LAB MANUAL

ANALYTICAL TECHNIQUES (I)

LABORATORY EXERCISES
COURSE NO: AC 407
2ND YEAR 3RD SEMESTER

1
S-NO CONTENTS PAGE NO

1 POTENTIOMETRIC LOCATION OF END POINT

2 DETERMINATION OF PHOSPHATE/ NITRATE ION

GIVEN FERTILIZER BY A ELECTRO ANALYTICAL
METHOD

3 DETERMINATION OF VITAMIN C IN GIVEN TABLET

4 DETERMINATION OF ACETIC ACID IN VINEGAR

5 PREPERATION OF BUFFER SOLUTIONS

6 PREPERATION OF BAUME SOLUTIONS

7 CONDUCTOMETRIC LOCATION OF END POINT

2
 INDEX
No. Date Experiment Page Initial Remarks
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           
           

3
 EXPERIMENT 1
OBJECT: POTENTIOMETRIC LOCATION OF END POINT
Chemicals:

1M NaOH, unknown acidic solutions A and B.

Theory:

Potentiometric titration is a volumetric method in which the potential between two electrodes is
measured (referent and indicator electrode) as a function of the added reagent volume. The most
common potentiometric measurement is that of pH. pH was defined originally as − log + H or
log(1/C + H) , where C+ H is the concentration of hydrogen ion. Today instead of C+ H one would
write a+ H , the activity of hydrogen ion.
The measurement of the pH of a solution is simple in principle, of it is based on the measurement
of the potential of hydrogen electrode immersed in the solution. The left-hand, i.e. the reference
electrode of the cell is typically a saturated calomel electrode (SCE) with potential E(cal). The
pH of the cell is therefore
E+ E ( cal )
pH=
( −RT
F ) ln10

Procedure:

Calibrate the pH meter with the help of standard buffer solutions of pH 7 & 4

Take 20 ml sample in 50 ml beaker, Dip the electrode & note the pH of sample. Now add 1 ml
base from burette and note the pH on each one ml addition of basic solution till the value is fairly
constant i.e. pH 14
Repeat same step for sample B

4
Observation:

FOR SAMPLE A

Volume of PH ΔH ΔPH ΔPH/ΔV Δ^2H/ΔV^2

NaOH
0          
1          
2          
3          
4          
5          
6          
7          
8          
9          
10          
11          
12          
13          
14          
15          
16          
17          
18          
19          
20          
21          
22          
23          
24          
25          
26          
27          
28          
29          
30          
31          
32          
33          
34          
35          

5
 36          
37          
38          
39          
40          

FOR SAMPLE B

Volume of PH ΔH ΔPH ΔPH/ΔV Δ ^2H/ΔV ^2

NaOH
0          
1          
2          
3          
4          
5          
6          
7          
8          
9          
10          
11          
12          
13          
14          
15          
16          
17          
18          
19          
20          
21          
22          
23          
24          
25          
26          
27          
28          
29          
30          
31          

6
 32          
33          
34          
35          
36          
37          
38          
39          
40          
41          
42          
43          
44          
45          
46          
47          
48          
49          
50          

Calculation:

1. Draw graphs b/w pH & vol. of base utilize & find out the concentration of unknown
acidic solutions.
2. Find the end point by First & Second derivative method and calculate the strength of
acids.

FOR SAMPLE A AND B

7
Result:

8
 EXPERIMENT 2
OBJECT: DETERMINATION OF PHOSPHATE/NITRATE ION IN
GIVEN FERTILIZER BY A ELECTRO ANALYTICAL
METHOD

Chemicals:

Fertilizer, 1 – 2M HCl, 0.01M NaOH.

Theory:

Ion exchange is an exchange of ions between two electrolytes or between an

electrolyte solution and a complex. In most cases the term is used to denote the processes of
purification, separation, and decontamination of aqueous and other ion-containing solutions with
solid polymeric or mineral 'ion exchangers'
Ion exchange resins are highly ionic, covalently cross-linked, insoluble polyelectrolytes supplied
as beads. There are two general types of ion exchange resins: those that exchange positive ions,
called cation exchange resins, and those that exchange negative ions, called anion exchange
resins.
The "reactivation" process is called regeneration and is carried out using a strong acid for the
cation (as a source of hydronium ions) and liquid caustic (sodium hydroxide) as a source of
hydroxyl ions for the anion. Resin is regenerated on site using hydrochloric or sulfuric acid and
sodium hydroxide (caustic) to regenerate the cation and anion resin respectively
When solution of fertilizer is passed through the column the cation ions present in it form acid
and washed out through the column which is then neutralize with base.

Procedure:

Prepare a column of cation exchange resin. The resin bed should be about 20 cm long and 1cm
wide and it should be free from air bubbles. Wash the column with 50 ml water then regenerate it
with 20 ml 1M HCl. Again wash it with 50 ml water to remove the excess HCl from column.

Weigh accurately 0.8 – 1 gm of given fertilizer and dissolve in 10ml distilled water. Introduce
concentrated hydrochloric acid 0.1 – 0.5ml (it converts all the phosphate to phosphoric acid/
nitrate to nitric acid). The pH of this solution should be less than 2. Pass the sample solution,
through resin column and collect the sample in another 250 ml beaker. Wash the column with
250 ml water. Now collect all the washing in separate beaker. After 150 ml of water has passed
out, freshly collect 20 ml solution in small beaker and note the pH. If pH of the effluent is more
than 4 it means washing of the column is complete.

Measure the total volume of affluent and titrate 20 ml of it with 0.01 M NaOH by using
potentiometer.

Observation:

9
S NO VOLUME OF BURETTE (ml) PH

10
 1    
2    
3    
4    
5    
6    
7    
8    
9    
10    
11    
12    
13    
14    
15    
16    
17    
18    
19    
20    

Volume of titrant=
Volume of solution=

Calculations:

Draw graph between pH & volume of NaOH utilize. First inflection point is at 4.5 pH and
second is at 8.5.
Take volume between the two inflection points and calculate the amount of phosphate/ nitrate
ion in given fertilizer.

11
RESULT:

EXPERIMENT 3
OBJECT: DETERMINATION OF VITAMIN C IN GIVEN TABLET

12
Chemicals:

1. 0.1 N Iodine solution.

2. Starch indicator.
3. Vitamin C tablet.

Theory:

Redox titrations are based on an oxidation-reduction reaction between the analyte and titrant.
These most commonly use a potentiometer or a redox indicator to determine the endpoint. There
are two types of redox titrations
1. Iodometric titrations
2. Iodimetric titrations

When an analyte that is a reducing agent is titrated directly with a standard iodine solution, the
method is called "iodimetry".

When an analyte that is an oxidizing agent is added to excess iodide to produce iodine, and the
iodine produced is determined by titration with sodium thiosulfate, the method is called
"iodometry".

Starch is the indicator of choice based on redox titrations involving iodine, since starch forms an
intense blue colored complex with iodine.

Procedure:

Dissolve the given tablet in 250 ml water. Take 25 ml of solution and titrate it with 0.1 N Iodine
solution by using starch indicator. First appearance of the deep blue color shows the end point
which exists for at least 1 minute.

Observation:

INITIAL FINAL
S NO. READING READING DIFFERENCE MEAN
  (ml) (ml) (ml) (ml)
1        
2        
3        
4        
5        

Calculation:

Calculate the number of mg of Vitamin C per tablet by using the given relation.
34 ml of 0.1 N of Iodine solutions react with 300 mg Vitamin C.

13
Percentage:

Result:

EXPERIMENT 4
OBJECT: DETERMINATION OF ACETIC ACID IN VINEGAR
Chemicals:
14
 1. 0.1 M NaOH
2. Phenolphthalein Indicator
3. Natural and synthetic vinegar

Procedure:

Dilute 10 ml vinegar in 250 ml water in volumetric flask. Pipette out 20/ 25 ml solution and
titrate it with 0.1 M NaOH by using phenolphthalein indicator. Repeat the same procedure for
both natural and synthetic vinegar.

Observation:
FOR NATURAL VINEGAR:
INITIAL FINAL
S NO. READING READING DIFFERENCE MEAN
  (ml) (ml) (ml) (ml)
1        
2        
3        
4        
5        

Volume of titrant=

FOR SYNTHETIC VINEGAR:

INITIAL FINAL
S NO. READING READING DIFFERENCE MEAN
  (ml) (ml) (ml) (ml)
1        
2        
3        
4        
5        

Volume of titrant=

Calculation:
Calculate the % acetic acid in viniger sample by using given relation.
1 ml 1 M NaOH required to neutralize 0.06005 gm of CH3COOH

15
16
Result:

EXPERIMENT 5
OBJECT: PREPERATION OF BUFFER SOLUTIONS.

17
Instrument

pH meter
Magnetic stirrer

Theory:

A buffer solution is one in which the pH of the solution is "resistant" to small additions of either
a strong acid or strong base. They are of two types

1. An acidic buffer solution is simply one which has a pH less than 7. Acidic buffer
solutions are commonly made from a weak acid and one of its salts - often a sodium salt.

2. An alkaline buffer solution has a pH greater than 7. Alkaline buffer solutions are
commonly made from a weak base and one of its salts.

(1) WALPOLE ACETATE BUFFER (pH 3.6-5.6)

Stock Solutions:

(i) 0.2 M Acetic acid

(ii) 0.2 M sodium acetate

Mix the stock solutions in the proportions given below and note the pH.

Acetic Acid Sodium Acetate pH Vol.

1. 2 18
2. 4 16
3. 6 14
4. 8 12
5. 10 10
6. 18 2
7. 16 4
8. 14 6
9 12 8
Unknown A 18.8 1.5
Unknown B 10.2 9.8

Calculations:

Draw graph between volume of acetic acid and volume of NaOH against pH

(2) MICHAELIS BORATE BUFFERS (pH 7.6-12.3):

Stock Solutions:
18
 0.1 M NaOH
0.1 M HCl
Borax: 3 gm boric acid + 25 ml 1M NaOH / 250 ml water.
Mix the stock solutions in the following proportions and note the pH.

FOR SAMPLE A
0.1 M NaOH Borax pH Vol
1. 2 18
2. 4 16
3. 6 14
4. 8 12
5. 10 10
6. 18 2
7. 16 4
8. 14 6
9. 12 8

FOR SAMPLE B
0.1 M HCl Borax pH Vol
1. 2 18
2. 4 16
3. 6 14
4. 8 12
5. 10 10
6. 18 2
7. 16 4
8. 14 6
9. 12 8

Calculations:

Draw graph between volume of Borax and volume of NaOH against pH, volume of Borax and
HCl against pH

19
3. Britlon Robinson Buffer (pH 2–12):

Stock Solutions:

 0.04M Acetic Acid

 0.04M Phosphoric Acid
 0.04M Boric Acid
 0.2 M NaOH

Take 10 ml of each acid and prepare 30 ml stock solution and note its pH value.. Now add NaOH
in given proportion and note the pH.

Sodium Hydroxide (ml) pH

1. 5
2. 10
3. 15
4. 20
5. 25
6. 30
7. 35
8. 40
9. 45
10

Calculations:

Draw graph between volume of NaOH against pH

20
 EXPERIMENT 6
OBJECT: PREPERATION OF BAUME SOLUTIONS.
Procedure:-

Transfer the given solution in 100 ml cylinder and with the help of Baume meter note the Baume
concentration. If °Be of solution is less than 33 then increase it with the help of given relation.

100 gm salt when dissolve in 100 ml water then solution is of 33-35°Be

Now transfer the solution again in beaker add 10 ml water in it, mix and transfer in 100 ml
measuring cylinder and again not the Baume concentration. Repeat the same procedure 10 times
and calculate the normality Or Molarity of the solutions.

OR

From the prepared solution of 33°Be make 31°Be, 29°Be, 27°Be, 25°Be and 23°Be solution by
using above given relation. Calculate the normality or molarity of prepared solutions.

Observation:

INITIAL FINAL
S NO. READING READING ADD WATER MEAN
  (ml) (ml) (ml) (ml)
1        
2        
3        
4        
5        

Calculation:

21
Result:

22
 EXPERIMENT 7
OBJECT: CONDUCTOMETRIC LOCATION OF END POINT
Chemicals:

0.1N NaOH, unknown acidic solutions A and B

Theory:

Conductometric titration is a type of titration in which the electrolytic conductivity of the

reaction mixture is continuously monitored as one reactant is added. The equivalence point is the
point at which the conductivity undergoes a sudden change.
In this experiment we shall be concerned with electrical conduction through aqueous solutions.
Although water is itself a very poor conductor of electricity, the presence of ionic species in
solution increases the conductance considerably. The conductance of such electrolytic solutions
depends on the concentration of the ions and also on the nature of the ions present (through their
charges and mobilities). Conductance behavior as a function of concentration is different for
strong and weak electrolytes.
The conductivity of a solution depends on the concentrations and mobilities of the ions present.
It is convenient to define a quantity, the molar conductance Λ,

1000 κ
Λ=
c
Where c is the molar concentration; that is expressed in mol.dm -3. 1000 is the factor arising from
the fact that 1 dm3 =1000 cm3. Thus, the molar conductance is expressed in S·cm 2 ·mol-1. The
molar conductance is sometimes described as the actual conductance of that volume of solution
which contains one mole of solute when placed between parallel electrodes 1 cm apart with a
uniform electric field between them

Procedure:

Set the measuring cell constant on the unit 1.00 cm–1 with control knob K = cm–1 First of all wash
the electrodes thoroughly with distilled water; note the conductance of distilled water at room
temp.

Pipette out 20 ml sample in 50 ml beaker, adjust the electrode and note the conductance of the
sample. Now add 0.5 ml base from burette and note the conductance on each 0.5 ml addition of
basic solution (continuously stir the solution with the help of glass rode).

The observed conductance may either in increasing or decreasing order.

23
Following titrations will have to perform.

1. Sample A with 0.1 M strong base

2. Sample B with 0.1 M strong base
3. Displacement titration ammonium chloride with 0.1 M strong base
4. Displacement titration sodium acetate with 1 M HCl.

Observation:

Normality of HCL=
Normality of NaOH=
Normality of CH3COOH=
SAMPLE A
S NO. VOLUME CONDUCTANCE
  (ml) (mS/cm)
1    
2    
3    
4    
5    
6    
7    
8    
9    
10    
11    
12    
13    
14    
15    

SAMPLE B
S NO. VOLUME CONDUCTANCE
  (ml) (mS/cm)
1    
2    
3    
4    
5    
6    
7    
8    

24
 9    
10    
11    
12    
13    
14    
15    

Calculation:

Draw the graph b/w conductance and volume of base / acid consumed. Find out the end point
from the graph and calculate the strength of unknown solutions.

25
Result:

26