TECHNICAL ANALYSIS

LABORATORY

DEPARTMENT OF CHEMICAL ENGINEERING

COIMBATORE INSTITUTE OF TECHNOLOGY

(An Autonomous Institution Affiliated To Anna University)

COIMBATORE – 641014
 TABLE OF CONTENTS
1. ANALYSIS OF WATER
2. ESTIMATION OF WATER OF HYDRATION AND NUMBER OF
WATER MOLECULES
IN A CRYSTALLINE SALT
3. ESTIMATION OF GLUCOSE
4. ESTIMATION OF AVAILABLE CHLORINE IN BLEACHING POWDER

5. ESTIMATION OF SULPHATE
6. ESTIMATION OF PURITY IN CALCIUM CARBONATE
7. ESTIMATION OF MANGANESE DIOXIDE IN PYROLUSITE
8. ESTIMATION OF COPPER
9. ESTIMATION OF AVAILABLE CALCIUM OXIDE IN QUICK LIME
10. ESTIMATION OF NITROGEN IN THE GIVEN SAMPLE OF
INORGANIC FERTILIZER
11. ANALYSIS OF TALCUM POWDER- ESTIMATION OF MAGNESIUM
SILICATE
12. ACID VALUE OF OIL
13. ANALYSIS OF CEMENT
14. SAPONIFICATION VALUE OF OIL
15. ANALYSIS OF SOAP
16. ESTIMATION OF KMnO4 BY SPECTROSCOPY
17. DETERMINATION OF SODIUM IN THE WATER SAMPLE BY FLAME
PHOTOMETRY
18. pH - METER
19. NEPHELOMETER
20. DETERMINATION OF IODINE VALUE OF OIL
21. ESTIMATION OF THE CELLULOSE CONTENT IN THE GIVEN
CELLULOSE BEARING MATERIAL
22. ANALYSIS OF BRASS
23. ANALYSIS OF BAUXITE
24. DETERMINATION OF CHEMICAL OXYGEN DEMAND
25. DETERMINATION OF CHLORIDE CONTENT IN THE GIVEN
WATER SAMPLE

1
OBSERVATIONS:

TOTAL DISSOLVED SOLIDS:

Weight of the empty dish =

Weight of the china dish + 50ml of water =
Weight of the china dish after evaporation =
Weight of residue =
Weight of residue per 50ml =
Weight of residue per 1000ml =
Total dissolved solids =

DETERMINATION OF TOTAL HARDNESS:

Pipette solution : Water sample

Burette solution : EDTA solution
Indicator : Erichrome black-T indicator
End point : Appearance of steel blue colour

Volume of Burette Reading Volume of Titre Value

Sl.
Solution in conical (ml) EDTA Used (ml)
No
flask (ml)
Initial Final
(ml)

Volume of EDTA consumed for 20ml of water =

1ml of EDTA solution prepared = 1 ppm of CaCO3
1000ml of the water consumes =
Total hardness of the sample =

2
 ANALYSIS OF WATER
Ex No: 1

AIM:
To estimate
 Total solids including suspended matter
 Temporary hardness
 Permanent hardness of the given water sample using the EDTA method

PROCEDURE:

Weigh accurately about 50ml of the water sample in a previously weighed china
dish and evaporate to dryness carefully on a sand bath. Dry the residue at 105˚C in an
oven for 30 minutes till constant weight is obtained. Cool the china dish in a desicator
and weigh the residual solids. Express it as parts per million parts of water.

TOTAL HARDNESS:

Pipette out 20 ml of the given hard water sample into a conical flask. Add exactly
10ml of the ammonia buffer and also a pinch of Erichrome black-T indicator. The colour
of the mixture changes to wine red. Add the standard EDTA solutions from the burette
and shake the conical flask thoroughly after each addition. When the end point is
approaching, a steel blue colour will appear along with wine red colour. At this stage add
EDTA solution carefully drop by drop with vigorous shaking till the solution changes to
steel blue colour. This is the end point. Note the burette reading. Repeat the experiment
till concordant values are obtained. Express the total hardness as ppm of CaCO3

PERMANENT HARDNESS:

Take 100ml of the given hard water into a clean conical flask. Keep the conical
flask on wire gauze and boil the solution to about 50ml (approximately) to destroy
temporary hardness. Cool the solution. Add 10ml of the buffer solution and a pinch of
Erichrome black-T indicator and titrate with the standard EDTA solution as given above
till the end point is reached. Calculate the permanent hardness as ppm of CaCO3

3
DETERMINATION OF PERMANENT HARDNESS:

Pipette solution : Water sample

Burette solution : EDTA solution
Indicator : Erichrome black-T indicator
End point : Appearance of steel blue colour

Sl. Volume of Burette Reading Volume of Titre Value

No pipette solution (ml) EDTA Used (ml)
(ml) Initial Final (ml)

Volume of EDTA consumed for 100ml water =

1000ml of the water contains =
Permanent hardness of the sample =

TEMPORARY HARDNESS:

Temporary hardness = Total hardness – Permanent hardness

=

TEMPORARY HARDNESS:

From the total hardness subtract the permanent hardness and report the balance as
ppm of CaCO3 as temporary hardness.

PREPARATION OF REAGENTS:

4
 EDTA SOLUTION:

Dissolve 3.72g of dissolved Ethylene diamine, Tetra acetic dihydrate in distilled

water and make up to 100ml in a standard flask. 1ml of this solution is equivalent to 1
ppm of CaCO3.

BUFFER SOLUTION:

Dissolve 67.5g of ammonium chloride in 570ml of liquor ammonia and dilute

with water to 1 litre.

ERICHROME BLACK - T

1gm of Erichrome black powder is mixed with 200g of Sodium Chloride. The
mixture is well ground in a mortar with a pestle so that both are well mixed uniformly.
A pinch of the above mixture is used in the titration each time.

RESULT:

The water sample is analyzed and the following were determined.

 The total dissolved solids =

 Total hardness =
 Permanent hardness =
 Temporary hardness =

OBSERVATIONS:

TOTAL DISSOLVED SOLIDS:

Weight of empty silica crucible =

Weight of crucible + salt before heating =
Weight of salt taken =
Weight of silica crucible + salt after heating =
Weight of water removed =
Weight of anhydrous salt =
5
Water of hydration loss in weight X 100 =
Weight of salt

18gms of water contains 6.023X 10 23

No. of molecules =
No. of gm moles of water =
No. of gm moles of anhydrous salt =
Ratio of no. of gm mole of water and salt =
Ratio of no. of gm moles of salt and water =

6
 ESTIMATION OF WATER OF HYDRATION AND
NUMBER OF WATER MOLECULES
IN A CRYSTALLINE SALT
Ex No: 2

AIM:

To determine the water of hydration in percentage and number of water molecules

in a crystalline salt.

PROCEDURE:

Weigh accurately about 1gm of the crystalline salt (Copper Sulphate or

Magnesium Sulphate) into a previously weighed silica crucible. Place the crucible over a
clay pipe triangle. Heat the crucible first gently and then strongly to a dull red colour.
Heat the crucible until constant weight is reached. Cool in a desicator and find the weight
of the anhydrous salt. Estimate the loss in weight as water of hydration and express it as
percentage. Calculate the number of molecules of water.

RESULT:

 Water of hydration as a percentage =

 No. of molecules of water =
 Ratio of number of gm mole of salt to water =

7
OBSERVATIONS:

Weight of the empty specific gravity bottle =

Weight of bottle +glucose =
Weight of bottle after transferring glucose =
Weight of glucose transferred =

STANDARDIZATION OF FEHLING’S SOLUTION:

Burette Solution : Glucose Solution

Pipette solution : 5ml of Fehlings ‘A’ + 5ml of Fehlings ‘B’ Solution
Indicator : Methylene Blue
End point : Disappearance of blue colour

Volume of Burette Reading Volume of Concordant

Sl.
pipette solution (ml) Glucose titre Value
No
(ml) Used (ml)
Initial Final
(ml)

180 g of glucose in 1000ml water =

X g of glucose in 100ml water =
Volume of glucose solution (V1) =
Normality of glucose solution (N1) =
Volume of Fehlings solution (V2) =

V1 x N1 = V2 x N2
N2 = V1 x N1 / V2

Normality of the Fehlings solution (N2) =

8
 ESTIMATION OF GLUCOSE

Ex No: 3

AIM:
To estimate the amount of glucose in the given sample.

PROCEDURE:

STANDARDIZATION OF FEHLING’S SOLUTION:

Prepare a standard solution of glucose by exactly weighing 0.4 – 0.5 g of glucose
and transfer it into a 100ml standard flask. Dissolve in water and make upto the mark.
Transfer the standard glucose solution to a burette.

Pipette out 5ml of Fehling’s A and 5ml of Fehling’s B solution into a 100ml
conical flask previously cleaned with con nitric acid. Add 6ml of cold standard glucose
solution from the burette and heat the cold mixture over a wire gauge without further
dilution and boil the contents for about one minute. See whether all the copper has been
reduced (by the appearance of bright red colour). If it is judged that all the copper has
been reduced, add 1 or 2 drops of Methylene blue indicator and without removing from
the flame. Add glucose solution in quantities of 0.5 ml at a time till the blue colour is
discharged. Note the burette reading, which is the approximate titre value.

HAVING THIS DETERMINED, THE EXACT TITRE VALUE PROCESSES ARE

AS FOLLOWS:

Pipette out 5ml of Fehling’s A and 5ml of Fehling’s B into a 50ml conical flask
and add a cold standard glucose solution from the burette, which is 1ml less than the
approximate titre value. Boil the contents over a wire gauge and keep in moderate boiling
for 1 minute. Without removing from the flame, add the glucose solution drop by drop.
Add methylene blue indicator and complete the titration as given above. Note the burette
reading, which gives the exact titre value. Calculate the amount of glucose equivalent to
10ml of Fehling’s solution.

9
ESTIMATION OF GLUCOSE:

Burette Solution : Glucose Solution

Pipette solution : 5ml of Fehlings ‘A’ + 5ml of Fehlings ‘B’ Solution
Indicator : Methylene Blue
End point : Disappearance of blue colour

Volume of Burette Reading Volume of Concordant

Sl.
pipette solution (ml) Glucose titre Value
No
(ml) Used (ml)
Initial Final
(ml)

V1 x N1 = V2 x N2

The normality of glucose solution (N2) = V1 x N1 / V2

Volume of Fehling’s solution (V1) =
Normality of Fehling’s solution (N1) =
Volume of Glucose solution (V2) =
The amount of glucose solution = Normality of Equivalent weight
Present in litre of the solution glucose solution of glucose

The amount of glucose present in

1000ml of the solution =
Amount of glucose present in 100ml
of the solution =

10
ESTIMATION OF GLUCOSE:

Make up the given glucose solution upto 100ml in the given standard flask.
Transfer this solution into the burette and titrate with 10ml Fehling’s solution as given
above and obtain the exact titre value. From the amount of glucose solution equivalent to
10ml of Fehling’s solution obtained from the titration, calculate the normality of glucose
solution from which the amount of glucose present in the whole of the given solution can
be calculated.

RESULT:

The amount of glucose present in whole of the given solution is ____________ g

11
OBSERVATIONS:

Weight of the empty weighing bottle =

Weight of Potassium dichromate + Weighing bottle =
Weight of Potassium dichromate transferred =
Weight of bleaching powder + weighing bottle =
Weight of bottle after transfer =
Weight of bleaching powder transferred =

STANDARDIZATION OF SODIUM THIO SULPHATE SOLUTION:

Pipette solution : Potassium dichromate solution

Burette solution : Sodium thio sulphate solution
Indicator : Starch indicator with KI solution and dil H2SO4
End point : Appearance of permanent green colour

Volume of Potassium Volume of

Dichromate solution Burette Reading Sodium Concordant
Sl. (ml) thiosulphate titre Value
No (ml) used (ml)
(ml)
Initial Final

Volume of Potassium dichromate solution (V1) =

Normality of Potassium dichromate solution (N1) =
Volume of Sodium thio sulphate (V2) =
Normality of Sodium thio sulphate (N2) = V1 x N1 / V2

12
 ESTIMATION OF AVAILABLE CHLORINE IN BLEACHING POWDER

Ex No: 4

AIM:
To estimate the amount of available chlorine in the given sample of bleaching
powder.

PRINCIPLE:
Bleaching powder is made by passing chlorine gas over dry slaked lime at
temperature ranging between 40 to 55oC. At higher temperatures beyond this limit, a
considerable amount to chlorine is formed. Hence a careful control of the temperature is
necessary. Chemically, bleaching powder is Calcium chloro hypochlorite which when
treated with water forms Calcium chloride and Calcium hypochlorite according to the
equation.
2 CaClOCl  CaCl2 + Ca (OCl) 2
The chlorine of the hypochlorite is the bleaching agent and is called the available chlorine
of the bleaching powder. The available chlorine is estimated by the Bunsen and Wagner
method.

PROCEDURE:
STANDARDIZATION OF SODIUM THIOSULPHATE SOLUTION:

Prepare a standard solution of 0.1N K2Cr2O7 by weighing accurately 0.5 g and

making it upto 100 ml in a standard flask and take 20 ml of the solution add to it, about
20 ml of 2N hydrochloric acid. Then add about 10 ml of a 10% KI solution, stir the
contents and wait for 1 minute to complete the liberation of iodine. Run from the burette
the given thiosulphate solution drop by drop with constant stirring. The color of the
solution will change from deep brown to light brown, yellow and then to greenish yellow.
At this stage, stop adding the thiosulphate solution and add about 1ml of starch indicator.
After the solution becomes deep blue color, continue the addition of thiosulphate drop by
drop with vigorous shaking till the blue color gets discharged. The solution suddenly
turns green due to the chromic salt. This is the end point. Repeat till the concordant
values are obtained. Calculate the exact normality of the Sodium thiosulphate.
ESTIMATION OF AVAILABLE CHLORINE:
13
 Pipette solution : Bleaching powder solution
Burette solution : Sodium thio sulphate solution
Indicator : Starch indicator
End point : Disappearance of blue colour

Volume of Bleaching Volume of

Sl. powder solution Burette Reading Sodium Concordant titre
No (ml) (ml) thiosulphate Value
used (ml)
Initial Final (ml)

1000ml of 1N Sodium thio sulphate solution contains 35.46g of chlorine

1N of 0.1ml sodium thio sulphate contains =

Amount of available chlorine present in 50ml of the solution =
Amount of available chlorine present in 500ml of the solution =
Percentage of available chlorine in bleaching powder =

14
ESTIMATION OF AVAILABLE CHLORINE:

Weigh accurately about 5g of bleaching powder sample and transfer into

porcelain mortar. Add a little distilled water and rub with a pestle to get a smooth paste.
Then add little more water and stir with the pestle and allow settling for a few minutes.
Pour off the clear liquid through a funnel into a 500 ml standardization flask. Again add
distilled water and pour off as before. Repeat the above operation until the whole material
is conveyed into the flask without any loss and repeat it until the mortar is washed and
fully cleaned. Make the solution upto the mark by adding distilled water, shake well.
Without allowing material to settle, pipette out 50ml of the turbid solution into a 250 ml
conical flask. Add about 10 ml of a 10% solution of KI followed by 10ml of acetic acid.
Titrate the liberated iodine against the standard sodium thio sulphate solution using the
starch indicator. The end point in this case, will be the colour change from blue to
colorless.

RESULT:

The percentage of available chlorine in the

given sample of bleaching powder = _________________

15
OBSERVATION:

Weight of empty silica crucible =

Weight of crucible + residue =
Weight of residue =

REACTION:

BaCl2 + SO4 2-  BaSO4 + 2Cl-

1gmole of BaSO4 contains 1gmole of “S”

Mol weight of BaSO4 = 233.8g/gmol
Mol weight of SO4 2- = 96g/gmol
233.8g of BaSO4 contains 96g of SO4 2-
____ g of BaSO4 contains = _________ g of SO4 2-
20ml of solution contains = _________ g of SO4 2-
100ml of solution contains = _________ g of SO4 2-

16
 ESTIMATION OF SULPHATE
Ex No: 5

AIM:

To estimate the amount of sulphate in the given solution

PROCEDURE:

The solution is made up in a standard flask (100ml) exactly upto the mark. It is
shaked thoroughly for complete mixing. Exactly 20ml of the made up solution is pipetted
out in a 250ml beaker and around 50ml of distilled water is added along with 2ml of con
HCl. The solution is heated nearer to the boiling point 70 to 80˚C BaCl2 solution is taken
in another beaker and heated to boiling. The hot BaCl2 solution is added to the hot ore
solution with constant stirring and boiling is continued. Complete precipitation is tested
by adding few drops of BaCl2 solution to the sides of the beaker. The solution is filtered
carefully, transferring the supernatant liquid to a gravimetric filter paper. Most of the
precipitate is made to remain in the beaker. It is allowed to settle and the supernatant
liquid is transferred to the filter paper. The process is repeated six times, after which the
precipitate is finally transferred. A final washing is made and the filtrate is tested for
chloride with few drops of silver nitrate. It is allowed to dry for sometime and is
transferred in a previously weighed silica crucible and is incinerated for sulphate. The
duplicate is carried out.

RESULT:

Amount of sulphate present in 100ml of the solution is _____________ g

17
OBSERVATIONS:

PREPARATION OF STANDARD OXALIC ACID SOLUTION:

Weight of the empty weighing bottle =

Weight of bottle + Oxalic acid before transfer =
Weight of bottle after transferring salt =
Weight of Oxalic acid transferred =
63g of Oxalic acid in 1000ml =1N
_____ g of Oxalic acid in 100ml = _________ N

PREPARATION OF SODIUM CARBONATE SOLUTION:

Weight of the empty weighing bottle =
Weight of bottle + Na2Co3 (before transfer) =
Weight of bottle (after transfer) =
Weight of Na2Co3 transferred =
53g of Na2Co3 in 1000ml =1N
_____ g of Na2Co3 in 100ml = _________ N

AMOUNT OF CALCIUM CARBONATE TAKEN:

Weight of the empty weighing bottle =

Weight of bottle + CaCO3 before transfer =
Weight of bottle after transferring salt =
Weight of CaCO3 transferred =
_____ g of CaCO3 in 100ml = _________ N

18
 ESTIMATION OF PURITY IN
CALCIUM CARBONATE
Ex No: 6

AIM:

To find out the purity of the given calcium carbonate sample.

PROCEDURE:

Prepare 0.1 N standard oxalic acid solution and standardize the given sodium
hydroxide solution using phenolphthalein indicator. Weigh accurately about 0.25 gram of
calcium carbonate sample and transfer it to a 250 ml conical flask. Add to it exactly 40
ml of 0.1N HCl by means of a pipette. Warm slightly to expel all the carbon di oxide
formed. Titrate the excess HCl using the standard NaOH solution from the burette using
phenolphthalein as indicator. The end point is the appearance of a pale pink color. Repeat
the experiment twice. Calculate the excess HCl acid used by Calcium Carbonate and
express it as a percentage.

CaCO3 + 2 HCl  CaCl2 + H2O + CO2

RESULT:

The purity of Calcium Carbonate in the given sample is ______________

19
 TITRATION-I
STANDARDIZATION OF SODIUM HYDROXIDE:

Burette solution : Oxalic acid

Pipette solution : Sodium hydroxide
Indicator : Phenolphthalein
End point : Disappearance of pink colour

Volume of
Sl. Volume of NaOH Oxalic acid Concordant
Burette Reading
No solution used titre Value
(ml)
(ml) (ml) (ml)
Initial Final

20

Volume of Oxalic acid (V1) =

Normality of Oxalic acid (N1) =
Volume of Sodium hydroxide (V2) =
Normality of Sodium hydroxide (N2) =

TITRATION-II
STANDARDIZATION OF HYDROCHLORIC ACID:

Burette solution : Hydrochloric acid

Pipette solution : Sodium carbonate solution
Indicator : Methyl orange
End point : Appearance of permanent pink colour

Sl. Volume of Na2CO3 Burette Reading Volume of HCl Concordant

No solution (ml) used titre Value
(ml) (ml) (ml)
Initial Final

20

Volume of sodium carbonate solution (V1) =

Normality of sodium carbonate solution (N1) =
Volume of hydrochloric acid (V2) =
Normality of hydrochloric acid (N2) =

20
 TITRATION-III
BLANK TITRATION OF HCl AGAINST NaOH:

Burette solution : Sodium hydroxide solution

Pipette solution : Hydrochloric acid
Indicator : Phenolphthalein
End point : Appearance of pink colour

Volume of
Sl. Volume of HCl Burette Reading NaOH used Concordant
No solution (ml) titre Value
(ml) (ml) (ml)
Initial Final

20 21.2

Volume of Sodium hydroxide required by 20ml of HCl (V1) =

TITRATION-IV
BACK TITRATION OF HCl AGAINST NaOH:

Burette solution : Sodium hydroxide solution

Pipette solution : Hydrochloric acid
Indicator : Phenolphthalein
End point : Appearance of pink colour

Volume of
Sl. Volume of HCl Burette Reading NaOH used Concordant
No solution (ml) (ml) titre Value
(ml) (ml)
Initial Final

6.5

Volume of Sodium hydroxide required in back titration (V2) =

21
AMOUNT OF CALCIUM CARBONATE PRESENT:

Volume of NaOH required by 20ml of HCl (V1) =

Volume of NaOH required in back titration (V2) =
Xml of HCl consumes = V2ml of NaOH
X = (20 X V2)/V1 =
Reacted HCl = (40 – X) =
1N 1000ml of HCl = 50g of CaCO3
____ N ____ml of HCl = _______________ g of CaCO3

Percentage purity of CaCO3 =Quantity of CaCO3 present X 100

Quantity of CaCO3 taken

22
 OBSERVATIONS:

(A) STANDARDIZATION OF POTASSIUM PERMANGANATE:

Weight of the empty weighing bottle =

Weight of bottle + Oxalic acid =
Weight of bottle after transfer =
Weight of Oxalic acid transferred =
Volume made up = 250ml
Strength of oxalic acid (N1) =

TITRATION OF POTASSIUM PERMANGANATE VS OXALIC ACID:

Burette solution : Potassium permanganate
Pipette solution : Oxalic acid
Indicator : Self
End point : Appearance of pale permanent pink colour

Volume of
Sl. Volume of Oxalic Burette Reading KMnO4 used Concordant
No acid (ml) (ml) titre Value
(ml) (ml)
Initial Final

N2 = Normality of KMnO4
V1N1 = V2N2
20 X N1 = V2N2
N2 = (20 X N1)/V2

23
 ESTIMATION OF MANGANESE DIOXIDE IN PYROLUSITE

Ex No: 7

AIM:

To estimate the amount of Manganese dioxide in the given sample of Pyrolusite ore.

PRINCIPLE:

Manganese dioxide oxidizes oxalic acid in the presence of dilute H2SO4 to CO2
and water as given below.

MnO2  MnO + [O]

(COOH) 2 + [O]  2CO2+H2O
MnO + H2SO4  MnSO4 + H2O
MnO2 = [O] = (COOH) 2 = 16 = 2 x 8 = equivalents
Equivalent Weight of MnO2 = Mol. Wt/2 = 87/2 = 43.5

The estimate depends upon adding a known excess standard oxalic acid to a
weighed amount of the substance and determining the unused oxalic acid by titration
against previously standardized permanganate.

PROCEDURE:

(A) STANDARDIZATION OF PERMANGANATE:

Prepare a 0.1N standard solution of oxalic acid in a 250 ml standard flask. Pipette
out 20 ml of this solution into a 250 ml conical flask, and add about 25ml of dilute
sulphuric acid. Heat to about 60 to 70ºC and titrate it against permanganate till the end
point is reached. (End point is the appearance of a pale permanent pink colour). Repeat

24
till concordant value is obtained. Note the amount of permanganate used. Calculate the
exact normality of the permanganate solution.

(B) ESTIMATION OF MANGANESE DIOXIDE:

Weight of the empty weighing bottle =

Weight of bottle + pyrolusite =
Weight of bottle before transfer =
Weight of bottle after transfer =
Volume of Oxalic acid transferred =
Weight of pyrolusite ore transferred =

TITRATION OF POTASSIUM PERMANGANATE VS EXCESS OXALIC ACID:

Burette solution : Potassium permanganate

Pipette solution : Pyrolusite
Indicator : Self
End point : Appearance of pale permanent pink colour

Volume of
Sl. Mass of Burette Reading KMnO4 used Concordant
No pyrolusite (ml) (ml) titre Value
(g) (ml)
Initial Final

Amount of oxalic acid used up (V4) = Amount of MnO2 in terms of KMnO4

= (2V2 – V3) ml
=
Strength of potassium permanganate (N2) =

1000ml 1N solution contains 43.5g MnO2

1000ml 0.1N solution contains 4.35g MnO2
(V4) ml of (N2) N solution contains (W) = (4.35/1000) X V4 X (N2/0.1)
25
 = _________ g of MnO2
% of MnO2 = W X 100 =
(Weight of ore taken)

(B) ESTIMATION OF MANGANESE DIOXIDE:

Weigh accurately about 0.1 to 0.15g of finely powered ore and transfer it to a
250ml conical flask. Add exactly 40ml of the standard oxalic acid using the pipette and
about 25ml of dilute H2SO4. Heat it to about 70ºC over a wire gauge till no black
particles are seen. Do not boil the contents since volatilizing with steam will lose oxalic
acid. After the reaction is over, dilute the solution with about 20ml of distilled water.
Heat if necessary to about 60ºC and titrate the excess oxalic acid present in the solution
with the standardized permanganate solution till the end point is reached. Calculate the
amount of oxalic acid as MnO2 and express it as a percentage of the weight of the sample
taken.

RESULT:

The amount of manganese dioxide in the given pyrolusite ore is ____________ %

26
OBSERVATIONS AND CALCULATIONS:

STANDARD SODIUM CARBONATE SOLUTION:

Weight of the empty weighing bottle =

Weight of the weighing bottle + sodium carbonate
 Before transfer =
 After transfer =
Weight of sodium carbonate transferred =
Normality of sodium carbonate solution =

STANDARDIZATION OF HYDROCHLORIC ACID:

Burette solution : Hydrochloric acid

Pipette solution : Sodium carbonate solution
Indicator : Methyl orange
End point : Appearance of pale pink colour

Volume of HCl
Sl. Volume of Na2CO3 Burette Reading used Concordant
No pipette solution (ml) (ml) titre Value
(ml) (ml)
Initial Final

Volume of sodium carbonate solution taken (V1) =

Normality of sodium carbonate solution (N1) =
Volume of hydrochloric acid consumed (V2) =
Normality of hydrochloric acid (N2) = V1 x N1 / V2
=

27
 ESTIMATION OF COPPER

Ex No: 8

AIM:

To estimate the amount of copper in 20ml of the given solution.

PRINCIPLE:
The copper salt solution is treated with a measured known volume of standard
sodium hydroxide solution. The precipitated calcium hydroxide is filtered off and the
excess unreacted sodium hydroxide solution is titrated with standard HCl solution. The
used sodium hydroxide is calculated to estimate the amount of copper.

CuSO4 + 2NaOH  Na2SO4 + Cu (OH)2

PROCEDURE:

Prepare a 0.1 N standard solution of sodium carbonate and standardize against the
given HCl acid taken in the burette and determine the exact normality.

Pipette out 20ml of the given copper sulphate solution in a 250ml beaker. Add
exactly 40ml of 0.1N sodium hydroxide solution from the pipette. Stir well and filter the
contents through the filter paper and collect the filtrate in a 250ml conical flask. Wash the
precipitate thoroughly with distilled water and combine the filtrate and washings and
titrate with the given standardized HCl using phenolphthalein indicator. Conduct a
titration using 20ml of sodium hydroxide solution. Calculate the sodium hydroxide used
up by copper and determine the amount of copper present in 20ml of the solution.

RESULT:
Amount of copper present in 20ml of the solution is ________________ g.

BLANK TITRATION:
28
 Pipette solution : Sodium hydroxide solution
Burette solution : Hydrochloric acid
Indicator : Phenolphthalein
End point : Disappearance of pale pink colour

Sl. Volume of NaOH Burette Reading

No sample (ml) Volume of HCl used
(ml) Initial Final (ml)

Volume of HCl required (V3) =

Normality of HCl (N3) =
Volume of NaOH used (V4) =
Normality of NaOH (N4) =

29
ESTIMATION OF COPPER:
Pipette solution : Sodium hydroxide solution
Burette solution : Hydrochloric acid
Indicator : Phenolphthalein
End point : Disappearance of pale pink colour

Sl. Volume of NaOH Burette Reading Volume of HCl Concordant

No Sample (ml) used titre Value
(ml) (ml) (ml)
Initial Final

Volume of HCl (V5) =

Volume of NaOH used = 40ml
Amount of NaOH used in terms of HCl (V6) = [2V3 – V5]

1000ml of 1N solution contains 63.54g of copper

1000ml of 0.1N solution contains 6.354g of copper

.˙. (V6) ml of (N2) solution contains = ___________ g of copper

30
OBSERVATIONS:

Weight of the empty specific gravity bottle =

Weight of bottle + oxalic acid =
Weight of bottle after transferring oxalic acid =
Weight of oxalic acid transferred =
Weight of the empty specific gravity bottle =
Weight of bottle + quick lime =
Weight of bottle after transfer of quick lime =
Weight of quick lime transferred =

TITRATION:

Pipette solution : Filtrate

Burette solution : Oxalic acid
Indicator : Phenolphthalein
End point : Disappearance of pink colour

Volume of solution in Volume of

Burette Reading
Sl. flask Oxalic acid Concordant
(ml)
No (ml) used titre Value
Initial Final (ml) (ml)

1ml of 0.1N oxalic acid = 0.0028g of CaO

Weight of CaO in 200ml of the filtrate =
___ml of ___N oxalic acid = (0.0028 X _____N X ____ml)/ 0.1
Weight of CaO in 20ml of the filtrate = ___________ g of CaO
Weight of CaO in 500ml of the filtrate = ___________ g of CaO
Available % of Calcium Hydroxide = Weight of CaO in 500ml X 100
Weight of quick lime initially taken

31
 AVAILABLE CALCIUM OXIDE IN QUICK LIME

Ex No: 9

AIM:

To estimate the amount of available Calcium Oxide in the given sample of

quick lime.

PROCEDURE:

Prepare a solution of oxalic acid of strength 0.1 N. Weigh 1gm of finely powdered
sample and add to it a little distilled water in a 250ml beaker. Boil for a few minutes until
the contents get thoroughly disintegrated. Cool and transfer the contents to a 250ml glass
stoppered bottle. Add about 200ml of water followed by 40g of cane sugar. Close the
bottle and mix the contents thoroughly by shaking every 15min or often for a period of 2
hours. Allow the contents to settle. Filter by suction on a buchner funnel and wash the
residue 3 times with distilled water. Make the filtrate upto 500ml in a standard flask.
Pipette out 20ml of made up solution in a conical flask and titrate it with 0.1 N oxalic
acid using phenolphthalein indicator. From the titration, calculate the value of Calcium
oxide and report the available lime as a percentage.

RESULT:

The available lime in the given sample is ____________________ g.

32
 OBSERVATIONS AND CALCULATIONS:

Weight of empty weighing bottle =

Weight of empty weighing bottle + ammonium chloride sample =

STANDARDIZATION OF THE GIVEN HYDROCHLORIC ACID:

Weight of empty weighing bottle =

Weight of empty weighing bottle + sodium carbonate =
Therefore, weight of sodium carbonate transferred =
Therefore, normality of sodium carbonate solution =

I.TITRATION:

Burette solution : Hydrochloric acid

Pipette solution : Sodium carbonate solution
Indicator : Methyl orange
End point : Appearance of pale permanent pink colour

Volume of HCl
Sl. Volume of sodium Burette Reading solution Concordant
No carbonate taken (ml) titre Value
(ml) (ml) (ml)
Initial Final

Normality of hydrochloric acid =

33
 BLANK TITRATION:
Burette solution : Hydrochloric acid
Pipette solution : Sodium Hydroxide
Indicator : Phenolphthalein
End point : Disappearance of pale pink colour

Sl. Volume of NaOH Burette Reading Volume of HCl Concordant titre

No solution (ml) used Value
(ml) (ml) (ml)
Initial Final

20 ml V2 =19

Normality of Sodium hydroxide =

34
 ESTIMATION OF NITROGEN IN THE GIVEN SAMPLE OF INORGANIC
FERTILIZER

Ex No: 10

AIM:
To estimate the amount of nitrogen present in the given sample of the inorganic
fertilizer.

PRINCIPLE:

The inorganic fertilizers are usually the ammonium salts of mineral acids which
reacts with sodium hydroxide and liberate ammonia, and forms the sodium salt of the
acid

(NH4) x (Y) + NaOH  NH3 ↑ + Nax (Y)

Where ‘Y’ is SO4-, Cl-, NO3-, PO4- etc…

In this estimation, a known excess volume of sodium hydroxide solution is added

to a definite volume of the fertilizer solution and the ammonia is boiled off. The excess
alkali is titrated with standard decinormal hydrochloric acid.

PROCEDURE:

Weigh accurately about 1.5g of solid ammonium chloride. Dissolve in distilled

water and make upto 250ml in a standard flask. Pipette out 20ml of the made up solution
into a 250ml conical flask and add to it, 40ml of 0.1N NaOH exactly and also a little
distilled water. Place a funnel in the mouth of the conical flask and also put 1 or 2
porcelain beads inside the flask for smooth boiling. Boil the contents for about 20
minutes till no more ammonia in found in the steam coming out as tested by a moist red
litmus paper. The contents of the flask should not be allowed to evaporate to dryness. If
necessary, add some distilled water into the flask to maintain the level. When no more
ammonia comes out, allow the flask to cool. Wash the funnel with a jet of distilled water
and remove it. Add 1 or 2 drops of Methyl orange indicator and titrate the excess alkali
TITRATION OF NH4Cl WITH NaOH SOLUTION AGAINST HCl:
35
 Burette solution : Hydrochloric acid
Pipette solution : Sample solution
Indicator : Methyl orange
End point : Appearance of pale permanent pink colour

Sl.
Volume of pipette Burette Reading
No
solution (ml) Concordant titre Value
(ml) Initial Final (ml)

V1 =5

20ml of NaOH = V2ml of HCl =

40ml of NaOH = 2V2ml of HCl =

20ml of fertilizer solution contains = 2.8 / 1000 x (2V2 – V1) / 2 x SHCl /0.1g Nitrogen

= 2.8 X (2V2 – V1) X SHCl

1000 X 2 X 0.1
=

Therefore 250ml of fertilizer solution contains = 250 X

20
=
Therefore percentage of Nitrogen =

36
against standardized 0.1N HCl till the end point is reached, required for the excess of the
alkalies as V1. Repeat the experiment till concordant values are obtained. Conduct a
blank titration by taking 20ml of the sodium hydroxide and titrating it against the
standard hydrochloric acid using methyl orange indicator. Let the volume be ‘V2’

RESULT:

 The percentage of nitrogen in the given sample =

 The theoretical value is =

37
Theoretical method
NH4Cl + NaOH NH4OH + NaCl
20 ml of ________N of NaOH consumes 20.7 ml of HCl
Reacted NaOH = 40-20 = 20 ml
1000ml of 1N Sodium Hydroxide = 14 g of nitrogen
20ml of ________N Sodium Hydroxide = 20X N X14
1000
=____________ g of N2
250ml of ________N Sodium Hydroxide = 250 X
20
=
Therefore percentage of Nitrogen =

38
 OBSERVATIONS:

Amount of MgCl2 dissolved in 250 ml = ________________ gm

X 1000
Strength of standard magnesium =
203.31X 250
= _________________ N

STANDARDIZATION OF EDTA
Strength of standard magnesium (N1) = _________________ N
Volume of standard magnesium (V1) = _________________ V
Volume of EDTA (V2) = _________________ ml
V1 XN1
Strength of EDTA (N2) =
V2
20 X
=
V2
=_________________ N

ESTIMATION OF MAGNESIUM SILICATE IN TALCUM POWDER

Amount of talcum powder taken for analysis = 1g
Volume of solution prepared = 250 ml
Volume of EDTA (V3) = ________________ml
Strength of EDTA (N3) =________________ N
Volume of talcum powder solution (V4) = 20 ml
V3 XN 3
Strength of Mg in talcum powder solution (N4) =
V4
= ________________ N

39
 ANALYSIS OF TALCUM POWDER- ESTIMATION OF MAGNESIUM
SILICATE

Ex No: 11

AIM:
To estimate the amount of magnesium silicate present in the given sample of
talcum powder.

PRINCIPLE:
Talcum powder contains essentially of magnesium silicate. On heating
magnesium silicate with concentrated acids gives magnesium ions. Magnesium
estimation is based on the complexometric titration. Magnesium is estimated by titrating
against EDTA using Erichrome Black- T indicator.

Mg2+ + EBT  [EBT-Mg2+]

Less stable- wine red

[EBT-Mg2+] + EDTA  [EDTA-Mg2+] + EBT

More stable- colourless Steel blue colour

PROCEDURE:

STANDARDIZATION OF EDTA:
A 50ml burette is washed, rinsed and filled with EDTA solution. 20ml of
standard 0.05N Magnesium ion solution is pipette out in to a clean conical flask. To this
5ml of ammonium buffer and 2 drops EBT indicator are added. This solution is titrated
against EDTA solution taken in the burette. End point is the colour change from wine red
to steel blue. The titration is repeated for concordant values. Let the volume of EDTA be
V1 ml.

40
 STANDARDIZATION OF EDTA:

Sl. Volume of Burette Reading Volume of Concordant

No standard (ml) EDTA used titre Value
magnesium (ml) (ml)
(ml) Initial Final

20 0 20.8 20.8

ESTIMATION OF MAGNESIUM SILICATE:

Sl. Volume of Burette Reading Volume of Concordant

No talcum powder (ml) EDTA used titre Value
solution (ml) (ml)
(ml) Initial Final

Amount of Magnesium silicate

present in sample = Strength of Mg X Mol.Wt

% of magnesium silicate present in the talcum powder = _____________

41
ESTIMATION OF MAGNESIUM SILICATE:

Weigh accurately about 1g of the talcum powder in to a beaker. Add 10ml of

conc.HCL and boil. Add water and filter through filter paper No 42. Collect the filtrate in
a 250ml standard flask and make up solution is 20ml pipette out in to a clean conical
flask. 5ml of ammonia buffer solution and 2 drops of Erichrome black- T indicator are
added and titrated against EDTA solution taken in the burette. The end point is the
change of colour from wine red to steel blue. The titration is repeated for concordant
values. Let the volume of EDTA be V2 ml.

RESULT

The percentage of Magnesium silicate present in the given sample of talcum

powder = ----------------------
(Sample used = )

42
OBSERVATIONS:

Quantity of the oil taken (W) = g

Volume of KOH solution (a) = 10 ml
Normality of KOH solution = 0.1 N
Volume of KOH solution required for blank (b) = 20 ml
Therefore volume of KOH equivalent to acid
Content of oil = (b – a) ml

Now,

1ml of 0.1 N KOH solution = 5 mg of KOH

Therefore (b – a) ml of KOH solution = (b – a) X 5mg of KOH
Therefore acid value of oil solution = (a – b) X 5 mg of KOH
W g of oil

43
 ACID VALUE OF OIL
Ex No: 12

AIM:
To determine the acid number of an oil

PRINCIPLE:

Acid value or acid number or neutralization number is defined as the milligrams

of potassium hydroxide required to neutralize the free acid contents of 1 gram of oil
sample.

PROCEDURE:

Weigh accurately 10g of the given sample in a dry 250ml conical flask. Add 50ml
of a mixture of equal volume of 95% alcohol and water. The whole mixture is agitated
and then heated to boiling point for 5 minutes and cooled. A drop of phenolphthalein
indicator is added and titrated against the standard solution of potassium hydroxide, till
the pink colour persists for 10 seconds.
A blank titration is performed by following exactly all the above described steps
without taking oil. The difference in the volume of potassium hydroxide required in these
two titrations will represent the equivalent of acid present in the oil.

RESULT:

The acid value of the given sample of oil = ____________

44
OBSERVATIONS:

LOSS ON IGNITION:

Weight of the empty weighing bottle =

Weight of the weighing bottle + cement
 Before transfer =
 After transfer =
Weight of empty Silica crucible =
Weight of empty Silica crucible + cement
 Before heating =
 After heating =
Weight of cement sample taken =
Loss in weight due to ignition =
Percentage loss on ignition =

INSOLUBLE RESIDUE:

Weight of the empty weighing bottle =

Weight of the weighing bottle + cement
 Before transfer =
 After transfer =
Weight of cement sample taken =
Weight of gravimetric filter paper =
Weight of the filter paper + residue after incineration =
Weight of insoluble residue =
Percentage of insoluble residue =

SULPHUR TRIOXIDE:

Weight of cement sample taken =

Weight of gravimetric filter paper =
Weight of the filter paper + residue after incineration =
Weight of barium sulphate precipitated =

45
 ANALYSIS OF CEMENT

EX No: 13

AIM:
To analyze the given sample of cement and estimate the loss on ignition, insoluble
residue, sulphur tri- oxide, silica, iron and aluminum oxides, lime and magnesia.

PROCEDURE:

(A) LOSS ON IGNITION:

Heat one gram of cement in a weighed silica (or porcelain) crucible placed in a
hole in an asbestos board, clamped horizontally so that 3/5th of the crucible projects
below the board, heat at full red hot for 15 minutes at 900 to 1000ºC and cool in a
desicator and weigh. Check the loss in weight in a second heating for 5 minutes. Take
care to wipe off particles that may adhere to a crucible when withdrawn from the board.
(OR)

Place the crucible in a muffle furnace heated to 900 to 1000 ºC for 15 minutes, cool in a
desicator and weigh. Check the weight in the second heating for 5 minutes. Report the
loss in weight as a percentage on the cement. (Do not use porcelain crucible with a
muffle furnace. Use a silica crucible.)

(B) INSOLUBLE RESIDUE:

Weigh 1gm of the cement sample accurately into a 100ml beaker. Add 10ml of
distilled water and 5ml of con HCl. Heat the solution and grind the material with
flattened end of a glass rod until it is evident that the decomposition is complete. Dilute
the solution upto 50ml and digest on a steam bath for 15 minutes. Filter and wash the
residue 6 times with distilled water. Combine the filtrate and washings and reserve for
sulphur trioxide determination. Ignite at a red heat in a weighed crucible to constant
weight. Cool and weigh as insoluble residue and express as a percentage.

46
 233g of barium sulphate contains 32g of sulphur
Weight of sulphur present =
80g of SO3 contains 32g of sulphur and 48g of oxygen
Therefore sulphur trioxide present =

SILICA:

Weight of the empty weighing bottle =

Weight of the weighing bottle + cement
 Before transfer =
 After transfer =
Weight of cement sample taken =
Weight of gravimetric filter paper =
Weight of the filter paper + residue after incineration =
Weight of silica residue =
Percentage of silica =

IRON AND ALUMINUM OXIDES:

Weight of cement sample taken =

Weight of gravimetric filter paper =
Weight of the filter paper + residue after incineration =
Weight of Iron and aluminum oxide residue =
Percentage of iron and aluminum oxide residue =

47
(C) SULPHUR TRIOXIDE:

Take the filtrate got from the above experiment in a 500ml beaker and heat to
boiling. Add to this boiling solution, a hot 10% solution of barium chloride, slowly drop
by drop with stirring and continue the boiling for 15 minutes. Cool the contents, allow the
precipitate to settle and test for complete precipitation. Filter through gravimetric filter
paper and wash the precipitate first with hot water, and then followed by distilled water
till the washings are free from barium chloride. Dry the filter paper in an oven and
incinerate in a weighed crucible to constant weight. Cool in a desicator and weigh as
barium sulphate. Calculate the Sulphur tri-oxide and report as a percentage.

(D) SILICA:

Weigh 0.5g of cement accurately and transfer to a china dish. Add 10ml of water
to prevent lumping and then 10ml of con HCl. Evaporate the contents to dryness on a
steam bath. Heat the residue to about 150ºC for half to one hour. Add 20ml of 1:1 HCl,
cover the dish and digest for 10 minutes on the steam bath. Dilute and filter through a
gravimetric filter paper, washing thoroughly. Place both the papers in the weighed
crucible, dry and incinerate to constant weight. Cool in a desicator and weigh as silica.

(E) IRON AND ALUMINUM OXIDES:

To the filtrate from silica determination (which should be about 250ml) add 5ml
of con HCl and a little bromine water. Add ammonium chloride and make up alkaline
with sufficient ammonium chloride and make up alkaline with sufficient ammonium
hydroxide. Boil until the odour of ammonia is nearly but not quite gone. Cool, allow the
precipitate to settle and filter through a gravimetric filter paper.
Wash the precipitate, first with hot water and then with ammonium nitrate
solution and again with hot water and finally with distilled water. Combine the filtrate
and washings and reserve for the estimation of lime. Dry the precipitate in an oven and
then incinerate in a weighed crucible to constant weight. Cool and weigh the iron and
aluminum oxides (Al2O3).

LIME:
48
 Weight of cement sample taken =
Weight of gravimetric filter paper =
Weight of the filter paper + residue after incineration =
Weight of lime residue =
Percentage of lime residue =

MAGNESIA:

% of magnesia =100 - {% of [loss of ignition + insoluble residue +sulphur

trioxide + silica + lime +iron and aluminum oxides] }

(F) LIME (CaO):

To the filtrate from iron and aluminum oxides, add 1ml of liquor ammonia and
heat to boiling. To this boiling solution, add 25ml of boiling saturated ammonium oxalate
solution. Continue the boiling for 5min, cool the contents and allow the precipitate to
settle. Test for complete precipitation and filter through a gravimetric filter paper and
wash the precipitate well with distilled water. Dry the precipitate in an air oven, ignite in
a weighed crucible, cool and weigh as lime.

(G) MAGNESIA (MgO):

To the filtrate got from the lime estimation, add a slight excess of dil HCl and boil
to about 150ml. make the contents alkaline by the addition of ammonium hydroxide.
Cool and add 10ml of saturated microscopic salt (NaNH4.HPO4) solution, followed by
ammonium hydroxide. Set aside the contents overnight and filter through a gravimetric
filter paper. Wash the precipitate with water containing 25 % NH3 (con ammonia diluted
to 1:9) followed by distilled water. Dry the filter paper, incinerate in a weighed crucible,
cool and weigh the magnesium pyrophosphate. Calculate to MgO and report as a
percentage.

RESULT:

49
 From the analysis of the given cement sample
 % Loss on ignition =
 Insoluble residue =
 Sulphur tri oxide =
 Silica =
 Iron and aluminum oxides =
 Lime =
 Magnesia =

OBSERVATIONS:

Normality of alcoholic potash = 0.5 N =

Volume of alcoholic potash taken for saponification = V ml =
Volume of alcoholic potash taken for blank titration = V ml =
Volume of N/2 HCl required in the saponification = a ml =
Volume of N/2 HCl required in the blank titration = b ml =

Therefore volume N/2 HCl equivalent to KOH

Used in saponification value = (a – b) ml =

Quantity of oil taken (W) = g

Saponification value = 56.1 x (b – a) / (2 x W) mg of KOH
= g of oil

50
 SAPONIFICATION VALUE OF OIL
Ex No: 14

AIM:
To determine the saponification value of a given sample of oil

PRINCIPLE:

The saponification value is the measure of saponificable matter in an oil, also it

gives an estimation of the non-fatty impurities present in the oil. It also gives the actual
amount of alkali required by an oil or fat for its conversion to soap.

PROCEDURE:

Weigh accurately about 5g of the oil, and transfer to a 250ml round bottom flask.
Add from the burette, 50ml of 0.5N alcoholic potash. A water cooled reflux condenser is
fitted to the flask and refluxed for 1 hour. A blank experiment is performed by following
the above steps by taking 50ml of 0.5N alcoholic potash alone in the round bottom flask.

The solution in the flask after reflux is titrated against a standard 0.5N HCl using
phenolphthalein indicator. The difference in these two volumes of acid is equivalent to
KOH used up for the saponification.

PREPARATION OF SOLUTIONS:

ALCOHOLIC POTASH:
Dissolve 30g of pure KOH in litre of 95% alcohol by volume, mix thoroughly and
allow it to stand for 1 or 2 days, till all carbonate has settled out. Take the clean solution
for use.

RESULT:
The saponification value of the given sample of oil = ______________
51
OBSERVATIONS:

Weight of empty china dish =

Weight of empty china dish + soap =
Weight of empty china dish + soap (after transfer) =
Weight of soap transferred = 20 g

TOTAL FATTY MATTER:

Weight of wax taken =5g

Weight of total fatty matter + wax = 18 g
Weight of total fatty matter alone =
100ml solution contains =
250ml solution contains =
Percentage of total fatty matter =

52
 ANALYSIS OF SOAP

Ex No: 15

AIM:

To determine the total fatty matter in the given sample of soap.

PROCEDURE:
About 20gm of the soap sample was weighed and it was dissolved in 150ml of hot
water. The solution was transferred while hot into 250ml standard flask and it was made
up to the mark.

TOTAL FATTY MATTER:

Pipette out 100ml of the made up original solution into a 250ml beaker. Add
concentrated nitric acid until the contents are slightly acidic. Heat the solution on the
water bath until the fatty acids have collected in a clear layer on top and the solution
below is perfectly clear. Weigh accurately about 5g of paraffin wax and add to the
contents of the beaker. Continue the heating on the water bath, till the wax completely
melts and gets mixed with the fatty acids as the top layer and the solution remains
perfectly clear. Cool in ice water or let it stand overnight. Remove carefully, the wax
layer containing fatty acids and wash it with distilled water. Dry carefully between the
faces of the filter papers and transfer to a previously weighed watch glass. Weigh
accurately the wax layer and subtract from it, the amount of wax previously taken. Report
as a percentage.

RESULT:

Percentage of total fatty matter present in the

given sample of soap = ___________________ %

53
OBSERVATIONS AND CALCULATIONS:

Concentration of KMnO4 in the standard solution:

Standard plot:

Reference : deionized water

Sample : KMnO4 solutions at different concentrations
Wavelength : 511nm

Sample Concentration (mg/l) Absorbance

no

1
2
3
4
5

Absorbance of the given sample solution at 511nm =

From the standard plot, the concentration of KMnO4 =

MODEL GRAPH:

Absorbance Unknown concentration

Concentration (mg/l)

54
 ESTIMATION OF KMnO4 BY SPECTROSCOPY
Ex No: 16

AIM:

To determine the concentration of potassium permanganate in the given sample

using a uv – visible spectrophotometer.

THEORY:

Colourimetric analysis is used to measure the connection of the given coloured

sample by measuring the transmittance or absorbance of a sample as a function of
wavelength. Spectrophotometer is one such equipment used for colourimetric analysis. In
the spectrophotometer transmittance ‘T’ is a fraction of the incident power which is
transmitted by a sample.

T = P/P0, where P and P0 are the incident and transmitted radiant powers.

The term log (P0/P) is called the absorbance and is denoted by “A”

Hence A = log (1/T) and %T = (P/P0) x 100

If ‘b’ is the length of path through the absorbing medium, then according to the
bougher beer’s law, A = abc when the concentration of the absorbing solute ‘c’ is
expressed in (g/l) or A = εbc, where c is in (moles/l). A and ε are absorptivity and molar
absorptivity respectively

ε = (a x M) where M is molecular weight, of the absorbing substance in the solution.

Absorption spectra is the plot of (absorbance vs wavelength).

ESTIMATION OF POTASSIUM PERMANGANATE BY

SPECTROPHOTOMETRY
55
OPERATION PROCEDURE

Step 1: Switch on the computer

Step 2: Click – start-program - UV-Vis spectrophotometer-119

Step 3: Click – Mode - single wave length - parameters

Step 4: Enter wavelength (511.0) and press OK

Step 5: Click – lamp - Vis

Step 6: Put reference solution in UV spectrophotometer

Step 7: Click – mode - single wavelength - sample

Step 8: Put sample and click OK

Step 9: Click – mode – Reference - OK

Step 10: Put reference and click OK

Step 11: Follow the steps from 7 to 11 for different concentrations.

PROCEDURE:

56
(A) STANDARD PLOT:

0.1g of KMnO4 is weighed accurately. It is dissolved in deionized water and is made

up to mark in a 1 liter standard flask. This would give the stock solution, whose
concentration is 100ppm. From this samples, different concentrations are prepared. The
absorbance of each samples against deionized water, as reference at wavelength of
511nm is determined using uv – visible spectrophotometer. Absorbance vs concentration
graph is plotted for above samples. The best straight line was drawn between the points.

(B) DETERMINATION OF KMnO4:

The absorbance of the given sample solution against deionized water is measured,
as reference at same wavelength used for standard plot. The unknown concentration of
KMnO4 is determined from the standard plot.

RESULT:

The concentration of potassium permanganate in the given sample =__________.

57
 DETERMINATION OF SODIUM IN WATER SAMPLE BY
FLAME PHOTOMETRY

S.No Concentration
ppm

The wavelength of light = nm

The dilution factor =
The concentration of unknown sample = ppm

58
 DETERMINATION OF SODIUM IN THE WATER SAMPLE BY FLAME
PHOTOMETRY
Ex No: 17

AIM:

To determine the amount of sodium present in the given sample using flame photometer

PRINCIPLE:

Flame photometry (or) flame emission spectroscopy is based on the principle of

emission of certain radiation in the visible region by a metal atom.

In this technique, metal atom is thermally excited from the ground state. The
excited atom emits light of a particular intensity while returning to the ground state
depending upon the concentration of the metal ions

A given sample to be analyzed is sprayed into the flame, where the water
evaporates leaving the fine salt particles. This salt decomposes into constituent atoms,
when they are heated to about 1700ºC. the vapors containing metal atoms are excited by
the thermal energy of the flame to higher energy state.

When the electrons fall down from the excited state to ground state they emit
radiation. The emitted radiation is measured and recorded.

The emission spectrum for each metal is different and its intensity depends on the
concentration of the atoms in the flame. Sodium produces a characteristic yellow
emission at 589nm.

Flame at Emission
NaCl Na* Na
1700ºC (excited state) (Ground state)

59
OPERATING PROCEDURE:

Step 1: Switch on the instrument

Step 2: Switch on the compressor
Step 3: Press 3 to set flame
Step 4: Aspirate distilled water, ignite flame, press enter
Step 5: Set fuel to get blue cone, press enter
Step 6: Adjust to fuel for best flame stability
Step 7: Press 1 to get operating mode
Step 8: Press 2 to get high concentration
Step 9: Press y to select element sodium, press enter
Step 10: Enter dilution factor as 1
Step 11: Enter number of standards
Step 12: Enter sodium standard concentration in decreasing orders
Step 13: Press 5 for calibration
Step 14: Aspirate standards in descending orders, between each standards you have to
aspirate distilled water
Step 15: Press 6 to get sample analysis and press enter
Step 16: Aspirate distilled water
Step 17: Aspirate sample
Step 18: Value will be shown
Step 19: Switch of the gas supply
Step 20: Aspirate distilled water for 5 minutes
Step 21: Aspirate air for 5 minutes
Step 22: Switch off the compressor
Step 23: Switch off the instrument

60
PROCEDURE:

DETERMINATION OF SODIUM IN THE GIVEN SAMPLE:

The instrument is switched ON and then followed by the compressor. The

instrument gas control is set to ignite position. The flame is ignited. It is adjusted to get
outer blue cone and inner red cone

The electronic module of the photometer is fed with the number of standard
solutions to be used. Using the standard solutions prepared, the system is standardized.
Distilled water is aspirated between two successive standardizations. The solution of
unknown concentrations is sprayed into the flame. The emitted light from the flame
passes through an optic filter to a photo detector. The output of the detector is processed
by the electronic unit and the result is directly displayed. This gives the value of
concentration of the required substance in the given sample.

RESULT:

The amount of sodium present in the sample =____________________.

61
 pH - METER

Ex No: 18

AIM:

To determine the pH of unknown solution by buffer using pH meter

PRINCIPLE:

The degree of acidity or alkalinity of a solution is expressed by the pH scale

which is a series of number between 0 and 7. The term pH was first coined in the year
1909 by Sorensen and was defined as the negative logarithm of hydrogen ion
concentration, which is expressed in molarity.

pH = - log[H+] (or) – log[OH+]

pH = (0.4573 – emf x 10-3 )/0.0591

PROCEDURE:

Keep the 0 - 7 /STD- BY/ 7 – 14 switch in STD-BY position. Switch on the

instrument. Allow 10 minutes to stabilize. Wash the electrodes by a jet of distilled water
and wipe them with soft tissue paper or filter paper. Do this washing and wiping before
each measurement. Immerse the electrodes in a beaker containing the standard buffer of
0.7 pH. Set the range switch in appropriate pH range (say 0-7 pH). Measure the
temperature of the buffer solution (in ºC) and set this value on the TEMP ºC control.
Meter indicates some value. Set this reading exactly to the buffer pH value (7.0) by
means of the ‘CAL’ control. Now check readings of 4.0 pH and 9.2 pH buffers.

Their readings should be 4.0 to 4.1 pH and 9.1 to 9.2 pH respectively, depending
upon the accurately of the buffer. Put the unit in STD-BY position. The instrument is
now to read unknown solution.
62
To measure the pH of the unknown solution, immerse the electrodes in that solution.
Select the proper pH range and read the pH indicated by the meter on the scale to which
the unit is set. Please read the scale 7-14 from left to right and the scale 0 – 7 from right
to left.

RESULT:

The pH of the given unknown buffer solution ___________________

63
TABULATION:

S.No Volume of sulphate solution Turbidity(NTU) Turbidity(ppm)

(ml)
1 0.5
2 1
3 1.5
4 2
5 2.5
6 unknown

CALCULATIONS:

100NTU = 250ppm
1 NTU = 2.5 ppm

MODEL GRAPH:

Turbidity

Concentration

GRAPH: It is plotted between the concentration of the solution and turbidity

64
 NEPHELOMETER
Ex No: 19

AIM:

To estimate the concentration of sulphate present in the given sample solution by

using turbiditymeter

REAGENTS:

Standard sulphate solution, NaCl-HCl solution, BaCl2, glycerol-ethanol solution

PRINCIPLE:

Nephelometer operates on the principle of Tyndall effect. The amount of

scattering of incident light by a dispersant of anion or element in a sample solution is a
measure of turbidity and from it, the concentration of ion in the sample is determined

TURBIDITY:

It is the optical property of a sample which causes light to be scattered and

absorbed rather than transmitted in straight lines through the sample. The dispersion is
actually an optical in homogeneity, resulting in light scatter. The intensity of the
particularly polarized component of scattered light are functions of the relative refractive
index. The size parameter, the angle of observation, as well as to the concentration of
dispersant

65
REPARATION OF REAGENTS:

PREPARATION OF STANDARD SULPHATE SOLUTION:

1.81g of dry potassium sulphate ion was dissolved in distilled

water and was made to 1 litre in a volumetric flask. This solution contains 1mg of
sulphate ion per ml -1000ppm.

SODIUM CHLORIDE-HYDROCHLORIC ACID REAGENT:

60g of sodium chloride was dissolved in 200ml of distilled water and 5ml of
pure concentrated hydrochloric acid was added and diluted to 250ml.

BARIUM CHLORIDE:
Crystals of Barium chloride was used.

GLYCEROL-ETHANOL SOLUTION:
One volume of pure glycerol was dissolved in two volumes of absolute alcohol,
Ethanol

PROCEDURE:
Standards of 0.5,1,2,2.5 and unknown ml of the standard potassium sulphate
solution was taken into separate 100ml volumetric flasks. To each flask 10ml of NaCl-
HCl solution,20ml of Glycerol-Ethanol solution,0.3g of BaCl2 was added and it was
dissolved to 100ml with turbidity free distilled water.
The reagent blank was prepared in a separate 100ml flask. The instrument was
calibrated using reagent blank solution to set 0 and with reference standard of highest
known concentration to set 100.Now the instrument was used to find the values of
turbidity of other concentration. A graph was drawn between Concentration Vs Turbidity.

RESULT:
The concentration of the sulphate present in the given unknown sample solution is
_______

66
Titration I
Standardisation of sodium thio sulohate solution:
Burette solution : Sodium thio sulphate
Pipette solution : Potassium dichromate
Additional solution : 20ml of KI + 20ml of Dil.H2SO4
Indicator : Starch
End point : Disappearance of blue color

S.NO Volume of Burette readings Volume of Tire value

burette Initial Final pipette (ml)
solution (ml) value(ml) value(ml) solution(ml)

Calculation:
Volume of Potassium dichromate(V1) =
Normality of Potassium dichromate(N1) =
Volume of Sodium thio sulphate(V2) =
Normality of Sodium thio sulphate(N2) =

Titration II
Blank titration:
Burette solution : Sodium thio sulphate
Pipette solution : 20ml of prepared solution
Indicator : Starch
End point : Disappearance of blue color

67
 DETERMINATION OF IODINE VALUE OF OIL
EX.NO 20

AIM:
To determine the iodine value of the given soil sample.

PRINCIPLE:
The iodine number is defined as the number of centigrams of iodine absorbed to
the one gram of oil (i.e.) percentage of iodine absorbed to one gram of oil. The iodine
number is measure of the unsaturation present in given sample of the oil due to the
presence of double bond in carbon chain. If iodine value is more than oil will be behavior
more of unsaturation and hence the oil will be quick drying in nature.

PROCEDURE:

STANDARDISATION OF SODIUM THIO SULPHATE:

Prepare a standard solution of potassium dichromate (K2Cr2O7) of normality 0.1N
by weighing accurately 0.49gm of the salt using weighing bottle and transferring it into a
100ml standard flask dissolved with distilled water and make up to the mark. Pipette out
20ml of the above made up solution and transfer it into 250ml conical flask and add about
20ml dilute H2SO4 and 20ml of 10%KOH and stir the contents wait for 30 seconds.
Titrate it against sodium thiosulphate solution. Add drop by drop slowly and stir
the solution becomes pale yellow in color. In this state stop addition of sodium
thiosulphate solution and add 1ml of starch solution .The solution becomes deep blue in
color. The continuous addition of sodium thiosulphate solution in burette the solution
becomes pale yellow green colour due to the chromium salt. Note the burette reading.
Calculate the normality of sodium thiosulphate solution.
DETERMINATION OF IODINE VALUE:
Weigh accurately 0.1gm of oil sample into 250ml in a beaker. Add 15ml of CCl 4,
25ml of Hanus solution (Iodine mono bromide) in a beaker. Moisten the stopper bottle
with 15% of KI solution. Allow to stand for 1 hour. Rinse the stopper bottle. Transfer the
solution in beaker into the stopper bottle and add 20ml 15% KI solution and 100ml of

68
 S.NO Volume of Burette readings Volume of Tire value
burette Initial Final pipette (ml)
solution value(ml) value(ml) solution(ml)
(ml)

Volume of sodium thio sulphate solution required (V1): ml

Titration III
Determination of iodine value;
Burette solution : Sodium thio sulphate
Pipette solution : 20ml of prepared solution
Indicator : Starch
End point : Disappearance of blue color
S.NO Volume of Burette readings Volume of Tire value
burette Initial Final pipette (ml)
solution value(ml) value(ml) solution(ml)
(ml)

Volume of sodium thio sulphate solution required (V2): ml

Calculation:
Weight of weighing bottle (W1) =
Weight of weighing bottle + oil transferred (W2) =
Weight of oil (W2 – W1) =
Iodine value of an oil = ((V1 –V2) * N2 *1.269)/(W2 – W1)

69
boiled water. For blank titration, take 20ml of the prepared solution and titrate it with
standardized sodium thiosulphate using starch as a indicator.
For sample titration, take 20ml of the prepared solution and 0.1gm of oil. Titrate it
with standardized sodium thiosulphate using starch as a indicator.

RESULT:
Iodine value of a given oil = ____________

70
OBSERVATIONS:

Weight of the sample taken =

Weight of the fibre present =
Percentage of total cellulose =

71
ESTIMATION OF THE CELLULOSE CONTENT IN THE GIVEN CELLULOSE
BEARING MATERIAL
Ex No: 21

AIM:

To estimate the amount of total cellulose present in the given cellulose

bearing material.

PROCEDURE:

Weigh about 5g of the sample accurately into a 500ml beaker and add 200ml of
1% caustic soda solution. Cover with a watch glass and boil gently for half an hour. Filter
with suction in a 5” Buchner funnel. A little of the fibre will run through the path, that is
tile plate, at first and must be poured back after a good mat is formed. Wash the boiled
fiber with a good volume of hot water, loosen up the fibre with a sharp pointed glass rod,
and transfer the fiber in to a 250ml conical flask. Add 5g of bleaching powder and water,
stir the contents for 5 to 10 minutes. After bleaching, wash the material with hot water.
Place the pulp in a 250ml beaker and treat the pulp with 150ml of 2% sodium sulphite
solution. Bring the mixture to boil, add 3ml of 10% sodium hydroxide and boil for 5
minutes. Again collect the pulp on the filter plates and wash with hot water until the
washings are colourless. Repeat the above operations till a white pulp is got. Wash the
pulp with a large amount of water, with alcohol, and finally with ether. Dry the product,
first with gentle heat and finally at 100 to 1500ºC until the weight is constant. Weigh the
dried pulp and report as a percentage.

RESULT:

The total cellulose has found to be _________ %

72
OBSERVATIONS:
Weight of empty weighing bottle = g
Weight of bottle + sample = g
Weight of bottle after transfer = g
Weight of brass transferred = g

ESTIMATION OF TIN:
Weight of gravimetric filter paper = g
Weight of filter paper + residue = g
Weight of residue = g
Weight of tin = (weight of residue*118.7/154.7)
= g
% of tin = (weight of tin/weight of brass transferred)
= g

ESTIMATION OF LEAD:
Weight of empty crucible = g
Weight of crucible + residue after = g
incineration
Weight of residue = g
303.19g of PbSO4 contains 207.19g of lead .
0.03g of PbSO4 contains = g
% of lead = g

STANDARDISATION OF SODIUM THIOSULPHATE SOLUTION:

Weight of empty weighing bottle = g
Weight of Bottle + Sample = g
Weight of bottle after transfer = g
Weight of K2Cr2O7 transferred = g
Normality of K2Cr2O7 = N

73
 ANALYSIS OF BRASS
Ex No: 22

AIM:
To analyze the given sample of brass and estimate tin, lead, copper and zinc.

PROCEDURE:

(A) TIN:
Weigh accurately about 0.5g of the given sample of brass and transfer into a
100ml beaker. Add about 20ml of 1:1 nitric acid slowly without allowing the material to
spurt and stir well with a glass rod. When the vigorous reaction is over, heat the beaker in
a sand bath and evaporate the solution to about 10ml. Cool, add about 20ml of water and
boil for 5 minutes. Cool the solution and then allow the precipitate of the m-stannic acid
to settle. Filter through a no.40 gravimetric filter paper and wash the precipitate
thoroughly with hot water and then with distilled water till the washings are free from
copper. Collect the filtrate and washings in a 250ml beaker. Dry the filter paper in an
oven and incinerate in a previously weighed crucible to constant weight. Determine the
weight of stannic oxide obtained and calculate the tin and express to a percentage.

(B) LEAD:
Evaporate the filtrate and washings obtained from the above experiment over a
sand bath to about 100 to 120ml. cool and add 10ml of dilute sulphuric acid and
evaporate till white fumes are evolved. All the nitric acid is to be removed. Cool and
dilute to about 100ml. if lead is present, a white precipitate of lead sulphate will be seen.
Filter the precipitate in a no.40 gravimetric filter paper, and wash the precipitate
thoroughly with hot water and then with distilled water till the washings are free from
copper. Transfer the precipitate into a previously weighed silica crucible and carefully
incinerate at a temperature not exceed 600ºC. Cool, add 1 or 2 drops of dilute sulphuric
acid and carefully incinerate till the contents of the crucible are white in colour. Cool and
weigh the lead sulphate. Calculate the lead and express as a percentage.

74
 Burette solution : Sodium thio sulphate
Pipette solution : K2Cr2O7 + Dil.H2SO4 + 15%KI
Indicator : Starch
End point : Appearance of permanent green colour.

Volume of pipette Burette Reading

Sl.
solution Concordant titre Value
No
(ml) (ml) (ml)
Initial Final

Volume of K2Cr2O7 (V1) = ml

Normality of K2Cr2O7 (N1) = N
Volume of Na2S2O3(V2) = ml
Normality of Na2S2O3(N2) = N

ESTIMATION OF COPPER:

Burette solution : Sodium thio sulphate

Pipette solution : Sample solution
Indicator : Starch
End point : Appearance of creamy white precipitate

Volume of pipette Burette Reading

Sl.
solution Concordant titre Value
No
(ml) (ml) (ml)
Initial Final

75
(C) COPPER:
Standardize the given sodium thio sulphate using potassium dichromate. Transfer
the filtrate and washings from the lead estimation to 250ml standard flask and make upto
the mark. Pipette out 20ml of the made up solution into a 250ml conical flask. Add
ammonium hydroxide solution drop by drop with stirring till a pale blue precipitate of
copper hydroxide is formed. Add 10ml of dilute acetic acid and 10ml of 15% potassium
iodide solution. Titrate the liberated iodine against the standardized sodium thio sulphate
solution using starch indicator, until the brown colour due to iodine has changed to
yellow. Add starch, continue the titration, stirring constantly until first drop changes the
colour from blue to yellowish white (not pure white). The end point is rendered sharp by
adding 1 or 2 drops of 0.1N silver nitrate. The yellowish colour of silver iodide
neutralizes the purplish tinge of cuprous iodide. Calculate the copper present in the whole
of the given solution and express to a percentage.

(D) ZINC:
From 100, subtract the total percentage of tin, lead, copper to report the remaining
as zinc.
RESULT:

The analysis of brass was made and the following were determined

 Tin = %
 Lead = %
 Copper = %
 Zinc = %

76
1000ml of 0.1N Na2S2O3 = 6.357g of copper
3.9ml of 0.09N Na2S2O3 contains = g of Cu
20ml of solution contains = g of Cu
250ml of solution contains = g
% of copper = %

ESTIMATION OF ZINC:
% of Zinc = 100 – % of (tin +copper + lead)

77
OBSERVATIONS:
LOSS ON IGNITION:

Weight of the empty weighing bottle =

Weight of the weighing bottle + bauxite =
Weight of bottle after transfer =
Weight of bauxite sample taken =
Weight of empty Silica crucible =
Weight of empty Silica crucible + bauxite
 Before heating =
 After heating =
Loss in weight due to ignition =
Percentage loss on ignition =

ESTIMATION OF SILICA:

Weight of the empty weighing bottle =

Weight of the weighing bottle + bauxite =
Weight of bottle after transfer =
Weight of bauxite sample taken =
Weight of gravimetric filter paper =
Weight of the filter paper + residue after incineration =
Weight of silica residue =
Percentage of silica =

ESTIMATION OF TOTAL R2O3:

Weight of the empty weighing bottle =

Weight of the weighing bottle + bauxite =
Weight of bottle after transfer =
Weight of bauxite sample taken =
Weight of empty silica crucible =
Weight of crucible after incineration =
Weight of total Iron and Aluminium oxide =

78
 ANALYSIS OF BAUXITE
Ex No: 23

AIM:
To estimate the following in the given sample of bauxite.
 Loss on ignition
 Silica
 Iron and aluminum oxides

PROCEDURE:

(A) LOSS ON IGNITION:

Ignite 0.5g of the ore in a weighed platinum or silica crucible, first over a Bunsen
burner and finally with a blast lamp to constant weight. Calculate the loss in weight to a
percentage, which is due to moisture and organic matter.

(B) ESTIMATION OF SILICA:

Weigh 1g of the powered sample into a 250ml beaker and 50ml of 1:1 sulphuric
acid. Digest the contents on a hot plate with the beaker covered for 3 hours and then
evaporate until white fumes come off strongly. Cool thoroughly, add 100ml of distilled
water and boil for 10min. filter and wash the contents with hot water. Ignite the insoluble
residue in a platinum crucible (which need not be weighed) and finally in a blast lamp for
15minutes, cool in a desicator and weigh. This residue contains SiO2 a little TiO2, Fe2O3
and Al2O3.

To determine silica, treat the insoluble residue in the platinum crucible with about
1ml of dilute sulphuric acid and fill it half full with HF. Evaporate and repeat the
operation once. Ignite the residue to drive off all H2SO4, then heat in full flame with a
mecker burner. Cool in a desicator and weigh. Report the loss in weight to % HF
treatment as a percentage and estimate silica.
ESTIMATION OF IRON OXIDE:
79
Volume of KMnO4 consumed in titration (V) =
For 50ml of the solution

1ml of 0.1N KMnO4 is equivalent to = 0.005585g of iron

___ ml of ___ N KMnO4 is equivalent to =

Therefore 500ml of the solution contains = g Fe

111.7g of Fe gives 159.7g of Fe2O3

_____ g of Fe gives = g Fe2O3

Percentage of Iron oxide =

ESTIMATION OF ALUMINUM OXIDE:

Amount of aluminum oxide = Total R2O3 – Iron oxide

Percentage of aluminum oxide =

80
(C) ESTIMATION OF IRON AND ALUMINUM OXIDE:

Grind the sample to a fine powder to pass through a 100 mesh screen. Weigh 2g of
the material accurately into a Kjedals digestion flask, together with 20g of 3:2 sulphuric
acid. Connect to a reflux condenser and boil for 3 hours. Cool immediately, dilute with
water, filter and wash into a 500ml standard flask and make upto the mark.

(D) TOTAL R2O3:

To 50ml of the above made up solution, add 10ml of dil HCl, add a little of
ammonium hydroxide, and let it stand on a steam bath for 15 minutes. Filter through a
gravimetric filter paper using a filter pump and a slight suction. Wash the precipitate 4
times with hot water, then followed by low heat in a weighed crucible with a smooth
glass rod, then ignite to constant weight, cool in a desicator and weigh. Calculate the
R2O3 to a percentage

(E) IRON OXIDE:

To 100ml of the above made solution, add a little zinc dust and evaporate it to
dryness, and destroy the organic matter by heating with an excess of KMnO4. Neutralize
with ammonium hydroxide and reduce the iron to ferrous state with a current of SO2. Boil
the excess SO2 carefully, cool and add a little of mercuric chloride solution to ensure the
removal of the traces of SO2. cool, acidify with dil H2SO4 and titrate with standard
KMnO4 solution. Calculate the iron to R2O3 and express as a percentage.

(F) ALUMINUM OXIDE:

Subtract the percentage of Fe2O3 from the total percentage of R2O3, and report the
rest as Al2O3

81
RESULT:
From the analysis of the given sample
 The amount of loss on ignition =
 The percentage of silica =
 The percentage of iron oxide =
 The percentage of Aluminum oxide =

82
OBSERVATIONS:

Weight of the empty weighing bottle =

Weight of weighing bottle + salt before transfer =
Weight of weighing bottle + salt after transfer =
Weight of salt transferred =
Normality of solution =

BLANK TITRATION:

Pipette solution : Distilled water

Burette solution : Ferrous Ammonium Sulphate
Indicator : Ferroin indicator
End point : Colour change from blue green to wine red

Volume of Burette Reading Volume of Concordant titre

Sl. pipette solution (ml) Ferrous Value
No (ml) Ammonium (ml)
Initial Final Sulphate Used
(ml)

Volume of Ferrous Ammonium Sulfate consumed =

83
 DETERMINATION OF CHEMICAL OXYGEN DEMAND

Ex No: 24

AIM:
To determine the chemical oxygen demand for the given sample.

PRINCIPLE:

The chemical oxygen demand is the measure of oxygen equivalent to the portion
of organic matter in a sample that is susceptible to oxidation by a strong chemical
oxidant. Normally this is expressed in mg/litre of oxygen consumed under specific
condition for the oxidation purpose. Many type of organic matter are completely oxidized
by a boiling mixture of chromic and sulphuric acid to produce CO2 and H2O. A measured
quantity of sample is refluxed with a known amount of potassium dichromate and
sulphuric acid. The excess of dichromate which remains unreacted is titrated against
ferrous ammonium Sulphate solution. The potassium dichromate consumed is
proportional to the amount of oxidizable matter measured as oxygen equivalent.

APPARATUS:

Reflux apparatus consisting of a 25ml flat – bottomed flask with a grounded glass
joint and a condenser.

REAGENTS:

 Standard 0.5N Potassium dichromate

 Sulphuric acid silver Sulphate reagent
 Standard ferrous ammonium sulphate solution
 Ferroin indicator
 Mercuric Sulphate crystal

84
TITRATION:

Pipette solution : Sample solution

Burette solution : Ferrous Ammonium Sulphate
Indicator : Ferroin indicator
End point : Colour change from blue green to wine red

Volume of Burette Reading Volume of Concordant titre

Sl. pipette solution (ml) Ferrous Value
No (ml) Ammonium (ml)
Initial Final Sulphate Used
(ml)

Volume of Ferrous Ammonium Sulfate consumed =

CHEMICAL OXYGEN DEMAND:

Strength of Ferrous Ammonium Sulfate (N) =

Volume of sample taken =
Blank titre value (V1) =
Sample titre value (V2) =
0.125 N potassium dichromate solution = 1mg of oxygen
Chemical oxygen demand (C.O.D of WA) = (V1 – V2) x N x 8 x 1000 mg/l
X

85
PROCEDURE:

Accurately weigh 1.96g and dissolve in 100ml of water to prepare 0.05N standard
solution of ferrous ammonium sulfate.

DETERMINATION OF CHEMICAL OXYGEN DEMAND:

Place 0.1g of mercuric sulphate in a flask and add 5ml of the sample or an aliquot
of the sample diluted and then add 5ml of distilled water. Mix well and add 2.5ml of 0.5N
potassium dichromate solution and 7.5ml of sulphuric acid – silver sulphate reagent while
continuously swirling the flask thoroughly. Connect the flask to the condenser and heat
slowly the flask, reflux for about 2 hours at a constant temperature of 145ºC. Cool and
wash the condenser with distillated water such that water falls into the flask. Dilute it to
about 50ml and titrate the unreacted 0.5N K2Cr2O7 with ferrous ammonium sulphate
using Ferroin indicator. The colour change from blue green to wine red is the end point.
Perform blank experiment with water instead of sample.

RESULT:

The chemical oxygen demand of given sample is ___________________ mg

86
 OBSERVATION:
Burette solution : 0.0141N AgNO3
Pipette solution : Sample solution
Indicato : Potassium Chromate
End point : Appearance of red colour

Volume of
Sl. Volume of sample Burette Reading AgNO3 used Concordant titre
No taken (ml) Value
(ml) (ml) (ml)
Initial Final

CALCULATION:
Volume of Silver nitrate solution (V1) =
Normality of Silver nitrate solution(N1) =
Volume of sample solution (V2) =
Normality of sample solution (N2) =
V1N1 = V2N2
N1 = V1N1 /V2
Normality of sample solution (N2) =

The amount of chloride present = Normality of the X 35.5 X 1000

in the sample sample solution

The amount of chloride present in the given water sample is ___________ mg/l

87
 DETERMINATION OF CHLORIDE CONTENT IN THE GIVEN WATER
SAMPLE
Ex No : 25
AIM:
To determine the chloride content of given water sample.
PRINCIPLE:
Chlorides occur naturally in all types of water. In natural freshwater its
concentration remains quite low and is generally less than that of sulphates and
bicarbonates. The most important source of chlorides in water is the discharge of
domestic sewage. Therefore the chlorides concentration serves as an indicator of
pollution by sewage. It is harmless upto 1500 mg/l but produces a salty taste at 250-500
mg/l level. Magnesium Chloride in water generates hydrochloric acid after heating,
which is highly corrosive. Silver nitrate reacts with chloride to form very slightly soluble
precipitate of AgCl. At the end when all the chlorides get precipitated free silver ions,
react with chromate to form silver chromate of reddish brown colour.

PROCEDURE:
Take 50 ml of the given water sample in a conical flask. Add 2 ml of 5%
potassium chromate solution and titrate with 0.0141N Silver nitrate solution until a
persistent red colour appears.

PREPARATION OF REAGENTS:

1. Silver Nitrate solution:

Dissolve 2.395g of AgNO3 in a 1000ml standard flask and make upto the mark.
2. Potassium Chromate, 5%
Dissolve 5g of K2CrO4 in a 100ml standard flask and make upto the mark.

RESULT:
The amount of chloride present in the given water sample is ___________ mg/l

88