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Applied Chemistry – Laboratory Manual

Department of Applied Science

Laboratory Manual
Subject: Applied Chemistry
CLASS: FE SEM: I
Name : …………………………………………………

Division : …………………………………………………

Roll Number : …………………………………………………

Batch : …………………………………………………

Expt. Title of the Date of Page Date of

Remarks
No. Experiment Expt. No. Submission

1. Determination of Moisture content

in coal.
2. Determination of ash content in
coal.
3. Determination of Cu in Brass

4. Determination of Zn in Brass

5. To preparation of urea
formaldehyde.
6. To preparation of phenol
formaldehyde.

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Moisture in Coal

Observations :-

1. Weight of empty crucible = W1 = ________ g.

2. Weight of crucible + Coal sample = W2 = _________ g.

3. Weight of Coal sample before heating = W2 – W1 = W3 = _________ g.

4. Weight of crucible + Sample after heating for 1 hr at 105 –110oC = W4 =_______ g.

5. Weight of Coal sample after heating = W4 – W1 = W5 = ___________ g.

6. Loss in weight of sample due to moisture = W3 – W5 OR W2 – W4 = WM = ______ g.

% Of Moisture in coal = Weight of moisture x 100 = WM x 100 Weight of coal (before heating)
W3 = _____ %

Calculation :-

Loss in Wt. (WM)  100

% of Moisture in coal =
Wt. of Coal taken (W3)

= ………… %

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_____________________________________________________________________________________

Expt. No 1 Date

Moisture in Coal

Aim :- To determine the amount of moisture in given sample of coal

Requirements : - Coal Sample, Crucible, Pair of tongue, weight box.

Theory :- Moisture in coal evaporates during the burnim of coal and it takes some of the liberated heat in
the form of latent heat of vaporisation. Therefore moisture lowers the effective calorific value of coal.
More ever, it quenches the fire in the furnace. Hence, lesser the moisture content, better the quality of coal
as a fuel. However, presence of moisture, up to 10% produces a more uniform fuel-bed and less of “fly-
ash” Moisture held within the coal itself is known as inherent moisture & is analysed. Moisture
reduces the calorific value of coal and considerable amount of heat is wasted in evaporating it
during combustion. Moisture content should be as low as possible.

Procedure :-

1) Take a silica crucible heat it at 1100C for about 10min.

cool it and then weighed silica crucible.

2) Take 1 gm of powdered sample of coal in silica crucible.

3) The crucible is placed by taking out the lid inside & electric hot air oven.
4) Maintain temp. at 1050C to 1100C the crucible is allowed to remain in oven for ½ hr. and then
taken out with the help of pair of tongs. Cool in Desicators& weighted.
5) The process of heating cooling & weighting of crucible is repeated till the constant weight is
obtained.
6) By knowing the loss in weight of coal the percentage of moisture can be determined.
Result :-

The moisture content in the given sample of coal is ------

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To determine ash content of a given sample of coal

Observations:
1. Weight of empty crucible = W1 = __________ g.

2. Weight of crucible + Coal sample = W2 = _________ g.

3. Weight of Coal sample (before heating) = W2 – W1 = W3 = ___________ g.

4. Weight of crucible + Sample after heating for 40 mins. at 725 ± 25 o C = W4 =______ g.

5. Weight of Ash formed = W4 – W1 = WA = __________ g.

Calculations:

𝑤𝑒𝑖𝑔ℎ𝑡𝑜𝑓𝑎𝑠ℎ(𝑊𝐴)
% of ash = 𝑥 100
𝑤𝑒𝑖𝑔ℎ𝑡𝑜𝑓𝑐𝑜𝑎𝑙(𝑊3)

= ________%

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Expt. No 2 Date

Aim: To determine ash content of a given sample of coal

Apparatus: Silica crucible with vented lid, electric oven, Muffle furnace, spatula,
desiccator, pair of tongs, weighing balance, , etc.

Chemicals: Powdered coal sample.

Theory: Coal is a primary, solid, fossil fuel. Coal sample has to be analysed before using it in
any field/industry to find out its quality & suitability. Moisture, volatile matter & ash content of
coal are determined under proximate analysis.

Ash: Ash content of coal is the non-combustible residue left after coal is burnt. It consists of
inorganic matter like silica, alumina, iron oxide, lime, magnesia, etc. Ash reduces the heating
value of coal, reduces air supply in furnaces and also requires labour (extra cost) for its regular
disposal. Therefore ash content of coal should be as low as possible.

Procedure:

Determination of Ash:Transfer about 1g (known quantity) of powdered air dried coal

sample into a previously weighed silica crucible. Heat the open crucible with sample in a Muffle
furnace maintained at 725 ± 25o C for about 40 minutes or till constant weight is obtained. Coal
burns in open and the residue left is ash. Take out the crucible from Muffle furnace carefully
using long legged tongs. Cool the hot crucible first in air and then in a disiccator. Weigh the
crucible and find out the amount of unburnt residue left (ash).

Result :-

The Ash content in the given sample of coal is = -----------%

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Applied Chemistry – Laboratory Manual

COPPER IN BRASS

OBSERVATION TABLE :-

[B] Standardization of Na2S2O3

Burette : Na2S2O3 Pipette : 10 ml of K2Cr2O7 (0.1n) + 20 ml of

2N H2SO4 + 10 ml OF 10% Kl

Indicator : Starch End point : deep blue to light green

REACTIONS :

K2Cr2O7 + 2H2SO4 K2SO4 + Cr2(SO4)3 + 4H2O + 3{O}

{2Kl + H2SO4 K2SO4 + 2Hl } × 3

{2Hl + O I2 + H2O }×3

K2Cr2O7 + 7H2SO4 +6Kl 6K2SO4 + Cr2(SO4)3+ 7H2O+ 3I2

I2 + 2 Na2S2O3 Na2S4O6 + 2Nal

Burette Pilot 1st in ml 2nd in ml 3rd in ml Mean in ml (V1)

reading Range in
ml

Final

Initial

Difference

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EXPT. NO: 3 DATE :

COPPER IN BRASS

AIM: To estimate the amount of copper in the given sample of brass.

REQUIREMENTS:

Brass turnings (clean & dry), Conc. HNO 3, Conc. H2SO4, 2N H2SO4, 2N CH3COOH, 10%
Na2CO3, 10% KI, 1% starch,

0.1 N K2Cr2O7 , 0.1 N Na2S2O3.

THEORY:

Brasses are alloys of copper & zinc containing 60 to 90% copper & 40 to 10% ZINC. They may
also contain small amounts of tin, lead & iron. Brasses posses greater strength ductility &
machinability than pure copper.

In the analysis of brass a known quantity of brass is treated with hot conc. HNO 3 Tin gets
precipitated as metastannic acid & can be removed by filtration. The filtrate containing soluble
salts of copper, zinc, tin & iron are treated with conc. H 2SO4 and are evaporate to dryness. The
dry mass comprising of PbSO4 is treated with distilled water & filtered. The clear filtrate
containing CUSO4 (blue), ZnSO4 (colourless) & FeSO4 (light green) is taken for estimation of
copper in brass. A known aliquot of the filtrate is treated with excess of KI in neutral or feebly
acidic medium, which reduces Cu 2+
to Cu 1+
& liberates an equivalent amount f .he of I2
liberated is estimated using Na2S2O3 solution using starch as an indicator. The amount of copper
in the filtrate is found out, hence the percentage of copper in the brass sample can be
calculated.

This is an iodometry titration, which deals with liberated I2 during the reaction.

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CALCULATIONS :

Normality of Na2S2O3

10 ml of 0.1 N K2Cr2O7  V1 ml of [XN] Na2S2O3.

N 2V2 10  0.1
N1V1  N 2V2  N1   N1   ...... Normality of Na 2S2 O 3 [XN] Where
V1 V1
, N1 = Normality of Na2S2O3.

V1 = Volume of Na2S2O3.

N2 = Normality of K2Cr2O7

V2 = Volume of K2Cr2O7

Normality of Na2S2O3 = …………………….. = [XN]

[C] Estimation Of Copper :

Burette : Na2S2O3 Pipette : 25 ml of diluted solution + 10% Na2CO3 till

(standardized) turbidity appears + 2N CH3COOH + 10 ml of 10% Kl

Indicator : Starch End Point : Deep blue to formation of chalk white

precipitate.
REACTIONS :

2Cu ++
(from brass) + 4Kl 2Cul  + I2 + 4K+

I2 + 2 Na2S2O3 Na2S4O6 + 2Nal

Pilot
Burette Mean in ml
Range in 1st in ml 2nd in ml 3rd in ml
reading (V2)
ml

Final

Initial

Difference

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PROCEDURE:-

[A] :-Preparation of solution of Brass sample

1. Weigh accurately 1.0 gm of brass alloy turnings & treat them with about 30 ml of conc.
HNO3 on a porcelain dish. Heat the solution to around 100 °c for 10 to 15 minutes when tin
separates out as metastannic acid (H2SnO3).

2. Cool & filter the solution. Washed precipitate can be taken for estimation of tin.

3. Take the filtrate & the washings in a porcelain dish, treat it with 50 ml of conc. H 2SO4 &
evaporate to dryness. Extract the dry mass with 100 ml of distilled water when lead appears as
a white precipitate of PbSO4. Filtered and washed ppt. can be taken for estimation of lead.

4. Collect the filtrate & washings containingCuSO 4, ZnSO4 & FeSO4 (in traces) in a 250 ml
volumetric flask. (You have been supplied with this filtrate).

[B]:- Standardization of Na2S203 solution:

1. Pipette out 10 ml of 0.1 N K2Cr2O7 solution in a stoppered bottle & to it add 20 ml of 2N

H2SO4 & 10 ml of 10% KI solution.

2. Stopper the bottle, shake the contents & keep it in the dark for 5-10 minutes.

3. Dilute the contents in the bottle with 25 ml of tap water & titrate the liberated iodine against
Na2S2O3 solution from the burette till a straw yellow colour is obtained.

4. Add about 2 ml of freshly prepared starch solution & continue the titration till the colour of
the solution in the stoppered bottle changes from dark blue to light green.

5. Repeat the procedure till you get two constant burette readings.

6. Note down this burette reading as V1 ml.

7. Calculate the normality of Na2S2O3 solution [XN]

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CALCULATIONS :

[C] Estimation of Copper:

1000 ml of 1N Na2S2O3  63.55 gm of Copper

63.55  V2  [ XN ]
 V2 ml of XN Na2S2O3  = [A] gm of Copper
1000

Thus 25 ml of pipette solution = [A] gm of Copper

Therefore 250 ml of stock solution = [A] × 10 gm of Copper

Thus 1 gm of brass sample contains 10 × [A] gm of Copper

 100gm of brass sample will have 10 × A × 100 = -------------% of Copper in the given brass
sample

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[C]:- Estimation of copper in brass:

1. Dilute the supplied processed brass solution to 250 ml in a standard flask. Shake well to get
a homogeneous mixture.

2. Pipette out 25 ml of the above diluted solution into a stoppered bottle & add to it 10%
Na2CO3 drop wise till a slight turbidity appears. Neutralize the excess of Na 2CO3 by adding 2N
CH3COOH till the turbidity disappears.

3. Add 5 ml of CH3COOH in excess to make the medium slightly acidic.

4. To the above mixture add 10 ml of 10% KI with a pipette, shake the contents & keep it in
the dark for 10 minutes.

5. Remove the bottle from dark & dilute the contents with 25 ml of distilled water.

6. Titrate the liberated iodine with standardized Na2S2O3 from the burette, till a straw yellow
colour appears. Add 2 ml of starch & continue the titration till the blue colour gets discharged &
a chalk like white precipitate appears in the bottle.

7. Repeat the same procedure till you get two constant burette readings

8. Note down this burette reading as V2 ml.

9. Calculate the percentage of copper in the given brass sample.

RESULTS:-

The given brass sample contains ----------------------% of copper.

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OBSERVATION TABLE :

[A] Estimation of Zinc

Burette : EDTA (0.1N) Pipette : 25 ml diluted solution + 20ml of buffer

of pH = 10

Indicator : Eriochrome End Point : Wine red to blue

black T

REACTIONS :-

Na2H2Y 2Na+ + [H2Y]-2

NaH2In H+ + Na+ + [HIn] Blue

Zn2+ + [Hin-] Zn HIn (wine red)

Zn HIn + Na2H2Y NnH2Y (colourless) + Na2HIn

Wine red Colourless (Zinc EDTA complex) + (Indicator is set free) Blue

M-In + EDTA M-EDTA + In

Less stable More stable Free Indicator

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EXPT. NO: 4 DATE :

ZINC FROM BRASS

AIM: -To estimate the amount of zinc in the given sample of brass.

THEORY:-

The major components of brass are copper & zinc. In order to improve the physical properties
of brass small amounts of tin, lead & iron are also added to brass.

Chemical analysis of brass is always done using freshly drilled brass turnings or powder. In the
analysis of brass a known quantity of brass is treated with hot conc. HNO 3 so that tin gets
precipitated as metastannic acid & can be removed by filtration. The filtrate containing soluble
salts of copper, zinc, tin & iron are treated with conc. H 2SO4 and are evaporated to dryness.
The dry mass comprising of PbSO 4 is treated with distilled water & filtered. The clear filtrate
containing CUSO4 (blue), ZnSO4 (colourless) & FeSO4 (light green) is taken for estimation of zinc
in brass. The pH of the filtrate is adjusted to 3 by using dil HCI, warmed & treated with
saturated H2S to precipitate Cu as CuS. Copper sulphide is filtered off, washed with water & the
filtrate is used for complexometric estimation of zinc from brass.

The filtrate is then boiled to expel excess of H2S. The pH of this solution is then adjusted to 10
using a buffer of NH4CI + NH4OH. This solution is then titrated against standard EDTA solution
to estimate the percentage of zinc from the given sample of brass.

PROCEDURE:

[A] Preparation of solution of the sample:

1. Weigh accurately 1.0 gm of brass alloy turnings on a porcelain dish & treat them with about
30 ml of hot concentrated nitric acid. Heat the solution to around 100 °c for 10 to 15 minutes
when tin separates out as metastannic acid (H2SnO3). Cool & filter the solution. Wash the
precipitate with hot water & tin can be estimated.

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Observation Table

Burette Pilot 1st in ml 2nd in ml 3rd in ml Mean in ml

reading Range in (V)
ml

Final

Initial

Difference

CALCULATIONS :

1000 ml of 1N EDTA  32.7 gm of Zn

V  0.1  32.7
 V ml of 0.1N EDTA   [Y] gm of Zn
1000

Thus Y gm of Zinc is present in 25 ml of pipetted solution

 250 ml of dilute solution will contain [Y] × 10 gm of Zinc

Thus 1.00 gm of Brass sample  [Y] × 10 gm of Zinc

Thus 100 gm of Brass sample 100 × [Y] 10 gm of Zinc

= ……………….% of Zn in the given Brass sample.

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2. Take the filtrate & the washings in a porcelain dish; treat it with 50 ml of conc.H 2SO4 &
evaporate to dryness. Extract the 'dry mass with 100 ml of distilled water when lead will appear
as a white precipitate. Filter & wash the precipitate with cold water & Pb can be estimated.

3. Collect the filtrate & washings containing CuSO4 , ZnSO4 & FeSO4 (in traces) in a 500 ml
beaker, add 100 ml of 2N HCI heat gently. Add saturated H 2S solution with constant stirring till
the smell of H2S comes from the beaker. Copper will precipitate as CuS (black). Filter off CuS &
test the filtrate for copper by addition of H2S to small portion of the filtrate. Boil the copper free
filtrate vigorously to expel H2S (test with lead acetate paper) & transfer the solution into a
250ml volumetric flask. This filtrate has been provided to you for estimation of zinc from brass.

[A] :-Estimation of zinc

1. Dilute the given solution to 250 ml in a volumetric flask. Make the solution homogeneous by
turning the flask upside down several times.

2. Pipette out 25 ml of the above solution in a conical flask & add 20 ml of NH 4Cl + NH4OH
buffer.

3. Mix & add few drops of Eriochrome black T indicator.

4. Fill the burette with EDTA solution (0.1N).

5. Titrate the above solution with EDTA from the burette till colour of the solution in the conical
flask changes from wine red to blue.

6. Repeat the same procedure till you get two constant burette readings.

7. Record the burette reading as V ml.

8. Calculate the amount of Zinc.

RESULTS:-

In the given sample of brass the amount of zinc is ----------------------%

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Applied Chemistry – Laboratory Manual

Aim :-To prepare urea formaldehyde resin.

Observations:-
1) Mass of the beaker (W1) = ---------g.
2) Mass of the beaker with urea formaldehyde (W2) = --------g.
3) Therefore mass of urea formaldehyde (W2 – W1) = --------g.

Reactions:

Properties:
1. They have good electrical insulating properties.
2. They are resistant to oil, grease and weak acids.
3. They are hard, resist abrasion and scratching.
4. They have good adhesive properties.

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Expt. No : 5 Date:

Aim :-To prepare urea formaldehyde resin.

Apparatus required:-Beaker, glass rod, funnel, filter paper and chemical balance.
Chemicals:-Urea, formaldehyde sol., conc. H2SO4, distilled water.
Theory:- Amino resins are condensation products obtained by the reaction of formaldehyde
with nitrogen bearing compounds such as aniline, amides for ex:- melamine formaldehyde, urea
formaldehyde etc.
Urea formaldehyde is prepared by condensation reaction between urea and formaldehyde in
acidic or alkaline medium. The first product formed during the formation of resin is
monomethylol and dimethylolurea.
Procedure:-
1. Place about 5 ml of 40% formaldehyde solution in 100 ml beaker.
2. Add about 2.5 g of urea with constant stirring till saturated solution is obtained.
3. Add a few drops of conc. H2SO4, with constant stirring.
4. A voluminous white solid mass appears in the beaker.
5. Wash the white solid with water and dry it in the folds of filter paper.
6. Weight the yield of product.

Precautions:-
1. While adding concentrated H2SO4, it is better to stay little away from the beaker since the
reaction sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.
Uses:-
1. They are used adhesive applications for the production of plywood and laminating.
2. They are used for the manufacture of cation exchange resins.
3. These also find use in the manufacture of electrical switches, plugs and insulating foams.
4. Their applications also include the treatment of textile fibers for improving their shrink
and crease resistance.
Result:-The yield of urea formaldehyde = -------------g

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To prepare Phenol formaldehyde (P-F) resin.

Reactions:-
Step 1: Formation of methylol phenol derivative.
Initially the monomers combine to form methylol phenol derivative depending upon phenol to
formaldehyde ratio.

Step 2: The phenol formaldehyde derivatives react among themselves or with phenol to give a
linear polymer or a higher cross linked polymer.
(a)Linear polymer (Novolac)

(b) Cross linked polymer (Bakelite)

A highly cross linked thermosetting polymer called Bakelite may be formed by further
condensation of novolac or methylol derivative. It was first prepared by Backeland. It is easily
formed if curing agent hexamethylenetetramine is added during synthesis.

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Expt. No. :6 Date:

Aim:To prepare Phenol formaldehyde (P-F) resin.

Chemicals required:Phenol (2g), 40% aq formaldehyde solution or formalin (2.5 mL),
glacial acetic acid (5 mL) and conc. HCl (8mL).
Theory:Phenol formaldehyde resin or P-F resin or phenolic resins (also called phenoplasts) are
important class of polymers which are formed by condensation polymerization of phenol and
formaldehyde in acidic or alkaline medium. Following steps are involved:

Procedure:
1. Place 5 mL of glacial acetic acid and 2.5 mL of 40 % aq formaldehyde solution in a 100 mL
beaker. Add 2 g phenol safely.
2. Wrap the beaker with a wet cloth or place it in a 250 mL beaker having small amount of
water in it.
3. Add conc. HCl drop wise with vigorous stirring by a glass rod till a pink coloured gummy
mass appears.
4. Wash the pink residue several times with to make it free from acid.
5. Filter the product and weigh it after drying in folds of a filter or in an oven. Report the yield
of polymer formed.

Observations:
1.Weight of empty watch glass = -----------W1 g
2.Weight of watch glass + poymer formed =----------- W2 g
3.Weight of polymer formed =-------------W2 – W1 g

Result:-The yield of Phenol formaldehyde = -------------g

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