1.

ESTIMATION OF MANGANESE DIOXIDE IN PYROLUSITE

AIM
To estimate the percentage of manganese dioxide present in the given sample of Pyrolusite
ore.
APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker
PROCEDURE
TITRATION - I
Standardization of Potassium permanganate
Pipette out 20 ml of std solution of 0.1N oxalic acid into a clean conical flask. Add 20ml of
8N sulfuric acid. Heat gently upto parable warm, titrate the warm solution with KMnO 4 taken
in the burette until just appearance of permanent pale pink color.
TITRATION II
Weigh out accurately above 0.25 gm of pyrolusite ore into a clean conical flask. Add 20ml
of dilute sulfuric acid and boiled for 10 minutes. Cool the flask then add 40ml of 0.1N oxalic
acid solution through pipette and heat gently up to 30 minutes. Titrate the content of the
conical flask against already standardized KMnO 4 taken in the burette, until the appearance
of permanent pale pink colour.
Standardization of Potassium permanganate
Standard Oxalic acid Vs KMnO4
Indicator: Self
End Point: Appearance of pale permanent pink color.

S. No Volume of Std Initial Final burette Volume of Concordant

Oxalic acid burette reading value
reading KMnO4
(ml) (ml) (ml)
(ml) (ml)

01
02
Volume of Oxalic acid V1 =20ml
Strength of Oxalic acid N1 =0.1N
Volume of KMnO4 V2 =
Strength of KMnO4 N2 = V1 N1 / V2

Estimation of Manganese di oxide in Pyrolusite ore:

Standardized KMnO4 Vs Pyrolusite + Standard Oxalic acid
Indicator: Self
End point: Appearance of pale pink colour.

Sl Volume of Std Oxalic Initial Final burette Volume of Concordant

acid burette reading value
.No reading KMnO4
(ml) (ml) (ml)
(ml) (ml)

Oxalic acid consumed by MnO4 in Pyrolusite ore = 2V1 - V2

2X40-9.4
= 70.6ml
Conversion factor
1ml of 0.1N oxalic acid consumes 0.00435 gm of MnO2.
=
RESULT

Percentage of MnO2 present in the given sample of pyrolusite = %

 2.ESTIMATION OF MAGNESIUM

AIM: To estimate the amount of Magnesium in the whole of the given solution of magnesium
sulphate.
APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker
PROCEDURE:
TITRATION 1:
Exactly 0.025 N solution of MgSO 4 7H2O is prepared in a 100 ml Standard flask.
Exactly 20 ml of this is taken in a 250 ml conical flask and diluted to about 100 ml. About 2 ml
of buffer of 10 PH and 2 to 4 drops of EBT indicator is added. The solution is warmed to 40 o C
and titrate against EDTA solution. The end point is change of color from wine red to pure blue.
The titration is repeated for concordant values. From the titre values, the strength of EDTA
solution is calculated.
TITRATION 2:
The given magnesium solution is made up to 100 ml in a standard flask a well shaken.
Exactly 20 ml of this solution is pipette out into clean conical flaks and diluted to about 100 ml.
About 2 ml of the buffer solution followed by a 3 or 4 drops of Eriochrome Black T indicator is
added to it. The solution is warmed to 40 oC and titrated against standardized EDTA solution
taken in the burette. At the end point, the wine red color changes to a pure blue. The titration is
repeated for concordance. From the titre values the strength of magnesium solution and hence its
amount is calculated.
TITRATION 1
Std EDTA Vs MAGNESIUM SULPHATE:

S. No Volume of Initial Final burette Volume of Concordant

burette reading value
MgSO4 7H2O reading EDTA
(ml) (ml)
(ml) (ml) (ml)

01
02
TITRATION 2

S. No Volume of Initial Final burette Volume of Concordant

burette reading value
MgSO4 7H2O reading EDTA
(ml) (ml)
(ml) (ml) (ml)

01
02

CALCULATIONS:

Strength of EDTA Solution: 20 x N1 / Titre Value = N2

Strength of the given Magnesium solution: N2 x Titre Value / 20 = N3

Amount of Magnesium present in the 100 ml of the given solution =

N3 x Atomic mass of Mg (24.01) / 100

RESULT:
Amount of Magnesium present in 100 ml of the given solution is = gm
 3. ESTIMATON OF COPPER IN BRASS
AIM:
To estimate the percentage of copper present in the given sample of brass
APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker
PROCEDURE:
TITRATION I: STANDARDIZATION OF TIOSULPHATE
Pipette out 20ml of the std. solution of 0.1Ncopper sulphate in to a conical flask; add 1:1
ammonia dropwise until the appearance of blue cupric ammonium complex. Add 1:1acetic acid
until the blue color just disappears. The add 15ml of 10% KI solution. Immediately titrate it with
thio taken in the burette, until the solution becomes light yellow. Add 1ml of freshly prepared
starch solution and continue the titration slowly until the solution becomes light blue .Repeat the
titration to confirm titre value
TITRATION II:
Weight out accurately about 0.5g of brass sample to a clean conical flask, Add above
10ml of 6Nnitric acid and the flask is gently heated, until the sample is completely dissolved.
Filter the solid metastanic acid and to the filtrate add 10ml of con sulphuric acid and evaporate it,
allow cooling and adding20ml of distilled water. To the filterate add ammonia until the
appearance of blue precipitate just disappears .then ad 2ml of precipitate just disappears, then
add 2ml of phosphoric acid cool the solution and transferred to a 100ml std flask make up to the
mark using distilled water. Pipette out 20ml of this solution to a clean conical flask. Add 15ml KI
and titrate against standardized thio as before using starch indicator
OBSERVATION AND CALCULATION:
STANDARDIZATION OF TIOSULPHATE:

Sl Volume of Burette Reading Volume of Concordant

thio run down value
No Copper sulphate Initial Final
solutio (ml) (ml)
(ml) (ml)
(ml)

Weight of watch glass (W1) gm =

Weight of watch glass and sample = (W2) =
Weight of the sample = (W2-W1) gm

Normality of copper solution = v2XN1/20

Atomic weight of copper= equivalent weight of copper
Amount of copper = (normality X atomic weight of copperX100)//1000= b gm
Percentage of copper= bX100/ (w2-w1) = C%

RESULT:

Percentage of copper present in the given sample of brass= %

 4. ESTIMATION OF NITROGEN BY KJELDOL METHOD

AIM:

To estimate the amount of nitrogen by Kjeldahl Method

APPARATUS REQUIRED:

Kjeldahl apparatus, conical flask

PROCEDURE:

The Urea whose quantity of Nitrogen is to be estimated is taken in a small amount of

weight 0.5 to 5g in Kjeldhal's flask. A known volume of concentrated H 2SO4about 20ml is added
to the organic compound and also about 8-10g of potassium sulphate is added to the kejaldahl's
flask.A few drops of Hg is added as catalyst.

The flask is fitted at the mouth by a glass stopper and is kept clamped in an inclined
position the Kjeldhal's flask is fitted with a safety trap and then heated in fume chamber.
Amonium sulphate gets formed and the colour of the solution changes.

The mixture in the flask boils slowly and the dark colour of the solution becomes colourless
slowly. After this, the flask is cooled and the content is diluted with distilled water and the
mixture is transferred to a round bottom flask. Caustic soda solution and a few pieces of zinc
granules are added to the flask .The condenser is fitted to the round bottom flask and a conical
flask is fitted to the condenser. As the round bottom flask is heated, the liquid begins to boil
slowly. Ammonia gas is released and it gets absorbed in the acid solution of the conical flask.
The unreacted acid of the conical flask is estimated by titration against standard solutions of
NaOH

CALCULATION:

Let the weight of organic compound be w gram

Volume of acid taken =V1 ml

Normality of acid =N

Volume of alkali of normality N required to neutralize unreacted acid =V 2 ml

Volume of acid to neutralize ammonia= V1 ml of acid - V 2 ml of acid (vV2 ml of alkali is the

same amount of acid neutralized as the normality is same for acid and alkali) = (V1 - V2) ml of
N acid soln. = (V1- V2) ml of alkali solution of N
normal.
Now 1000 ml of (N) ammonia soln. Has 17 g NH3 ie 14 g Nitrogen

So (V1-V2) ml (N) NH3 has [14 x (V1--V2) ml x 1/w x 1/1000 gram

So the % of N in the w gm organic compound is 14 x (V1 -V2) x1/w x 1/1000 x 100

ie 1.4 x (v1-v2)/w %N

RESULT:

The amount of nitrogen is = gm

 5. POLARIMETRIC ESTIMATION OF SUGAR.

AIM: To estimate the percentage of sugar present in the given solution using Polarimeter.

APPARATUS REQUIRED:
Standard volumetric flasks, beaker, Polarimeter.

PROCEDURE:
Part A.
Prepare a known concentration of (say 2%, 4%, 6%, 8%, 10% 12%, 14%, 16%) sugar
solutions in different 50 ml standard volumetric flasks. Measure its optical rotations using a
standard Polarimeter. Plot a graph of between optical rotations and concentration. Measure the
optical rotation of the given solution and find out its concentration with the help calibration
curve.
Part B
Measure the optical rotation of the given sugar solution. Calculate the specific rotation
using the following formula [] = 100 /CL Where

[] = Specific rotation.

= Optical rotation.
C = Concentration.
L = Length of Potentiometric tube in dm.
Knowing the optical rotation of unknown sugar solution, the concentration of sugar
solution is determined by applying the values of specific rotation from above formula. The
specific rotation of sugar is a constant value.
OBSERVATION AND CALCULATION:

Angle of
Concentration of sugar rotation Specific
SL No.
solution Rotation
(R = r01 r0)

1.

2.

3.

4.

5.

RESULT:
The percentage of sugar present in the given solution
By calculation
By graph:
 6. ESTIMATION OF PHENOL

AIM:

To estimate the amount of phenol present in the whole of given solution

APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker
PRINCIPLE:

The estimation is based on the following reaction

However a standard solution of bromine is not used for this purpose. Instead a mixture of
bromate bromide (wrinklers solution) which readily liberates bromine in the presence of acid is
used. Also the strength of the thio sulphate solution does not vary with this and this is fairly
stable the excess of bromine is treated with KI, so that the liberated iodine could be treated
against sodium thiosulphate, which inturn is standardised by potassium dichromate solution.

PROCEDURE:

Standardardization of sodium thiosulphate:

Prepare a standard solution of potassium dichromate

(i) Pipette out 20ml of std. Potassium dichromate solution in a clean conical flask
and add 5ml of conc. HCL and 40ml of 10% KI and titrate the liberated iodine
against sodium thiosulphate in burette.
(ii) When the solution becomes pal yellow add one drop of starch indicator and
continue the titration
(iii) The end point is the appearance of green colour.
(iv) Repeat the titration for the concordant value

Estimation of wrinklers:solution:

(I) Conduct a similar experiment to standardise the bromate bromide mixture

(II) Pipette out 20ml of this solution into a clean conical flask
(III) Add 5ml of conc. HCL and 10ml of 10%KI and titrate the liberated iodine against
sodium thiosulphate solution using starch indicator.
(IV) End point is the disappearance of colour
(V) Repeat the titration for concordant value

Estimation of phenol:

(i) Make up the given phenol solution into 100ml in a std. measuring flask
(ii) Pipette out 20ml of the solution into stoppered conical flask
 (iii) Dilute it by adding 50 ml of water
(iv) Add 40ml of wrinklers solution from burette slowly with constant shaking
(v) Then add 5ml of conc. HCL 10ml of 10% KI solution
(vi) Titrate the liberated iodine against thiosulphate using starch indicator
(vii) End point is the disappearance of colour
(viii) Repeat the titration for concordant value

STD DICHROMATE Vs THIOSULPHATE

S.No Volume of Burette reading Volume of Concordant

dichromate sodium value
(ml) thiosulphate
solution solution (ml)

V1(ml) V2 (ml)

Initial Final

Strength of K2Cr2O7 (N1) =

Volume of dichromate solution (V1) =

Volume of sodium thiosulphate solution (V2) =

Strength of thiosulphate solution (N2) =

According to law of volumetric analysis,

V1XN1 = V2XN2

ESTIMATION OF WRINKLERS SOLUTION:

S.No Vol of Burette reading Vol of Concordant

Wrinklers Initial Final Thiosulphate Value

Solution (ml) (ml) Solution (ml)

V1 (ml) V2 (ml)

ESTIMATION OF PHENOL:

S.No Vol of Burette reading Vol of Concordant

phenol Initial Final Thiosulphate Value

Solution (ml) (ml) Solution (ml)

V1 (ml) V2 (ml)

RESULT:

Amount of phenol present in the given solution = gm

7. DETERMINATION OF TOTAL RESIDUAL CHLORINE IN WATER SAMPLE

AIM:-
To determine the total residual chlorine in the given water sample.
APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker

PROCEDURE:
Standardization of thio solution:
About 20 ml of std thio of K 2Cr2O7 solution taken in a clean conical flask. Add 20 ml of
10% KI solution and 20 ml of 4N H2SO4. Titrate the solution till it turns light yellow in colour.
Add 1 ml of freshly prepared starch and titrate till it appears steel blue.
Estimation of residual Cl2:
Transfer 100 ml of given H2O sample in a clean conical flask and add 10 ml of KI
solution and about 3 ml of glacial acetic acid to maintain pH of 3- 4. Cover the flask with stop
cork and mix the solution by dil. H2O. Titrate against std. Na2S2O3 solution with 1 ml of starch
indicator till the blue colour disappears.

STD DICHROMATE Vs THIOSULPHATE

S.No Volume of Burette reading Volume of Concordant

dichromate sodium value
(ml) thiosulphate
solution solution (ml)

(ml) (ml)

Initial Final

TITRATION I
ESTIMATION OF RESIDUAL CL2 Indicator : Starch
End point : Disappearance of blue colour

Sl Volume of Burette Reading Volume of thio Concordant

H2O value
No Initial Final Sulphate
(ml) (ml)
(ml) (ml) (ml)

CALCULATION:

Free Cl2 in 100 ml of sample =

Normality of H2O w.r.t free Cl2 present =

=
Amount of Cl2 in given H2O =
=

RESULT:-

The amount of total residual chlorine in given sample of water = ______gm

8. ESTIMATION OF CHEMICAL OXYGEN DEMAND

AIM:
 To estimate the amount of chemical oxygen demand for the given water sample
APPARATUS REQUIRED:
Reflux apparatus, heating mantle, and burette
PROCEDURE:
Place o.2gm of silver sulphate in the reflux flask,20ml of unknown water sample ,10ml of
0.1N potassium di chromate solution are taken in the flask together with glass beads, Add slowly
30ml of 8N sulphuric acid and mix thoroughly .connect the flask to the condenser , mix the
contents before heating. Improper mixing results in bumping and sample may be blown out.
Reflux for a minimum period of 2hrs, cool and wash the condenser with distilled water. After
cooling to room temperature ,titrate excesses dichromate with 0.1N ferrous ammonium sulphate
using ferrion indicator sharp color change from blue green to wine red indicate the end point
.Reflux blank in the same manner using distilled water instead of sample
OBSERVATION:

Burette Reading
Sl Volume ofH2O Initial Final Volume of Concordant
thio run down value
No (ml) (ml) (ml)
(ml) (ml)

CALCULATION:
Quantity of ferrous ammonium sulphate added for blank = Aml
Quantity of ferrous ammonium sulphate added for sample = Bml
COD = ((A-B) XN FASX8X1000)/quantity of water sample taken
RESULT:
The amount of COD in the given water sample =

9. ESTIMATION OF DISSOLVED OXYGEN IN WATER

AIM
To determine the amount of dissolved oxygen in the given water sample by wrinkles
method.
APPARATUS REQUIRED:
 Conical flask, Burette, pipette, beaker
PROCEDURE
Part - I
Standardisation of sodium thiosulphate
The burette is washed and filled with sodium thiosulphate solution, 20ml of 0.01N
potassium dichromate solution is pipette out in to a clean conical flask, 5ml of sulphuric acid snd
15ml of potassium iodide. This is titrated against thio sulphate, when solution turn straw yellow
color, starch indicator is added. Then titration is continued till blue color becomes green
Part II
Standardisation of Dissolved oxygen
100-150ml of the water sample is taken in the iodine flask, 2ml of manganese sulphate
and 2ml of potassium iodide are added. The stopper is replaced and the flask is shaking for
several times. the water sample is titrated against thio sulphate solution when the solution
becomes light yellow, starch indicator is added, titration is continued until the blue color is
disappears . hence the amount of dissolved oxygen is calculated

STANDARDIZATION OF SODIUM THIO SULPHATE

Standard thio sulphate Vs potassium di chromate
Indicator: starch
End Point: Appearance of pale green color.
Sl Volume of Burette Reading Volume of Concordant
thiosulphate value
No K2Cr2O7
Initial Final ml ml
ml
ml ml

Volume of thio sulphate V1 =

Strength of thio sulphate N1 =
Volume of K2Cr2O7 V2 =
Strength of K2Cr2O7 N2 = V1 N1 / V2

ESTIMATION OF DISSOLVED OXYGEN:

Standardized Water Vs thio sulphate
Indicator: starch
End point: Disappearance of blue color.
 S. No Volume of Water Initial Final burette Volume of Concordant
burette reading value
ml reading thio sulphate
ml ml
ml ml

Volume of thio sulphate V1 =

Strength of thio sulphate N1 =
Volume of water sample V2 =
Strength of Water sample N2 = V1 N1 / V2
Amount of dissolved oxygen = NormalityX Eq.wt. Of oxygenX1000
RESULT
Amount of dissolved oxygen in given water sample = gm

10.ANALYSIS OF POLYMER

AIM: To determine the molecular weight using Ostwald viscometer as 1% soln is provided

APPARATUS REQUIRED:
 Polyvinyl alcohol, hot water, viscometer
PROCEDURE: Polymer soln of different concentration say 0.1, 0.2, and 0.5%are prepared
from the given polymer stock soln, Take 10mlof the solvent is taken in a viscometer and sucked
through the capillary tube, Now note the time of the flow of the solvent to lower mark, Now fill
the viscometer with 10ml of one of the polymer concentration in to the viscometer and
determine the flowtime as before , similarly the flow time of the other polymer soln are formed,
from the flow time reduced. Viscoscity can be calculated.
CALCULATION:

SL CONCENTRATION FLOW TIME rel= /o sp=t/to-1 red=sp/c

NO g/100ml (t)
Sec = t/to

Molecular weight of the polymer:

i=kMa

log i= log k + a log m

log m = 1/a ( log i - log K)

k= 20x10-5 ; a = 0.76

Logm=logn-logk/a

Degree of polymerization:

= mx Dp

Dp=

RESULT:
Molecular weight of the given polymer is =
Degree of polymerization =
11. CONDUCTOMETRIC TITRATIONS

AIM:
To find out the strength of hydrochloric acid and acetic acid in a mixture of both
(strong acid - weak acid) by titrating it against sodium hydroxide solution
conductometrically.
APPARATUS:
Conductivity meter, conductivity cell, std. flasks, magnetic stirrer etc.

PROCEDURE:
Prepare the following stock solutions in water 0.01N HCl, 0.01N CH3COOH, 0.1N
NaOH., Pipette out 25cc of acid mixture [10cc HCl + 15cc CH3COOH] to a clean beaker, placed
on the magnetic stirrer, Dip the conductivity cell in it and record the reading. (See that the point
foil is completely immersed in the solution). Fix the filled NaOH solution in a micro burette on a
stand. Add NaOH drop wise in an increment of 0.2ml (5drops), Stir the solution and record the
conductance after stopping the stirring. Continue the process until the conductivity value first
decreases, reaches a minimum, then increases gradually and latter increases rapidly, Plot the
points for observed conductance Vs the volume of NaOH added in ml,Draw straight lines
passing through a maximum number of points, Record the points of intersection and note V1 and
V2.
OBSERVATION:

Volume of NaOH. Conductance (mho/ cm-1)

ml

Nature of the Graph:

Conductivity
(mho/ cm-1)
 Volume of NaOH
From graph: V2, volume of NaOH added for HCl=

CALCULATION:
V1 N1 = V2 N2
(HCl) (NaOH)

V2 x N2
Normality of HCl N = ----------
V1

Amount of HCl present in 1 ltr = N x eq.wt of HCl = g/litre

RESULT:
The strength of each acid in the given mixture is

Hydrochloric acid =

12. ESTIMATION OF FERROUS IRON BY POTENTIOMETRIC METHOD

AIM:
To determine the amount of ferrous ion present in the whole of the given solution by
potentiometrically
APPARTUS REQUIRED:
Potenetiometer , micro burette, beaker
PROCEDURE:
First a preliminary titration is carried out by adding std di chromate solution is portion of
1ml of emf of the cell is measured after addition , the addition of dichromate is continued even
after the end point , the volume of dichromate is calculated

Volume of di Conductance (mho/ cm-1)

chromate.
ml

Volume of Di chromate(ml) Emf E/V

ml V

CALCULATION:
Volume of Dichromate =
Strength of ferrous ion =
Amount of ferrous ion present in 100ml of the given soln= x55.83x100/1000

RESULT:
The amount of ferrous ion present in 100ml of the given solution = gm
13. DETERMINATION OF SODIUM AND POTASSIUM BY FLAME PHOTOMETER
AIM:
To determine the amount of sodium and potassium using flame photometer
APPARATUS REQUIRED:
Flame photometer, conical flask

PROCEDURE:
DETERMINATION OF SODIUM AND POTASSIUM IN WATER
Sodium chloride solution of 8ppm is sent and reading is adjusted for 100, now the
instrument is said to be calibrated, the solution of sodium chloride is sent one by one & reading
is noted
The same procedure is fallowed in the determination of potassium as in the sodium

DETERMINATION OF SODIUM IN WATER

SL CONCENTRATION INTENSITY
NO OF SODIUM
 CHLORIDE
PPM

DETERMINATION OF POTASSIUM IN WATER

SL CONCENTRATION INTENSITY
NO OF POTASSIUM
CHLORIDE
PPM

RESULT:

The amount of sodium in given water = ppm

The amount of potassium in the given water = ppm

14.ESTIMATION OF BARIUM

AIM:
To estimate the amount of barium present in the given soln
APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker

PROCEDURE:
Make up the barium salt solution to100ml in a std flask , pipette out 20ml of this made up
solution into 400ml beaker ,add 1ml con.Hcl &dilute the solution to about 100ml by adding
water, heat the content of the beaker to boiling & added 15ml of 0.5N sulfuric acid . The
precipitate is formed within 15min, dry the precipitation air oven, Weight the crucible & the
content is determined

CALCULATION:
Mass of empty crucible =
Mass of Barium sulfate crucible =
Mass of Barium sulfate =

Amount of Barium in 100ml of given solution =

=

RESULT:
The amount of the Barium ion in the whole of the solution = gm

15. ESTIMATION OF NICKEL

AIM:
To estimate the amount of nickel in whole of the given solution
PROCEDURE:
Make up the nickel salt solution to 100ml in a volumetric flask, pipette out 20ml of this
made up solution in to a clean 400ml beaker with glass rod & water. Add 5ml of 1:1Hcl & dilute
the solution, Heat the contents of beaker to about 80ocover a water bath, Add 25ml of DMG and
add 1% alcoholic ammonia , Repeat the processes for drying & cooling until const weight is
obtained

CALCULATION:
Mass of empty crucible = gm
Mass of Nickel = gm
Mass of DMG= gm

Amount of nickel present in 100ml of solution =

=
RESULT:
The amount of nickel present in whole of the solution= gm

16.ESTIMATION OF ASPIRIN DRUG IN TABLETS

AIM:
To estimate the amount of Aspirin in the given tablet using pH meter.

APPARATUS REQUIRED:

Burette, pipette, beaker, pH meter etc.

PROCEDURE:
Accurately weigh the given tablet, grind it in a porcelain mortar to fine powder.
Dissolve the powder in 95% ethanol and transfer the whole into a 100ml standard flask and make
up to the mark using 95% ethanol. Pipette out 20ml of the made up solution into a conical flask.
Add 5 drops of thymol blue indicator and titrate it against std. 0.05 alcoholic KOH solution taken
in the burette. The end point is the change of colour from yellow to blue.
Standardize the pH meter using pH 4 buffer solution. Wash the electrodes with distilled
water. Pipette out 20ml of the drug solution into to a clean beaker. Immerse the electrode in to
the drug solution. Note the pH value by the addition of each 1ml of 0.05 alcoholic KOH
solution. From the burette after well stirring, continue the addition up to a pH of 13. After the
jump, repeat the experiment by adding 0.1 ml nearing the end point.
Draw a graph by plotting pH Vs the volume of std. alcoholic KOH solution.
Calculate the strength of acetyl salicylic acid in the given drug sample by knowing the volume of
alcoholic KOH from the graph. The molecular weight of Aspirin is 180.

Pilot Titration

Volume of Alcoholic KOH pH

(ml)

FAIR TITRATION

Volume of alcoholic KOH PH pH/V

(ml)
Equivalence point =0.8

Normality of drug solution = V1 x N 1

------------
N2

Weight per litre = Equivalent mass x Normality = g

56.11 x
Amount of the substance in 100 ml of the solution = 56.11 x
=
RESULT:
The amount of Aspirin in the given sample Using pH metric analysis = gm

17. ESTIMATION OF AMMONIA IN AMMONIUM SALTS

AIM:
To estimate the ammonia in the given ammonium salt.

APPARATUS REQUIRED:
Conical flask, Burette, pipette, beaker

PROCEDURE:

Take 0.1 N Sodium hydroxide is prepared in a 250 ml std. Flask and standardized with
0.1 N oxalic acid. 0.1 N HCl is prepared and standardized using standardized sodium hydroxide.
In a Pyrex glass conical flask 0.15 grams of the given ammonium slat is taken and 50 ml of 0.1 N
Sodium Hydroxide solution is added. A small funnel is placed in the mouth of the conical flask
in order to prevent mechanical loss and the mixture is boiled till all the ammonia is evolved
which is checked up by using a wet mercruous nitrate paper. If the vapors of ammonia ceased to
come the paper does not turn black. At this stage cool the solution and titrate the excess alkali
with standard Hydrochloric acid solution in presence of methyl orange indicator. The
determination is repeated till identical results are obtained.

TITRATION: I
Std Hcl Vs ammonium chlorids
 S. No Volume of Initial Final burette Volume of Concordant
ammonium burette reading HCl value
chloride reading
(ml) (ml) (ml)
(ml) (ml)

01
02

CALCULATION:
Titre Value x Normality of HCl
Volume of NaOH unreacted = ----------------------------------------- = z
Normality of NaOH

Volume of NaOH consumed:

Gram equivalents of NaOH = Normality x Volume of NaOH reacted / 100 = x
=
Amount of ammonia
Percentage of ammonia present in the sample = --------------------------------- x 100
Weight of the sample taken

RESULT:
The percentage of ammonia present in the given sample is = %
CH2307 TECHNICAL ANALYSIS LAB LTPC
0032
LIST OF EXPERIMENTS
1. Ore Analysis
 Estimation of manganese in pyrolusite ore.
Estimation of magnesium in dolomite.
2. Analysis of alloys .
3. Analysis of fertilizer.
Estimation of nitrogen in urea by kjeldal method.
4. Sugar Analysis .
5. Estimation of phenol by Iodimetry / UV-Vis Spectrometer.
6. Water Analysis
Determination of total residual chlorine in water.
Determination of chemical oxygen demand.
Determination of dissolved oxygen.
7. Polymer analysis .
8. Conductometric Titration.
9. Potentiometry.
Estimation of iron.
Determination of standard electrode potential of Zn , Fe , Copper.
10. Estimation of sodium and potassium by flame photometry.
11. Gravimetric analysis
Estimation of barium in barium sulphate.
Estimation of nickel as DMG.
12. pH metry (acid basic titration ) not basic.

* Minimum 10 experiments shall be offered TOTAL : 45 PERIODS

INDEX
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1. ESTIMATION OF MANGANESE IN PYROLUSITE ORE

2. ESTIMATION OF MAGNESIUM IN DOLOMITE ORE

3. ANALYSIS OF ALLOYS (ESTIMATION OF COPPER IN BRASS)

4. ESTIMATION OF NITROGEN IN UREA BY KJELDAL METHOD

5. SUGAR ANALYSIS(POLARIMETRIC ESTIMATION OF SUGAR)

6. ESTIMATION OF PHENOL BY IODIMETRY

7. DETERMINATION OF TOTAL RESIDUAL CHLORINE IN WATER.

8. DETERMINATION OF CHEMICAL OXYGEN DEMAND.
9. DETERMINATION OF DISSOLVED OXYGEN.
10. POLYMER ANALYSIS.
11. CONDUCTOMETRIC TITRATION.
12. POTENTIOMETRY.
13. ESTIMATION OF SODIUM AND POTASSIUM BY FLAME PHOTOMETRY.
14. ESTIMATION OF BARIUM IN BARIUM SULPHATE.
15. ESTIMATION OF NICKEL AS DMG

16. ESTIMATION OF ASPIRIN DRUG IN TABLETS

17. ESTIMATION OF AMMONIA IN AMMONIUM SALTS