Assignment 1

01. Practical: Determination of End Point of Titration Using pH Meter

Frequently an acid or a base is quantitatively determined by titration using pH meter to
detect the equivalence point rather than using a visual indicator. After running a
titration with the drop wise addition of titrant (NaOH, C = 0.2M) to find out the location
of the equivalence point, the obtained results are mentioned in the below table.
i. Plot a graph which shows the general pattern of how the pH changes when a
strong acid reacts with a strong base using excel sheet.
ii. Find out the volume of NaOH required for complete neutralization of HCl from
the graph.
iii. Find out the unknown concentration of HCl. (Volume of titrand, HCl is 40.00 cm 3)

Volume of Volume of Volume of

NaOH added pH NaOH added pH NaOH added pH
(cm3) 3
(cm ) 3
(cm )
0.00 1.15 8.50 1.52 17.00 11.54
 0.50 1.16 9.00 1.56 17.50 11.60
1.00 1.17 9.50 1.58 18.00 11.74
1.50 1.18 10.00 1.67 18.50 11.79
2.00 1.19 10.50 1.71 19.00 11.82
2.50 1.20 11.00 1.76 19.50 11.84
3.00 1.21 11.50 1.81 20.00 11.89
3.50 1.22 12.00 1.92 20.50 11.93
4.00 1.25 12.50 1.98 21.00 11.95
4.50 1.29 13.00 2.08 21.50 11.97
5.00 1.30 13.50 2.23 22.00 12.00
5.50 1.32 14.00 2.31 22.50 12.04
6.00 1.33 14.50 2.51 23.00 12.05
6.50 1.37 15.00 3.01 23.50 12.06
7.00 1.39 15.50 10.49 24.00 12.07
7.50 1.42 16.00 11.28 24.50 12.09
8.00 1.44 16.50 11.48 25.00 12.13

02. Practical: Conductometric Titration - Determination of the concentration of

an acid solution using conductometric titrations.

Volume of NaOH added (cm3) Conductance (µS) 24.00 4.22

0.00 19.08 24.50 4.36
 0.50 18.46 25.00 4.49
1.00 17.91 26.00 4.75
2.00 16.71 27.00 4.96
3.00 16.08 28.00 5.21
4.00 15.13 29.00 5.42
5.00 14.22 30.00 5.57
6.00 13.45 31.00 5.76
7.00 12.66 32.00 6.02
8.00 11.89 33.00 6.25
9.00 11.15 34.00 6.39
10.00 10.51 35.00 6.58

11.00 9.84

12.00 9.21

13.00 8.68

14.00 8.06

15.00 7.44

15.50 7.09

16.00 6.84

16.50 6.56

17.00 6.42

17.50 6.16

18.00 5.83

18.50 5.49

19.00 5.30

19.50 5.10

20.00 4.93

20.50 4.60

21.00 4.38

21.50 3.94
 22.00 3.81

22.50 3.90

23.00 4.01

23.50 4.13
Conductometric method can be used to determine the end point of ionic titrations as
conductance of electrolyte depends upon i) number of free ions, ii) changes on the free ions
and iii) mobility of the ions on the substitution of one ion by another of different mobility
(speed of ions).

When hydrochloric acid solution (HCl) is titrated with sodium hydroxide solution (NaOH), the
highly mobile hydrogen ions are progressively replaced by slower moving sodium ions and the
conductance of the solution decreases. After the end point, the conductance of the solution
rises sharply due to the presence of excess, highly mobile hydroxide ion. Thus the neutralization
of a strong acid by addition of a strong base leads to a minimum conductance at the end points.
This is due to the disappearance of H+ ions and their replacement by slower moving Na + ions of
the base followed by the presence of highly mobile OH– ions after the end point.

After running a titration with the drop wise addition of titrant (NaOH, C = 0.1M) to find out the
location of the equivalence point, the obtained results are mentioned in the above table.

i. Plot a graph between conductance and volume of titrant (NaOH solution) using
an excel sheet. Two intersecting lines will be obtained and the points of
intersection of these lines represent the equivalent point.
ii. Find out the volume of NaOH required for complete neutralization of HCl from
the graph.
iii. Find out the unknown concentration of HCl.(Volume of titrand, HCl is 40.00 cm 3)
 03. Practical: Determination of concentration of KMnO 4 solution using UV-Vis

spectroscopy.

UV- Vis spectroscopy is a technique that uses the absorbance of light in UV and Visible part of
the electromagnetic spectrum by an analyte at a certain wavelength to determine the analyte
concentration. Permanganate ions absorb visible light at 520 nm. It is possible to determine the
concentration of unknown KMnO4 solution by UV-Vis spectroscopy with the help of Beer
Lambert Law.

The measured absorbance values of prepared standard KMnO 4 solutions and unknown KMnO4
solution are mentioned in the table below. (Chosen wavelength is 520nm)

i. Plot a calibration curve using an excel sheet.

ii. Find the concentration of unknown KMnO 4 solution (C) from the plotted calibration
curve.

Concentration of standard KMnO4 solution Absorbance value at 520 nm wavelength

(mol dm-3)
0.0001 0.214
0.0002 0.421
0.0003 0.650
0.0004 0.846

Concentration of unknown KMnO4 solution Absorbance value at 520 nm wavelength

(mol dm-3)
C 0.722
 04. Practical: Measurement of Chemical Oxygen Demand.

The chemical oxygen demand (COD) is a measure of the amount of chemicals (usually organics)
that consume dissolved oxygen. Organic matter in aqueous samples may be determined by
oxidation with dichromate. The amount of O 2 that is chemically equivalent to the dichromate
consumed is defined as the chemical oxygen demand (COD) of the water sample. The excess
dichromate is determined by means of an oxidation-reduction titration with ferrous ammonium
sulfate using an Fe(II)-orthophenanthroline complex as an indicator. This method is a “back
titration” in analytical chemistry. Since it is difficult to express the concentration of the myriad
of oxidizable organic substances in a sample, COD results are expressed as the amount of
oxygen (in mg O2/L) necessary to carry out the oxidation of the sample to CO2 and H2O.

The experiment was carried out as follows:

Add 50.00ml of standard 0.02M K2Cr2O7 into a 500ml Erlenmeyer flask.
While stirring slowly add 50ml of 9M H2SO4.
Cool down the mixture to room temperature under a stream of tap water.
Add 25.00ml of waste water sample and mix well.
Boil the solution for 1 hour while covering the sample with small watch glass to minimize the
evaporation loss.
Then dilute the content of the flask to about 250ml with deionized water and cool the solution
to room temperature.
Add five drops of ferroin indicator.
Titrate with 0.15M ferrous ammonium sulphate.
Continue the test for 3 replicate samples and 3 blank tests using distilled water as the blank.
At the end point of titration:
The average volume of ferrous ammonium sulphate for the blank sample (ml): 38.70 ml
The average volume of ferrous ammonium sulphate for the waste water sample (ml): 32.20 ml
 i. Write down complete balanced equations for the reactions with half reactions and
derive the formula to determine COD.
ii. Calculate the chemical oxygen demand (COD) with the following formula.
 ( A−B ) ×t×8000
COD ( mg O2 / L )= ×f
V
where:
A = volume iron ammonium sulfate solution for the blank (mL)
B = volume iron ammonium sulfate solution for the Sample (mL)
t = normality of the iron ammonium sulfate solution (N)
V = volume Sample (mL)
f = dilution factor

Assignment 2
1. Label the diagram using glassware names correctly.

a
b
2. When add 2 ml of Na2SO4 into 1 ml of acidified BaCl 2
c
solution, what observations can be obtained.

3. The flames obtained

d by heating some group 1 and group
2 cation containing samples (CaCO3, KCl, NaNO3, SrCl2)
were given ebelow. Identify the compound and cation
present ina each b c by observing its flamedcolour.
sample
4. About 2 ml of colourless solution was mixed with 3 ml of FeSO 4 solution in a test tube and it
was kept in an ice bath. When add 2 ml of chilled conc. H 2SO4 through the wall of the test tube
into previous chilled mixture brown colour ring was observed at the interface of solutions as
given below. Identify the anion present in the colourless solution.

Brown ring

5. How to prepare standard solution of 500.00 ml of 0.05 M Potassium dichromate solution.

6. When you mix same volumes of 2 M HCl and 2 M NaOH into a test tube, you feel the test
tube is heated. What is the reason for this observation?

7. When you heat Mg ribbon in a bunsen flame white powder was observed.

i. What compound contains in above mentioned white powder.

ii. Explain the above reaction with the type of chemical reaction.

8. When place Cu metal in a 15 ml of 0.4 M AgNO 3 solution for 15 minutes to react undisturbed,

i. What observations can be taken on the metal and explain it using a chemical equation.

ii. What observations can be taken in the solution and explain it using a chemical equation.

iii. Write the overall reaction for above reaction.

9. Write the balanced chemical equations for the following reactions.

i. Pb(NO ) (aq) + CuSO (aq)

32 4
ii. NaCl (aq) + AgNO  (aq)  
3

10. The results obtained after carrying out the benedict test for sucrose, glucose and starch are
given below.

Sample A: The following colour change was observed.

Sample B: No observe any colour change. But when doing the benedict test after
addition of HCl, the above mentioned colour change was observed.

Sample C: No observe any colour change even after addition of HCl.