LAB MANUAL

Lab Name : ENGINEERING CHEMISTRY LAB

Branch : ALL

Year : B.Tech I YEAR

Jaipur Engineering College and Research Centre, Jaipur

Department of Chemistry
(Rajasthan Technical University, KOTA)

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 JECRC

Department of Chemistry

Semester-I&II

Engineering Chemistry Lab

Lab Outcomes

Students will be able to:

• Carry out, record and analyze the results of chemical experiments through different
titrations.

• Analyze water with respect to dissolve impurities and coal with respect to proximate
analysis.

• Determine the flash and fire point, cloud and pour point, viscosity of different
lubricants and calorific value of coal, also to synthesize Aspirin.

Co Po Mapping for Engineering Chemistry Lab

PROGRAM OUTCOMES
COURSE
OUTCOMES
1 2 3 4 5 6 7 8 9 10 11 12

LO1 1 1 - 1 - - - - 1 2 - -

LO2 2 2 - 1 - - 1 - 1 2 - -

LO3 2 2 - 1 - - 1 - 1 2 - -

Average 1.66 1.66 - 1 - - 0.66 1 2 - -

PROGRAM OUTCOMES

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1. Engineering Knowledge: Apply the knowledge of mathematics, science, engineering
fundamentals, and an engineering specialization to the solution of complex engineering
problems.
2. Problem analysis: Identify, formulate, research literature, and analyze complex
engineering problems reaching substantiated conclusions using first principles of
mathematics, natural sciences, and engineering sciences.
3. Design/development of solutions: Design solutions for complex engineering problems
and design system components or processes that meet the specified needs with
appropriate consideration for the public health and safety, and the cultural, societal, and
environmental considerations.
4. Conduct investigations of complex problems: Use research-based knowledge and
research methods including design of experiments, analysis and interpretation of data,
and synthesis of the information to provide valid conclusions.
5. Modern tool usage: Create, select, and apply appropriate techniques, resources, and
modern engineering and IT tools including prediction and modeling to complex
engineering activities with an understanding of the limitations.
6. The engineer and society: Apply reasoning informed by the contextual knowledge to
assess societal, health, safety, legal and cultural issues and the consequent
responsibilities relevant to the professional engineering practice.
7. Environment and sustainability: Understand the impact of the professional
engineering solutions in societal and environmental contexts, and demonstrate the
knowledge of, and need for sustainable development .
8. Ethics: Apply ethical principles and commit to professional ethics and responsibilities
and norms of the engineering practice using.
9. Individual and team work: Function effectively as an individual, and as a member or
leader in diverse teams, and in multidisciplinary settings.
10. Communication: Communicate effectively on complex engineering activities with
the engineering community and with society at large, such as, being able to
comprehend and write effective reports and design documentation, make effective
presentations, and give and receive clear instructions.
11. Project Management and finance: Demonstrate knowledge and understanding of the
engineering and management principles and apply these to one’s own work, as a
member and leader in a team, to manage projects and in multidisciplinary
environments.
12. Life –long Learning: Recognize the need for, and have the preparation and ability to
engage in independent and life-long learning in the broadest context of technological
changes needed.

INSTRUCTIONS OF LAB

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DO’s
1. Please switch off the Mobile/Cell phone before entering Lab.
2. Enter in the Lab with complete Lab Uniform.
3. Intimate the lab In charge whenever you are incompatible of doing experiment.
4. Arrange all the apparatus and seats before leaving the lab.
5. Keep the bag in the racks.
6. Enter the lab on time and leave at proper time.
7. Maintain the decorum of the lab.
8. Utilize lab hours in performing the allotted experiment.
9. Switch off the equipment immediately after completing the experiment.
10. Handle the equipments carefully in the lab.

DON’TS
1. Don’t mishandle the equipments.
2. Don’t make noise in the lab.
3. Don’t enter in the lab without permission of lab Incharge.
4. Don’t litter in the lab.
5. Don’t delete or make any modification in lab manual files.
6. Don’t carry chemicals outside the lab.
We need full support and cooperation for smooth functioning of the lab.

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 GENERAL LABORATORY INSTRUCTIONS / PRECAUTIONS

Your own safety and that of other students in the laboratory is largely determined by your work practices.
Accidents in the laboratory can be prevented to a large extent by working carefully, with full concentration,
neatly and unhurriedly. Accidents in the laboratory can have serious consequences and one must believe in
the fact that prevention is better than cure. Here are some instructions that you must follow:

1. Student should bring the following items before coming to the laboratory:
(a) Laboratory coat
(b) Chemistry practical note book
(c) Rough notebook
(d) Pen, Pencil and Eraser
2. It should be compulsory to wear laboratory coat while working in chemistry laboratory.
3. For real understanding of principle, techniques and procedure, the students should plan his or her
work carefully in advance and work purposefully during laboratory period.
4. All chemicals in the laboratory are hazardous in some way or the other. They should be handled
carefully.
5. To prevent accidents, suitable precautions should be taken while working in lab. Always follow the
instructions exactly and in sequence given by the instructor.
6. Do not throw waste material into the sink. Throw them only in the wastebasket.
7. Pieces of Sodium metal should not be thrown into the sink or waste jar. It may be destroyed by
reacting it with alcohol. Sodium must be kept in toluene or kerosene.
8. Experiments should be done only in the presence of an instructor. Never work alone in the
laboratory.
9. All the doors and windows must remain open while working in laboratory.
10. Equipments, glassware, reagents and bottles and other items should be placed in a schematic
manner.
11. Check all the glassware before use. Never use unclean, ordinary and cracked glassware for any
reaction.
12. If a student has broken any apparatus bring this fact immediately to the notice of laboratory staff.
13. The experimental work should be done systematically.
14. Start noting down the readings/ observations of the experiments simultaneously and get it checked
by the teacher concerned.
15. While heating a test tube never point its mouth towards yourself and any other else.
16. Clean all the glassware after completing the experiment.
17. Do not take the chemicals or glassware out of the laboratory.
18. Follow all the instructions given by the supervisor.

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 JECRC

DEPARTMENT OF CHEMISTRY

ENGINEERING CHEMISTRY LAB

List of Experiment:-

1.To determine the hardness of given water sample by complexometric method using EDTA.

2. To Determination the amount of residual chlorine in a given sample.

3. To determine the amount of dissolved oxygen (D.O.) present in given water sample.

4. To determine the strength of Ferrous Ammonium sulphate (FeSO4(NH4)2SO4.6H2O)

solution by titrating it against potassium dichromate K2Cr2O7 (N/40 )solution using

internal indicator diphenyl amine indicator.

5. To determine the strength of unknown solution of copper sulphate(CuSO4.5H2O) by

titrating it against standard solution of sodium thio-sulphate N/40 (Na2S2O3.5H2O)

(iodometrically).

6. To determine the strength of sodium hydroxide ( NaOH) and sodium carbonate

(Na2CO3 )in the given alkali mixture (or in water sample) by titrating against an

Intermediate hydrochloric acid ( HCl N/20 ) using phenolphthalein and methyl orange as

indicator .

7. To carry out proximate analysis of given solid fuel (coal).

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8.(A)To determine the flash and fire points of a given lubricating oil sample using Pensky

Marten’s apparatus.

8.(B) To determine cloud and pour points of given lubricating oil sample using cloud and

pour point apparatus.

9. To determine the viscosity of a given sample of lubricating oil by using Redwood

Viscometer.

10.Synthesis of Aspirin/ Paracetamol.

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 Experiment No. 1

Object: To determine the hardness of given water sample by complexometric method using EDTA.

Apparatus/Reagents required : Burette, pipette, conical flask, beaker, burner, standard M/100 EDTA
solution, Eriochrome Black- T indicator, NH4Cl-NH4OH buffer solution of pH 10, hard sample.

Preparation of M/100 EDTA solution: Dry 5 gm of commercially available A.R. EDTA in an air oven at
80˚ C for 1 ½ hour. Cool and accurately weigh 3.7224 gm and dissolve it in distilled water and make up to
1 litre. This may be used as standard solution.

Preparation of NH4Cl- NH4OH of pH10: Take 70 gm of A.R.NH4Cl and 568 ml concentrated ammonia
solution. Stir and dilute the solution to 1 litre with deionised water.
Preparation of Erichrome Black- T indicator: Dissolve 0.5 gm of Erichrome Black-T indicator in 100 ml
alcohol.

Theory: Ethylene diamine tetra acetic acid (EDTA) is a well known powerful complexing agent.
HOOC.H 2C CH 2COOH

N CH 2 CH2 N

HOOC.H 2C CH 2.COOH

EDTA form complexes with Ca2+ and Mg2+ ions as well as with many other metal cations. These complexes have the
general formula as-

O=C-O O-C=O

H 2C N N CH 2

-
OOCCH2 CH2 CH2 CH2COO-

where M=Ca+2 or Mg+2

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When hard water is titrated against EDTA solution, then EDTA or its sodium salt forms complex ions with
Ca+2 or Mg+2 ions in water.
M + EDTA M-EDTA

(Stable complex)

The titration is carried out in presence of an indicator Erichrome black-T. When indicator is added to hard water
which is buffered at pH 10, then it combines with Ca+ 2, Mg+2 ions to form weak complex of wine red colour. When
an excess of EDTA is added then colour changes to blue due to Ca+ 2 / Mg+2 .EDTA complex. Thus change of wine red
colour to distinct blue marks the end point of titration.

M + EBT [M-EBT]

(Unstable wine red complex)

[M-EBT] + EDTA EBT + M-EDTA

(Blue) (Stable)

Procedure:

(1) Pipette out 10 ml of std.hard water in conical flask.

(2) Add 2 ml of buffer solution and 2 drops of EBT as an indicator .
(3) Titrate the solution against std. M/100 EDTA solution from burette till the colour changes from wine red
to blue.

(4) Repeat it to get concordant titre reading.

(5) Repeat the process with sample hard water to get two concordant readings.
(6) Pipette out 10 ml of boiled water sample in conical flask and add 2 ml of buffer solution and 2 drops of
Erichrome Black-T.

(7) Titrate it with M/100 EDTA solution till blue colour appears at end point.
(8) Repeat the procedure to get concordant value. This corresponds to permanent hardness.

Observation:
Titration: EDTA V/S std. hard water (V1 ml)

S.No. Volume of water Burette Reading(ml) Concordant

reading (ml)
sample (ml) Initial Final

1 10.0 0.0

2 10.0 0.0

3 10.0 0.0

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 Titration: EDTA V/S sample hard water (V2 ml)

S.No. Volume of water Burette Reading(ml) Concordant

reading (ml)
sample (ml) Initial Final

1 10.0 0.0

2 10.0 0.0

3 10.0 0.0

Titration: EDTA V/S boiled hard water (V3 ml)

S.No. Volume of boiled water Burette Reading(ml) Concordant

reading (ml)
sample (ml) Initial Final

1 10.0 0.0

2 10.0 0.0

3 10.0 0.0

Calculation:

Total hardness = V2/V1 x 1000 ppm

Permanent hardness = V3/V1 x 1000 ppm

Temporary hardness =Total hardness – Permanent hardness

Expected outcome: The temporary, permanent, and total hardness of water sample comes out to be…….ppm.

Achieved outcome: The temporary, permanent, and total hardness of water sample is ….ppm.

Precautions:

(1) Titration should be performed slowly near end point.

(2) There should not be any tinge of reddish blue colour at end point.
(3) pH of the solution maintained properly.

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 Experiment No. 2
Object: To determine the amount of free chlorine in given water sample.

Apparatus and Reagents: Burette, pipette, conical flask, volumetric flask, KI solution, glacial acetic acid, starch, hypo
(Na2S2O3)solution (0.06N).

Theory: The germicide action of Cl2 gas depends upon the following reactions:

Cl2 + H2O HOCl + HCl

HOCl HCl + [O]

Hypochlorus acid (HOCl) and nascent oxygen [O] both are powerful germicides. If chlorine is more
than a certain limit, it will make potable water unfit for drinking purposes, because it is injurious to human
metabolism process. Therefore it is necessary to determine its amount in municipal water to iodide (KI)
take place by the free chlorine present in the water. The liberated iodine is estimated by titrating against std.
hypo solution N/40 using starch as an indicator.
Cl2 + 2KI 2KCl + I 2

I2 + 2Na2S2O3 Na 2S4O6 + 2 NaI

I2 + Starch Iodostarch complex ( Blue colour )

Procedure:

1. First wash all the apparatus with distilled water.

2. Fill the burette with std. hypo solution and note down the initial reading of burette.
3. Take 10 ml of water sample in a conical flask, than add 2-3 ml of glacial acetic acid (to maintain 3-4 pH) and
add 1-2 ml of KI solution.
4. Titrate the water sample with hypo till the solution in the conical flask becomes faint yellow.
5. Then add 2-3 drops of starch indicator,a blue colour appears.
6. Add hypo drop wise with constant shaking till the blue colour disappears, it indicates end point. Note down
again the burette reading.
7. Repeat the titration till the same reading is obtained.
5. Observation:

S.No. Volume of water Burette Reading(ml) Concordant

reading (ml)V2
sample (ml)V1 Initial Final

1 10.0 0.0

2 10.0 0.0

3 10.0 0.0

6. Calculation: From normality equation:

N 1 x V1 = N 2 x V2

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 (Water sample) (Hypo)

N 1 = N2 x V2/ V1

∴ Free chlorine = N1 x E (E= equivalent wt. of chlorine)

= N 1 x 35.5 g/L

= N 1 x 35.5 x 1000 ppm

Expected outcome: The free chlorine present in given sample of water is ……….ppm.

Achieved outcome: The free chlorine present in given sample of water is ……….ppm.

Precautions:

1.Starch solution should be freshly prepared.

2.KI solution is used carefully.

Experiment No. 3
Object: To determine the amount of dissolved oxygen (D.O.) present in given water sample.

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Apparatus & reagent required: Pipette, burette,BOD bottles.glass rod, conical flask,standard sod.
thiosulphate( hypo) solution (N/40), sod. azide solution (5%), KI solution, MnSO 4 solution(4.8%), starch solution,
conc. H2SO4.

Theory: The principle involved in the determination of D.O. is to bring about the oxidation of KI to iodine with the
dissolved oxygen present in the water sample after adding MnSO 4, KOH & KI, the basic maganic oxide formed acts
as an oxygen carrier to enable the dissolved oxygen in the molecular form to take part in the reaction. The liberated
iodine is titrated against standard hypo solution, using starch as indicator.

MnSO4 + 2KOH Mn(OH) 2 +K2SO4

2Mn(OH) 2 + O2. 2MnO(OH) 2

Basic maganic oxide (white ppt.)

MnO(OH) 2 + H2SO4 MnSO 4 + 2H2O + [O]

2KI + H2SO4 + [O] H 2O + I2 + K2SO4

(yellow brown colour)

I2 + 2Na2S2O 3 Na 2S4O6 +2NaI

Starch + I2 Iodo-starch complex

(Blue colour)

Procedure:

1. Take 300 ml water sample containing D.O. in it in a BOD bottle.

2. Add 1 ml MnSO4 alkali, iodide, & azide solution (NaOH, KI, NaN3) to the bottle containing water sample.
Brown ppt. of Mn(OH)2 appears in the bottle .
3. After 15-20 minutes, add 2 ml of H 2SO4 and shake the bottle properly. The ppt. get dissolved and reddish
brown colour solution appears due to liberated iodine.
4. Take 10 ml of above solution in a conical flask and add some sodium thiosulphate(hypo) solution to
it. till the solution become light yellow, add 3-4 drops of starch solution to it. A blue colour appears in the
conical flask.
5. Again add hypo from burette to conical flask till blue colour disappears. Note the reading, this represents
the end point.
6. Repaet the titration till you get concordant reading.

Observation:

S. No. Volume of water Concordant

Burette reading reading

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 sample taken(ml) Initial(ml) Final(ml) (ml)V2

10.0 0.0

10.0 0.0

10.0 0.0

Calculation:

Formula used for calculation is- N1V1 (Water Sample) = N2V2( Hypo Solution)

D.O.(mg/L) = ml of titrant x normality of hypo solutionx 8 x 1000

* *
V 1 (V1 -V) / V1

*
V1 = Volume of BOD bottle ml (300 ml)

V1 = Volume of the contents titrated (10 ml)

V = Volume of MnSO4 and iodide, azide (1+1=2 ml)

V2= ml of titrant( volume of hypo solution used)

Expected outcome: The amount of the D.O. comes out to be…………………mg/L.

Achieved outcome: The amount of the D.O. is…………………mg/L.

Precaution:

1. After the addition of the reagents in water sample taken inside BOD bottle, the bubble check should be
done and its removal should be done if formed
2. Special care should be taken in sampling.
3. As far as possible the sample should not come in contact with air.

1.1.1 Experiment No. --4

1.1.2
Object: To determine the strength of ferrous ammonium sulphate [FeSO 4.(NH4)2.SO4.6H2O] solution by titrating it
against potassium dichromate (K2Cr2O7 ) solution(N/40) using diphenyl amine as an internal indicator.

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 Apparatus/ Reagent required: Burette, pipette, conical flask, unknown FAS aq. solution, K 2Cr2O7 aq. solution N/40,
diphenylamine, dil. H2SO4.

Theory: In presence of dil H2SO4 or dil HCℓ, the potassium dichromate acts as an oxidising agent and gives three
atoms of oxygen for oxidation of reducing agent (acid).

K2Cr2O7 + 4H2SO4 K2SO4 + Cr2(SO4)3 + 4H2O + 3[O]

[O]

Fe 2+ Fe 3+

The oxygen so liberated oxidizes Fe2+ to Fe3+ in FAS solution and by adding 2-3 drops of diphenylamin (as an
indicator) the green colour of the solution changes to light purple red colour at the end point due to oxidation of
indicator (benzenoid form converts into quinonoid form.

6[FeSO4.(NH4)2.SO4. 6H2O] + K2Cr2O7 + 7H2SO4 3Fe2 (SO4)3 + K2SO4 + Cr2(SO4)3

+ 6(NH4)2 SO4 + 43H2O

oxidation
2 NH NH NH

Diphenyl benzidine
( Benzenoid form) ( Colourless)

N N N N

Diphenyl benzidine ( quinoidform)

+ 2H + + 2e ( violet colour)

Procedure:

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 1. Take 10 ml of unknown FAS solution into the conical flask and add 8-10 ml of dil H 2SO4 into it and shake it
properly.
2. Fill the burette with N/40 K2Cr2O7 solution and note the initial reading (0.0 ml).
3. Add 3-4 drops of diphenylamin into the conical flask.
4. Add K2Cr2O7 solution from burette into FAS aq. solution with constant shaking and observe the colour
change.
5. The appearance of purple colour from greenish indicate the end point..
6. Addition of final drop of K2Cr2O7 suddenly changes the green colour to purple reddish tinge. This indicates
the end point.
7. Repeat the titration until the concordant reading is observed.

Observation:

Titration between unknown F.A.S. solution and standard Pot. dichromate solution

S.No. Volume of FAS Burette reading (ml) Concordant

Solution (ml) (Volume of K2Cr2O7 solution) Reading (ml)

Initial Final

1. 10.0 0.0

2. 10.0 0.0

3. 10.0 0.0

4. 10.0 0.0

5. 10.0 0.0

Calculation:

The formula for calculation is

N1V1=N2V2

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 Where N1= Normality of FAS solution (unknown)

V1= Volume of FAS solution taken = 10 ml

N2= Normality of K2Cr2O7 solution (N/40)

V2= Volume of K2Cr2O7 solution (concordant reading)

Concentration / Strength of unknown FAS solution = Normality x equivalent weight of FAS

N2XV2X392.14

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Expected Outcome: The strength of given unknown FAS solution is 9.80 g/L

Achieved Outcome: The strength of given unknown FAS solution comes out to be ………….g/L .

Gap between Expected Outcome and Achieved Outcome:

Precaution:

1. All the volumetric apparatus should be washed properly.

2. Drop of analyte is taken time to time and observe carefully whether blue colour appears or not.

3. K2Cr2O7 solution should be added drop by drop.

4. End point should be observed carefully.

Experiment No. 5

Object: To determine the strength of unknown solution of copper sulphate (CuSO 4.5H2O) by titrating it against
standard solution of sodium thiosulphate (Na 2S2O3.5H2O) iodometrically.

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Apparatus / Reagents required: Burette, pipette, conical flask, distilled water, unknown CuSO 4.5H2O, Na2S2O3.5H2O
(N/40), 10% KI solution, Starch indicator.

Theory: Copper sulphate is determined by iodometric method. When KI is added to CuSO 4 solution, cuprous iodide
is precipitated and equivalent amount of iodine gets liberated. This free iodine is then titrated against standard
solution of hypo, using starch as an indicator. The blue colour of iodo-starch complex will disappear till all the
liberated iodine gets changed to NaI. Due to formation of cuprous iodide the colour of precipitate in conical flask
will be white. This indicates the end point.

2CuSO4 + 4KI 2Cu 2I2 + 2K2SO4 + I2 ↑

(White)

2Na2S2O3 + I2 Na 2S4O6 + 2NaI

sod. tetrathionate

Starch + I2 Iodo-Starch complex

(Blue)

2CuSO4.5H2O ≡ I2 ≡ 2Na2S2O3. 5H2O [Equivalent equation]

Procedure:

1. Take 10ml of unknown copper sulphate aq. solution into conical flask with the help of pipette.

2. Add 3-5 ml of 10% KI solution to the conical flask and stir the solution thoroughly red brown or dark brown colour
appears into it.

3. Fill the clean burette with hypo solution and titrate the CuSO 4 solution in the conical flask until yellow colour
commences to decrease (till it becomes pale yellow).

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4. Add 2-3 drops of starch to it. Blue colour appears due to the formation of iodo-starch complex.

5. Add hypo solution to it again, till blue colour disappears and solution turns milky white due to the formation of
Cu2I2.

6. Repeat the titration to get concordant reading.

Observation:

Titration between unknown copper sulphate solution and standard

Sod.thiosulphate solution

S.No. Volume of CuSO4 Burette reading Concordant

solution reading
Volume of hypo solution (ml)
(ml) (ml)
Added

Initial Final

1 10.0 0.0

2 10.0 0.0

3 10.0 0.0

4 10.0 0.0

Calculation:

2CuSO 4.5H2O ≡ 2Na2S2O3. 5H2O

Formula used for calculation is- N1V1 = N2V2

Where N1 = Normality of aq. Copper sulphate solution (unknown)

V1 = Volume of aq. Copper sulphate solution (unknown)

N2 = Normality of hypo aq. Solution = (N/40)

V2 = Volume of hypo aq. solution consumed (burette reading)

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 N 1 x 10 = N2 x V2

N 1 = N2 x V2/10

Strength of aq. Copper sulphate solution = Normality x equivalent weight CuSO 4.5H2O

= 1/40 x V 2/10 x 249.5 g/L

Expected Outcome: The strength of given copper sulphate solution is 6.23g/L

Achieved Outcome: The strength of given copper sulphate solution comes out to be --------------- g/L.

Gap between Expected Outcome and Achieved Outcome:

Precaution:

1. The clean glass apparatus is used for each titration.

2. Fresh reagents and solutions should be prepared.
3. Exact volume of aq. copper sulphate solution is taken with the help of pipette.
4. End point should be observed carefully.

Experiment No. 6

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Object: To determine the amount of sodium hydroxide (NaOH) and sodium carbonate (Na 2CO3) in the given alkali
mixture (or in water sample) by titrating against an intermediate hydrochloric acid (HCℓ N/20) using
phenolphthalein and methyl orange as indicators.

Apparatus/ Reagent required: Burette, pipette, mixed alkali (NaOH + Na 2CO3) solution, hydrochloric acid (N/20),
phenolphthalein, methyl orange, and sodium carbonate solution.

Theory: It is a double indicator titration method; hence different indicators are used at two different stages of the
titration. In this titration when sodium carbonate and sodium hydroxide mixture solution is titrated with
hydrochloric acid, the neutralization occurs in two stages. In the first stage, sodium hydroxide is completely
neutralized while Na2CO3 partially neutralized.

Phenolphthalein is used as an indicator.

NaOH + HCℓ NaCl + H 2O

Na2CO3 + HCℓ NaHCO 3 + NaCl

NaHCO3 + HCℓ NaCl + H 2O + CO2

At the first end point [P] the pink colour of phenolphthalein disappears with change of pH 8.3 – 10.0. At this stage
indicator methyl orange is added and the titration is continued. At the next end point [M] the yellow colour of the
solution turn to cherry red in the pH- range 3.1 – 4.4

Here reading [M] means total volume of HCℓ used, from the beginning of the experiment.

[P] = NaOH + (1/2) Na 2CO3

[M] = NaOH + Na 2CO3

[M] – [P] = (1/2) Na 2CO3

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 P NaOH + ½ Na 2CO3

2 ( [M] - [P] ) = Na 2CO3

2 [P] – [M] = NaOH

II

Procedure:

1. Wash the apparatus with distilled water.

2. Prepare solution of Na 2CO3 in volumetric flask. Standardize the intermediate HCℓ solution.

3. Rinse the burette with HCℓ solution, then fill the burette with HC ℓ solution, make sure there are no air
bubbles in the burette.

4. Note down the burette reading.

5. Rinse the pipette with mixed alkali solution. Transfer 10ml of mixed alkali solution to washed conical
flask.

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 6. Add 2 - 3 drops of phenolphthalein indicator to mixed alkali solution in conical flask, a pink colour is
appeared.

7. Add HCℓ from burette solution drop wise with constant shaking, observe the colour change.

The disappearance of pink colour indicates the first end point [P].

8. Add 2 - 3 drops of methyl orange. Continue the titration with same solution in the conical flask.

9. Add more HCℓ from burette drop - wise into mixed alkali solution and observe the colour change. The
change of colour from yellow to cherry red indicates the second end point. Note down the burette
reading [M].

10. Repeat the titration till concordant readings are obtained.

Observation:

Titration between unknown mixed alkali solution and standardized HCℓ

S.No. Volume of Volume of HCl aq. solution (ml) Concordan Concordant

mixed alkali t reading reading (ml)
aq. solution (burette reading ) (ml) [P] [M]
(ml) Initial phenolphthalein Methyl
end point [P] orange end
point [M]

1. 10.0 0.0

2. 10.0 0.0

3. 10.0 0.0

Calculation:

Calculation for strength of NaOH

HCℓ NaOH

N 1V1 N 2V2

N1 = Normality of HCℓ = N/20

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V1 = Volume of HCℓ consumed with NaOH only = [2P– M]

N2 = Normality of NaOH

V2 = Volume of alkali mixture taken (10 ml)

Strength of NaOH in alkali mixture (g/L) = N 2 × equivalent weight of NaOH = N2 × 40

Calculation for strength of Na2CO3

HCℓ Na2CO3

N 1V1* = N3V3

N1 = Normality of HCℓ = N/20

V1* = Volume of HCℓ consumed with Na2CO3 only (i.e- 2 [M - P] )

N3 = Normality of Na2CO3

V3 = Volume of alkali mixture taken (10 ml)

Strength of Na2CO3in alkali mixture (g/L) = N3 × equivalent weight of Na2CO3

= N 3 × 53

Expected Outcome: 1.Presence of Na2CO3 = 0.670g/L

2. Presence of NaOH = 0.403g/L

Achieved Outcome: Alkalinity of given water sample due to:

1. Presence of Na2CO3 = …….g/L

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 2. Presence of NaOH = …….g/L

Gap between Expected Outcome and Achieved Outcome

Precautions:

1. Solution titrated must be cold enough.

2. Use indicator carefully (only 1-3 drops).

3. Loss of CO2 must be prevented by keeping the tip of the burette immersed in the solution present in the conical
flask.

4. Observe decolourisation of phenolphthalein indicator at the end point carefully.

Experiment No. 7

Object: To carry out proximate analysis of given solid fuel (coal).

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Apparatus /Reagent required: Coal sample, electric oven,dessicator, silica crucible, long legged tongs.

Theory: Proximate anlysis is an empirical but important analysis dealing with the determination of moisture
content, volatile matter, ash content and fixed carbon. It provides beneficial informations in accessing the quality of
coal.

Moisture content: It is the weight loss on heating and expressed in the percentage as

Loss in weight

% of moisture = x 100

Wt. of coal sample

Lesser the moisture content, better the quality of coal as a fuel as it reduces calorific value of coal. However,
presence of moisture upto 10 % produces a more uniform fuel – bed and less of fly ash.

Volatile matter: It is not a constituent of coal, but it consists of a complex mixture of gaseous and liquid products
resulting from the thermal decomposition of the coal substance. A high volatile matter containing
coal burns with a long flame high smoke and has low calorific value. Hence lesser the volatile
matter, better the quality of the coal.

Loss in wt. due to removal of V.M

% of volatile matter(V.M ) = x 100

Wt. of coal sample

Ash: It is a useless, non a combustible matter left after burning of the organic matter from the coal. It is usually
consists of silica, alumina, iron oxide and small quantities of lime magnesia etc. Ash reduces the heating value
of a coal. The presence of ash also early wear of furnace walls, burning of apparatus, feeding mechanism and
production cost. So lower the ash content, better the quality of coal.

wt. of ash left

% of ash = x 100

Wt. of coal sample

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Fixed carbon: The amount of fixed carbon increases from low ranking coals to high ranking coals i.e. peat to
anthracite side. More the amount of fixed carbon in coal more will be its calorific value.

% of fixed carbon = 100 − % of (Moisture + V.M + Ash)

Procedure:

1. Clean the crucible ,dry and weight.

2. Dry coal sample in air , transfer 1 g. of coal sample to the crucible and weigh it again .

3.Keep the crucble in the electric oven maintained at 105-110 0C for about 1 hour.

4.After heating, remove the crucible, put into a dessicator for cooling & weigh it.

5.The difference in the weight is reported in % as the amount of inherent moisture in coal.

6. Heat the dried sample of coal covered with a lid in a muffle furnace maintainrd at 925 ± 20˚C for
around 7 – 10 minutes. Cool and weigh after putting the crucible first in air, then into the desiccator
for some times, loss in weight corresponds to volatile matter content.

7.Heat the above treated sample in the crucible without lid inside the muffle furnace at 700 ± 50˚C for
half an hour or until a constant weight is obtained.

8.Cool as usual and weigh the amount. The residue is reported as ash on percentage basis.

Observation:

Wt. of empty crucible = X gm.

Wt. of empty crucible + sample = Y gm.

Wt. of Sample = Y – X= a gm

sample, after heating at 105 - 110 0C = b gm.

sample, after heating at 925 -9520 0C = c gm.

sample, after heating at 700 - 750 0C = d gm.

Calculation:

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 Y-b

(i) % of moisture = x 100

b–c

(ii) % of volatile matter = x 100

d-X

(iii) % of Ash = x 100

(iv) % of fixrd carbon = 100 –(% of moisture + % of volatile matter + % of ash ).

Results: Proximate analysis of given sample of coal has given the following results.

(i) % of Moisture.............gm
(ii) % of Volatile matter.............gm
(iii) % of Ash..............gm
(iv) % of Fixed carbon...............gm

Precaution:

1. The weighing should be taken upto 4 th decimal place.

2. After the heating, the crucible should be removed with the help of long legged tongs carefully.
3. The heating should be done by raising the temp. at slow rate.

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 Experiment No. 8 (A)
Object: To determine the flash and fire points of a given lubricating oil sample using Pensky-Marten’s apparatus.

Apparatus/Reagents required: Pensky-Marten’s apparatus, given lubricating oil sample.

Theory: Flash point of oil is the lowest temperature at which the combustible liquid gives off sufficient vapours that
ignite for a moment when a small flame is brought near the liquid surface under specified conditions. The fire point
of oil is also the lowest temperature at which the vapours of oil will begin to produce a continuous flame above the
oil at least for 5 seconds. A liquid having flash point less than 140 0F is called inflammable liquid and those with flash
point above 1400F are called combustible liquids. Normally, the fire point of oil is 5 to 40 0C higher than its flash
point. The flash and fire points don’t have any bearing with the lubricating property of the oil but these are important
when oil is exposed to high temperature services. Depending upon the requirements, any of three apparatus (Abel’s,
Pensky Martens apparatus or Cleveland’s open cup apparatus may be selected). Pensky-Martens apparatus is the
most commonly used apparatus for determination of flash & fire points of oils. The essential features of the apparatus
are as follows:

Pilot burner

Shutter

control

Test flame burner

Themometer

oil level Opening

pointer

Stirrer

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Oil cup

Pensky-Marten’s apparatus

i) The oil cup consists of brass and is of a standard size having a mark up to which the oil has to be filled.
ii) The lid of the oil cup has four openings which are meant for a special type of stirrer, thermometer, an air
inlet and a device for introducing the standard flame. The shutter provided at the top of the cup has a
lever mechanism.
iii) The assembly is heated in a controlled manner by keeping it on an electrical
heater

30
Procedure:

1. Clean the oil cup and other parts thoroughly before starting the experiment.

2. Put the apparatus on a level steady table to avoid any damage or accident.

3. Fill the oil to be tested in the cup up to the level mark.

4. Cover the lid and insert the thermometer, stirrer device and flame exposure device carefully in
its opening.

5. Heat the apparatus homogeneously by using the air bath with the help of burner or hot plate
and stirrer (approx. 60 revolutions per minute).

6. When the temperature rises within the range of anticipated flash point, at every 2 0C rise, flame
is introduced for a moment with the help of shutter.

7. Record the flash point at the temperature at which a flash appears in the form of weak sound
and light. This temperature is flash point. Allow to cool the oil for some time, heat again and
test the flame for a distinct flash. Repeat the process 3-4 times.

8. The procedure is continued as before until oil vapour catches fire which stays minimum for
five seconds. The temperature at which this ignition takes place is recorded as the fire point of
the oil.

Observation:

S. No. Temperature (0C ) Observation

1. No flash

2. ,,

3. Flash Point (Little bit spark with pop sound)

4. No fire

5. ,,

6. ,,

7. Fire Point (Flame stays minimum for 5 Sec.)

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Expected Outcome:

The flash point of given lubricating oil sample = 35-60 0C.

The fire point of given lubricating oil sample = 68-720C.

Achieved Outcome:

The flash point of given lubricating oil sample =……..0C.

The fire point of given lubricating oil sample = ………0C.

Gap between Expected Outcome and Achieved Outcome

Precaution:

1. The oil cup and apparatus should be cleaned and dried properly.

2. The bulb of the thermometer should be in touch properly with the oil surface.

3. Stirring of oil and heating should be stopped at the time of the application of test flame.

4. Breathing over the surface of the oil should be avoided.

5. For each experiment the fresh oil has to be used to get correct value of flash and fire points.

Application: Flash and fire points of all petroleum products tell us about its inflammability as well as
combustibility, respectively. These points ensure safety against fire hazards during the storage, transport and
use of the lubricating oil. The flash points and fire points are used to indicate the fire hazards of petroleum
products and evaporation losses under Pensky-Marten’s apparatus. Flash and fire point of all petroleum
products except fuel oils and those having flash point below 175 0F can be measured by this apparatus. A good
lubricant should have a flash point at least above the temperature at which it is to be used. Fire points are 5-
400C higher than the flash point.

32
 Experiment No. 8(B)

Object: - To determine cloud and pour points of given lubricating oil sample using cloud and pour point
apparatus.

Apparatus /Reagents required: - Cloud and pour point apparatus, lubricating oil sample, freezing mixtures.

Theory : - Most of the petroleum lubricants contain dissolved paraffin wax and asphaltic impurities. When the
oil is cooled, these impurities have a natural tendency to crystallize and separate out. As
petroleum oil is cooled under specified conditions, it gets cloudy at first and then solidifies. The
temperature at which a cloudy or hazy appearance is noticed is called the ‘cloud point’ of the oil.
Likewise, the temperature at which the oil just solidifies is called the ‘solid point’. The
temperature at which the oil ceases to flow or pour or become semisolid is known as ‘pour point’.
Important examples of cloud and pour points are refrigerator plants and air craft engines, which
may be required to start and operate at sub-zero temperatures. The apparatus employed for the
determination of cloud and pour point is shown in figure known as cloud and pour point

Thermometers

Flat bottomed test tube

Jar Air jacket

Cork disc

33
 Ring Cooling mixture

jacket

Cloud and Pour point apparatus

It consists of the following parts:-

i) Flat bottomed tube: - It is made of glass with standard dimensions (12cm height and 3cm
diameter). This tube is enclosed in a glass or metal jacket which is firmly fixed in a cooling
bath having suitable freezing mixtures and a thermometer.
ii) Cooling bath: - Containing cooling mixture.
iii) Thermometer
iv) A cork disc to support the tube.

Procedure :-

1. Thoroughly clean and dry the flat bottomed tube.

2. Fill the oil inside the tube and then fit the cork.

3. Adjust the thermometers inside the oil properly and in the cooling bath.

4. The tube is then kept in the freezing mixture. Prepare freezing mixtures in a way as mentioned
below-

Mixture Composition Temperature Range

A Ice + water Up to 100C

B Ice + NaCl Up to -100C

34
 C Ice + CaCl2 Up to - 250C

D Solid CO2 + Acetone Up to - 600C

5. The temperature of the oil falls on cooling. Take out the tube from the freezing mixture after
every 10C fall in temperature and then inspect for a moment. It is restored if the cloudiness has
not formed. This step should be completed within 3 seconds.

6. Note the temperature for hazy appearance which is the cloud point of the lubricating oil. .

7. For determining pour point, continue the cooling process. After every 3 0C fall of temperature,
the tube is withdrawn and tilts to horizontal position for about 5-10 seconds.

8. When oil stops flowing out of the tube, note the temperature which is the pour point.

Observation:-

S.No Temperature( 0C) Observation

1. t1 No hazy appearance

2. t2 Cloudy appearance (Cloud

point)

3. t3 No pour point

4. t4 Pour point (cease to flow)

Expected Outcome:-

The cloud point of the given lubricating sample is 210C.

The pour point of the given lubricating sample is 170C.

Achieved Outcome:-

The cloud point of the given lubricating sample is __________ 0C.

35
 The pour point of the given lubricating sample is ________ 0C.

Gap between Expected Outcome and Achieved Outcome

Precautions : -

1. The observation of tube should be completed within 3 to 5 seconds.

2. A suitable freezing mixture should be chosen depending upon the pour point of the oil.

3. When the wax crystals start separating from the oil, care should be taken to see that the oil and
the thermometer in it are not disturbed unduly. Otherwise, great care should be taken to see
that the oil and the thermometer are not disturbed

4. The flat bottomed tube should not be kept directly in the freezing mixture.

Application: - Cloud point is useful for estimating the temperature at which filter screens in the fuel intake
system of diesel engines might become clogged because of wax separation. Filterability
depends upon the type and nature of wax (either micro-crystalline or amorphous). The
amorphous wax is sticky in nature and more easily clog the filter screen. Values of
petroleum and non petroleum lubricants are significant as many operations must function in
sub freezing conditions.

36
 Experiment No. 9

Object: To determine the viscosity of a given sample of lubricating oil by using Redwood Viscometer.

Apparatus/Reagents required:- Redwood viscometer , stop watch, given sample of lubricating oil.

Theory: The absolute viscosity of a fluid oil can be defined as the tangential force per unit area required to
maintain a unit velocity gradient between two parallel planes in the fluid unit distance apart. For academic
purpose, viscosity is usually expressed in centipoises (1/100 poise) or centistokes. The ratio of absolute
dynamic viscosity to density for any fluid is known as its absolute kinematic viscosity

ν = --------

where ν = Absolute kinematic viscosity

η = Absolute dynamic viscosity

ρ = Density of the fluid

37
 Viscosity is usually determined with three types of viscometer namely Redwood, Engler and
Saybolt. Viscosity of an oil can be measured in terms of the time ( or seconds ) taken by the oil to flow
through the particular standard apparatus used

Thermometers

Stirrer blade

Metallic heating

Bath Pointer

Water bath Stirrer shield

Heating tube Oil valve rod

Agate jet of 1.82mm

dia.& 10mm Length

Water outlet

kohlrausch flask

Leveling screw

38
 Redwood Viscometer

The redwood viscometer is available in two sizes i.e. Redwood no.1 and no.2. Both the apparatus are
similar in principle, shape and working. They differ only in dimensions of the orifice.

Viscometer Diameter of orifice Length of the jet Capable in testing for

RW 1 1.62mm 10mm Light or thin oils

(Kerosene, Mustard oil)

RW 2 3.8mm 50mm Highly viscous oils (Fuel

oil, Mobile oil, Glycerol)

Redwood viscometer consists of the following parts:

1. Oil cup – It is a silver plated brass cup which is opened at the upper end. The bottom of the cylinder is
fitted with an agate jet that can be kept closed or opened by a valve ‘rod’ fitted with a thermometer,
which indicates the oil temperature.
2. Heating bath – Oil cup is surrounded by a cylindrical copper bath containing water with an outlet for
taking out of water, a stirrer with four blades and a thermometer.
3. Kohlrausch flask – A special type of receiver for receiving the oil. Its capacity is 50ml up to the mark
in its neck.

Procedure:

1. On the basis of nature of oil, select the viscometer and clean the oil cup with a suitable solvent
e.g. CCl4, ether, benzene, petroleum spirit and dry properly.

2. Level the instrument with the help of the leveling screw on the tripod.

3. Fill the bath with water or oil according to the temperature of the experiment.

4. Keep the brass ball in position to seal the orifice.

5. Pour the sample oil into the oil cup upto the tip of the pointer.

6. Put the receiver below the jet.

7. Maintain the desired temperature by stirring the water in the heating bath or oil in the oil cup.

8. Lift the ball valves and simultaneously start a stopwatch. Note the time for collecting the oil
up to the mark in the receiver.

39
 9. Replace the ball valve in position to seal the cup and refill the sample oil up to indicator mark.
Perform same experiment for several times to get precise results.

10. Repeat the experiment at three different temperature and note the respective times
Observations:

S. No. Temperature 0C Time taken to flow in seconds (t) Redwood

seconds
(T) Trial 1 Trial 2 Trial 3
(average)

1. 40 0C A1 A2 A3 A1+ A2 +A3

2. 50 0C B1 B2 B3 B1 +B2 +B3

3. 60 0C

Calculation : v = At --

T 0C

v = kinematic viscosity (in centistokes, Cst), t= time of flow in seconds

Where A and B are instrument constants.

A = 0.264, B = 190 for t = 45 – 85 seconds

A = 0.247, B = 65 for t = 85 – 2000 seconds (100Cst = 1stoke)

40
Expected Outcome: (a) The viscosity of given sample of lubricating oil at T 0C is ___________seconds.

(b) As the temperature increases, viscosity decreases.

Achieved Outcome: (a) The viscosity of given sample of lubricating oil at T0C is ___________seconds.

(b) As the temperature increases, viscosity decreases.

Gap between Expected Outcome and Achieved Outcome

Precaution:

1. Before starting the experiment and after each reading, the cup and receiver should be properly
washed.

2. The receiver is so kept that the oil jet touches inside layer of the flask and does not cause
foaming.

3. Filter the oil through a mesh wire sieve before testing for its viscosity.

4. The temperature of bath and oil cup should be maintained identical throughout the
experiment.

Applications:

Viscosity is the property of a lubricating oil that determines its ability to lubricate .Viscosity
values are used in evaluating load carrying capacity in denoting the effect of temperature changes for
establishing uniformity in shipments and for determining the presence of contaminants in used oil
during service. Absolute viscosity values are required to use in all bearing design calculations and
other lubrication engineering technical design problem. Kinematic values are applied for oil blending
procedures. Redwood Viscometer is mainly used for determining viscosity of any lubricating oil for
the above purposes.

41
 Experiment:10
Theory:Aspirin acetylsalicylic acid was first synthesized in 1893 by Felix Hofmann, a chemist for the
German firm of Bayer.This compound had the medicinal properties of salicylic acid.

Aspirin is both an organic ester and an organic acid.It is used extensivelyin medicine as a pain
killer(analgesic)and a fever-reducing drug(antipyretic).

Preparation: Aspirin (molar mass of 180.2g/mol) is prepared by reacting salicylic acid (molar
mass of 138.1g/mol) with acetic anhydride (molar mass of 102.1g/mol).Aspirin is a weak
monoprotic acid.

42
Procedure Day 1 – Synthesis 1. Use a centigram balance to weigh a 50 mL Erlenmeyer flask. Place
about 2 g of sylicylic acid in the flask and weigh again. In the fume hood, the instructor will transfer 5.0 mL of
acetic anhydride from a buret into the flask. Add 5 drops of 85% phosphoric acid (catalyst) to the flask

2. Clamp the flask in a beaker of tap water supported on a ring stand over a burner flame. Stir if needed to
dissolve the salicylic acid. Heat the water to boiling, and shut off the flame. Keep the flask in the hot water
bath for 10 more minutes.

3. While the flask is still in the water bath, slowly add 2 mL of distilled water to the flask to decompose any
excess acetic anhydride.

4. After a minute, remove the flask from the water bath and add 20 mL of distilled water. Let the flask cool
to room temperature. As the solution cools, crystals of aspirin will appear. Cool the solution further by
placing the reaction flask in an ice bath. Chill 5-10 mL of distilled water in a separate container.

5. Weigh a watch glass and filter paper on the centigram balance.

6. Set up a Büchner funnel on a vacuum flask connected to a water aspirator. Place the filter paper in the
funnel and moisten with distilled water from a squirt bottle. Turn on the aspirator and transfer the aspirin
slurry into the funnel. Wash the crystals with 5 mL of the cold DI water.

7. Transfer the filter paper and aspirin to a pre-weighed watch glass and allow to air dry in your locker until
the next lab period.

8. It is safe to discard of the filtrate down the sink with water.

Day 2 – 1. Weigh the dry product to obtain the yield of the reaction. Calculate the theoretical yield and
percent yield of the reaction.

Safety Precautions:
1. Wear safety glasses.
2. Acetic anhydride is corrosive and its vapour is irritating to the respiratory system.
3. Avoid skin contact and inhalation of the vapours.
4. If the vapours are inhaled, move to an area where fresh air is available.
5. Sulfuric acid is corrosive.Avoid skin contact.

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