6. QUANTITATIVE SALT-ANALYSIS
6.1 Volumetric Analysis: Definition and Principle
6.2 Use of chemical Balance
6.3 To prepare the standard solution
6.4 Titration
6.5 Script of titration experiment
6.6 Calculation of titration
37
38
Example :
HCL=H++ ClH2SO4=2H++SO4
39
40
2[39+55=16x4]=5x16=10x1
Or 2[158]=10x8=10x1
Or 316/10=8=1 Or 31.6=8=1
Therefore, the equivalent weight of KMno4
is 31.6 into the acidic medium. In the similar
way.
The equivalent weight of oxidization
agent=Molecular weight of substance x2x
Number of atom of the obtain oxidization
agent.
(Note- Hence 2 is multiplied in formula because
the atomic weight of oxygen is 16 is eight times
more then the equivalent weight of oxygen).
Equivalent weight of KMnO4 in the neutral
medium2KMnO4+H2O=2MnO2+2KOH+3O
2KMnO4=3O=6H
2x158=3x16=6H
316=6x8=6H Or 316/6=52.66=8=1
Therefore the equivalent weight of KMnO4
in the neutral medium is 52.66.
Equivalent weight of KMnO4 in basic
medium2KMnO4+2KOH=2K2MnO4+H2O+O
2KMnO4=O
2x158=16=2x8
Equivalent weight=2x158/2=158.
In this way, the equivalent weight of KMnO4 in
Table
Molecular
Weight
36.5
63
98
60
126
56
40
315
35
106
Basisity
Acidity
1
1
2
1
1
x
x
x
x
x
x
x
x
x
x
1
1
2
1
2
Equivalent
Weight
36.5
63
49
60
63
56
40
15705
35
53
41
Marked Bar
Adjustable Screw
Hollow
Stand
Indicator
Scale
Key
42
Weight
50 gm.
20 gm.
10 gm.
5 gm.
2 gm.
1 gm.
Weight of Gram
Figure:
Rider
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
4. The method of taking the reading by rider:Use the rider for weighting below 10 ml.
The zero is marked at the middle of the
balance rod of chemical balance and both sides
have 10-10 blocks., which have 1 to 10
number are marked.
43
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
Weight of Gram
Weight
50 gm.
20 gm.
10 gm.
5 gm.
2 gm.
1 gm.
3.
Fig : Rider
44
(a)
Rider
(b)
Procedure of weighing :
Before taking
weight pan of balance should be cleaned first
and see whether the balance is at equal level. To
bring it in equal level screws then screws on the
edges of the marked rod can be set by rotator if
needed. Rotate the handle and see whether the
indicator goes to and from zero equally or not. If
it does not move equally and screws on the edges
of the marked rod can be set by rotating. The
direction in which indicator covers the more
distance that pan is the lighter one. To make it
right, rotate the screw inside from the heavier pan
or rotate the screw outside from the light is pan.
After checking whether the balance working
properly keep substance in the measuring tube
(clean & dry) in the left pan from the left
window. Keep weight in the right pan from
the right window. First start weighing with
larger weight, then smaller weight are used in
place of larger weight sequentially. After
putting each weight it is cheeked that which
pan heavier.
The direction in which indicated covers more
distance that pan is lighter one. If there is the
need for the weight of less than one gm then
start putting weight of mg. If the weight less
than 10 mg is needed then rider is used. At
first rider is kept on one end point of the right
side of the marked bar and it moves to and
fro from the zero. Observe this situation
carefully this is the exact measurement. Now
take out the weight from the pan & note the
reading.
6. Calculation of weight : Suppose the
following weights are kept on the right pan
for weighing tube & weight of substance.
Gram weight = 5 gm + 2 gm + 1 gm = 8 gm.
Milligram = 500 mg + 200 mg + 200 mg +
20 mg + 10 mg.
= 950 mg = 0.959 gm.
Rider = 3 main parts on the right side + 2
subparts
= 3 0.001 gm + 2 0.0002 gm.
45
= 0.003 gm + 0.0004 gm
Total weight = 8 gm + 0.95 gm + 0.0034 gm
= 89534 gm
weighing tube + weight of substance = 8.9534gm
Similarly,
the weight of weighing tube = 5.3246 gm.
8.
Fig. 6.4
2.
3.
4.
5.
1.
46
Acid :
2.
E N V
gm
1000
When
W = Weight of solote (substance)
E = Equivalent weight of substance
N = Normality
V = Required Volume
From the above formula the required weight
of substance in calculated to prepare standard
47
3.
5.
4.
Fig 6.8 To pour the solution in the flask upto last drop.
Fig 6.9 To wash the funnel and fill the measuring flask
Fig 6.10 To fill the mearuring flask with the help of pipette
48
6.4 Titration
6.4.1 Titration
A known volume and concentration of one
substance is reacted with a known volume of
another substance whose concentration is to
be determined this process is called. titration.
Titration is classified into 3 categories depending
upon the nature of the reaction which happen in
the solutions.
(i)
(ii)
External Indicator
(iii)
Self Indicator
49
H+
Me + + OH
S.No
Solution
used in Titration
Suitable Indicator
for Titration
1.
Methyl Orange or
Phenophthelim one
of them
2.
Methyl Orange
3.
Phenolphthalein
4.
50
Acid
base
Salt
Water
(36.5) (40)
(58.5) (18)
It in clear from the equation that for complete
neutralizes 40 gram of NaOH must react with
36.5 gram of HCl.
i.e one gram of equivalent of NaOH
Completely neutratizes one gram equivalent
of HCl. If Normal Solution of both reagents
are used then one litre of each solution or any
same volume of both solutions will be
required for complete netralisation i.e. end
point
ml, =
N1 V1
1000
gm equivalent
N 2 V2
1000
gm. equivalent
N1 V1
N 2 V2
N1 V1
1000
Fig 6.11
(a) Stopper of burette.
(b) pinch cock burette.
51
2.
52
3.
5.
6.
53
2.
3.
4.
Fig : 6.16 (i) To fill the solution in the pipette (ii) To stop the solution with finger (iii) To bring the solution upto the
marked point (iv) To pour the solution in the conical flask (v) To remove the last drop of the pipette.
(Record of Titration-Experiment)
Correct result is obtained after completing
Volumetric analysis with accuracy. It is to be
carefully recorded in the practical note book.
Here the method are given for recording the
practical work related with titration.
54
Experiment No.1
Object
Formula
Calculation
as an indicator
Method :
1.
Clean all the apparatus with water. Wash
the burette with given NaOH and fix it
to the stand, fill it with acid. In case, if
there is a air bubbles in the rubber of
pinch cock then remove them and put
the surface of base at zero.
2.
3.
4.
Right page
1.
2.
3.
4.
5.
6.
7.
8.
Experiment No 1.
Object : To find out the concentration of
hydroxide. solution by titrating it against the
| phenol-ph+nalein
COONa
|
COOH
Observation Table :
Table number 1
S.No.
Volume
of acid
Reading of
Burate
Starting
1.
2.
3.
25 ml
25 ml
25 ml
0.01 ml
0.01 ml
0.01 ml
20.3 ml
20.3 ml
20.3 ml
Volume
End
of base
20.0ml
55
Formula : N1 V1 = N 2 V2
Standard solution = Solution of unknown
concentration.
Calculation
N1 V1 = N 2 V2
(acid) (base)
N
25 = N 2 20
10
N 25 N
N2 =
=
10 20 8
1.6562
8 1000
Concentration of
Na2CO3 = (1.6570 4gm / littre)
56
Table No. 1
S.No
Volume
Volume of
Na2CO3
Reading of Burrete
Start
End
of H 2SO4
1.
2.
20 ml
20 ml
1.7 ml
3.2 ml
22.9 ml
24.3 ml
21.2 ml
21.1 ml
3.
20 ml
6.2 ml
24.3 ml
21.1 ml
Calculation : N1 V1 = N 2 V2
Normality=Concentration equivalent weight
3.
= N1 = 1.6570 4 N = 0.1257
53
V1 = 20 ml
N2 = ?
V2 = 2101 ml
0.125 N 20 = N 2 21.1
N 2 = 0.125 N
20
20.1
2.50
= 0.123 N
20.1
2.50
4.9
20.1
1225
201
Observation table
S.No.
Volume of Reading
the base of Start
Burette
End
1.
2.
3.
25 ml
25 ml
25 ml
26.7 ml
26.4 ml
26.4 ml
= 6.09 litre.
Experiment no. 3 :
Objective:To find out the concentration of HCl
solution with the help of standard solution of N/
10. Sodium Carbonate,
Principle : When HCl is added into the sodium
carbonate then the reaction is completed into two
steps :
(i)
Na2CO3 + HCl NaHCO3 + NaCl
(ii)
Na2CO3 + HCl NaCl + H 2O + CO2
In the first step the Carbonate is converted in
to the bicarbonate. In the 2nd step the bi carbonate reacts with acid and gives carbondie-oxide.
In this titration methyle orange is used as a
indicator and acid solution is be taken in to
the burette.
0.0 ml
0.0 ml
0.0 ml
Used
Volume
of acid
26.4 ml
N2 =
N
25
25
=
N
10 264 264
56
57
1000
N
10
1.2
= 6 gm
200
= 40 N = 4 gram /litre
10
4 2 = 8 gram
Result -2 litre solution of caustic soda contains
8 gram solvent
Solution 2:
100 ml of solution contains .53 grams
solution
0.53 1000
= 5.3 gm
100
Normality =
Strength
Equivalent weight
5.3
53
1
N
=
10 10
4.76 500
= 2.38 gm
1000
58
N2 =
N
25
2.5
=
10 23.8 23.8
or
2.5
238 N
= N1 V1 = N 2 V2
= base
= 0.105 N
N
25 = N 2 27.3
10
N2 =
or
acid
25
N
10 27.3
= 0.091 N
5.3
1
N
=
=
53 10 10
Exercise Question
Q.1
Q.2
Q.3
Q.4
What is the difference between dinormal & decimolar solution of Sulphuric acid?
Q.5
Which indicator is suitable for titration between oxalic acid and caustic soda
solution?
Q.6
Q.7
What is the normality of Na2CO3 solution prepared by dissolving 10.6 gram in 500 ml
flask?
Q.8
Q.9
Q.10
How much water must be added in 6 NHNO3 acid solution so that it becomes 2 N
concentration?
59
Q.11 How much water must be added in 1 litre 0.125 N NaOH solution so as to make on
0.100 N solution ?
Q.12 Find the amount of KOH dissolved in it was completely neutralized by 25 ml of N/10 HCl
Solution ?
58
Q.13 0.5 N HCl Solution completely neutralized by 22.5 ml Caustic Soda Solution, find the amount
of Caustic Soda dissolved in the Solution ?
Q.14 To neutralized 35 ml of H 2SO4 of unknown strength 28.6 ml. N/10 NaOH was used. Find
the normality of H 2SO4 .
Q.15 20 ml of N/20 was completely neutralized by N/10. Calculate the used quantity of acid ?
Q.16 31.00ml of 1 base was neutralized by 25 ml of N/10 HCl solution. If strength of base is 4.5
gm/litre then find the equivalent weight of base.
Answer
(7) 0.4 N
(8) 2 gm
(11) 250 ml
(12) 0.14 N
(15) 100 ml
(16) 55.8
(9) 26.5 gm
(13) 0.45 gm
(10) 1 : 2
(14) 0.0817 N