction of the indicator
solution from wine red to blue which is the end point of
Erichrome Black T which colours the
Ca2+ + EDTA titration.
Ca(EDTA)
Mg* + EDTA Mg(EDTA)
Procedure:
A.
Standardization of EDTA solution with Standard Hard water (S.H.W.):
Pipette out 25 ml of standard hard water, into a conical flask. Add to it 2 ml of
buffer
solution (NH,CI+ NHÊOH, pH - 10)and 4 drops of Erichrome Black -T indicator. Titrate it
against EDTA solution taken in a burette. At the end point the colour changes from wine red
to pure blue. Repeat the titration for three concordant readings. Let the
volume of EDTA
consumed be 'X'ml.
Caleulation:
X
Amount of EDTA with S.H.W.(25 ml)
Amount of EDTA with U.H.W.(25 ml) Known hardness in ppm
Unknown hardness in ppm
Department of Che:nisry ET
EXPERIMENT NO. 2
THEORY
% purity=
Weighi of CaCO, in lime stone sample iak:en x 100
Total weight of iimestone taken
PROCEDURE
A Known weight of limestone sample (0.5 - 1gm.) is dissolved in exscily 25, m!. ci 2rN
(approximately) HCI in a beaker (warm the solution i# the reaction is slow but do not bo). Afry
the evolution of carbon dioxide is over it is cooled and the solution is transered to a 280 nL
measuring flask. The beaker is washed 3 to 4 times with smal quantities oi wete: ano thu
washings are transferred to the same measuring flask and finaiiy diluted uc to the ars b
adding required amount of water. (Solution -)
in another 250 m. measuring flask exactly 25 mi. of the 2N HCI used above is taken ana ci
withwater up to the mark (solution-l).
Exactly 10 mi. of the supplied N/10 NaOH solution is teksn in a conica! iesk an: tia:
separately witn solutions- and solutions-! taken in a bursie using methvi orenge as indice:
OBSERVATIONS
Procedure:
The water sample is taken in a 500 ml glass stoppered bottle leaving about 10 ml
empty space at the top. To it approximately 1ml of MnSO4 solution is added followed by
approximately 1 ml of alkaline KI solution with the help of a pipette taking care that the
solutions are delivered well below the surface of the water. (The alkaline KI
solution contains
sodium azide which takes care of any oxidizing agents present that are likely to
liberate
iodine from KI). If any air space is stillleft it is filled up with water sample
bottle is then made upside down several times to ensure proper
immediately. The
mixing and the precipitate
formed is allowed to settle for a few minutes. Then HSO4 is added
drop wise to the solution
with shaking till the precipitate is dissolved giving a clear yellow
solution (addition of excess
HSO, is to be avoided) 100 ml of the solution was pipetted out and
titrated with standard 40
Na,S,O; using an indicator (1-2 mlof starch is used for every titration).
Table:
S. No,
Volume of water Burette Reading Volume of NazS,0,
sample taken Initial (mL) Final (mL) (X mL)
Calculation:
Strength of sodiumthiosulfate solution = 1.02
40
Result:
The amount of
dissolved oxygen in water observed is
Estimation of Iron by titration with
Aim: Estimate the
potassium permanganate
amount of ferric ion (Fe3+) in the
Apparatus: Burette, Pipette(10 mL),conical flask given solution.
Chemicals: Iron Sample, 0,0IN KMn04, (250mL), Measuring jar (100mL).
Introduction. standard oxalic acid, Concentrated
H2S04 (4N).
In this
experiment you will use potassium
an
unknown solution. permanganate (KMnOa) to determine the of iron (as Fe)in
Permanganate reduces to a manganese(I1) ion in the acidic solution. This
reaction requires 5 electrons ion
and 8
MnOa+ 8H* + 5e’ Mnt + hydrogen ions:
40
Only one electron is
Fe2t ’ Fet + e necessary to reduce Fe(lll) to Fe(l)
Therefore, Imole of MnO4(the oxidizing agent)
5 moles of Fe and I reacts with 5 moles of Fe?* (the
mole of Mn,Thus, in net ionic reducing agent) to form
MnO4+ SFe*+ 8H ’ SFet + Mn2 +4H)0 form:
The 1:5 mole ratio with
respect to the amounts of
stoichiometric basis for allof the calculations in this MnOa'and Fet consumed will provide the
experiment.
Procedure.
A.
Standardisation of KMnO4 Solution:
Pipette out 10 ml of oxalic acid solution into a
conical flask. Add ~0 ml of dil. H2S04 and heat to
°C. Titrate the hot solution
against the KMn04 solution taken in the 40-50
the solutionchanges from burette. At the end point the color of
colorless to light pink color. Repeat the titration for three
Reactions concordant readings.
B. Estimation of
unknown Fe(I) solution
You receive a solution of unknown
mark.
concentration in 100 mL volumetric flask. Dilute it carefully to
1. Pipette out 10 mL of an unknown
solution into an conical flask.
2. Using a graduated
cylinder, add 10 mL of 1 MH,SO4 to the flask.
3. Titrate the solution with the
KMn04 solution from a burette. The pinkish
drop of excess KMnO4 signals the end color produced by the î
point for the titration. Repeat the
readings. titration for three concorda
MnO, + 8H + 5e ’ Mn* +
4H,0
Fe2t ’ Fet + e] x5
Overall re action: MnO, + 8H + SFe+ ’
5Fet + Mn+ + 4H,0
Calculation:
1000 ml of IN KMn04 = 55.8 g
of Fe
xml of yN
KMn04 = (55.8X xXy) /1000 =wg
10 ml of
unknown iron solution contains wgof Fe
100 mlof
unknown iron solution contains wX 10 gof Fe.
Rate constant of hydrotysis of thylacetate
Aim: Demine ratexnstant othyitnhsis ot an ester suach as ethyl avetate catalyzevi h
ApAaS Themostat, cnical flasks with ot, burtte and stoy watch.
Chemicals: Ethyl avetatt, 0.$ MHC, 0.$ M NaOland phenophthalein indicater.
Thon:
The hydrolysis of ethyl acctate gives ethyl alcohol and acetic acid.
CHCO0CH +H;0 CHCO0H + CHOH
The reaction is catalyzed by il. HCl and is a
of water is in large amount and does not reaction of first order as the concentration
fist onder reaction. change significantly during the reaction. lt is pseudo
The rate constant is determined by using the
following kinetie equationof first order
2.303
t
Where a= initial
concentration.
a -x
=concentration after time t.
The values of a, a-x and t are taken
from experimentally determined
experimental solution of known concentration of ethyl acetate and HCl are values. an actual
In
kept on water bath at room mixed together and
at an interval of 5-10 temperature. Known volumes of the reaction mixtures are withdrawn
minutes, added to chilled water in a conical
standard NaOH solution using flask and titrated against
phenolphthalein as an indicator. The
corresponds to the total acid formed i.e. HCI and acetic acid by volume of NaOH used
mixture. The final reading is noted after keeping the the hydrolysis in the reaction
or keeping it in hot water at reaction mixture on water bath for 24 hours
50-60° C for an hour.
K= 2.303 Voo- Vo
t
vii) Finally the reaction mixture flask was placed on a water bath at 50-60° Cfor about an 30
min.
Pipette out 10ml of the reaction mixture and titrate it against 0.5 M NaOH. This NaOH
volume is Vao.
Observation:
Example:
When time (t) = 10 minutes. K=
2.302\08yo-V1o
10
Calculate the values of K at intervals of time. Thevalue of K gives the value of rate constant, K.
Result:
The rate constant for acid catalyzed hydrolysis ofethyl acetate is ...... .min!.
Precautions:
Temperature of reaction mixture should be constant throughout the course of the reaction.
ii) The reaction must be stopped before carrying out the
to ice cold water. titration of the sample by adding it
Partition coefficient of succinie acid
Aim: Determine the
partition coefficient of
liquids. succinic acid in system of two immiscible
Apparatus: 4
beakers.
separation funnels (100 m), 4
titrimetric
flasks, 2 burettes, pipcttes, 8
1.
Prepare 4 mixtures of butanol, water and
succinic acid into separationfunnels
following the Table 1.
2.
Shake gently the separating funnels with
3. Put them to the holders and prepared solutions for 20 min.
wait a few minutes until the
separated into two clear layers: lower layer is water mixture is apparently
(Org). (Wat), andupper layer is butanol
4. Pour carefully the water phase into a
beaker using the
5
Transfer the water solution from the beaker into two funnel's valve.
using pipette (V=5 ml). titrimetric flasks, 5 mlper flask,
6.
Add 2-3 drops of
7. phenolphthalein.
Fill aburette with a standard solution of
8. NaOH (titrant) and performtitration.
When the endpoint of titration has been
the burette (Vr). Write it down tothe table
reached, read the used volume ofNaOH from
9 Table 2.
Repeat the procedure for funnels 2 -4.
l0.
Proceed in the same way the upper layer
1-4. (butanol) of the mixtures in thefunnels
No,
Calculation:
Calculate the average volume of titrant (V)from 2titrations of the
2
the Table 2.
Succinic acid is a diprotic acid. Process of titration is
samesolution in
based on theneutralization
reaction:
CH,-COOH CH,-COONa
CH,-COOH +2 NaOH ’ |
CH,-COONa +2 H,0
3.
Calculate the concentration of succinic acid in the
respectively, for each composition of the partitionwater and organic phase,CWat, COrg
titration). Remember, theanalyte is the mixture(according to manual for
Calculate the partition coefficient ksuccinic
4.
acid.the volume of VA=5 ml.
of succinic acid at
thepartition mixture. each composition of
k= CorCwatg
5.
Express the average value of the
partition coefficient k fromn four
Table.1. Composition of experiments.
Funnel partition mixtures.
1
2.
NumberSuccinicacid
20
(mL) Water (mL)
1-butanol (mL)
10 15
3 15
15 15
4
10 15
10
15
Table 2.
Experimnental data.
No. Volume of titrant VT (mL)
1-butanol K=
Mean (Corg) I Water Corg
1. II
2.
Mean (Cwat) Cwat
3.
4
Determination of the Strength of an Aeid by pH Meter
(0.5N
Aim:
Determinethe
strength of a weak acid (acetic acid) by titrating with strong base
NaOH) using pH meter and in 250 ml of
estimatec the amount of an acetic acid present
the given nsolution. (You are provided with 0.5N standard NaOH solution).
Measuring
Apparatus: pH - meter, Calomel and glass electrodes (pH-cel), Beaker, Burette,
jar.
Chemicals: ..5N NaOH, Acetic acid. Buffer solutionn(pH =4.0), Acetic acid.
Principle:
pH of the exterior
up the
At 25°C the potential of a glass electrode, depends upon
solution according to the following equation.
Eç = E + 0.0591 log [H*]
Eç = E - 0.0591 pH
electrode with
The pH of the solution can be determined by combining the glass
eference electrode like calomel electrode as follows.
0.1 NHCt/Pt
Pr/Hg, H9;Cl,/KCl (satd. soln. )//Experimental sol./glass,
25°C = 0.242 V
The potential of the saturated calomel electrode at
Ecels =ER - E,
Eçell Eç - Ecalonel
Eçell = (E- 0.05916 pH) - 0.242 V
0.05916 pH =E- 0.242 V- Ecel
E- 0.242 V - Ecell
pH = 0.0591
Procedure:
of the pHmeter at 30°C.
a) Fix the temperature controller
solution (pH-4).
b) Standardize the pH meter using a buffer
acid (acetic acid) in a beaker. Dip the calomel and glass
c) Take 100 ml of the given
electrodes into the solution.
pH value on the pH meter before adding alkali.
d) Read the
standard 0.5N NaOH solution from the burette, stir the solution
e) Add 1 ml of the
carefully and read pH.
readings.
time) and note the pH
addition of NaOHI mlat a few
of
more additions the alkali,.
f) Continue the slowly. Afer a
pH changes ml is the end point
g) In the beginning the observed which is let V,
sudden rises in the pH of
the solutionis
five more readings. endpoint. Take new
batch of acetic
and thereafter take at least exact
order to get the notethepH value. Continue the
h) Repeat the experiment in NaOH solution and
acid solution and add V,-3 m of and note down the pH each time
total of V+3 mL
addition of 0.2 mL of NaOH up to
carefully.
Observation:
ph
Endpoint V, ml
NaOH (ml)
dpH
Plot of -Vsvolume of NaOH.
dV
dpH
ba End point V, ml
V NaOH
Normality of given acid:
We know that.
=NV: (Acetic acid Solution)
N,V, (NaOH solution) V,= 100 ml
V,= (firom graph 2)
N =0.5N N =?
N, VË N
Normality of the acetic acid = N2= V2
Result:
Normality of given acid is = N
Amount of acid present in the 250 ml of the solution =
Conductometric Titrationof strong Acid vs Strong Base
Principle: (1) is
titrations works on the principle of Ohm's law. As current
Conductometric as
Resistance (R) and the reciprocal of resistance is termed
inversely proportional to
(mho) cm
Conductance, and its unit is Siemen on the number of ions and
their
of a solution depends
The electrical conductivity NaOH, the addition of a base (NaOH) to
titration of HCI versus
mobility. For example, in the conductivity of the solution, due to the replacement
cause changes in the ions (Na). Such a
an acid (HCI)would less mobile sodium
hydrogen ions (H) by the end
of the highly mobile
intersects at a particular point, known as the
one line which
titration curve consists of
point or equivalence point.
Conductance
titration of a strong
Fig, 1: Conductometric
base (NaOH).
cm'of Na)H acid (HCI) vs.a strong
Procedure:
by using standard 0.1 N KCI
meter is calibrated or standardized
1. The conductivity cm).
(14.12 millisiemens /
solution
beaker and then it is make up to
pipette out in a clean
HClsolution is
2. 10 ml of given water. of
by adding 90 ml distilled beaker and the initial conductance
100 ml the
conductivity cell isimmersed in constant.
3. Now, the solution and keeping it
stirring the
taken by
the solutionis
4.
Then, 0.S ml portions of NaOH is added from the burette and stirred well. The
6.
conductance of the solution for each addition is to be noted.
Upon addition of NaOH there values till the end point
of acid is reached. will be decrease in conductance
7.
er tnat, the conductivity values increases suddenly due to the
ions. conductance of OH
8
O ne graph with resDect to the vounme of
NaOH consumed versus corrected
conductance. From the intersection point on the graph which gives one minimunm
of the
9 conductance value represents the equivalence points of HCI.
The conductivity is corrected by v+V
multiplving with the factor where '' is the
ordne OT base added and 'V' is the volume of acid solution initially
beaker. taken in the
10.
From known concentration of NaOH
solution. calculate the concentration of HCT
present in 100 ml of the solution.
12.
Graphical calculations and other calculations are to be shown in
formulas, units, results etc. format vwith all
Table:
S.No.
Volume of
NaOH
consumed, V(ml) Conductance (C) CorrectedConductance
C'=C 100+V)
100
Known Unknown Known Unknown
Concentration of NaOH(N)=
Volume of the NaOH at end point (Vi) =
Volume of the HCI has taken initially (Vi) =
Concentration of HCI(N) = ?
As we know
N, V,(NaOH) =N, V2 (HCI)
N,V
Concentration of HCI (N)
V
1. The values of the corrected conductivity are plotted as ordinate (y - axis) against the
volume of NaOH solution added as abscissa (x -axis).
2 The point of intersection of the 2 curves gives the volume of NaOH solution at the
equivalence point.
3 The volumes of the unknownacid solution and the amount of HCland HCl present in
100 ml of the supplied solution are to be calculated.
Note:
Handle the instrument, electrodes (cell), glassware with care. Avoid parallax error
while taking the readings. The electrode should not touch the walls of the beaker.
Results
Strength of HCI= .. . . . . . .
Aim:: Determine the
Viscosity of oil by
redwood
viscosity of oil by viscometer
Apparatus:
Ivatch.
Redwood
Redwood viscometer (with viscometer method.
variable
Chemicals: oil (300ml).
temperature setup), thermometer and stop
Theory
Viscosity is the
measure of fluid friction
resulting when alayer of fluid is which can
due to the forces of made to move in be considered as the intermal friction
Viscositymay be detined cohesionbetween
as "the
the molecules of relationship
the fluid.
to another layer. It is
mainly
unit velocity gradient tangential force per unit area which is required to
system is poise. between twoparallel layers. It is denoted byn(eta). Its unitmaintain a
in CGS
The kinematic viscosity (also
called "momentum diffusivity") is the ratio of the
the density of the fluid p. viscosity n to
Redwood Viscometer
Redwood Viscometer determines the viscosity in terms of seconds, a time
through a standard orifice and collection of the same oil in 50 cc flask. taken by oil to pass
The redwood viscometer consist of vertical cvlindrical oil cup with an orifice in the center of
its base. The orifice can be closed by a ball. Ahook pointing upward serve as a guide mark
for filling the oil. The cylindrical cup is surrounded by the water bath. The water bath
maintain the temperature of the oil tobe tested at constant temperature. The oil is heated by
heating the water bath by means of an immersed electric heater in the water bath, The
provision is made for stirring the water, to maintain the uniform temperature in the water bath
water bath. This viscometer
and to place the thermometer to record the temperature of oil and
From the kinematic viscosity the
is used to determine the kinematic viscosity of the oil.
dynamic viscosity isdetermined.
Viscosity = Apt - Bp/t
Kinematic viscosity = viscosity /p = At - B/t
for 50 m! of oil, and
are
B instrument constants, t is the time of flow in second
Where A and
density of oil. The values of Aand B are:
pis the
B
A
Time offlow in seconds 1.79
0.00260
34-100 0.50
0.00247
>100
Procedure
water.
1. Fillthe outer bath with level indicated br marker point.
with oil to the required oii alo
2. Fillthe oil cup temperature by lifting the baliabove the orifice hole and
3. Take a reading at room stop watch) and collect 50 ml
of oi! in the
pass through it (start the
the oil to
volumetric flask. Note down the time.
temperature to 100 °C.
4. Heat the water at uniform lift the bal! above theorifice hole.
temperature of oil is attained.
S. When required watch) and collect 5 m! of oi! in, the
through it (start the stop
6. Allow the oil to pass
volumetric flask.
viscosity of oil measured.
The measured seconds is in terms of
7
Cand 0°C.
8. Repeat the experiment to get more readingS at 90 °C, 80 °C. 79 °C. 60
Graph :
The following graph has to be drawn
(1)Temperature Vs Redwood seconds
(2)Temperature VsKinermatic Viscosityry
oCis
RESULT: The viscositv of given oil sample sing Redwood viscometer a:
PRECAUTIONS::
1. Theoi! shou!d be filtered thoroughly a muslin cloth to remove solid vartieles that mav
clog the jet.
2, The receiving flask should be placed in such a manner ihai the oil strean îom ie:
strikes the neck of receiving flask and do not cause any toaming.
3. After each reading the oil should becompletely drained out of receiving ilesk.