B1-CONDUCTOMETRIC ESTIMATION OF ACID MIXTURE

Take given acid mixture (HCI & CH,COOH) in a clean 100 ml beaker. Dip the conductivity cell
in the solution and note down the specific conductivity of the solution i.e., when the volume
of NaOH added zero. Now, add standard NaOH solution from the burette in increments of
0.5 mL.
After each addition stir the solution gently and note down the specific conductivity. As the
titration proceeds, the specific conductivity decreases gradually then rises slowly and finally
rises sharply. Continue the titration until the conductance more or less the same as it was
beginning.
Plot a graph of specific conductivity against volume of NaOH to get three straight lines and
determine the concentration of both HCl and CHCOOH. Knowing the normality and amount
of NaOH required for neutralization, amount of HCl and CH,COOH is calculated.
Observations and calculations:
Solution taken in the burette: Standard NaOH (NNaOH = .....N
Solution taken in the beaker: (HCI + CH,COOH) (50 ml of test solution)
Electrode: conductivity cell

Volume of NaOH(VB ml) Specific conductivity, k (mS • cm'

0.5

Estimation of HCI :
Volume of NaOH required to neutralize HCl from the graph = V,
N1V1, = N2V2 or Nnaoh*Vhcl=Nnaoh*Vnaoh
* Normality of HC1 = Nнcl = Nnaoh *Vnaoh/Vhcl =….*…/50 N
The amount of HCl in the given solution = Nhcl X Equivalent weight of HCI (36.5) g/L
=...... × 36.5 g/L = g/L
Estimation of CH3COOH :
Volume of NaOH required to neutralize CH,COOH from the graph = V3 = (V2- Vi) = ...... ml
It is known that, NIV, = N2V3 or NcH,соон × V сн,соон = NNaOH × VNaOH
Normality of CH,COOH = NcH3COOH = NaoH * VaOH/CH3 COOH=……*……/50N
The amount of CH COOH in the given solution =
NcH,coo X Equivalent weight of CH,COOH (60) g/L =
= × 60 g/L
= g/L
B2. POTENTIOMETRIC ESTIMATION OF (FAS) BY USING K,CR207
Take the given volume of FAS solution in a beaker. Add one test tube full of dilute H2SO4.
Immerse the calomel electrode & platinum electrode into the solution. Connect the
electrodes to a potentiometer & measure the cell potential. Now, add K2C20, from a micro-
burette in increments of 0.5 ml with subsequent measurements of cell potential after each
addition. A sudden rise in cell potential is observed at the equivalence point. Take at least 6-
8 readings after crossing the equivalence point.
Plot a graph of AE/AV against Volume of K2C20, & determine the equivalence point. From
normality and volume of K2Cr20, consumed, calculate the normality & weight of FAS in the
given solution
Observations and calculations:
Solution taken in the burette: Standard K2Cr2O7 (Nk2cr207=0.5N___)
Solution taken in the beaker: 25 ml FAS + 1 test tube full of dilute H2O4
Electrodes: Platinum electrode (Indicator electrode) + Calomel electrode

Volume of E mV Delta E mV delta V ml DELTAL E/Delta

K2Cr2O7 (ml) V
0 ---- ==== ----
0.5
Equivalence point from the graph = Vk2cr2o7= ml
N1V1=N2v2 or Nfas x Vfas = N K2CR207, x VK2 CR207
Normality of FAS, NFAS= NK2CR207 *VK2CR207 /VFAS =…*…./25N
The amount of FAS in the given solution = Nfas x Equivalent weight of FAS (392) g/L
=____x 392 g/L
DETERMINATION OF pKa VALUE OF VINEGAR USING pH
SENSOR
Take the given volume of weak acid in a beaker and immerse the combined glass electrode
into the solution. Connect the electrode to a pH-meter and measure the pH. Now, add NaOH
from the micro-burette in increments of 0.5 ml with subsequent measurements of pH after
each addition. A sudden rise in pH is observed at the equivalence point. Take at least 6-8
readings after crossing the equivalence point.
Plot a graph of ApH/AV against Volume of NaOH & determine the equivalence point. Plot
another graph of pH against Volume of NaOH & determine pKa value of the given weak acid.
Observations and calculations:
Solution taken in the burette: NaOH solution
Solution taken in the Beaker: Given volume of Weak Acid
Electrodes: Combined glass electrode (Ag-AgCl + glass electrode)

Volume of pH Delta pH Delta V Delta pH/Delta

NaOH (ml) V

0.5
1. Equivalence point
from the graph, Delta pH / Delta V vs volume of NAOH =P=__ML
2. Half equivalence point= P/2=__ml
3. pKa value of the given weak acid (from the graph- pH vs Volume of NaOH)=___
B4. ESTIMATION OF TOTAL HARDNESS OF WATER BY EDTA
METHOD
A. Preparation of standard Na EDTA solution:
Weigh the given Na2EDTA crystals into a clean 250 ml standard flask. Add 5 ml of 1:1
ammonia, a little of distilled water, dissolve the crystals and dilute up to the mark with
distilled water. Shake the solution well. Calculate the molarity of solution.
molarity of NA2EDTA =weight of NA2EDTA *four /molecular weight of NA2ETA (372 )
B. Determination of total hardness of water:
Burette : Standard Na2EDTA solution
conical flask : 25 ml of hard water sample + 2 ml NH4OH - NH4Cl buffer solution (pH = 10)
Indicator : Eriochrome black - T (a pinch of indictor)
Colour change at end point: Wine red to clear blue
From the molarity and volume of NazEDTA consumed, calculate the total hardness of the
given water sample
Observations:
A. Preparation of standard NazEDTA solution:

Weight of weighing bottle + Na2EDTA crystals=W1=___g

Weight of weighing bottle after transferring Na2EDTA crystals=W2=____g
Weight of Na2EDTA transferred = W = w1-w2= ____g
Molarity of Na2EDTA solution, Y= 4 *W/372.25=____M

reading Trial 1 trial 2 trial 3

Final burette reading
initial
difference
Calculation:
It is known that
1000 ml of 1M NazEDTA solution = 100 g of CaCO3
(Molecular weight of CaCO3 = 100)
1 ml of 1M Na2EDTA solution= 0.1 g of Caco3
V ml of YM Na2EDTA solution= 0.1 *V *Y g of CACO3
Z=____ g of CACO3
25 ml (= 25 g) of hard water = Z =__g of CACO3
10^6 ml (= 10(6)g) of hard water= Z *10(6)/25=__g of CACO3
Total hardness of given sample of water=___ppm

Estimation of Copper present in electroplating effluent by optical sens. (colorimetry)

Take 5ml, 10ml, 15ml, 20ml & 25ml of given cupric sulphate solution into a 5 separate 50 ml
volumetric flasks. Add 5 ml of 1:1 ammonia to each one of them and also in the test solution
of unknown volume. Dilute up to the mark with distilled water & shake well. Prepare a blank
solution by diluting 5 ml of 1:1 ammonia with distilled water up to the mark in a 50 ml
standard flask and shake well. Measure the absorbance of each of the standard solution
against blank solution at 620 mm on the colorimeter.
Plot a calibration graph of Absorbance (O.D.) against volume of copper sulphate solution &
determine the volume of copper by comparison. Calculate the volume and amount of
copper in the test solution

Volume of CuSO,(ml) Volume ofAmmonia(ml) Absorbance

5,10,15,20,25 5
Test solution, blank sol 5

Calculations:
Given, 1ml of stock solution contains 8 mg of CuSO4.5H20
249.55 mg of CuSO4.5H20 = 63.55 mg of copper
8mg of CuSO4 5H20= 63.55×8/249.55 = 2.037MG of cu
i.e., 1 ml of stock solution = 2.037 mg of Copper
Volume of the test solution from the graph = z=__ml
Therefore, Weight of Copper in the given test solution = 2.037 X Z mg=__mg
C2-DETERMINATION OF VISCOSITY COEFFICIENT OF LUBRICANT
USINGOSTWALD'S VISCOMETER
Fix a clean & dry viscometer vertically in a thermostat. Pipette out 25 ml of the given organic
liquid into wider limb of the Ostwald"s viscometer. Suck the liquid into the capillary limb.
Allow the liquid to flow. Determine the time for its flow from upper mark (above the glass-
bulb) to lower mark (below the glass-bulb). Repeat for concurrent readings. Pour out the
liquid, wash, rinse with acetone & dry it in the oven and then cool Fix the viscometer
vertically. Pipette out 25 ml of distilled water into the wider limb & determine the flow time
for water. Knowing the densities of water and test liquid, and viscosity of distilled water at
thermostat temperature, the viscosity of the test liquid can be calculated.
Viscosity coefficient of liquid, nl= nw *tl*dl/twdw
where, tl, tw are flow times and dl, dw are the densities of the test liquid and distilled water
respectively and wis viscosity coefficient of water.
Observations and calculations
Temperature of the thermostat = 28c

Flow time (seconds)

Trial 1, trial2, trial3 average
Test liquid, water Tl, tw

Time of flow of test liquid t1=15.133 s

Density of test liquid D1=0.9963g/cm3
Time of flow of water tw=14.967s
Density of water DW= _0.9967____g\cm3
Viscosity coefficient of water nw= __8.545__ milipoise
Viscosity coefficient of the test liquid, n, =nw *t1 *D1/ tw *dw =___ milipoise/Nm2

C5. DETERMINATION OF COD OF WASTE WATER

A. Preparation of standard FAS solution:
Weigh the given FAS crystals into a clean 250 ml volumetric flask. Add 1 test tube full of
dilute H2O4. Add a little of water, dissolve the crystals, dilute up to the mark with water and
shake
Normality of FAS =weight of fas * 4 /Equivalent weight of FAS (392.13)
B. Determination of COD of waste water sample:
Solution taken in the burette: Standard FAS solution
Solution taken in the conical flask: 25 ml of waste water sample+ 10 ml of K2CrO, solution +
1 test tube full of 1:1 H2504
Indicator: Ferroin (3 drops)
Color change at end point: Bluish green to reddish brown
Perform a blank titration in the same way as above except waste water. Knowing the
normality and volume of FAS consumed for main titration and for blank titration, calculate
the COD of the given water sample
Observations:
A. Preparation of standard K2Cr2O7 solution:
Weight of weighing bottle + K2Cr2O7crystals=W1=___g
Weight of weighing bottle after transferring K2Cr2O7crystals=W2=____g
Weight of K2Cr2O7 crystals transferred = W = w1-w2= ____g
Normality of K2Cr2O7solution, Y= 4 *W/392=____N

reading Trial1 Trial2 Trial3

Final burette
reading,initial,
differencein(ml)
Concordant reading (v)= ml
Blank titer value B= ml
Calculations:
It is known that,1000 ml of 1 N FAS = 8 g of oxygen
1 ml of 1 N FAS= 0.008 g of oxygen
Consumption of K2Cr20, by 25 ml waste water in terms of FAS= (B - V) ml of Y molar FAS
(B - V) mi of Y molar FAS = Y x (B - V) x 8 mg of oxygen
= Z=0. 0290816x8 mg of oxygen
25 ml of waste water requires, Z=1.4192 mg of oxygen
1000 ml of waste water requires z*1000/25 __ mg of oxygen
The chemical oxygen demand (COD) of the given sample of waste water____ppm/mg/L