RAJALAKSHMI ENGINEERING COLLEGE

(An Autonomous Institution)

Affiliated to Anna University, Chennai-602105.

DEPARTMENT OF CHEMICAL ENGINEERING

CH23721 CHEMICAL REACTION ENGINEERING

LABORATORY
R 2023
DEPARTMENT OF CHEMICAL ENGINEERING

VII SEM B. TECH CHEMICAL

CH23421ENGINEERING

TECHNICAL ANALYSIS LABORATORY MANUAL

0
 DEPARTMENT OF CHEMICAL ENGINEERING
Vision

To be a center of excellence in chemical engineering to provide well prepared

professionals to the industries and society.

Mission

i. To provide state of art environment to the students for better

learning to cater for the chemical industries and pursue higher
studies.
ii. To provide space to the students in research to think, create and innovate
things.

PEOs’

I. To produce employable graduates with the knowledge and competency

in Chemical Engineering complemented by the appropriate skills and
attributes.
II. To produce creative and innovative graduates with design and soft skills
to carry out various problem solving tasks.
III. To enable the students to work as teams on multidisciplinary projects
with effective communication skills, individual, supportive and
leadership qualities with the right attitudes and ethics.
IV. To produce graduates who possess interest in research and lifelong
learning, as well as continuously striving for the forefront of technology.

Program Outcomes(POs)
Engineering Graduates will be able to
1. Engineering Knowledge:

Apply the knowledge of mathematics, science, and engineering fundamentals,

to solve the complex chemical engineering problems

ii
2. Problem analysis:

Identify, formulate, review research literature, and analyze complex chemical

engineering problems reaching substantiated conclusions using first principles
of mathematics, natural sciences and engineering sciences.
3. Design/development of solutions:

Design solutions for complex chemical engineering problems and design

system components or process 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 proceed 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
chemical 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 chemical engineering practice.
7. Environment and sustainability:

Understand the impact of the professional chemical 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 chemical engineering practice.
9. Individual and team work:

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Function effectively as an individual and as a member or leader in diverse
teams, and in multidisciplinary settings.
10. Communication:

Communicate effectively on complex chemical 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 in chemical engineering.

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 DEPARTMENT OF CHEMICAL ENGINEERING
TECHNICAL ANALYSIS LABORATORY
LIST OF EXPERIMENTS

S.NO EXPERIMENTS Page No

1 ESTIMATION OF TDS, SS AND HARDNESS OF WATER 1

2 ESTIMATION OF DO BY USING SENSORS 7

3 DETERMINATION OF pH OF A SAMPLE OF WATER 10

4 TURBIDITY METRY 13

5 ANALYSIS OF SOAP 15

6 DETERMINATION OF SAPONIFICATION VALUE OF OIL 19

7 ESTIMATION OF IODINE VALUE OF OIL 22

8 ANALYSIS OF BLEACHING POWDER 25

DETERMINATION OF SILICA CONTENT IN CEMENT

9 27

10 DETERMINATION OF MIXED OXIDE CONTENT IN 30

CEMENT
DETERMINATION OF CALCIUM OXIDE CONTENT IN 32
11 CEMENT

12 DETERMINATION OF FLASH AND FIRE POINT 34

13 DETERMINATION OF CLOUD AND POUR POINT 36

14 VERIFICATION OF BEER-LAMBERTS LAW 37

DETERMINATION OF ABSORPTION COEFFICIENT

15 OF A SOLUTION 39
DETERMINATION OF ABSORPTION COEFFICIENT
16 OF DYE SOLUTIONS 40

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COURSE OBJECTIVES

1. To train the students on basic principles involved in estimation and

characterization
2. of industrially important materials.

2. To provide clear understanding of basic concepts of scale up processes

3. To identify the pollutants present in water, waste water, solvents and
fuels
4. To understand the principles of polymer synthesis and characterization
5. To train the students to identify the common impurities in domestic
chemicals

COURSE OUTCOMES

1. The student would have a thorough understanding on the estimation

and analysis of water pollutants.
2. The student would have a clear understanding of scale up of industrial
processes
3. The student could acquire skills in polymer synthesis and
characterization
4. The students will be able to analyze the common composition of
domestic utilities
5. The students would be aware of handling spectroscopic instruments for
their research

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MAPPING OF PO’S with Course Outcome:

PO
CO
1 2 3 4 5 6 7 8 9 10 11 12

I 3 3 3 3 3 3 3 1 3 2 1 3

II 3 3 3 3 3 3 3 1 3 2 1 3

III 3 3 3 3 3 3 3 1 3 2 1 3

IV 3 3 3 3 3 3 3 1 3 2 1 3

V 3 3 3 3 3 3 3 1 2 2 1 3

CO-PSO MAPPING

CO PSO
1 2 3
1 3 3 3
2 3 3 3
3 3 3 3
4 3 3 3
5 3 3 3

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 TECHNICAL ANALYSIS LABORATORY
DOs and DONTs in the Laboratory

 Before coming to the laboratory, understand the theory behind the reaction
you are going to carry out.

 Keep the work - bench and sink neat and clean. Don’t allow filter paper,
broken bits of glass, sticks of matches etc., to lie on the table or in sink. Put
these things in the dustbin placed at the worktable.

 Apparatus should be in non-greasy condition.

 Keep the apparatus clean and properly arranged on the work - bench.

 If any piece of apparatus is broken, report at once to the staff members / Lab
Assistant.

 Once you have transferred a reagent from a reagent bottle, never pour it
back even if there is some excess.

 Arrange reagent bottles in their proper places after use and see that they are
properly stoppered.

 Handle reagent bottles / chemicals carefully.

 Use only minimum possible quantity of chemicals / Reagents for any

reaction.

 Close the water tap immediately after use; do not waste water.

 Precautions should be taken to avoid fire accidents.

 After the class, before you leave the laboratory, wash the apparatus clean,
wipe the table and keep the apparatus in proper place.

 Wearing lab coats and shoes is mandatory inside the laboratory

 Wear gloves while handling the chemicals

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 DEPARTMENT OF CHEMICAL ENGINEERING TECHNICAL
ANALYSIS LABORATORY

S.NO Date of Name of the Experiment Date of Signature of

Expt Submission Staff

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 ANALYSIS OF WATER
ESTIMATION OF TDS, SS AND HARDNESS OF WATER

Exp. No.1 Date:

Aim

To find out the amount of suspended matter, total dissolved solids, temporary
hardness and total hardness of the given sample water.

Principle
Suspended matter may be due to the presence of the dust and colloidal particles in water.
Water may contain many dissolved solids, which may lead to corrosion and scale
depending upon its hardness. Hardness is the property of water, not lathering with soap,
due to the presence of calcium and magnesium salts. The presence of bicarbonates leads to
the temporary hardness whereas chlorides and sulphates lead to permanent hardness. The
sum of the temporary and permanent hardness of water represents the total hardness. The
temporary hardness is determined by titrating against Std. HCl and permanent hardness is
determined by EDTA method.

Ca(HCO3 )2+ 2 HCL →CaCl 2+ 2 H 2 O+2CO 2

Mg (HCO3 )2+2 HCL → MgCl 2 +2 H 2 O+2 CO 2

The EDTA method of estimation is based on complexometric titration. The total hardness
of water is estimated by titrating it against EDTA using EBT indicator.

n+ ¿ pH =9−10 EBT − M ¿
unstable complex (winered colour )
EBT + M →

[ EBT −M ] + EDTA pH=9−10 EDTA−M + EBT

→ stable complex steel blue colour

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 EBT indicator forms wine red coloured complex with hardness causing metal
ions present in water. On addition of EDTA, metal ions preferably form
complexes with EDTA and steel blue EBT indicator is set free. Therefore
change of colour from wine red to steel blue denotes the end point.

Procedure

1.Suspened mater:
Filter 250ml or the sample water to a dry weighed filter Paper. After filtration keep the
filter paper in an oven for dry. Cool it in a desiccator and weigh it. From the
difference in weight of filter paper, calculate the amount of the suspended matter present
in 250 ml of sample water. Report the value in ppm.

2. Total dissolved solids:

Evaporate 40ml of the filtered sample water in a preweighed china dish. Cool the china
dish in desiccator and weigh it. The difference in weight gives the amount of total
dissolved solids present in 40ml of the sample. Report the value in ppm.

3. Temporary hardness:
(a) Standardization of HCl:
Prepare 100ml of the N/20 Na2CO3 std. solution. Pipette out 10ml of this solution and
titrate it against dilute HCl using methyl orange as an indicator. The endpoint is the color
change from yellow to pink.
(b) Estimation of temporary hardness:
Titrate 40ml of filtered sample against standardized HCl using methyl orange as
indicator. Report the value of hardness as calcium carbonate in ppm.

4. Total hardness:
Standardization of EDTA Solution:

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Pipette out 20ml of the given standard water. Add 10ml of ammonia buffer solution and
titrate against EDTA using Erichrome Black- T as indicator. The end point is the color
change from wine red to blue.

Estimation of total hardness:

Pipette out 20ml of sample water. Add 10ml of the buffer solution and titrate against
standardized EDTA using Erichrome Black- T as indicator. The end point is the color
change from wine red to blue. Report the value of total hardness as CaCO3 in ppm.

Result
Suspended matter = _____ ppm.
Total dissolved solids =_____ ppm.
Temperary hardness = ____ ppm (CaCO3)
Total hardness = ______ ppm (CaCO3)

3
Calculations
1. Suspended Matter:
Weight of filter paper =_______ g
Weight of filter paper after filtration and drying =_______ g
Weight of filtrate =_______ g
Amount of suspended matter present in 250 ml of sample water =_____ g
Amount of suspended matter present in 1000 ml =______ g
Amount of suspended matter = ______mg/lit =_____ ppm.

2. Total Dissolved Soilds:

Weight of empty china dish =_______ g
Weight of china dish after evaporation =______g
Amount of total dissolved solids =_______g
Amount of TDS in 40ml of sample water =_____ g
Amount of TDS present in 1000 ml =______ g
Amount of TDS = ______mg/lit =_____ ppm.

3. Temporary Hardness:
Standardization of HCl
Standard Na2CO3Vs HCl
Indicator : Methyl Orange
Volume of Burette Reading(ml)
Sodium
S. No. Carbonate(ml) Initial Final Volume of HCl(ml)

Volume of Na2CO3, V1 =
Normality Na2CO3, N1 =
Volume of HCl,V2 =
Normality of HCl, N2 = _________

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Estimation of temporary hardness
40ml of filtered water sample Vs Standardized HCl
Indicator: Methyl orange
Volume of Burette Reading(ml)
water sample
S. No. (ml) Initial Final Volume of HCl(ml)

Volume of HCl, V2 =
Normality of HCl, N2 =
Volume of filtered sample water,V1 =
Strength of filtered sample water, N1 = _________ N
Equivalent weight of Calcium carbonate = 50.045g
Temporary hardness of sample water as CaCO3 = NormalityX50.045
=______g/l
=________mg/l or ppm

4. Total Hardness:
Standardization of EDTA
Standard hard water+10mlbuffer solution Vs EDTA
Indicator: EBT

Strength of standard water = _______ N

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(Standard hard water is prepared by dissolving known amount of CaCO3 in HCl and the
making upto 1 litre using distilled water.)

Volume of standard water, V1 =

Normality of standard water, N1 =
Volume of EDTA Solution, V2 =
Normality of EDTA, N2 = _________ N

Estimation of Total hardness

40ml of filtered water sample + 10ml buffer solution Vs Std EDTA ample
Indicator: EBT

Volume of EDTA Solution, V1 =

Normality of EDTA N1 =
Volume of filtered water sample,V2 = 40ml
Normality of filtered hard water sample, N2 = _________ N
Total hardness of sample water as CaCO3 = Normality X 50.045 =________g/l
=________mg/l
=________ppm

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 ESTIMATION OF DO BY USING SENSORS

Exp. No.2 Date:

Aim
To determine the dissolved oxygen present in given water sample.

Apparatus
Digital Dissolved Oxygen Meter with the electrode.

Reagents
Potassium chloride solution (7.5%).

Principle
Oxygen dissolved in water, often referred to as DO, is a very
important parameter of water quality and is an index of physical and
biological process occurring in water. There are two main sources of
dissolved oxygen in water i) Diffusion from air ii) Photosynthetic
activity within water. Diffusion of oxygen from air to water is physical
phenomenon and depends upon solubility oxygen, which in turn, is
influenced by factors like temperature, water movement, salinity etc.

DO Measurement Method

Preparation of Solution
Take 7.5gm of potassium chloride and mix it in 100 ml distilled water.
Fill potassium chloride solution (7.5%) in the electrolyte tube.

DO probe Assembly
1. Fit the membrane on the lower part of the electrolyte tube. Be careful to handle its
membrane.

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2. Fix the ring in the electrolyte tub, covering the sides of the membrane.
3. Fill potassium chloride solution in the electrolyte tube to its top.
4. Insert the electrode in the electrolyte tube and tightly screw it up. Now the probe is
ready for use.

DISSOLVED OXYGEN SATURATION

VALUE OF DISTILLED WATER
Temp. Temp. Temp.
Oxygen Solubility Oxygen Solubility Oxygen Solubility
o o o
C (ppm) C (ppm) C (ppm)
21 8.82 25 8.06 29 7.60
22 8.67 26 8.22 30 7.50
23 8.41 27 7.90 31 7.40
24 8.36 28 7.76 32 7.30

S. No Types of Water Temperature (oC) DO value

1 Distilled Water
2 Tap Water
3 Waste Water

Procedure
1. Set the temperature knob to the solution temperature and CAL knob to extreme
right position, and Zero knob to extreme left position.\
2. Place the DO probe in 2% sodium sulphite solution. Allow the display to attain
equilibrium. Set the Zero knobs to bring the display to read 0.00 by keeping
temperature knob to actual temperature of the solution. Calibrate knob should be at
extreme right position.
3. Now calibrate the instrument with known value of DO solution.
4. Take 250 ml flask and fill 2/3 of it with distilled water.
5. Stopper the flask and take it for 20 seconds. Remove the stopper back and swirl the
water back and repeat the procedure 4 times.
6. Measure the temperature of water and set the temp knob, knob a temp. of water in

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 the flask.
7. Hold the probe in the flask and agitate the water. If necessary adjust the meter
reading with CAL knob.
8. Now, the instrument is ready to take measurements of DO value of any unknown
solution.

Precautions:
1. 7.5 % KCL solution acts as a good electrolyte in DO probe. Presence of any other
salt in electrolyte solution may damage the probe.
2. The electrolyte tube should not contain any air bubble. If it is present, it will cause
fluctuations in the readings.
3. Movement of the solution should be about 2 ft/sec for accurate measurement.

Result:
Dissolve Oxygen present in the following water sample is
(i) Distilled Water = -------- mg/l
(ii) Tab water = -------- mg/l
(iii) Waste water = -------- mg/l

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 DETERMINATION OF pH OF A SAMPLE OF WATER

Exp. No.3 Date:

Aim
To determine the pH of the given water sample.

Apparatus
pH meter, pH electrode filled with KCl solution, buffer solutions of pH4 and pH 7.

Reagents
pH = 7 and pH = 4 buffer solutions.

Principle
The term “pH” refers to the measurement of hydrogen ion
activity in the solution. Since the direct measurement of the pH is very
difficult, specific electrodes are needed for quick and accurate pH
determination. pH is measured on a scale of 0 to 14, with lower values
indicating high H+ (more acidic) and higher values indicating low H+
ion activity (less acidic). A pH of 7 is considered as neutral. Every
whole unit in pH represents a ten-fold increase in or decrease in
hydrogen ion concentration. Most natural waters possess the pH values
ranging from 5.0 to 8.5. Rain water have a pH value of 5.4 to 6.0
which then reacts with the soils and minerals causing the reduction in
H+ ion concentration and thus the water may become alkaline with a
pH 0f 8.0-8.5. More acid water (pH<5) and more alkaline (pH >9) and
other immediate changes in the hydrogen ion concentration (pH)
suggest that the quality of the water is adversely affected due to the
introduction of some toxic contaminants in water bodies. pH is
measured using pH meter, which comprises a detecting unit consisting

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 of a glass electrode, reference electrode, usually a calomel electrode
connected by KCl bridge to the pH sensitive glass electrode and an
indicating unit which indicates the pH corresponding to the
electromotive force is then detected. Before measurement, pH meter
should be calibrated by using at least two buffers.

Precautions 1. The pH meter can be standardized by measuring the 7-pH buffer solution or
any other solution of standard pH. 2. The electrodes have to be inserted into the water so
that it does not touch the bottom of the beaker. Bottom contact may cause damage to the
electrodes. 3. Any cause of slow response due to the polarization can be solved by
washing the electrodes thoroughly. 4. Periodic check has to be conducted to check the
electrodes 5. During the electrode storage, they have to be kept moist. And also follow the
instructions of the manufacturer.

Procedure:
1. Plug in the pH meter to power source and let it warm up for 5 to 10 minutes
2. Wash the glass electrode with distilled water and clean slowly with a soft tissue.
3. Note the temperature of water and set the same on the pH meter
4. Place the electrode in pH 7 buffer solution and set the value of 7 on the pH meter
turning the Calibrate knob on the meter.
5. Take out the electrode, wash with DW and clean
6. * Dip the electrode in the pH 4 buffer solution. Adjust the value on the pH readout
meter by the Slope switch . Repeat with pH 7 and pH4 buffers till a correct and
stable reading is displaced.
7. While moving and cleaning the electrode, put the selector switch on standby mode.
Turn to pH mode for recording the pH.
8. Now place the electrode in the water sample whose pH is to be determined.
9. You can take a number of simultaneous readings for different samples until the
power is on pH Meter.

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 ‘pH meter

S. No Types of Water Temperature (oC) pH value

1 Distilled Water
2 Tap Water
3 Sample Water

Result:
The pH of the samples of water found using the pH meter are as follows:
(i) Distilled Water = -------- mg/l
(ii) Tab water = -------- mg/l
(iii) Waste water = -------- mg/l

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 TURBIDITY METRY
Exp. No.4 Date:

Aim
To find the turbidity of the given sample of solution.

Apparatus required
10 ml graduated pipette, 100ml standard flask, 100ml beaker, specimen tubers, Nephelo
turbidity meter.

Procedure
Preparation of 400 NTU stock solution:
Solution 1:
Weigh exactly 1g of hydrazine sulphate and dissolve it in 100ml distilled water.
Solution 2:
Weigh exactly 10g of hexamethylene tetramine and dissolve it in 100ml distilled water.
Stock solution: Mix 5ml of solution 1 and 5ml of solution 2 and allow to stand it for 24
hours. Then make up the 10ml mixture to 100ml using distilled water. The made up
solution is the 400NTU standard solution for Turbidity meter. Calibrate this instrument by
using distilled water to zero reading and using the stock solution.

Preparation of sample solutions:

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Prepare the solutions of the given sample of roughly 100NTU, 200NTU, 300NTU and 400
NTU, using 100ml standard flasks. Find the NTU values of the prepared samples using
the instrument. Then find the NTU of given unknown solution. Draw a graph between
readings and find the NTU of unknown solution from the calibration graph.

Graph:
Plot meter reading (y-axis) Vs concentration (x-axis)
Determination of Composition
From the graph explained above, the percentage concentration of unknown
solution is determined for the corresponding mater reading of the unknown
composition.

Result:
Turbidity of the given unknown solution is ______________NTU

14
 ANALYSIS OF SOAP

Exp. No.5 Date:

Aim
To determine the percentage of moisture content, total alkali and total fatty
matter present in a given sample of soap.
Principle
Soap is salt of fatty acid used for cleaning action. The common cleaning soaps used are
generally sodium salt of fatty acid. The salt is hydrolysed in hydrochloric acid to give
fatty acid and NaCl. The acid remaining after the reaction is found using titration with
standardised NaOH. From the quantity of unreacted acid the amount of acid that has
reacted with the alkali in the soap, and hence the quantity of alkali in the soap is
calculated.

Procedure
1. Determination of Moisture and Volatile Matter:
 Weigh 2 to 3 g sample of soap in the form of fine flakes using a watch glass.
 Keep it in an oven for 2 hours. Cool the contents using the desiccator and weigh it.
Find the difference in weight. From this calculate the percentage of moisture content.
2. Determination of Fatty Matter and Total Alkali:
 Weigh accurately 5g of given soap sample in the form of fine flakes. Dissolve this
sample using 100ml of warm water.
 Take the contents in a beaker. Taking care that no lather is formed. Make the solution
into 250ml standard flask.
 Pipette out 100ml of this solution in a beaker and add 40 ml of N/2 HCl. Heat the
contents over a water bath for 30 minutes.

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 Cool the contents in a cold water bath for overnight. This will enable the fatty matter
to become a crust.
 Separate this using a separating funnel by dissolving the fatty matter in
ether/ethanol(approximately 50ml). shake well in the separating funnel to separate
aqueous layer from fatty matter.
 Titrate 10 ml of the excess acid in the aqueous layer with standard N/2 NaOH solution
using methyl orange as indicator.
 A blank titration of HCl Vs NaOH must be performed. From this calculate Na 2O
content in the given sample.
3. Determination of Fatty Matter:
 Take the organic layer of fatty matter in the beaker and dissolve it with excess ether if
required.
 Transfer the contents carefully to a preweighed and dried china dish and evaporate the
contents using a water bath. Ether/ethanol will evaporate leaving the oily matter
residue.
 Weigh the residue and calculate the percentage of total fatty matter.

Result
Percentage of moisture content and volatile matter =______ %
Percentage of total alkali =______ %
Percentage of fatty matter =_______ %

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Calculations:
Moisture Content and Volatile Matter
Weight of the soap = _____ g
Weight of soap after taken from oven = _____ g
Difference in weight =_____ g
Percentage of moisture content and volatile matter = (Difference in weight/weight of soap
taken)*100= ___%

Total Alkali Estimation

Standardization of HCl
Standard Na2CO3Vs HCl
Indicator Methyl Orange
Volume of Burette Reading(ml)
Sodium
S. No. Carbonate(ml) Initial Final Volume of HCl(ml)

Volume of Na2CO3, V1 = 10ml

Normality of Na2CO3, N1 =________N
Volume of HCl, V2 = ________ml
Normality of HCl, N2 =V1*N1/V2 = _________ N
Standardization of NaOH
Standard HCl Vs NaOH
Indicator : Methyl orange

17
 Volume of HCl Burette Reading(ml) Volume of NaOH
S. No. (ml) Initial Final (ml)

Volume of HCl, V1 = ___________ ml

Normality of HCI, N1 = __________ N
Volume of NaOH, V2 = __________ ml
Normality of NaOH, N2 = _________ N

10ml Aqueous soap layer Vs NaOH

Indicator: Methyl Orange

Volume of Burette Reading(ml)

Volume of NaOH
aqueous soap
S. No. Initial Final (ml)
layer (ml)

Calculation of the alkali content in soap:

Volume of aqueous layer (excess acid) = z ml
10ml of aqueous layer corresponds to x ml of NaOH
z ml of excess acid = x* z ml = x2 ml
Volume of HCl unreacted (excess) = x2 ml
Amount of HCI reacted with alkali in soap = 40 – x2 = x3 ml

1000ml of 1N HCl =1000ml of 1N NaOH =40g of NaOH=31g of Na2O

x3 ml of ___ N HCl =(x3ml *Normality of HCl used*31)/1000*1N = _____ g of Na2O
[Note: 80g of NaOH corresponds to 62g of Na2O]
Percentage of Total alkali = __________%

Fatty Matter

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Weight of china dish = __________ g
Weight of fatty matter + china dish = __________ g
Amount of fatty matter = _________ g
Percentage of fatty matter = ______ %

ANALYSIS OF OIL

DETERMINATION OF SAPONIFICATION VALUE OF OIL

Exp. No.6 Date:

Aim
To determine the amount saponification value of the given oil.

Principle
Oils and fats are the triesters of the fatty acids and trihydroxy
alcohol, glycerol. Saponification is the alkaline hydrolysis of esters
resulting in the formation of soap. The saponification value of an oil is
defined as the number of milligrams of potassium hydroxide (alkali)
required to neutralise the fatty acids resulting from the complete
hydrolysis of 1 g of the sample.
C 3 H 5 ( C 17 H 35 COO )3+ 3 KOH → C3 H 5 ( OH )3 +3 C 17 H 35 COOK
Stearin Glycerol Potassium
stearate

The esters of the fatty acids of lower molecular weight require

more alkali for saponification, so the saponification value is inversely
proportional to the mean of the molecular weights of the fatty acids in
the glycerides present. Saponification value is useful for detecting the
presence of oil and fats which contain a high proportion of lower fatty
acids.
Apparatus

19
Bulb condensers, Erlenmeyers flasks (50-300 ml depending on sample size), water bath,
Pipettes and Burette.
Reagents
Standard solution of Na2CO3
0.5N HCl standard solution
0.5N Ethanolic potassium hydroxide standard solution
[Weigh 35 g of KOH, dissolve in 20 ml of water and then make up to 1000 ml with 95%
(v/v) ethanol or absolute alcohol].
Indicator Phenolphthalein
[Take 1 g of phenolphthalein and make up to 100 ml with 95% ethanol]
Indicator Methyl orange
[Take 0.05 g of methyl orange dissolve it in 100 ml of distilled water]

Procedure
1. Standardise the HCl solution with standard Sodium Carbonate solution.
2. Take 0.2 to 0.5 g of oil in a 50-100 ml Erlenmeyer flask.
3. Add 10 ml of 0.5N ethanolic potassium hydroxide solution and mix.
4. Heat at 80-85°C in a water bath for 30 min.
5. Cool to 30-40°C and titrate against 0.5N HCl standard solution (Add 2-3 drops of
indicator).
6. Carry out a blank test (without oil).
Result
The saponification value of the given oil sample is found to be =___________ .

20
Standardization of HCl
Standard Na2CO3Vs HCl
Indicator Methyl Orange
Volume of Burette Reading(ml)
Sodium
S. No. Carbonate(ml) Initial Final Volume of HCl(ml)

Calculations
Volume of Na2CO3, V1 = 10ml
Normality of Na2CO3, N1 =________N
Volume of HCl, V2 = ________ml
Normality of HCl, N2 =V1*N1/V2 = _________ N

Determination of Saponification value

Sample/Blank Vs Std. HCl
Indicator: Phenolphthalein
Burette Reading(ml)
S. No. Titrant(ml) Initial Final Volume of HCl(ml)
1 Blank A

21
 2 Sample B

( A−B) x 56.11 x Normality of HCl

Saponification value (mg/g) =
Weight of the Oiltaken

ESTIMATION OF IODINE VALUE OF OIL

Exp. No.7 Date:

Aim
To determine the amount of unsaturation present in the given oil (To determine the iodine
value of an oil).

Principle
Unsaturated compounds absorb iodine ( in suitable form) and
form saturated compounds. Iodine value is expressed in grams of
iodine absorbed by 100 g of oil or fat. Iodine value is a measure of the
degree of unsaturation of the constituent fatty acids in an oil or fat.
When a halogenating agent is treated with an unsaturated oil , the
halogen get added into the double bond quantitatively and convert it
into saturated molecule. From the amount of halogenating agent used
the extent of unsaturation in the oil is calculated.
NOTE: No oil has zero iodine value and oils are classified as drying, semi drying and non
drying on the basis of iodine value. Oleic acid containing 1 double bond absorbs 90% of
iodine, linoleic acid (2 double bonds) absorbs 181% iodine and linolenic acid (3 double
bonds) absorbs 274% iodine. Non drying oils have 1 double bond and absorbs iodine
below 90%. Semi drying oils contain some proportion of double bonds and have iodine
value below 140. Iodine value for coconut oil is about 8, for olive oil about 88, and for
linseed oil is about 200.

22
Procedure
Standardisation of Thio
1. Pipette out 20 ml of 0.1 N potassium dichromate solution into a clean conical flask.
2. Add 1 test tube of dilute H2SO4 and 10 ml of KI solution to the conical flask.
3. Titrate against thiosulphate from the burette until it turned into pale yellow.
4. Add 1 ml of starch indicator and titrate against thiosulphate solution.
5. End point is disappearance of blue color.
6. Repeat the titration for concordant value.
Estimation of Iodine Value
1. Weigh 1ml of oil and transfer into Iodine flask.
2. Add 10 ml of carbon tetrachloride to dissolve the oil and warm slightly and cool for 10
minutes.
3. Add 25 ml of Wij’s solution in the same flask and shake vigorously.
Note: Wiji’s solution is Iodine monochloride in acetic acid used as a halogenating agent
for unsaturated molecules.
4. Allow the flask to stand for half an hour in dark place.
5. Add 10 ml of KI solution and titrate the solution against 0.1 N Sodium thiosulphate
solution until the appearance of yellow color.
6. Add 1 ml of starch indicator and continue the titration against the sodium thiosulphte
solution from the burette.
7. Disappearance of blue color indicates end point.
Result:
The iodine value of the given oil sample is found to be =___________ .

Standardization of Na2S2O3 (Thio)

Standard Potassium dichromate Vs Na2S2O3
Indicator:Starch

23
 Volume of Burette Reading(ml) Volume of Thio
S. No. K2Cr2O7(ml) Initial Final (ml)

Determination of Iodine value

Sample/Blank Vs Std. Na2S2O3
Indicator: Starch
Volume of titrant Burette Reading(ml)
+
Wij’sSolution(ml Volume of
S. No. ) Initial Final HCl(ml)
1 Blank A
2 Sample B

CALCULATION

( B− A) x 127 x Normality of Thio

Iodine value of the given oil =
Weight of the Oil taken

Equivalent weight of Iodine -127

24
 ANALYSIS OF BLEACHING POWDER
Exp. No.8 Date:

Aim
To determine the available chlorine in the given bleaching powder sample.

Principle
Bleaching powder consist of essentially a mixture of calcium hypochloite CaOCl2
and the basic chloride Ca(OH)2, H2O, CaCl2, some free slaked lime, is usually
present. The active constituent is hypochlorite, which is responsible for bleaching action.
The available chlorine refers to the chlorine liberated by dilute acids and is expressed as
percentage weight of the bleaching powder. The following reaction takes place when
heated with dilute acid.
CaO Cl 2 +2 HCl → CaCl 2+ H 2 O+Cl 2

When bleaching powder suspension is treated with an excess solution of KI and strongly
acidified with acetic acid/sulphuric acid. The reaction is
+ ¿+I 2 + H 2 O ¿

CaO Cl 2 +2 KI +2 H + ¿→Ca Cl +2 K
2 ¿

25
The liberated iodine is titrated against standard Na 2S2O3 (sodium thiosulphate/thio)
solution. From the amount of Iodine liberated the amount of bleaching powder and hence
the chlorine equivalent of that is calculated.
Note: The thio solution should not be acidified with HCl, as it may react with CaOCl 2 that
may be present in the sample, in the presence of Kl and will liberate additional amount of
I2 This may lead to higher estimation of available Cl2.

Procedure
1. Standardization of Na2S2O3:
Prepare 100ml of exactly N/10 K2Cr2O7 solution.
Pipette out 10 ml of this solution into a clean conical flask.
Add 10ml of dil. HCl and 10ml of 10% KI solution.
Titrate the liberated I2 against sodium thio sulphate solution. When the colour of the
solution becomes pale yellow add starch indicator continue the titration until the colour
changes from blue to colorless.
2. Standardization of available chlorine:
Weigh accurately about 0.5g of a fresh bleaching powder in a weighing bottle. Transfer to
a mortar, add 2ml of water and grind to a smooth paste.
Quickly transfer it into a 250ml standard flask make upto the mark.
Pipette out 20ml of this solution into a clean conical flask.
Add 10ml of the dilute acid and 10ml of 10% Kl solution, titrate against standard thio
solution.
Add starch indicator near the end point. The end point is the disappearance of blue colour.
Result
Percentage of available chlorine present in the given sample of bleaching powder is
______ .

26
Calculations
Standardization of thio
10ml standard K2Cr2O7 + 10m of dil. H+ + 10ml of 10% Kl
Vs Sodium thio Sulphate
Indicator: Starch

Volume of K2Cr2O7, V1=10ml

Normality of K2Cr2O7, N1 = __________N
Volume of Na2S2O3,V2 = __________ml
Normality of Na2S2O3, N2 = V1N1/V2 =__________N
Determination of available chlorine
Weight of bleaching powder = __________ g
20ml of bleaching powder solution + 10ml of H+ + 10ml of 10% Kl
Vs Sodium thio sulphate
Indicator: Starch

27
Volume of K2Cr2O7, V1=10ml
Normality of K2Cr2O7, N1 = __________N
Volume of bleaching solution, V2 = __________ml
Normality of bleaching solution, N2 = V1N1/V2 =__________N
Amount of available chlorine = Normality of bleaching solution × 35.5

% of available chlorine =
Normality of bleaching solution×35.5 X 10
Weight of bleaching powder taken
ANALYSIS OF CEMENT

DETERMINATION OF SILICA CONTENT IN CEMENT

Exp.No:9 Date:

Aim
To estimate the silica content present in the given cement sample.

Apparatus / Reagents required

1:1 HCI solution, Watmann Filler paper No. 40, china dish, silica crucible and
standard flask.

Principle
Cement is a mixture of oxides. The oxides dissolve in concentrated Hydrochloric acid and
leaves silica as suspended matter. The soluble oxides generally contains oxides of
aluminium, iron and calcium. The insoluble silica is filtered and weighed to find the
percentage of silica in the given cement sample.

28
Procedure:
1. Weigh about 1g of the given cement sample and transfer into a beaker.
2. Add half test tube of water and test tube of 1:1 HCl and evaporate it to dryness on
a hot plate.
3. A duplicate analysis can also be performed side by side.
4. Dissolve the content in two test tube of water and digest it for 10 minutes.
5. Filter the contents using whatmann 40 filter paper and wash the residue formed
with hot water, to remove the yellow stains.
6. Dry the residue and incinerate it in a preweighed crucible using a furnace.
7. Cool and weigh the crucible.
8. The difference in weight gives the weight of silica in the cement sample.
9. Calculate it to percentage weight.

Calculations
Weight of cement = S = ____ g
Weight of silica crucible = A = ____ g
Weight of silica crucible with silica residue = B =____ g
Weight of silica in cement =B-A=_____ G
( B− A)×100
Percentage of silica in the cement sample =
S

Result
The percentage of silica in the given cement sample is ________ .

29
 DETERMINATION OF MIXED OXIDE CONTENT IN CEMENT

Exp.No:10 Date:

Aim
To determine the mixed oxide (aluminium and iron oxides) of the given cement sample.

Apparatus / Reagents required

1 : 1 HCI solution, NH 4 Cl, NH 4 OH, watmann Filler paper No. 40, China dish,
silica crucible and standard flask.

Principle
Cement is a mixture oxides of calcium, aluminium, iron and silica. The oxides dissolve in
concentrated hydrochloric acid and leave silica as residue. The filtrate contains
aluminium, iron and calcium oxides. Aluminium and iron oxides in the filtrate can be
precipitated as hydroxides using ammonium hydroxide. The precipitate upon strong

30
heating produce the respective oxides. The filtrate may be used for calcium oxide analysis
of cement.
Al2O3+4NH4OH → 2Al(OH)3 +4NH3+H2O
Fe2O3+4NH4OH → 2Al(OH)3 +4NH3+H2O

Procedure
The filtrate obtained in the silica estimation of cement is collected and made upto 250ml in
a standard flask.
Pipette out 20ml of the solution into a beaker, add 2g of NH4Cl and boil for 5-10 minutes.
Add NH4OH in excess to make the solution alkaline and digest the contents for 5 minutes.
A pale brown jelly precipitate is obtained.
Cool the precipitate and filter through a whatmann 41 filter paper.
Wash the precipitate with hot water and incinerate in a prewighed silica crucible. Cool
and weigh the crucible.
Using the difference in the weight, the amount of aluminium and iron oxides present in the
sample can be calculated.
Calculate it to percentage wight.

Calculations
Weight of cement = S = ____ g
Weight of silica crucible = A = ____ g
Weight of silica crucible with mixed oxide residue = B =____ g
Weight of mixed oxide in cement =B-A=_____ G
( B− A)×100
Percentage of mixed oxide in the cement sample =
S

Result
The percentage of mixed oxides in the given cement sample is ________ .

31
 DETERMINATION OF CALCIUM OXIDE CONTENT IN CEMENT

Exp.No:11 Date:

Aim
To determine the mixed oxide (aluminium and iron oxides) of the given cement sample.
Apparatus / Reagents required
1 : 1 HCI solution, NH 4 Cl, NH 4 OH, whatman Filler paper No. 40, china dish,
silica crucible and standard flask.

Principle
Cement is a mixture oxides of calcium, aluminium, iron and silica. The oxides dissolve in
concentrated hydrochloric acid and leave silica as residue. The filtrate contains
aluminium, iron and calcium oxides. Aluminium and iron oxides in the filtrate can be
precipitated as hydroxides using ammonium hydroxide. The precipitate upon strong

32
heating produce the respective oxides. The filtrate collected is treated with ammonium
oxalate solution to precipitate calcium oxalate. Calcium oxalate upon strong heating gives
calcium oxide.

CaCl2+(NH4)2C2O4 → CaC2O4 +2NH3+2HCl

Procedure
Prepare ammonium oxalate solution by dissolving 1g of ammonium oxalate crystal in
10ml of boiling water.
Filter the solution and make use of the filtrate as oxalate solution.
Make up the filtrate collected in the analysis of mixed oxide in cement upto 250ml in a
standard flask.
Pipette out 20ml of the solution into a beaker, add the oxalate solution to obtain white
precipitate of calcium oxalate.
Filter the precipitate through whatman 40 filter paper and wash the residue with hot water.
Dry the residue and incinerate the residue in a preweighted silica crucible.
From the difference in weight, the percentage of calcium oxide can be calculated.

Calculations
Weight of cement = S = ____ g
Weight of silica crucible = A = ____ g
Weight of silica crucible with calcium oxide residue = B =____ g
Weight of calcium oxide in cement =B-A=_____ g
( B− A)×100
Percentage of calcium oxide in the cement sample =
S

Result
The percentage of calcium oxide present in the given cement sample is
________.

33
 DETERMINATION OF FLASH AND FIRE POINT

Exp. No.12 Date:

Aim
To determine the flash and fire point of the given fuel/lubricating oil and their mixture
using Pensky Martin’s flash point apparatus.

Principle
The lowest temperature at which a product gives just sufficient vapor to form an
inflammable mixture with air under the conditions of standard test is called flash point.
The temperature of a liquid fuel that gives off enough vapour to support continuous
combustion is called as fire point. The flash and fire point can be determined using pesky
martin’s closed cup apparatus. A sample of oil is heated in a closed vessel until a

34
temperature is reached at which the vapor in the air space above are sufficient to form an
inflammable mixtures and ignite when a flame is applied. The flash thus determined is the
closed flash point. If the test is carried out with the some sample cup uncovered.An open
flash point is determined. On further heating a temperature is reached at which the
combustion will continue for a few seconds, it is called fire point.

Apparatus
Pensky Martin’s flash point apparatus, stirrer, thermometer and beakers.
Description of Apparatus:
It is used for oils having flash point of about 120 degree Fahrenheit. It consists of an oil
cup with an indicator marked around the interior provided with a lid carrying the
thermometer. There are three opening in the lid: 1. For admitting the test flame. 2. For
thermometer 3. For observing the flash. The cover of the lid is operated by a spring
handle passing through the lid into the stirrer consisting of two – propeller maintained on
the steel shaft.

Procedure

1. Fill the oil cup with the given fuel oil to the indicated level and place the lid on the
of cup and set in the burner.
2. Introduce the thermometer in the opening provided.
3. Adjust the test flame in size to about 0-16”.
4. Apply the Heat at a constant rate of not less than 90 o F and not more than 110 o F.
Rotate the stirrer at a rate of 1-2rps.
5. Record the flash point temperature at which the distinct flash becomes visible in
two observation ports.
6. To determine the fine point, continue heating at a specified rate of 90 o F to 110o F
per minute.
7. Apply the test flame at specified intervals.

35
 8. Repeat the above procedure until the oil gets ignited and continue to burn for a
period of 5 seconds.
9. Note the corresponding thermometer reading.

Result
The flash and fire points are found out for fuel and their mixtures. The graph is plotted
with the percentage of fuel against the flash point.
The flash point of the unknown fuel mixture = _________oC
The fire point of the unknown fuel mixture = __________oC

DETERMINATION OF CLOUD AND POUR POINT

Exp.No:13 Date:

Aim
To determine the cloud point and pour point of the given lubricating oil/liquid fuel.

Principle
The pour point of a liquid is the temperature below which the liquid loses its flow
characteristics. When a petroleum or a lubricating oil is cooled slowly under specified
condition, it will form a hazy appearance at a particular temperature. The temperature is
known as cloud point. Upon further cooling the oil, the oil ceases/stops to flow at a
temperature, which is referred as pour point. High pour point of liquid fuel is generally

36
associated with a high paraffin wax content. Cloud and pour points indicate the suitability
of lubricants in cold conditions.

Apparatus required
Cloud and pour point apparatus, stirrer, thermometer and beakers.

Procedure
A cloud point apparatus basically consists of a flat bottom tube enclosed in an air jacket.
The jacket is surrounded by freezing mixture(ice + CaCl2) contained in a jar.
Fill half of the tube with the oil under test and introduce a thermometer into the oil. Cool
the oil slowly with the freezing mixture. As the oil is cooled slowly, withdraw the tube
from the jacket for a moment and examine for hazy appearance. Record the temperature
at which cloudiness appears as cloud point of the oil. Continue the examination by tilting
the tube and checking until the oil ceases to flow. Record the temperature as pour point of
the oil.

Result
1. The cloud point of the given lubricating oil = _______°C.
2. The pour point of the given lubricating oil = _______°C.
ABSORPTION SPECTROMETRY
VERIFICATION OF BEER-LAMBERT’S LAW
Exp.No:14 Date:

Aim
To verify Beer-Lambert’s law.
Principle
Atoms and molecules absorb UV/Visible radiation of
electromagnetic radiation, based on their electronic structure. The
wave length of absorption can be found using a spectrophotometer or a
colourimeter. According to Beer Lambert’s law the relation between
absorbance(A), a measure of relative intensity of light absorbed at a

37
 given wavelength, the concentration of the molecules in solution (c )
and path length (d in cm) of light in solution are mathematically given
as A = Ɛcd, where Ɛ is the molar extinction coefficient of the
molecule under analysis. The Ɛ value is the characteristic value for a
given molecule and d is a constant for the given instrument ( usually
1cm).
The law is verified by plotting the A values of different concentrations of same analyte
under study against the concentration values.

Procedure
1. Prepare a known concentration (0.1M) solution of CuSO4.
2. Prepare atleast five dilutions of the above bulk solution using distilled water in standard
measuring flasks of 25ml.
3. Take 1 ml each of known solutions of copper sulphate and treat with 1 ml of ammonia
individually in 100ml standard flasks. Make up the CuSO 4 +NH3 complex solution upto
100ml in each of the standard flask. Mix the solutions for uniformity.
4. Calibrate the colorimeter/spectrophotometer set to zero absorption using distilled water
in the sample holder.
5. Take 2ml of one of the CuSO 4 complex solution prepared in the sample holder and do
wavelength scan, in the spectrophotometer/colorimeter. Tune the monochromator to light
rays of wavelengths 400-700nm one by one and note the wavelength (λ max)of maximum
absorption (620nm).
Note: The filters in the spectrophotometer/ colourimter are to be set accordingly, as
wavelength is changed.
6. Set the filter/monochromator as per the wavelength of maximum absorption.

38
7. Take 2ml of each of the above CuSO 4 +NH3 solutions prepared, one by one in the
sample holder/cuvette, keep it in the spectrophotometer/colourimeter and note the
corresponding absorbance values.
8. Plot A Vs c i.e., Absorbance Vs concentration of the solutions on a graph sheet.

S. No. Conc.(c in M) Absorbance(A)

Result
As A is directly proportional to c, a straight line graph of y=mx form confirms Beer
Lambert’s law.
DETERMINATION OF ABSORPTION COEFFICIENT OF A SOLUTION
Exp.No:15 Date:

Aim
To determine the absorption coefficient of the given CuSO4 solution.

Principle
Atoms and molecules absorb UV/Visible radiation of
electromagnetic radiation, based on their electronic structure. The

39
 wave length of absorption can be found using a spectrophotometer or a
colourimeter. According to Beer Lambert’s law the relation between
absorbance(A), a measure of relative intensity of light absorbed at a
given wavelength, the concentration of the molecules in solution (c )
and path length (d in cm) of light in solution are mathematically given
as A = Ɛcd, where Ɛ is the molar extinction coefficient of the
molecule under analysis. The Ɛ value is the characteristic value for a
given molecule and d is a constant for the given instrument ( usually
1cm). For a given solution of known concentration, if the absorbance
value is found using the spectrophotometer/colourimeter, substituting
the d and other known values Ɛ can be calculated.

Procedure
1. Prepare a known concentration (0.1M) solution of CuSO4.
2. Prepare atleast five dilutions of the above bulk solution using distilled water in
standard measuring flasks of 25ml.
3. Take 1 ml each of known solutions of copper sulphate and treat with 1 ml of ammonia
individually in 100ml standard flasks. Make up the CuSO 4 +NH3 complex solutions upto
100ml in each of the standard flask. Mix the solutions for uniformity.
4. Calibrate the colorimeter/ spectrophotometer set to zero absorption using distilled water
in the sample holder.
5. Take 2ml of any one of the CuSO 4 +NH3 complex solution prepared in the sample
holder and do wavelength scan, in the spectrophotometer/colorimeter. Tune the
monochromator to light rays of wavelengths 400-700nm one by one and note the
wavelength (λmax) of maximum absorption (620nm).
Note: The filters in the spectrophotometer/ colourimter are to be set accordingly, as
wavelength is changed.
6. Set the filter/monochromator as per the wavelength of maximum absorption.
7. Take 2ml of each of the above CuSO 4 +NH3 solutions prepared, one by one in the
sample holder/cuvette, keep it in the spectrophotometer/colourimeter and note the
corresponding absorbance values.

40
8. For every values of A obtained, substituting the value of A, c and d, calculate the value
of Ɛ. Find the average of the Ɛ values obtained.

Molar absorption
S. No. Conc.(c in M) Absorbance(A)
coefficient(Ɛ)

Average value of Ɛ =_____________

Result
The absorption coefficient of the given CuSO 4 + NH3 complex solution = ____________
M-1cm-1.

DETERMINATION OF ABSORPTION COEFFICIENT OF DYE

SOLUTIONS
Exp.No:16 Date:

Aim
To determine the absorbance the given dye solutions.
Principle

41
Molecules absorb UV/Visible radiation of electromagnetic radiation, based on their
electronic structure. The wavelength of absorption depends on the energy required for the
electronic excitation in the molecule. Dyes are coloured organic substances, they usually
due to the presence of П electrons and/or due to the presence of non bonded electrons in
their structure undergo electronic excitation like П→П*, n→П* by absorbing UV/Visible
radiation. The wave length of absorption is shifted based on the number of pi bonds and n
electrons. The wavelength of absorption unique characteristic for the particular type of
bond interaction in a molecule, can be found using a spectrophotometer or a colourimeter.
Procedure
1. Prepare various known dilute solutions of the given dye (water
soluble) in distilled water.
2. Calibrate the colorimeter/ spectrophotometer set to zero
absorption using distilled water in the sample holder.
3. Take 2ml any one the dye solution prepared in the sample holder
and do wavelength scan, in the spectrophotometer/colorimeter.
Tune the monochromator to light rays of wavelengths 400-
700nm one by one and note the wavelength of maximum
absorption.
Note: The filters in the spectrophotometer/ colourimter are to be set accordingly, as
wavelength is changed.
4. Set the filter/monochromator as per the wavelength of maximum absorption.
5. Take 2ml of each of the above dye solutions prepared, one by one in the sample
holder/cuvette, keep it in the spectrophotometer/colourimeter and note the corresponding
absorbance values.
6. Repeat the same procedure for the other dyes given.
S. No. Λmax(nm) Conc.(c in M) Absorbance(A)

Dye 1

Dye 1

42
Dye 3
Result
The characteristic absorption wavelength and the absorbance values of the given dyes are
found and tabulated.

43