Chemistry Lab Journal Write Up

FE [ALL Sinhgad Institute of Technology, Engineering
BRANCHES] Lonavala Chemistry
SINHGAD TECHNICAL EDUCATION SOCIETY’S

SINHGAD INSTITUTE OF TECHNOLOGY
Kusgaon (Bk), Lonavala 410401
DEPARTMENT OF FIRST YEAR ENGINEERING SCIENCES
LABORATORY MANUAL
ENGINEERING CHEMISTRY [107009]
F.E. ALL BRANCHES (SEM – II)
AY 2020-2021
TEACHING SCHEME EXAMINATION SCHEME

Practical: 2 Hrs/Week Term Work : ----
Practical : 25 marks
1
DEPARTMENT OF ENGINEERING SCIENCES
CERTIFICATE
This is to certify that Mr. /Ms._______________Aastha Singh_________________________________
of class FE Div. _____B___ Roll No. _____01___ Examination Seat No./PRN No. ._ __72150001D___
has completed all the practical work in Engineering Chemistry [107009] satisfactorily, as
prescribed by Savitribai Phule Pune University, Pune in the academic year 2019 -2020 (Semester II).
Course In-charge Head of Department Principal
Date:
2 DEPARTMENT OF ENGINEERING SCIENCES

INDEX
Planned Date of Marks
Date of Sign of
SN Title of experiment Date performa Obtained
Submission Faculty
nce (10)
To determine hardness of water by EDTA 21/05/21 11/07/21

1
method
2 To determine alkalinity of water 28/05/21 11/07/21
3 Titration of a mixture of weak acid and 04/06/21 11/07/21

strong acid with strong base using
conductometer
To determine strength of strong acid using 04/06/21 11/07/21

4
pH meter
To determine maximum wavelength of

absorption of CuSO4/FeSO4/ KMnO4, verify 11/06/21 11/07/21
5
Beer’s law and find unknown concentration
of given sample.
Preparation of polystyrene/phenol- 25/06/21 11/07/21

6
formaldehyde/urea-formaldehyde
resin
To determine molecular weight/radius of

7 macromolecule polystyrene/ polyvinyl 25/06/21 11/07/21
alcohol by viscosity measurement.
8 Proximate analysis of coal. 25/06/21 11/07/21
Name & Signature of Course In-charge

Name of the Student: Roll no:
CLASS: - FE Division: Course: - ENGINEERING CHEMISTRY

Experiment No. 01
To determine hardness of water by EDTA method
Marks: /10
Date of Performance: / /20 Sign with Date
Aim : To determine hardness of water by EDTA method
Objectives:
1. Understand the EDTA method to find out hardness in hard water sample.
2. To analyse hard water sample and find out the quantity of salt impurities.
Outcomes: At the end of this experiment students should be able to:

1. Find out types of hardness in water.
2. Decide the quality of water.
3. To use salt free water for industrial purpose, domestic pur[pose.
PEOs, POs, PSOs and COs satisfied:

PEOs: I, II, IV POs: i, ii, iii, iv, v, vi, ix PSOs: 1 COs: 1
APPARATUS: Titration apparatus i.e. burette, pipette, conical flask, stand etc.
CHEMICALS: EDTA, Buffer solution, EBT indicator, ZnSO4, Hard water sample.

THEORY:
Hardness is the property of water that does not allow water to produce lather when
soap is mixed with it but to form a curdy white precipitate. The hardness of water is due
to the presence of dissolved bicarbonates, sulphates, chlorides and nitrates of calcium
and magnesium. Hardness of water is expressed in terms of ‘ppm’ i.e. parts per million
of CaCO3 equivalents.
To find the magnitude of hardness of water sample, we use di-sodium salt of
ethylene di-amine tetra acetic acid (Na2EDTA) and perform a complexometric titration.
Na 2EDTA forms a 1:1 complex with divalent Ca+2 and Mg+2 ions.
The indicator used for the titration is Eriochrome black-T dye. This indicator when
added to hard water at PH 10 produces wine red stable complex with Ca+2 and Mg+2
ions, in water sample. When it is titrated against EDTA solution the color complex is
changed from wine red to original sky blue showing the end point.
Structure of EDTA
STRUCTURE OF COMPLEX: Metal – EDTA complex

PROCEDURE:
PART 1: Preparation of standard hard water (1 ppm)
1. Weight accurately 0.718 grms of pure Zinc Sulphate (ZnSO4.7H2O) on watch glass.
2. Transfer it to a beaker and dissolve in little quantity of distilled water.
3. Transfer it to 250 ml volumetric flask and take washing of beaker also.
4. Dilute the solution up to the mark using distilled water.
5. Shake well to make the solution homogeneous. Transfer this std. hard
water (SHW) to a 250ml beaker.
PART 2: Standardization of EDTA solution
1. Wash, rinse & fill the burette with given Na2EDTA solution taking usual
precautions.
2. Pipette out 10 ml of SHW in a titration flask. Add 2 to 3 ml of buffer solution.
3. (pH = 10) & 2-3 drops of Eriochrome black-T indicator. The solution becomes wine
red.
4. Titrate this solution titrated against Na2EDTA from burette till wine red coored
solution becomes sky blue.
5. Record the burette reading. Take three such readings. Note the constant burette
reading (V1 ml).
6. Express 1ml of Na2EDTA solution in terms of mg CaCO3.
PART 3: Total hardness of given water sample
1. Pipette out 20 ml given hard water sample in a titration flask. Add 5-7ml of buffer
solution (pH = 10) & 2-3 drops of Eriochrome black-T indicator. The solution
becomes wine red.
2. Titrate this solution titrated against Na2EDTA from burette till the solution becomes
sky blue
3. Record the burette reading. Take three such readings. Note the constant burette
reading (V2ml).
4. Calculate the hardness of given sample in ppm.

OBSERVATIONS: PART 2: Standardization of EDTA solution
Burette: Na2EDTA solution Indicator: Eriochrome black-T
Pipette: 10 ml of SHW (ZnSO4.7H2O) End Point: wine red to sky blue.

.
Reading in Pilot I II III C.B.R.

ml Reading (ml) (ml) (ml) (V1ml)
Initial
Final
Difference
PART 3: Total hardness of given water sample
Burette: Na2EDTA solution Indicator: Eriochrome black-T

Pipette: 20 ml of HWS End Point: wine red to sky blue.
Reading in Pilot I II III C.B.R.

ml Reading (ml) (ml) (ml) (V2ml)
Initial
Final
Difference

CALCULATION: PART 2: Standardization of EDTA solution
Normality of Na2EDTA solution: ------- N Burette reading: (V1ml)------------ml
1ml of SHW ≡ 1 mg of CaCO3  10 ml of SHW ≡ 10 mg of CaCO3
But 10 ml of SHW required ml (V1ml) of EDTA
 ml (V1ml) EDTA react with 10 ml CaCO3 equivalent
1 ml EDTA solution determines = 10 ÷ V1 = (A) mg of CaCO3
PART 3: Total hardness of given water sample: Burette reading (V2 ml)
1 ml EDTA determines = 10 ÷V1 = __ (A) mg ofCaCO3
10 ml of hard water sample reacts with = V2 __________ml of EDTA
 V2 ml EDTA determines = (A X V2) = ___________(B) mg of CaCO3
10 ml of hard water sample contain = ______________(B) mg of CaCO3
Hence, 10 0 0 m l hard w a t e r sample contain = (B X 1 0 0 ) = _______ mg of CaCO3
But 1mg/lit CaCO3 = 1 ppm
Therefore, total hardness = _____________ ppm of CaCO3

RESULT:
1. 1 ml EDTA solution determines = ppm of CaCO3

2. Total hardness of water sample = ppm of CaCO3
Conclusion:
By performing this experiment, it can be concluded that disodium salt of EDTA forms
stable complex with hardness producing salts and determines concentration of salts as
hardness in water in EDTA volumetric titration method.
Sign. Of Teacher with date –


Experiment No. 02
To determine total alkalinity of water sample.
Marks: /10
AIM: To determine total alkalinity of water sample.
Objectives:
1. Understand volumetric acid base titrimetric method to find out alkalinity
in alkaline water sample.
2. To analyse alkaline water sample and find out the quantity of alkaline
salt impurities.
1. Find out types of alkalinity in water sample.
2. Decide the quality of water.
3. To use alkaline free water for industrial purpose.

APPARATUS: Titration apparatus i.e. burette, pipette, conical flask, stand
etc. CHEMICALS: HCl, methyl orange, phenolphthalein.and water sample

THEORY: The knowledge of Alkalinity of water is necessary for controlling the
corrosion, in conditioning the boiler feed water (internally), for calculating the amounts
of lime and soda needed for water softening etc.
The Alkalinity of water is due to the presence of hydroxide (OH), carbonates (CO 3 2- )
and bicarbonates (HCO3-) present in the given sample of water. These can be estimated
separately by titration against standard acid, using phenolphthalein and methyl orange
as indicators. The chemical reaction involved can be shown by the equations given
below.
[OH-] + [H+] → H2O
[CO32-] + [H+ ] → [HCO3-]
[HCO3-] + [H+] → H2O + CO2
The titration of water sample against a standard acid up to phenolphthalein

endpoint shows completion of reactions (i) & (ii) only. This amount of acid used thus
corresponds to hydroxide plus one half of the normal carbonate present. The titration of
water sample further continued to methyl orange endpoint marks them completion of
reaction (i),(ii) & (iii).Hence, the amount of acid used after the phenolphthalein
endpoint corresponds to one half of normal carbonate plus all the bicarbonates. While
the total amount of acid used represents the alkalinity (due to hydroxide, bicarbonate
and carbonate ions)
The possible combinations of ions causing alkalinity in water are:
Only OH- , or only CO3 2- or only HCO3- , OH- and CO3 2-,or CO3 2- and HCO3-
together. The possibility of OH- and HCO3- ions together is not possible since they
combine together to form CO3 2- ions.
OH- + HCO3- → CO3 2- + H2O
 PROCEDURE:
1. Fill the burette with given acid solution taking usual precautions.
2. Pipette out 25 ml of the water sample into a conical flask.
3. Add 2-3 drops of phenolphthalein indicator and titrate this sample against HCl
from the burette until the pink color caused by phenolphthalein just disappears.
4. Note down this reading as phenolphthalein endpoint [P].
5. Now to the same solution add 2 drops of methyl orange indicator. It will give
light yellow color.
6. (Do not fill the burette). Continue the titration against HCl from the burette until
the yellow color changes to red.
7. Now note the total volume of acid (Volume from the beginning of the
experiment). This is methyl orange endpoint.
8. Repeat the procedure twice to obtain the [P] and [M] readings.
11DEPARTMENT OF ENGINEERING SCIENCES
Reactions & Reference table:
1. OH¯ + H H2O (one step neutralization, P =M) Detected by Methyl orange

Indicator
2. HCO3¯ + H H2 + CO3 (one step neutralization, M) Detected by
Phenolphthalein Indicator
3. CO3 -- + H HCO3¯ (first step)
Type of Alkalinity (ppm)

Conditions and Relation between Alkalinity
OH CO3 HCO3
If phenolphthalein end point is zero, then

V1 = 0 / P = 0 --- --- M
alkalinity is due to only bicarbonate
If methyl orange end point is zero & only
V1 = V2 / P = M there is phenolphthalein end point, then the P --- ---
alkalinity is due to hydroxide alone.
If phenolphthalein end point is exactly
V1= ½ V2 / P =
half the total titration, then only carbonate --- 2P ---
½M
alkalinity is present.
If phenolphthalein end point is greater than
V1 > ½ V2 / P >
half the total titration, then alkalinity is due to 2P-M 2(M-P) ---
½M
both carbonate & hydroxide.
If phenolphthalein end point is less than half
V1 < ½ V2 / P < the total titration, then alkalinity is due to
both carbonate & bicarbonate --- 2P M-2P
½M
 OBSERVATIONS:
In Burette : 10 ml Water sample

In Pipette : 0.01N HCl solution
Indicators : 1) Phenolphthalein 2) Methyl orange
Endpoints : 1) Pink to colourless 2) Yellow to Orange
1
2
OBSERVATION TABLE:
Reading 1 2 3 Mean
P 2.1 2.2 2.3 V1 = 2.2 ml
M 3.4 3.5 3.6 V2 = 3.5 ml
Type of We get Relation of V1 & V2

Alkalinity Thus, type of alkalinity P > ½ M
Volume of 0.01 N HCl equivalent to Hydroxide = [X] = 2.2

Volume of 0.01 N HCl equivalent to Carbonate = [Y] = 2.2
Volume of 0.01 N HCl equivalent to Bicarbonate = [Z] =3.5
ml
CALCULATIONS:
RESULT:
Alkalinity due to Hydroxide = 45 ppm
Alkalinity due to Carbonate = 130 ppm
Alkalinity due to Bicarbonate = 00 ppm
Conclusion:
With the help of this volumetric titration it can be concluded that alkalinity of water
sample be determined by acid -base volumetric titration.
Sign. Of Teacher with date
3

Experiment No. 03
Conductometric titration
Marks: /10
AIM: Titration of mixture of weak acid and strong acid with strong base using
conductometer.
Objectives:
1. To Understand the conductometric titration method to find out strength of acid
mixture solution.
2. To analyse acidic solution by instrumental method by using conductometer.

1. Apply analytical method to find acidic impurities in solution.
2. T o check acid free water and to use in boiler to prevent boiler corrosion.
3. Apply this method in industries to check the quality of product.

Apparatus: Conductance measurement assembly, conductivity cell.
Chemicals: 0.1 N mixtures of HCl and CH3COOH, 0.5 N NaOH solution, conductivity
water

Theory:
Conductance of a solution depends upon the nature & amount of ions present in it.
If an ion is removed or replaced from the solution then the conductance of the solution
changes. This is the basic principle of a conductometric titration.
In the acid mixture, the strong acid gets neutralize first, followed by the neutralization
of weak acid.
Hydrogen ions have maximum mobility therefore acid mixture shows a high value
of conductance. As the strong acid starts getting neutralized, hydrogen ions get replaced
by slow moving metallic Na+ ions. Thus, the conductance values keep on decreasing
rapidly, till neutralization of the strong acid is complete. After this point, neutralization
of weak acid starts. Now, the conductance decreases till further but this decrease is
slow. This is due the fact that the salt formed shows common ion effect & suppress the
dissociation of weak acid. On further addition of strong base, the conductance of ions
of the salt formed exceeds that of the weak acid, thus conductance increases slowly.
When the weak acid gets neutralized
Procedure:
1. Rinse the conductivity cell with distilled water

2. Take 10 ml of mixture of acid solution in a small beaker; add about 40 ml of
conductivity water. Dip the conductivity cell in this solution and see that the
electrodes are completely covered by the solution.
3. Stir the solution well. Measure its conductance.
4. Fill the burette with 0.5 N NaOH solutions.
5. From burette add 0.2 ml NaOH solution to the acid solution in the cell. Stir the
solution and note the conductance. Take at least 16 readings.

5
Observation table:
Obs. No ml of 0.5 N NaOH Resistance R Conductance 1/R
added (ohm) (ohm-1)
1 0.0 9.94
2 0.5 8.45
3 1.0 6.89
4 1.5 5.32
5 2.0 4.11
6 2.5 ml – X1 3.13
7 3.0 3.36
8 3.5 3.71
9 4.0 3.98
10 4.5 4.30
11 5.0 4.68
12 5.5 ml – X2 4.75
13 6.0 6.75
14 6.5 7.50
15 7.0 8.35
16 7.5 ml 9.15
Graph: Plot the graph of conductance Vs ml of NaOH added

1
6
Calculations:
1. X1 ml of 0.5 N NaOH is required to neutralize HCl solution and (X2-X1) ml of
0.5 N NaOH is required to neutralize CH3COOH solution.
2. Find the concentration of HCl in mixture:
N1V1 = N2V2
(Acid) (NaOH)
N1 x 10 = 0 .5 x X1
N1 = normality of HCl in mixture = 0.5 x X1
10
3. Find the concentration of CH3COOH in acid mixture:

N1V1 = N2V2
(Acid) (NaOH) N1
x 10 = 0 .5 x (X2-X1)
N1 = normality of CH3COOH in mixture = 0.5 x (X2-X1)
10

7
Result:
1 Volume of 0.5 N NaOH required to X1 2.5……… ml
neutralize HCl from the mixture
2 Volume of 0.5 N NaOH required to (X2-X1) …3.0……… ml
neutralize CH3COOH from the mixture
3 Normality of HCl in the mixture ……0.125……. N
4 Normality of CH3COOH in the mixture ……0.15……. N
Conclusion:
With the help of conduct meter it can be concluded that instrumental analysis gives out
accurate end point of the equivalence reaction and find out accurate strength of
electrolyte solution.

8

Experiment No. 04
PH metric Titration
Marks: /10
Aim: Determination of dissociation constant of weak acid (acetic acid) using pH meter.
Objectives:
1. To understand the PH metric titration method to find out dissociation constant of
weak acid solution by using instrument PH meter.
2. To analyse the acidic solution accurately by instrumental analytical method.

1. Apply analytical method to find acidic impurities in solution.
2. To check acid free water and to use in boiler to prevent boiler corrosion.
3. Apply this method in industries to check the quality of product.
4. To use glass electrode as indicator electrode to detect PH of chemical content.

Apparatus: pH meter, calomel and glass electrode, burette, pipette, stirrer etc.
Chemicals: 0.1 N (approx) of a given weak acid, 0.5N (exact) NaOH, 0.05M potassium
hydrogen phthalate (pH=4)

Theory: Dissociation of a weak acid e.g. CH3COOH may be represented by the
equation
When the acid is half neutralised, the concentration of acid and the
concentration of its salt in the solution will be equal. For a weak acid the concentration
of undissociated acid molecules can be assumed to be unchanged by a small fraction
which dissociates to provide the hydrogen ions. The salt can be regarded as fully
dissociated and hence the concentration of CH3COO- ions can be assumed to be equal
to that of the salt formed up to any stage of titration.
For the half neutralisation stage, [CH3COOH] = [CH3COO]
[CH3COO−] [𝐻+]
Ka = [𝐶𝐻3𝐶00𝐻]
[CH3COO−]
Ka = [𝐶𝐻3𝐶00𝐻] X [H+]
∴ Ka ≈ [H+] ∴ -log Ka = -log [H+]
pKa = pH
Thus the dissociation constant can be evaluated either by knowing the
[H+] or the pH value for the half neutralised solution of the acid.
Procedure:
PART – I Standardization of pH meter
1) Switch on the instrument by turning the control ‘ON’. Allow it to warm up for 10
minutes.
2) Adjust temperature dial to 250C.
3) With the help of special cable provided connect the electrode terminal and 7 pH.
4) Now remove the wire from 7 pH and connect to 4.2 pH Adjust ‘SLOPE’ to read
4.20.
5) Now remove the wire from 4.20 pH and connect to 9.20 pH. The reading displayed
must be 9.20.
6) If the above procedure works then the instrument is ‘OK’.
7) If not report it to instructor.

PART – II Determination the pKa value of weak acid
(1) Standardise the pH meter using 0.05 M potassium hydrogen phthalate solution
(2) Take 20 ml of the .given weak acid and about 50 ml of water in 100 ml beaker
(3) Place the stirrer and calomel - glass electrodes into the beaker. See that the
electrodes are properly dipped into the solution.
(4) Fix burette containing the strong base i.e. O.5N NaOH above the beaker.
(5) Measure the pH of the acid solution.
(6) Add O.2 of O.5N NaOH from the burette to the acid solution. Stir well
and note the pH of the solution.
7) Repeat the procedure by adding 0.3 ml NaOH each time. Record the pH of
the solution at each time, continue the addition of NaOH solution till the end point
exceeds by 2 ml

1
Observations
Obs. Volume of pH ∆pH ∆V ∆pH

No. 0.5N NaOH ∆V Mean V
added V(ml)
1. 0.0 4.40 0.40 0.5 0.8 0.25
2. 0.5 4.80 0.23 0.46 0.75

3. 1.0 5.03 0.20 0.4 1.25
4. 1.5 5.23 0.33 0.66 1.75
5. 2.0 5.56 0.17 0.34 2.25
6. 2.5 5.73 0.28 0.56 2.75
7. 3.0 6.01 0.27 0.54 3.25
8. 3.5 6.37 2.98 5.96 3.75
9. 4.0 9.35 1.13 2.26 4.25
10. 4.5 10.48 1.89 3.78 4.75
11. 5.0 12.37 0.18 0.36 5.25
12. 5.5 12.55 0.34 0.68 5.75
13. 6.0 12.89 --------- ------------ ------
22
Graph: Plot the following graphs.
Calculations:
From the graph (1) note the equivalence point of the titration as X ml. Find
the half neutralization point as X/2 ml.
At half neutralization point (X/2 ml.) find the pH of the solution from the
plot 2. The pH value at half neutralization point is the pKa value of the acid.
Now, pKa = -log Ka
Ka = antilog (-pKa )
Result:
1 Equivalence point of the titration …3.75…ml

2 pKa of the given weak acid ……
3 Dissociation constant (Ka) of the acid ……
Conclusion:
With the help of PH meter it can be concluded that instrumental method of analysis
gives accurate equivalence point of acid base titration and correct strength of solution.

3

Experiment No. 05
Colourimetry
Marks: /10
AIM: - DETERMINE  max AND CONCENTRATION OF GIVEN SOLUTION OF

CuS04.
Objectives:
1. To understand colourimetric method to find out concentration of unknown
coloured solution and verify Lambert-Beers’s Laws.
2. To find out coloured ion impurities from the sample solution.

1. Apply instrumental analytical method to find ionic impurities.
2. To use colorimeter apparatus in industries to check ionic impurities.

APPARATUS: Colorimeter
CHEMICALS: CuSo4, NH3 etc.

THEORY: - Lambert- Beers Law states, for the given system and the thickness of the
medium, the absorbance of the solution is directly proportional to the concentration of
an absorbing species.
PROCEDURE:
A) Prepare various solutions as per the table given below.
Cone of CuS04 0.1 M CuS04 Liquor NH3

Flask Total volume after
Solution Solution taken added
No. dilution(ml)
(M) for dilution (ml) (ml)
1 0.01 10 ml 12 ml 100 ml
2 0.02 20ml 12 ml 100 ml
3 0.04 40 ml 12 ml 100 ml
4 0.06 60 ml 12 ml 100 ml
5 Unknown Given volume 12 m 100 ml
B) Selection of  max (wavelength of maximum absorption)

It is found that solution does not absorb various incident monochromatic
wavelengths. But the certain wavelength is absorbed maximum known as  max.
Sr. No. Filter (Wavelength) Absorbance

1 400 nm 0.09
2 420 nm 0.19
3 470 nm 0.21
4 500 nm 0.15
5 530 nm 0.16
6 620 nm 0.23
7 660 nm 0.23
8 700 nm 0.25

25
C) 1. Before instrument is switched ON, check that required filter is rotated in the
instrument.
2. Allow the instrument to warm up for 15-20 minutes.
3. Insert the test tube filled with solvent (Blank) in its place.
4. Do not disturb the test tube. Adjust 100% (Coarse and line) knobs till display
reads 100.
5. Record absorbance for solution from flasks 1, 2,3,4,5 with disturbing adjustment
done.
6. Plot the graph or absorbance against concentration.
7. Determine graphically the concentration of unknown solution.
OBSERVATIONS:- SELECTED FILTER 700 NM
SR.
FLASK NO. CONCENTRATION ABSORBANCE
NO.
1 1 0.02 0.08
2 2 0.04 0.16
3 3 0.06 0.30
4 4 0.08 0.33
5 5 Unknown 0.14
PLOT A GRAPH: ABSORBANCE VS CONCENTRATION
Abs.
Conc.

RESULTS:
1. Graph is a straight line passing through origin: Lambert -Beer's Law verified.
2. Concentration of given unknown solution is:
Conclusion:
With the help of colourimetry experiment it can be concluded that strength of
coloured solution can be determined and verified Lambert-Beer’s Law.


Experiment No. 06
PREPERATION OF POLYMER
Marks: /10
Aim: Preparation of urea formaldehyde and its characterization

Objectives:
1. To understand polymerization reaction to prepare polymer in chemical industries.
2. To know the suitable condition for polymerization reaction.
Outcomes:
1. At the end of this experiment students should be able to write
reaction mechanism of polymerization reaction.
2. Apply suitable polymerization synthetic method to manufacture the polymer.
3. To add useful additives to improve the quality of polymer.

Apparatus:- Glass rod, Watch glass, Beaker
Chemicals: 40% formaldehyde, urea, conc. H2SO4

Theory: Phenolic resins are condensation polymerization products of phenolic
derivatives with aldehydes. Urea formaldehyde resin are prepared by the condensation
reaction between urea and neutral or alkaline conditions.
Procedure:
1. Take 10 ml of 40% formaldehyde solution in a 100 ml beaker.
2. Add about 5gms of urea with constant stirring till saturated solution is obtained.
3. Pour little quantity of this saturated solution on a watch glass.
4. Add few drops of conc. H2SO4 in this solution carefully.
5. Within 2 minutes, a white solid mass appears in the watch glass.
6. Wash the white solid with water and dry it in the folds of filter paper.
7. Place it in plastic bag and staple to your sheet.
Reaction:
Test for characterization of Urea formaldehyde

(A) Water soluble / miscible
Substance + cold water shake
(B) Water Insoluble / immiscible
Substance i.e. Urea formaldehyde is Water Insoluble
Type Determination of Substances

Sr. Test Observation Inference
No.
1 10 mg substance + Soluble with effervescence Acid is present and
10 drops 10% of CO2 and reprecipitated confirmed.
NaHCO3 by conc. HCl
2. 10 mg of substance Completely soluble and Phenol is present and
+ 10 drops 10% reprecipitated with conc. confirmed
NaOH HCl
3 10 mg substance + Completely soluble and Base is present and
10 drops of 1:1 HCl reprecipitated with 10 % confirmed

& shake NaOH
4 If all the tests (1), Then  Substance isNeutral.
(2), (3) are negative
Conclusion : Type of the substance is Acidic / Phenolic / Basic / Neutral

Type of the substance is
Detection of Saturation/Unsaturation
Sr. No. Test Observation Inference

1 KMnO4 Test : i) Pink colour of
10 mg substance + 10 KMnO4 Unsaturated compound
droops 10 % Na2CO3 + disappears present.
4 drops of dilute ii) No
KMnO4 and shake well decolourisation  Saturated compound
(Pink colour present
persists)
Detection of Aliphatic/Aromatic Nature
Sr. No. Test Observation Inference

1 Heat a little (10 mg) i) Sooty flame  Aromatic compound
substance on a clean ii) Non present
copper gauze sooty flame Aliphatic compound
present
Conclusion: Polymer compound is:

(i) Acidic/ Phenolic / Basic / Neutral
(ii) Saturated / Unsaturated
(iii) Aromatic / Aliphatic

0
Result Table: Polymer compound is……Urea Formaldehye.
 Conclusion: With the help of qualitative analysis of polymer students able to

detect nature and structure of polymer


Experiment No. 07
MOLECULAR WEIGHT OF POLYMER
Marks: /10
Aim: Determination of molecular weight of a polymer.

Objectives:
1. To understand the method that is applicable for the determination of molecular
weight of polymer.
2. To know the properties of polymer which are depends upon the molecular weight
of polymer.

1. Apply suitable method to find out the molecular weight of polymer.
2. Able to feed required quantity of monomers in synthetic reactors to have good
strength of polymer.

Chemicals: Polyvinyl alcohol
Apparatus: Ostwald’s viscometer, stopwatch.

Theory: Polymers have molecular weights, which may vary from several thousands to
several millions. It is related to the chain length and the extent of cross –linking between
different chains.
Addition of even a very small amount of a polymer to a solvent of low viscosity causes a
sharp increase in its viscosity. The magnitude of increase in viscosity depends on the
molecular weight of the polymer.
When a liquid is made to flow through a capillary tube by a pressure gradient and the
time for a given volume to flow along the tube is measured, then at a constant
temperature, the coefficient of viscosity, η , is given by Poiseuille’s equation .
Л Pr4 t
Η=
8VL
V – Volume of liquid that flows through the tube.
P - Difference in pressure at the two ends of the tube.
r - Radius of the tube.
L - Length of the capillary tube in centimeter.
t – Time of flow in seconds
When viscometer is used for the measurements the liquid flows vertically down the
capillary tube and the driving force is given by P = h p g
By using an Ostwald’s viscometer, relative viscosity (viscosity ratio) η r = η / ηo can be
found out . Here η is the viscosity of polymer solution and ηo is the viscosity of pure
solvent.
ηr = ηs / ηo = ps ts / po to
ps and po are densities of unknown liquid (polymer solution) and pure solvent
respectively and ts and to are the corresponding flow times.
For a dilute polymer solution (C < 0.6% ), the density of the solution may be taken as that
of the solvent, i.e., ps = po
η r = t s / to
The specific viscosity, ηsp, of the polymer solution is obtained by dividing (η sp - ηo ) the
increase in viscosity of the solvent due to the presence solute by η o the viscosity of the
pure solvent .
ηsp = (ηsp - ηo) / ηo = ηr – 1
The ratio of the specific viscosity of the solution to its concentration C, expressed in g/
100 ml is called reduced specific viscosity or simply reduced viscosity ηred.
 ηred = ηsp / C

Both ηr and ηsp vary sharply with concentration, the variations of η red with concentration
is somewhat less and regular, and the plot of ηred versus concentration is a straight line
given by the equation.
2.303 X log η ηred = ηsp

C η0 C
}η }η
%C %C
The value of the constant is given by the intercept on the ordinate. This constant, which
becomes independent of concentration is the limiting value of the reduced viscosity and
is termed as limiting viscosity or intrinsic viscosity, [η].
Mathematically,
lim ηred
[η] = C→ O
C
Or ηsp /C = mC + [η]
For linear polymer the intrinsic viscosity [η] and the molecular weight M are generally
found to obey the Mark – Kuhn – Houwink empirical equation.
[η] = KMa
Where K and a are constants for a particular polymer / solvent / temperature system. K
and a, values are known for a polymer / solvent combination, M may be calculated from
the determined value of [η] .

The values of K and a are given below for some polymers (250C).
Sr. No. Polymer Solvent K A
1. Cellulose acetate Acetone 1.49 X 10-4 0.82
2. Polystyrene Toluene 3.70 X 10-4 0.62
3. Polymethyl Methacrylate Benzene 0.94 X 10-4 0.76
4. Polyvinyl alcohol Water 2.00 X 10-4 0.76
Procedure:
Part – A: To determine the time of flow for a given pure solvent
1. Take a clean and dry Ostwald’s viscometer.
2. Clamp the wider arm of the viscometer to the retort stand in such a way that
viscometer is in perfectly vertical position.
3. Introduce 30 ml of pure solvent into wider arm of viscometer.
4. Attach a rubber tube to a narrow arm of viscometer and suck the pure solvent by
rubber tube till it rises above the upper mark of narrow arm above bulb B
5. Allow the pure solvent to flow down, and start the stopwatch as the liquid crosses
the upper mark.
6. Stop the stopwatch as the liquid crosses the lower mark.
7. Note the time in seconds required by solvent to flow from upper mark to lower
mark on narrow arm of viscometer.
8. Take two such readings and find out the mean time in seconds required to flow for
the solvent.
Part – B: To determine the time flow for given polymer solution.
1. Drain out the water from viscometer and rinse the viscometer using 4-5 ml of 0.2%
polymer solution.
2. Now introduce 30 ml of 0.2 % of polymer solution ( polyvinyl alcohol in water
) in clean viscometer and repeat the procedure as in part A to take two readings.
3. Find mean time of flow for 0.2 % of polymer solution.
4. Similarly repeat the procedure for 0.3 %, 0.4 %, 0.5 % and 0.6 % polymer
solution and record the time.

Observation table:
Sr. Solvent/ Time
No Polymer ‘t’ (seconds) ηr = η / ηo = ηsp= ηr – ηred = ηsp / C (2.303/C) *
solution 1 2 Mean t / to 1 (log η / ηo)
1 0 % (Pure
solvent)
2 0.2 %
polymer soln
3 0.3 %
polymer soln
4 0.4 %
polymer soln
5 0.5 %
polymer soln
6 0.6 %
polymer soln
Calculations:
From appropriate values of K and value of [η] from graph find out molecular weight of
polymer by using equation
1) η = KMa
Ma = 𝜂
𝐾

a log M = log
k

3
6
Result Table:
Polymer used Molecular weight
Conclusion:
With the help of Oswald viscometer by measuring the viscosity of polymer solution the
molecular weight of polymer can be determined.
3
7

Experiment No. 08
PROXIMATE ANALYSIS
Marks: /10
AIM: To determine moisture, volatile matter and ash content in a given sample of coal.
Objectives:
1. To understand the proximate analysis method to analyse the coal sample.
2. To know the quality of coal sample.
Outcomes: At the end of this experiment student should be able to:

1. Apply the proximate analytical method to select good quality of coal for
application purpose.
2. To remove undesirable contents from coal sample.
3. To use good quality of coal sample wherever applicable.

APPARATUS/INSTURMENTS: Oven, Muffle Furnace, Crucible

CHEMICALS: Coal sample

THEORY:
In order to find suitability of coal for a particular domestic or industrial use proximate
analysis is carried out. Proximate analysis is the simplest type of analysis of coal and it
gives information about the practical utility of coal. In the proximate analysis, moisture,
volatile matter, ash and fixed carbon are determined.
Moisture is absorbed by porous coal. It decrease with increasing rank and is a rough
indicator of the age or degree of coalification. It reduces the calorific value of coal. A
lot of heat is wasted in evaporating the moisture during combustion.
Coal with high volatile matter burns with long smoky flame. Volatile matter consists of
combustible gases like CO, H2, CH4 & HC and incombustible gases like CO2 and N2.
The calorific value of such coals is less as the heat produced is distributed over large
space.
Ash is non-combustible matter left over after burning of coal. It reduces the calorific
value of coal. Ash carried with coal increases its weight without adding to the calories
available. Ash usually consists of silica, alumina, iron oxide, lime, magnesia etc.
PROCEDURE: PART A: MOISTURE CONTENT IN COAL
1) Clean a porcelain crucible. Dry the crucible by heating in a oven at 100 oC for 5
minutes. Cool the crucible in desiccator and weigh it accurately.
2) Weigh exactly about 1 gram of powdered coal sample in the crucible.
3) Place the crucible without lid in hot air oven. Heat it to 105 - 110 ~ for about one
hour. Remove the crucible from oven and cool it in desiccator. Weigh it
accurately.
4) Repeat the procedure by heating and cooling the crucible till constant weight is
obtained.
5) Hence calculate percentage of moisture in coal.

9
OBSERVATIONS:
Sr. No. Observation Symbol Value
1 Wt of dry porcelain crucible W
2 Wt of dry porcelain crucible + coal W1
3. Wt of coal taken X
4 Wt of crucible + coal after heating W2
5 Wt of moisture content W1 - W2
CALCULATIONS:
loss in weight of coal

Percentage of moisture =----------------------------------* 100
weight of coal taken
PART B : VOLATILE MATTER IN COAL
1. Clean a crucible. Dry it in oven. Dry the crucible by heating in a oven at 100 oC
for
5 minutes. Cool the crucible in desiccator and weigh it accurately.
2. Weigh exactly about 1 gram of powdered coal sample in the porcelain crucible.
3. Place the crucible without lid in a muffle furnace maintained at 950 +-20 oc for
about 7 minutes.
4. Take out the crucible .First bring down its temperature rapidly ( to avoid
oxidation of the contents) by placing it on a cold iron plate.
5. Then transfer the warm crucible to a desiccator to bring it to room temperature.
6. Take the weight of crucible and its contents and find the percentage of volatile
matter in coal.

OBSERVATIONS:
Sr.
Observation Symbol Value
No.
3 Wt of coal taken X
5 Wt of volatile matter content W1 - W2
CALCULATIONS:
Loss in weight of moisture free coal

Percentage of volatile matter = -------------------------------------------- * 100
Weight of coal taken
PART C: ASH CONTENT IN COAL
Weigh exactly about 0.5 gm of powdered coal sample in a previously dried and
weighed silica crucible.
1. Heat crucible without lid in muffle furnace at 750 +- 20o C for half an hour.
2. Remove crucible from furnace. Cool it in air initially & then in desiccator.
3. Weigh it accurately and find the percentage of ash in coal.
41DEPARTMENT OF ENGINEERING SCIENCE

Sr.
Observation Symbol Value
No.
3 Wt of coal taken X
5 Wt of volatile matter content W1 - W2
CALCULATIONS:
Weight of ash / residue

Percentage of ash =-------------------------------------* 100
Weight of coal taken
Percentage of carbon = 100 - % of (moisture + volatile matter + ash)

=
RESULT TABLE:
Sr. No. Observations Percentage
1 Percentage of moisture
2 Percentage of volatile matter
3 Percentage of ash
4 Percentage of carbon
Conclusion:
In proximate analysis of coal step by step we the % of moisture, V. M. ash content and
fixed carbon percentage from known mass of coal sample can be calculated.

2

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FE [ALL Sinhgad Institute of Technology, Engineering

BRANCHES] Lonavala Chemistry

SINHGAD TECHNICAL EDUCATION SOCIETY’S

DEPARTMENT OF FIRST YEAR ENGINEERING SCIENCES

TEACHING SCHEME EXAMINATION SCHEME

This is to certify that Mr. /Ms._______________Aastha Singh_________________________________

Course In-charge Head of Department Principal

2 DEPARTMENT OF ENGINEERING SCIENCES

To determine hardness of water by EDTA 21/05/21 11/07/21

2 To determine alkalinity of water 28/05/21 11/07/21

3 Titration of a mixture of weak acid and 04/06/21 11/07/21

To determine strength of strong acid using 04/06/21 11/07/21

To determine maximum wavelength of

Preparation of polystyrene/phenol- 25/06/21 11/07/21

To determine molecular weight/radius of

8 Proximate analysis of coal. 25/06/21 11/07/21

Name & Signature of Course In-charge

3 DEPARTMENT OF ENGINEERING SCIENCES

CLASS: - FE Division: Course: - ENGINEERING CHEMISTRY

Date of Performance: / /20 Sign with Date

Aim : To determine hardness of water by EDTA method

Outcomes: At the end of this experiment students should be able to:

PEOs, POs, PSOs and COs satisfied:

4 DEPARTMENT OF ENGINEERING SCIENCES

STRUCTURE OF COMPLEX: Metal – EDTA complex

5 DEPARTMENT OF ENGINEERING SCIENCES

PART 1: Preparation of standard hard water (1 ppm)

PART 2: Standardization of EDTA solution

PART 3: Total hardness of given water sample

DEPARTMENT OF ENGINEERING SCIENCES

Burette: Na2EDTA solution Indicator: Eriochrome black-T

Pipette: 10 ml of SHW (ZnSO4.7H2O) End Point: wine red to sky blue.

Reading in Pilot I II III C.B.R.

PART 3: Total hardness of given water sample

Burette: Na2EDTA solution Indicator: Eriochrome black-T

Reading in Pilot I II III C.B.R.

7 DEPARTMENT OF ENGINEERING SCIENCES

Normality of Na2EDTA solution: ------- N Burette reading: (V1ml)------------ml

1ml of SHW ≡ 1 mg of CaCO3  10 ml of SHW ≡ 10 mg of CaCO3

But 10 ml of SHW required ml (V1ml) of EDTA

 ml (V1ml) EDTA react with 10 ml CaCO3 equivalent

1 ml EDTA solution determines = 10 ÷ V1 = (A) mg of CaCO3

1 ml EDTA determines = 10 ÷V1 = __ (A) mg ofCaCO3

10 ml of hard water sample reacts with = V2 __________ml of EDTA

 V2 ml EDTA determines = (A X V2) = ___________(B) mg of CaCO3

10 ml of hard water sample contain = ______________(B) mg of CaCO3

Hence, 10 0 0 m l hard w a t e r sample contain = (B X 1 0 0 ) = _______ mg of CaCO3

But 1mg/lit CaCO3 = 1 ppm

Therefore, total hardness = _____________ ppm of CaCO3

DEPARTMENT OF ENGINEERING SCIENCES

1. 1 ml EDTA solution determines = ppm of CaCO3

Sign. Of Teacher with date –

9 DEPARTMENT OF ENGINEERING SCIENCES

CLASS: - FE Division: Course: - ENGINEERING CHEMISTRY

Date of Performance: / /20 Sign with Date

AIM: To determine total alkalinity of water sample.

PEOs, POs, PSOs and COs satisfied:

APPARATUS: Titration apparatus i.e. burette, pipette, conical flask, stand

etc. CHEMICALS: HCl, methyl orange, phenolphthalein.and water sample

10 DEPARTMENT OF ENGINEERING SCIENCES

The titration of water sample against a standard acid up to phenolphthalein

1. OH¯ + H H2O (one step neutralization, P =M) Detected by Methyl orange

Type of Alkalinity (ppm)

If phenolphthalein end point is zero, then

This is to certify that Mr. /Ms._Aastha Singh___________________