2020 21 Ec Lab Manual Student Version

ENGINEERING CHEMISTRY LABORATORY
MANUAL (A2 Regulation)

<<
Name
Regd. No
By
DEPARTMENT OF CHEMISTRY
Maharaja Vijayaram Gajapathi Raj College of Engineering (Autonomous)

(Approved by AICTE, New Delhi and permanently affiliated to JNTUK)
Chintalavalasa, Vizianagaram -535005
Engineering Chemistry lab manual 2020-21
INDEX
Subject Name: Engineering Chemistry Lab Subject Code: A2CYI101
Name: Dept.: Reg. No:
S. No Experiment Date Signature Grade

1 Introduction to engineering chemistry laboratory –
Molarity, Normality, Primary, Secondary Standard
solutions, Volumetric titrations, Quantitative and
Qualitative analysis etc.,
2 Determination of concentration of a strong acid HCI
using standard Na2CO3 solution.
Cycle I
3 Determination of strength of an acid in Pb-Acid battery.
4 Estimation of calcium oxide in port land Cement.
5 Determination of Total Hardness of water using
standard EDTA solution.
6 Preparation of a polymer.
7 Preparation of nano materials.
8 Adsorption of acetic acid by charcoal.
9 Determination of acid number and saponification
number of a test sample of lubricating oil.
Cycle II
10 Determination of iron (Fe+3) with potassium thiocyanate
(KSCN) (Spectrophotometer).
11 pH metric titration between strong acid and strong base
(pH metery).
12 Strong acid and strong base (Conductometric
Titrations).
12 Weak acid and strong base (Conductometric Titrations).
13 Determination of Ferrous iron with standard K2Cr2O7
solution by Potentiometric titration method
(Potentiometric titration).
14 Determination of viscosity of polymer solution using
survismeter.
15 Project based learning
16 Grade average
Faculty Signature
M V G R College of Engineering (Autonomous), Vizianagaram. Page 1

S. No. CONTENTS Page. No.

1 Index 1
2 Introduction to Engineering chemistry laboratory – Molarity, Normality,
Primary, Secondary Standard solutions, Volumetric titrations, 3-4
Quantitative and Qualitative analysis etc.,
3 Essential conditions for accurate titrimetry. 4
4 Terms used in volumetric analysis. 4-8
5 Classification of reactions in volumetric analysis. 8-9
6 Laboratory safety. 9
5 General safety precautions. 9-10
7 Waste disposal. 11
8 Instructions to the students 12
9 Instructions to write lab record 13
10 Undertaking by the student 14
11 Determination of concentration of a strong acid HCI using standard 15-20
Na2CO3 solution.
12 Determination of Strength of an acid in Pb-Acid battery. 21-29
13 Estimation of calcium oxide in port land Cement. 30-40
14 Determination of Total Hardness of water using standard EDTA solution 41-48
15 Determination of iron (Fe+3) with potassium thiocyanate (KSCN) using
49-56
Spectrophotometer.
16 pH metric titration between strong acid and strong base (pH metry). 57-70
17 Strong acid and strong base (Conductometric Titrations).
71-87
18 Weak acid and strong base (Conductometric Titrations).
19 Determination of ferrous iron with standard K2Cr2O7 solution by
88-98
Potentiometric titration method (Potentiometric titration).
20 Determination of acid number and saponification number of a test 99-108
sample of lubricating oil.
21 Preparation of a polymer. 109-113
22 Determination of viscosity of polymer solution using survismeter. 114-119
23 Adsorption of acetic acid by charcoal. 120-129
24 Preparation of nano materials. 130-136
25 Project based learning. 137-140

INTRODUCTION TO CHEMISTRY LAB
Chemical analysis is carried out to understand the composition of the materials. This will
enable to assess the properties of materials and if necessary, modify the properties for technical
and scientific applications. Chemical analysis is the resolution of a chemical compound into
proximate or ultimate parts. Traditional manual chemical analysis is divided into two types.
a. QUALITATIVE ANALYSIS: It deals with the identification and confirmation of the nature of
the substance or impurities present in a given sample.
b. QUANTITATIVE ANALYSIS: It deals with the estimation of, how much of each component or
of specified components, are present in a given sample, including in trace quantities. The
substance determined is analyte and the minor or the trace quantities are impurities. The
complete quantitative analysis consists of five steps: sampling, dissolution of the sample,
conversion of the analyte into a form suitable for measurement, measurement, calculation
and interpretation of data.
Quantitative chemical analysis is further divided into two types:
a. VOLUMETRIC ANALYSIS: It is based on a chemical reaction and the calculations are on the
simple stoichiometric relations of chemical reactions. It is a quantitative chemical analysis by
measure, which consists essentially in determining the volume of solution of accurately
known concentration required to react quantitatively with solution of substance being
determined. The weight of the substance to be determined is then calculated from the
volume of the standard solutions and the known laws of chemical equivalence/
stoichiometry. The standard solution is usually added from a graduated glass vessel called a
burette. The process of adding the standard solution until the reaction is just complete is
termed as a titration and the substance to be determined is said to be titrated. Hence, this is
also referred to as titrimetric analysis. The point at which the titration is completed is called
the equivalence point or the theoretical (stoichiometric) endpoint. The completion of the
titration should, as a rule, be detectable by some change, unmistakable to the eye, produced
by the standard solution itself or more usually by the addition an auxiliary agent, known as
indicator. The indicator should give a clear visual change in the solution being titrated. In the
ideal titration, the visible endpoint will coincide with the stoichiometric or theoretical
endpoint. However in practice, a very small difference usually occurs, referred to as titration
error. Volumetric analysis, which involves the accurate measurements of volume of

solutions, though one or two weighing’s may also, be needed. The indicator is a chemical
substance and choice of the indicator depends on the nature of the chemical reaction.
Volumetric methods need simpler apparatus and the processes are quickly performed. They
require a balance for weighing, calibrated measuring vessels like burettes, pipettes and
volumetric flasks and substances of known purity for the preparation of standard solutions.
b. GRAVIMETRIC ANALYSIS: Unlike volumetric analysis where measurements of volumes are
involved, gravimetric method involves separation of the analyte into a solid form as
precipitate. The measurement step in gravimetry is weighing. The element or a definite
compound of the element in as pure form as possible, is isolated and weighed. The weight of
the element or compound may then be readily calculated from the formula knowledge of the
compound and the atomic weights of the constituent elements. The isolation of the required
species is achieved by precipitation methods, volatilization, evolution methods or electro
analytical methods.
The advantage of gravimetric method over volumetric analysis is that the constituent
may be seen and examined for the presence of impurities. A correction can be applied if
necessary. The disadvantage of gravimetry is that it is more time consuming compared to
volumetric analysis. Of the two methods, gravimetric analysis is accurate, but volumetric
analysis is much more readily and quickly carried out. The error allowed in volumetric
analysis is 0.2%.
ESSENTIAL CONDITIONS FOR ACCURATE TITRIMETRY
1. Clean glass apparatus must only be used in titrimetric analysis. Glass apparatus must be free
from grease and thoroughly rinsed with distilled water and dried in an oven before use.
Graduated apparatus need not be dried in oven, as they may cause error due to expansion.
2. The stoichiometric equation governing the reaction must be known.
3. The reaction should be practically instantaneous or proceed with sufficient speed. Addition
of a suitable catalyst may help to increase the speed of the reaction. The reaction must go to
completion, without any complicating side reactions.
4. There must be some marked change in some physical or chemical property of the titrate to
assess the completion of the reaction (usually an indicator is employed).
5. An indicator should be available, which should sharply define the end point of the reaction.
6. The standard solution must not alter in its strength during the period of experimentation.
The solution must be stable to light, atmosphere and must not react with the solvent or
containers.
7. The balance must be accurate, stable, and sensitive and give the same result in successive
weighings. Calibrated weights must be used. If a digital balance is used, its operation must
be fully understood and proper care be taken to obtain accurate results to the specified
decimals.
TERMS USED IN VOLUMETRIC ANALYSIS

a. TITRATION: It is a process of adding one solution from the burette to another known
volume of solution in a conical flask, in order to complete the chemical reaction. Out of
the two solutions one must be standard i.e., whose concentration is known by
preparation or by previous standardization.
b. TITRANT: The reagent being added through a burette is called as titrant.
c. TITRATE: The substance being titrated in the reaction vessel is termed as Titrate.
However, these terms titrant and titrate are relative.
d. EQUIVALENCE POINT or STIOCHIOMETRIC END POINT: It is the point at which the
amount of reagent (titrant) and substance (titrate) being determined are
stoichiometrically equivalent according to the equation representing the chemical
reaction or it is the exact stage at which the chemical reaction involved in the titration is
just complete.
e. INDICATOR: The substance which helps in the visual detection of the completion of the
reaction in the titration is known as indicator.
f. PIPETTE: A glass apparatus with which a fixed volume of solution as marked on the
pipette can be delivered. It should be previously rinsed with the solution of titrate
Solution is drawn by suction above the mark and the end is closed with pointing finger
tightly, with three fingers on one side and thumb on the other side. By slow release of
pointing finger, the level is adjusted to the mark and transferred into the titration vessel.
Care must be taken to see that air bubbles are not present while drawing solution and
the solution drop in the nozzle is never released by blow off.
g. BURETTE: Burettes are long cylindrical tubes of uniform bore throughout the graduated
length with a closed bottom with stop cock and nozzle at the end. Titrant is filled into the
burette including the nozzle and clamped to the stand vertically for five minutes before
use, to eliminate air bubbles, if any. Initially the burette is filled with titrant up to its zero
mark. The stop cock can release solution as a continuous flow, but gentle operation will
enable drop wise addition. Burette releases sufficient measured volume of solution into
the titration vessel till the reaction is complete as indicated by change in color of
indicator. The volume released can be noted immediately as titer value. The reading of
the lower meniscus coinciding with graduation will be taken as the burette reading.
Burette should be fixed in stand and clamp vertically during and after use.
h. CONICAL FLASK: It is the reaction vessel containing titrate and indicator solution in
distilled water. It should be rinsed with distilled water only before and after each
titration.
i. WEIGHING BOTTLE: This is used to weigh a required quantity of specified solid for
preparing standard solutions. The difference in weights before and after use gives the
weight of the substance transferred.

j. ANALYTICAL BALANCE: It is a two pan balance with graduated beam holding aluminum
rider. It is closed on all sides to prevent air disturbances and all weighings must be
carried out while closing these windows. Gentle lifting of the bottom knob will lift the
beam to give free oscillations of the attached pointer within the scale. Before weighing, it
should show equal oscillations on both sides of the scale failing which; the help of
teacher in charge may be sought. No part of balance must be touched, while the beam is
raised with knob and it is on free oscillations. Usually the balance is supplied with a
weight box having weights 200g to 1 g and fractional weights of 500mg to 10mg. The
weights should be handled with forceps only otherwise errors in weights are likely to
interfere. Its accuracy is up to 0.1 mg. i.e., to fourth decimal place of a recorded weight.
Digital balance can also be used for specific decimal places. A digital balance gives direct
reading of weight to specified decimal places on the panel.
k. MEASURING CYLIDER OR JAR: This is a graduated cylindrical glass vessel to draw

approximate volumes of solution.
l. VOLUMETRIC FLASK: This is a stoppered glass vessel with flat bottom and pear shape
with a long narrow neck containing a thin line mark etched on the neck. The volume
specified on the flask is up to the mark only. This is used to prepare solutions with
definite concentrations.
m. PORCELAIN TILE: A ceramic plate of 6”x6” size glazed white on one side and placed
under the conical flask or any titration vessel during titration, which helps for better
detection of colour change at the equivalence point.
n. END – POINT: The point at which the colour change of the indicator is visible is called
the end point. Since this depends upon the sensitivity of the eye, the appearance of the
first change in the faint color must be noted carefully, lest errors should creep into the
measurement of volumes of solutions. A glazed white porcelain tile or a white paper in
the back ground of the titration vessel will improve the visibility of the color change in
observing and recording the end point accurately.
o. TITRATION ERROR: Ideally, the visible end – point and the equivalence point should
coincide, but in practice there is always a difference between the two, this difference
being called the titration error. It is because the color change of indicator takes place
only after the completion of the chemical reaction and addition of small excess of the
titrant. Also it is possible that the indicator itself may also cause or join the chemical
reaction.
Many errors occur due to analyst or method or reagent or uncalibrated glassware and
interference of the indicator. To avoid these errors statistical treatment of the titration values is
necessary. Hence, ‘Most Probable value’ is taken as the result.
MOST PROBABLE VALUE: Even when a quantity is measured with possible accuracy, the
results of a successive observation differ among themselves. The average value of these results
is taken as most probable value. Hence, it is not a true value.

ABSOLUTE ERROR: The difference between observed or measured value to a true or most
probable value is known as absolute error. It is measure of accuracy.
ACCURACY: It is the concordance between measured value and most probable value or true
value.
PRECISION: Precision is a measure of reproducibility of measurements.
If the values are accurate, they may be precise, but if they are precise, they may not be
accurate.
STANDARD SOLUTION: A solution of known strength is called as standard solution. It is

prepared by dissolving a definite weighed amount of the substance in a small volume of solvent
in a volumetric flask of prescribed volume. It is dissolved and made up to the mark in the
volumetric flask in the total volume being as stipulated on the volumetric flask. Later it is
thoroughly made homogeneous before use and every reuse by shaking for uniformity in
concentration.
PRIMARY STANDARD SUBSTANCE: A Primary Standard Substance should satisfy the

following requirements.
a. The substance used as a primary standard should be available in a state of high purity
and preserved in a pure state. It is known as Analytical Reagent or AR grade.
b. The substance should maintain its composition during storage and unaltered in air
during weighing. It should be neither oxidized by air nor effected by carbon – dioxide.
c. It should not be hygroscopic, deliquescent or efflorescent.
d. The total amount of impurities should not in general, exceed to 0.01 to 0.02%. The
impurities to the trace level must be specified to take necessary precautions to avoid
possible interferences.
e. It is preferred to have high equivalent weight, so as to minimize the errors in weighing.
f. The substance should readily be soluble under the conditions in which it is employed.
In practice an ideal primary standard is difficult to be obtained and a compromise in the

above ideal requirements may be necessary.
PRIMARY STANDARD SUBSTANCES COMMONLY EMPLOYED:
In acidimetry and alkalimetry: Sodium carbonate (Na2CO3), Borax (Na2B4O7. 10H2O), and
Potassium hydrogen phthalate (KHC8H4O4) etc.

In precipitation titrations: Sodium chloride, Potassium chloride, etc.
In oxidation-reduction titrations: Potassium dichromate, sodium oxalate, arsenium oxide etc.
In Complexometric titrations: Zinc sulphate solution
SECONDARY STANDARD SUBSTANCES: Those substances which do not loose water of

crystallization such as sodium bicarbonate, ferrous ammonium sulphate, copper sulphate, silver
nitrate etc.
CLASSIFICATION OF REACTIONS IN VOLUMETRIC ANALYSIS:
For convenience sake, reactions in volumetric analysis are classified into four types.
However the classification is not strictly followed and overlap may occur.
1. Neutralization reactions (acidimetry and alkalimetry): These reactions are based on

the principle of neutralization of a free acid or free base. The free bases or those formed
from salts of weak acids by hydrolysis are titrated with a standard acid (acidimetry) or
vice versa (alkalimetry). The basic common reaction involves the interaction of
hydrogen and hydroxyl ions to form water molecule. Selective acid base indicators are
only employed to mark the sudden change in pH during these titrations.
2. Oxidation reduction reactions (redox reactions): These reactions involve a change in
the oxidation number or transfer of electrons amongst the reacting substances. The
standard solutions are oxidizing or reducing agents. The oxidation reduction indicator
should mark the sudden change in the oxidation potential in the neighborhood of the
equivalence point.
3. Complex formation reactions: They involve the combination of ions (other than
hydrogen and hydroxyl ions) to form a soluble, slightly dissociated ion or compound.
Special metallochromic indicators are employed here.
4. Precipitation reactions: They involve the combination of ions (other than hydrogen
and hydroxyl ions) to form a simple precipitate. No change in valency occurs. Special
adsorption indicators help the detection of the equivalence point.
Concentration of a standard solution is generally expressed in following chemical units.
MOLARITY: Molarity of a solution is defined as the number of gram moles of solute present in
one liter of the total solution.
NORMALITY: The normality of a solution is defined as the number of gram – equivalents of

solute present in one liter of the total solution.

Ppm: Parts per million (Ppm) is a better notation for expressing concentrations of trace
quantities of species present. This system is convenient for expressing the concentrations of
very dilute solutions. It specifies the number of parts of solute in one million parts of solution
and is expressed mathematically as
Ppm = w x106/W
Where w is the number of grams of solute and W is no of grams of solvent.
One liter of water at room temperature weighs approximately 106 mg; hence a convenient
relationship to remember is that one milligram of solute in one liter of water is a concentration
of 1ppm. For even more dilute solutions the system parts per billion (Ppb) is employed.
Ppb = w x 109/W
LABORATORY SAFETY
Safety in the laboratory is of the utmost importance. Work carried out within a
laboratory will often involve the use of chemicals and/or equipment which is potentially
harmful to yourself or those working around you; therefore, proper training is required. Most
laboratories will have an explicit standard operating procedure (SOP) associated with a
particular test, piece of equipment etc.
Most companies will have safety training unique to their site which will be mandatory
for all employees. The following section will detail some common safety measures; however, all
personnel should be familiar with the specific safety requirements of the laboratory in which
they work.
GENERAL SAFETY PRECAUTIONS
1. When student entering into in a laboratory you must always:

 Wear eye protection (safety glasses)
 Wear a laboratory coat
 Wear suitable footwear (closed toe shoes)
 Tie long hair back
 Wear appropriate clothing/jewelry
 Follow good hand hygiene protocols
Wear appropriate gloves as needed and change regularly (Note: not all gloves have the
same chemical resistance and specific types of gloves may be needed when handling particular

chemicals. This information can be provided by glove manufacturers) Use barrier creams when
advisable
2. Avoid touching face/eyes when in the laboratory:
 Be familiar with the use and location of eyewash bottles, safety showers etc.,
 Be aware of emergency/evacuation procedures, location and type(s) of
firefighting equipment, fire alarm points, muster/assembly areas
 Know how to call first aiders
 Know how to report an accident/incident
3. In the laboratory you should never:
 Eat
 Drink
 Smoke
 Apply cosmetics
4. Before carrying out any laboratory work make sure that:
 You are familiar with the experiment you are performing
 You know how to use all of the required equipment, glassware, chemicals etc.,
correctly and safely
 You are aware of any hazards associated with the chemicals being used (consult
the appropriate material safety data sheet (MSDS))
 Prepare or read the Experimental Risk Assessment
5. Before leaving the laboratory you must:
 Wash your hands
 Ensure that all equipment is either turned off (if required) or operating correctly
if it will run over night
 If required follow any SOP for leaving experiments/equipment running overnight
 Water taps, gas connections and fans, lights etc., may kindly be switched off when
they are not required
6. The bottles and other apparatus should not be moved from one place to another
unless instructed by teacher. Reagent bottles should be replaced to their original
position soon after use. Otherwise it becomes difficult for another user to trace it.
7. All doors and windows must be kept open while working in the laboratory. Fans and
lights should be switched off, if they are not required.
8. Dry alkalis and concentrated acids should never be touched with hands or spilled over
on the skin. In case it happens, the skin exposed must be washed under tap water
immediately.
9. The test tubes and open vessels are to be heated with caution. The face of the vessel
being heated should not be kept towards your neighboring colleague in lab, as the liquid
inside may be ejected on to his face.
10. Heating must be done gradually and carefully. The articles, test tubes or others for
heating must be dry or wiped dry to prevent breakage.

11. The nozzles of burettes and pipettes must be protected against casual handling resulting
in breakage, as the entire apparatus becomes useless, if its nozzle is broken. If any of the
equipment supplied to you is found cracked or broken, immediately report to the lab in
charge. Never handle the apparatus carelessly or roughly as it may result in damage or
breakage.
12. The glass corks of the volumetric flasks should be tied through a small thread to prevent
mixing of stoppers. Replace caps on bottles immediately after use lest they should be
interchanged.
13. All electrical devices should be plugged in with a dry hand only, preferably with dry
shoes.
14. The balance pan must be clean and dry. Chemicals should not be weighed directly on the
pan of the balance. A watch glass or paper may be used and necessary tare may be made.
15. Students should not sit on the work tables or keep hands for rest on tables for their own
safety.
16. Never return unused solutions or solids to the stock containers as they can contaminate
the stock chemicals.
17. The floor space in the laboratory shall be clean and free from spillage, broken glass or
pieces, straw, cloth pieces or paper to avoid accidents. Leave the laboratory only when
your work bench is cleaned and all the apparatus supplied to you is properly returned to
the lab technician.
18. When fire originates, all gas taps must be cut off immediately.
19. In case of emergency, do not get panicky and be brave enough to handle the situation.
Medical attention should be requested immediately. If skin comes into contact with acid
solutions, it should be washed with water and sodium bicarbonate solution alternately
and continuously till skin is smoothened. Similarly exposure to caustic alkalis may be
treated with dilute acetic or boric acid solutions and water. Fire scar can be washed
thoroughly with water in a tap in the sink and a little oil or pipette be applied. If eyes
come into contact with chemicals, wash them with plenty of water and clean them with a
dry fresh cloth.
20. WASTE DISPOSAL
Separate waste as follows:
a. All waste solid materials, broken glass, filter papers etc., shall be dumped into dust bins
provided. Disposal of solutions or water or washing of apparatus shall be into the water
sink only. Insoluble solids should be put in dust bins but not in water sinks. The work
tables and working space must be kept neat, dry and clean always before, during and
after experiment. Any spilling of material should be cleaned immediately.
b. Solutions containing strong acids should never be poured directly into the sink. They
should be diluted with sufficiently excess water and discharged into the nearby sink
slowly.
c. Gloves used in lab are to be disposed of in the containers labeled “Used Gloves Only”
located next to the sinks in each lab.

d. Other trash that is not glass and is not contaminated by hazardous chemicals should be
placed in the large waste baskets near the front of the lab room.
INSTRUCTIONS TO THE STUDENTS
The following instructions are offered to the students for acquiring curriculum based skills in
Chemistry laboratory, since chemical analysis is a basic component in all branches of
Engineering & Technology, which will be useful in later courses of study, research and technical
job requirements.
1. The student shall make himself completely familiar with the experiment he/she is
about to perform, its theory, procedure and precautions, before the beginning of the
experiment.
2. This lab manual is intended to help in this aspect. Each apparatus is designed to be
used in a specific manner to give expected results. Even if the experiment is
performed in a batch of two or three, each student shall record his/her own
observations separately in his observation note book. Students are advised to
familiarize themselves with each of the apparatus with the help of this lab manual
and further supporting instruction from the teacher.
3. All students should carry laboratory manual, make a record of every observation in it
during experimentation immediately. They are advised to perform the experiment in
the manner prescribed in the procedure or as instructed by the teacher. If there is a
doubt in experimentation, they may consult the teacher and follow the instruction.
4. The student should read the procedure of the experiment and conduct it accordingly.
For better results, the precautions to be taken shall be adhered to strictly. Better
results are not accidental and they are due to contiguous effort.
5. Students should not use excess amount of reagents or chemicals. The quantities to be
used are prescribed in the procedure given in this manual. Sometimes use of excess
reagents may lead to adverse results, in addition to wastage of chemicals.
6. After completion of the assigned experiment and proper record of all necessary
observations on the note book, the apparatus may be returned to the in charge.
Calculations shall be completed in the note books to arrive at the results.
7. If there is breakage of supplied equipment or abuse of any instrument the concerned
student shall be charged as per present price list. Hence students are advised to
verify equipment/ instrument before they obtain and give satisfactory report to lab
in charge.

INSTRUCTIONS TO WRITE LAB RECORD

1. Write on the right hand page the following order:
a. Serial number and date of performance (in the margin)
b. Name and number of the experiment as given in the list.
c. Aim of the experiment.
d. Description of the apparatus.
e. Procedure including sources of error and precautions taken to eliminate or to
minimize them.
f. Inference or Result.
g. Explanation, if necessary of any divergence in the expected result.
2. Left hand page should contain the following in their proper places.
a. Observation in tabular form.
c. Calculation in tabular form.
d. Graph sheets and other papers to be attached.
8. Students should submit a record of the previous experiments in the subsequent week
9. Every student shall complete the prescribed number of experiments and submit
record for certification & evaluation by the concerned teachers and Head. A student
without the certified record will not be allowed for external examination at the end of
the semester.
10. An experiment is deemed to be complete when it is satisfactorily performed and the

results shall be shown to the teacher and his approval in the form of his signature
must be obtained and then recoded.

UNDERTAKING BY THE STUDENT
I …………………………………………………………. here by undertake to state that, I have

read all the general instructions and safety precautions to be followed in the
ENGINEERING CHEMISTRY LAB. Comprehensive understanding of glassware,
handling of chemicals etc., were learned and trained to carry out experiments in
the curriculum.
Name:
Regd. No.
Signature

ACIDIMETRY – ALKALIMETRY
DETERMINATION OF HYDROCHLORIC ACID
OBJECTIVES:
 Determination of strength of HCl

 Comparison/interpretation of results
AIM: To determine the concentration of hydrochloric acid in a given volume (100ml) of solution
with standard sodium carbonate solution.
APPARATUS & CHEMICALS REQUIRED: Burette, pipette, volumetric flasks, funnel, conical flask,
wash bottle with distilled water, glazed tile, a digital balance, weighing bottle, anhydrous sodium
carbonate AR (solid), methyl orange indicator solution.
PRINICIPLE:
2HCl + Na2CO3 2NaCl + H2O + CO2
According to the principle of neutralization reactions, a free acid reacts with a base to form
salt and water, in which the hydrogen ions of the acid combine with the hydroxyl ions of the free
base in stoichiometric proportions, this being common for all acid- base reactions.
PROCEDURE:
STEP-1: Preparation of 0.05 M sodium carbonate solution

1.325 g of anhydrous sodium carbonate transferred into a 250 ml volumetric flask through
a glass funnel. The substance is dissolved completely in a minimum amount of distilled water and
the solution is made up to the mark. The concentration of sodium carbonate solution is calculated
using the given formula.
OBSERVATIONS:
S. No Contents in the pan grams milligrams Total weight(g)
1 W1
2 W2
CALCULATIONS:
W1 = Weight of weighing bottle with sodium carbonate = g
W2 = Weight of weighing bottle after transferring the sodium carbonate = g
Amount of the sodium carbonate transferred = W1–W2 = g
Concentration of the sodium carbonate = X 1000/250 = M
Gram molecular weight (GMW) of sodium carbonate = 106g

STEP-2: Determination of the concentration of the given hydrochloric acid solution
The given HCl solution is made up to the mark with distilled water (in the 100 ml
volumetric flask). The burette is filled with hydrochloric solution; 10 ml of the standard sodium
carbonate solution is drawn through a pipette into a 250 ml clean conical flask. To this, 10ml of
distilled water, 2-3 drops of methyl orange indicator solution are added to give a yellow colour.
This mixture is then titrated with the hydrochloric acid solution till the colour of the solution
changes from yellow to pale pink. The same procedure of titration is repeated until concurrent
readings are obtained.
OBSERVATIONS:
S. No Volume of sodium carbonate Burette reading Volume of HCl run down in ml

taken, in ml Initial Final
1
CALCULATIONS:
V1 = Volume of HCl consumed =

V2 = Volume of sodium carbonate taken = 10 ml
M1 = Molarity of HCl solution = ?
M2 = Molarity of sodium carbonate =
n1 = No of moles of HCl = 2 (as per the equation)
n2 = No. of moles of sodium carbonate = 1 (as per the equation)
Concentration of the supplied HCl solution = M
SIGNIFICANCE:
The determination of hydrochloric acid or principle of acidimetry or alkalimetry

assumes importance in industries, (for example manufacture of soaps, fine chemicals, drugs,
fertilizers etc.,) where acids and bases are used as a raw material and also commercially
available as a byproduct in other industries. The industrial effluent analysis may also require
these methods. The acids and bases are widely available in natural products and also in gastric
juices. Hence these methods are important in biochemistry and for evaluation in clinical
chemistry.

Note: Lab concentration of HCl in a fresh bottle is 11.3 molar
Lab concentration of HCl = 10 x Specific gravity x % purity of HCl/GMW of HCl
STUDENT REPORT : Write the report by answering the below questions
1. Why HCl is titrated with standard sodium carbonate

2. Is HCl can be titrated with NaOH directly
3. Is there any other indicator that can be used in the place of methyl orange
4. What is standard solution and how many types are there
5. What is difference between primary and secondary solutions
6. What is the difference between end point and equivalence point in a titration
7. How many types of reactions in volumetric analysis
8. What is the principle in the present titration
9. Compare the concentration of HCl (result) with standard lab concentration of HCl
10. Give the industrial applications of the present experiment

EXPERIMENT NO. 1 Date:
Name of the experiment
AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Preparation of 0.05M sodium carbonate solution
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

STEP-2: Determination of the concentration of the given hydrochloric acid solution
OBSERVATIONS:
S. No Volume of sodium carbonate Burette reading Volume of HCl run down in ml

taken, in ml Initial Final
1
CALCULATIONS:

Concentration of the given HCl solution = M
RESULT:
Given Reported % of error
STUDENT REPORT:

Determination of Strength of an acid in Pb-Acid battery

OBJECTIVES:
 Determination of strength of an acid in lead acid battery

 Comparison/interpretation of results
THEORY/PRINCIPAL
A storage cell is that which can work both as voltaic cell as well as electrical cell. During
its operation it works as a voltaic cell i.e., it supplies electrical energy due to a chemical energy
and it becomes discharged. Then during its charging, it works as an electrolytic cell i.e.,
chemical is produced by supplying of electrical energy. It is also called as lead storage battery.
Anode : Lead (Pb)
Cathode : Lead dioxide (PbO2)
Electrolyte: Dil. H2SO4
A lead storage battery consists of 6 cells each producing 2V output. To increase the
current output of each cell, the cathode plates are joined together and the anode plates are also
joined together and connected in series, we get an output of 12V as shown in figure.
Electrode reactions during discharge
Anode : Pb → Pb2+ + 2e-
Pb2+ + SO42- → PbSO4
Cathode : PbO2 + 4H+ + 2e- → Pb2+ + 2H2O
Pb2+ + SO42- → PbSO4 .
Net reaction: Pb + PbO2 + 4H+ + 2SO42- → 2PbSO4 + 2H2O
Electrode reactions during charging
Anode : PbSO4 + 2e- → Pb + SO42-
Cathode : PbSO4 + 2H2O → PbO2 + SO42- + 4H+ + 2e-
Net reaction: 2PbSO4 + 2H2O → Pb + PbO2 + 4H+ + 2SO42-
The PbSO4 forms during discharge is a solid and sticks to the electrodes. So, it is in a
position to gain or receive the electrons during electrolysis.

Such type of cell is generally used for electrical vehicles, automobiles, railways, hospitals,
power stations, in telephone exchange, UPS system etc.
An acid–base titration is a method of quantitative analysis for determining the concentration

of an acid or base by exactly neutralizing it with a standard solution of base or acid having
known concentration. A pH indicator is used to monitor the progress of the acid–base reaction.
Indicator Approximate Color Change When selecting an indicator for acid-base

pH Range for titrations, choose an indicator whose pH
Color Change
range falls within the pH change of the
Methyl orange 3.2-4.4 Red to yellow
Bromthymol 6.0-7.6 Yellow to blue
reaction. For example, in the titration of a
blue strong acid with a strong base, the pH
Phenolphthalein 8.2-10 Colorless to pink quickly changes from 3 to 11. Hence
Litmus 5.5-8.2 Red to blue phenolphthalein indicator suits the best for
Bromcresol 3.8-5.4 Yellow to blue this titration. Selection of indicator depends
green
on the pH range. The following table
Thymol bule 8.0-9.6 Yellow to blue
illustrates different acid base indicators and
their pH range.
In a lead acid battery, 20% (V/V) sulphuric acid is used as an electrolyte. Concentration of the
acid has a significant effect on the voltage of the battery. The following diagram explains the
concept.

From the above figure, it is noticed that, as the concentration of the acid decreases, voltage of
the battery drops gradually. Hence maintaining the acid concentration is very important in lead
acid batteries. Hence, the present experiment gains its importance in proper maintenance of
the battery.
PROCEDURE:
STEP-1: Preparation of standard oxalic acid solution
0.025M Oxalic acid primary standard solution is prepared by dissolving 1.575g of Oxalic
acid solid in 100 ml distilled water.
OBSERVATIONS:
1 W1
2 W2
CALCULATIONS:
W1 = Weight of weighing bottle with Oxalic acid = g
W2 = Weight of weighing bottle after transferring the Oxalic acid = g
Amount of the sodium carbonate transferred = W1–W2 = g
Gram molecular weight (GMW) of Oxalic acid = 126 g
W1 - W2
GMW of Oxalic acid
x 1000
100
STEP-2: Standardization of sodium hydroxide solution
Take 10ml of oxalic acid solution into a conical flask, add 20 ml of distilled water and a
drop of phenolphthalein indicator then titrate against sodium hydroxide solution taken in a

burette until color of the solution changes from colorless to pale pink. Repeat the titration for
concurrent readings.
OBSERVATIONS:
S. No Volume of oxalic acid taken in ml Burette reading Volume of NaOH run

Initial Final down in ml
1
2
3
CALCULATIONS:
V1 = Volume of oxalic acid taken = V2 = Volume of NaOH rundown =
M1 = Molarity of oxalic acid = M2 = Molarity of NaOH = ?
n1 = No. of moles of oxalic acid =1 n2 = No. of moles of NaOH = 2
Concentration of the supplied sodium hydroxide solution = M
STEP-3: Determination of acid strength of lead acid battery:
The given test sample solution is made up to the mark using distilled water. 10 ml of this
solution is transferred into a conical flask. Add 20 ml of distilled water and a drop of
phenolphthalein indicator and titrated against sodium hydroxide solution taken into a burette
until color of the solution changes from colorless to pale pink. Repeat the titration for
OBSERVATIONS:
S. No Volume of the acid taken in ml Burette reading Volume of NaOH

Initial Final run down in ml
1
2
3
CALCULATIONS:
V1 = Volume of acid taken = V2 = Volume of NaOH rundown =

M1 = Molarity of acid =? M2 = Molarity of NaOH =

n1 = No. of moles of acid =1 n2 = No. of moles of NaOH = 2
Concentration of the supplied test sample solution = M
STUDENT REPORT:
Write a report on the result by comparing the obtained value with the true or standard
value of acid concentration in batteries (4-6M), and answer the below questions.
1. Phenolphthalein is a suitable indicator for the present experiment- justify

2. What is the relation between concentration and specific gravity?
3. Can you study the effect of concentration of acid on the lead acid battery
4. Explain the phenomenon of neutralization
5. Reason for drop in voltage while drawing current from a battery.
6. Write the chemical equations involved during discharging and charging cycle.
7. Collect the data of concentrations observed from all the students of the batch and
plot a graph to explain the variation of voltage with concentration

EXPERIMENT NO. Date:
AIM:
PRINICIPLE:
PROCEDURE:
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

OBSERVATIONS:
S. No Volume of oxalic acid taken in ml Burette reading Volume of NaOH run

1
2
3
CALCULATIONS:
STEP-3: Determination of acid strength of lead acid battery:

OBSERVATIONS:
S. No Volume of the acid taken in ml Burette reading Volume of NaOH

1
2
3
CALCULATIONS:
Concentration of the supplied test sample solution = M
STUDENT REPORT:


DETERMINATION OF TOTAL CALCIUM OXIDE IN PORTLAND CEMENT BY

RAPID EDTA METHOD
OBJECTIVES:
 To determine the amount of total calcium oxide in the given test sample of cement
 To compute the percentage of total calcium oxide.
 Comparison of result with the industrial standard.
INTRODUCTION
Cement is a binder, a substance that sets and hardens and can bind the other materials
together such as sand, bricks and other building blocks. (What is cement?).
The raw materials used in the manufacturing of cement are Calcareous materials and
argillaceous materials (What are the raw materials used in the manufacturing of cement?).
Cement contains oxides of Calcium, Silicon, Aluminum, Magnesium, Iron and Calcium
Sulfate, Sulfur Trioxide and Alkali metals (in small amounts). (What are the constituents of
cement?)
(Percentage composition may vary depending on the grade of cement)
These oxides interact with one another in the kiln at high temperature to form more
complex compounds. The relative proportions of these oxide compositions are responsible for
influencing the various properties of the cement.

Functions of Calcium oxide in the cement:

 It is the principal constituent of the cement. (What is the main constituent of cement)
 Presence of lime in a sufficient quantity is required to form silicates and aluminates of
calcium.
 Excess of lime reduces the strength and makes the cement to expand and disintegrate.
 Deficiency in lime causes cement to set quickly and also reduce the strength of the
cement.
Preparation of cement solution
Cement solution is prepared by weighing accurate sample of cement, dissolved in
minimum concentrated HCl, warmed and then diluted with distilled water.
Calcium oxide in the cement is determined by complexometric titration method.
Complexometric titration is a form of volumetric analysis, in which formation of colored
complex is used to indicate the end – point of a titration. Complexometric titrations are
particularly useful in determining a metal ions or mixture of metal ions in solution. (Source:
Wikipedia:. https://en.wikipedia.org/wiki/Complexometric_titration).
These titrations are based on complexing a metal ion with a ligand (?). Ligand is an
electron donating species (may be of either Organic, Inorganic and either charged or neutral).
Simple complexing agents such as ammonia are rarely used as a titrating agent because
a sharp end point cannot be observed due to improper complexation. The ligands having
multiple donor sites are used as complexing agents. The common ligands used in the
complexometric titrations are Ethylene diamine tetra acetic acid (EDTA), 1, 2-cyclohexane tetra
acetic acid (CDTA), Dimethylgyloxime, Nitrilo tri acetic acid etc.,
The accuracy of these titrations is high and the concentration of the metal ion can be
determined even at milli mole level. EDTA is one such good complexing agent.
How to determine the end–point of the reaction in a complexometric titration?

The end–point of the complexometric titration is determined by using a metal–ion
indicator or complexometric indicator. Commonly used metal–ion indicators are Organic
dye stuffs viz. Eriochrome Black–T, Fast Sulphon Black–F, Murexide, Calcein, Patton–Redeer’s
indicator, xylenol orange etc.,
How EDTA is helpful in determining the Calcium oxide content in cement?
EDTA forms a stable complex with almost all metal ions and this reaction is the
basis for general analytical method for determination of these metal ions.
EDTA is ethylenediamine tetra acetic acid has four carboxylic acid groups and two amino
acid groups. It is a hexa dentate ligand having six donor sites. All the six donor sites will form
co-ordinate covalent bonds with the metal ion and form a stable metal complex. The ligancy of

EDTA is 6. It has 6 donor sites. Four replaceable hydrogen atoms and two lone pair of
electrons in two nitrogen atoms
EDTA forms 1:1 complex with metal ion present in the test sample irrespective of the
valency of the metal ion. Pure EDTA is insoluble in water and EDTA disodium salt is used
instead of EDTA.
EDTA di sodium salt when in aqueous form forms a stable complex with metal ions
present in the solution. The reaction is pH sensitive and has to be carried out at a pH value 10.2.
Since both the reactants are colorless, a suitable metal – ion indicator is to be employed.
Indicator first reacts with the metal ion and form Metal Indicator complex, which is unstable.
This reaction mixture when titrated with EDTA solution, EDTA replaces the indicator and form
a stable complex with the metal.
Now when the test solution is taken, the metal – ion indicator used is Murexide. The
reactions between Calcium, EDTA and Murexide is as follows.
In the first step, Murexide reacts with calcium ion and form an unstable wine red color complex.
In the second step, EDTA reacts with metal indicator complex, replaces the indicator with EDTA
molecules.

This method is called rapid EDTA method because, the calcium ions are determined directly
and quickly without eliminating the other metal ions.
Influence of pH in the above reaction:
EDTA ionizes in four stages (pK1 = 2.0, pK2 = 2.67, pK3 = 6.16 and pK4 = 10.26) and
form a stable complex in alkaline solution. If pH is less than 10.26 complete complexation of
EDTA will not take place. The so formed Metal – EDTA complexes are quite stable in ammonical
solutions and hence ammonical buffer solution is used to control the pH of the reaction mixture.
The experiment involves a series of steps.
STEP-1: Preparation of standard ZnSO4 solution:
Around 1.45g of Zinc sulphate heptad hydrate (ZnSO4. 7H2O) is weighed accurately and
transferred into a 100ml volumetric flask using a funnel. This is dissolved in a minimum
amount of distilled water and finally made up to the mark.
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:
W1 = Weight of weighing bottle with zinc sulphate = g
W2 = Weight of weighing bottle after transferring the zinc sulphate = g
Amount of the zinc sulphate transferred = W1–W2 = g
Concentration of the zinc sulphate= x = M
Gram molecular weight (GMW) of zinc sulphate = 287.54g
Therefore, the molarity of ZnSO4 = M.
Preparation of EDTA solution:
Around 4.65g of EDTA disodium salt is weighed accurately and transferred into 250 ml
volumetric flask using a funnel. This is dissolved in a minimum amount of distilled water and
finally made up to the mark.
Preparation of Buffer solution:
17.42g of NH4Cl is weighed accurately and transferred into a beaker. To this 142 ml of
NH4OH is added, mixed properly and is finally made up to 250 ml with distilled water. The pH is
adjusted to 10.2 by adding either NH4Cl of NH4OH using a pH meter.

Preparation of 5M Sodium Hydroxide solution:

50g of NaOH is weighed and transferred into a 250 ml beaker. This is dissolved in
minimum distilled water and finally made up to the mark with distilled water.
Preparation of test sample solution:
1.25g of test cement sample is weighed accurately and transferred into a 500 ml beaker.
This is dissolved in 20 ml of concentrated hydrochloric acid and then diluted up to 500 ml with
distilled water.
STEP–2: Standardization of EDTA solution:
10 ml of standard ZnSO4 solution is pipetted out into a 250 ml conical flask. To this 10 ml
of distilled water is added. 5 ml of pH 10.2 buffer and 2–3 drops of EBT indicator is added and
then the reaction mixture is titrated with EDTA from the burette until the wine red colored
solution changes to blue. The volume of EDTA rundown is recorded and the titration is
repeated until concurrent values are obtained and the values are tabulated.
OBSERVATIONS:
S. No Volume of ZnSO4 Burette Reading Volume of EDTA

taken in ml Initial Final run down in ml
1
2
3
CALCULATIONS:
V1 = Volume of zinc sulphate taken = V2 = Volume of EDTA rundown =
M1 = Molarity of zinc sulphate = M2 = Molarity of EDTA =?
n1 = No. of moles of zinc sulphate = 1 n2 = No. of moles of EDTA =1
Concentration of the supplied EDTA solution = M
Step –3: Determination of CaO content in Cement sample:

10 ml of cement solution is pipetted out into a 250 ml conical flask. 20 ml of distilled
water is added followed by 10 ml of 4 M NaOH solution to the flask (NaOH acts as a masks

other metal ions.). The flask is then thoroughly shaken for 2 minutes. 5 ml of glycerol (to get
sharp end – point), 5 ml of diethylamine (to maintain the pH of 12–13) and a pinch of Patton
- Reeder’s indicator is added. The contents are then titrated with EDTA from the burette until
wine red colored solution changes to blue. The readings are then tabulated and then percentage
of CaO is calculated. NaOH acts as a masking agent to mask other metal ions.
Observations:
S. No Volume of test Burette Reading Volume of EDTA

sample taken in ml Initial Final run down in ml
1
2
3
CALCULATIONS:
V1 = Volume of test sample taken = V2 = Volume of EDTA rundown =
M1 = Concentration of total CaO = ? M2 = Molarity of EDTA =
n1 = No. of moles of Cao = n2 = No. of moles of EDTA =
Concentration of the total CaO in test sample solution = M
We know,
Percentage of Total Calcium Oxide:

SIGNIFICANCE:
When hydrochloric acid is added to the test sample, the metal oxides are converted into
their metal chlorides and they are dissolved in solution. Now, a small quantity of sodium
hydroxide is added which precipitates Fe2+, Al3+ ions as their corresponding hydroxides. The
Ca2+ ions left in the solution is then determined by EDTA using Murex ide indicator.
This experiment helps in significantly determining the total Calcium oxide content in the
various cement samples and also helps in grading the cement.
Chemical composition of CaO in various grades of ordinary Portland cement
S. No % of CaO Grade
1 66.67 53
2 60.41 43
3 57.5 33
4 37.5 High alumina cement
Analysis and conclusion of Results:

From the available industrial standards, the percentage of Calcium oxide present in the
given sample of cement is in between 60–66%. The value obtained from the above
computations is comparable with the industrial standards, then the cement sample is said to be
of a particular grade and quality.
References:
1. Vogel’s text book of quantitative analysis, 5th Edition.
2. Text book of quantitative analysis, I.M. Kolthoff, 3rd Edition.
3. Engineering Chemistry, Jain and Jain, 16th edition, Dhanpat Rai Publications.
STUDENT REPORT: Compare the result with amount Cao in various grades of cement and
answer the following questions.
1. How do you determine the total CaO content in the cement

2. Importance of Calcium Oxide in cement
3. Name the indicators used in the experiment
4. Why EBT is not used in the determination of Calcium Oxide
5. Role of glycerol
6. Role of NaOH
7. Function of diethyl amine
8. Importance of pH in the experiment

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Preparation of standard ZnSO4 solution:
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

STEP–2: Standardization of EDTA solution:
OBSERVATIONS:
S. No Volume of ZnSO4 Burette Reading Volume of EDTA

taken in ml Initial Final run down in ml
1
2
3
CALCULATIONS:
Step –3: Determination of CaO content in Cement sample:

OBSERVATIONS:
S. No Volume of test Burette Reading Volume of EDTA

sample taken in ml Initial Final run down in ml
1
2
3
CALCULATIONS:
Percentage of Total Calcium Oxide:
STUDENT REPORT:


COMPLEXOMETRY
DETERMINATION OF TOTAL HARDNESS OF WATER
OBJECTIVES:
 To perform a complexometric titration to determine the hardness water from various

sources
AIM: Determination of total hardness of a water sample with EDTA.
APPARATUS & CHEMICALS REQUIRED: Burette, pipette, volumetric flasks, funnel, conical
flasks, wash bottle, with distilled water, burette stand, EDTA solution, zinc sulphate AR(solid),
Eriochrome black T (EBT) indicator solution, buffer solution (NH4Cl +NH4OH) of pH 10.
THEORY: The total hardness of water is generally due to dissolved calcium and magnesium
salts.
Hardness of water is expression for the sum of the calcium and magnesium ion
concentration in a water sample.
The standard way to express total hardness of water is in ppm.
Ethylene diamine tetra acetic acid (EDTA) form a complexes with Ca2+ and Mg2+ ions,
which are more stable at pH 10. The success of an EDTA titration depends upon the precise
determination of the end point. Ordinary indicators fail hence metal ion indicators or
metallochromic indicators like SBT (Solochrome Black-T), EBT (Eriochrome Black T) are used.
The indicator reacts with Ca+2 and Mg+2 ions to give a
wine red color. Upon the addition of EDTA is, the free Metal
ions (Ca+2 and Mg+2) present in the water sample are first
complexed to EDTA forming the most stable M-EDTA complex.
On further addition of EDTA, forms a pale blue color,
which indicates elimination of all the bivalent cations
responsible for hardness. The appearance of the pale blue
EBT Structure color of the indicator marks the end point of the titration.
S. No Hardness (ppm) Type of water Application

1 up to 50 Soft Industrial
2 51-100 Moderately Soft
Laundry
101-150 Slightly Hard
3 151-250 Moderately Hard
Agriculture
4 251-350 Hard
5 over 350 Excessively Hard Drinking
*Above data is as per WHO and BIS

PRINCIPLE:
M2+ + EBT M-EBT (Wine Red)
M-EBT + EDTA [M-EDTA] + EBT

(Colorless)
PROCEDURE:
STEP-1:– Preparation of 0.01M zinc sulphate solution:
About 0.71 g of zinc sulphate is weighed and transferred into a 250 ml volumetric flask.
The substance is dissolved completely in distilled water and the solution is made up to the
mark.
OBSERVATIONS:
1 W1
2 W2
CALCULATIONS:
W1 = Weight of weighing bottle with zinc sulphate = g
W2 = Weight of weighing bottle after transferring the zinc sulphate = g
Amount of the zinc sulphate transferred = W1–W2 = g
Concentration of the zinc sulphate = x = M
Gram molecular weight (GMW) of zinc sulphate = 287.54g
STEP-2: Standardization of EDTA solution:
10 ml of the ZnSO4 is pipetted out into a clean conical flask to this add 3 ml ammonia
buffer solution and 1 or 2 drops of EBT indicator, this produces wine red color. Titrate with
EDTA solution from the burette until the color changes from wine red color to pale blue.
OBSERVATIONS:
S. No Volume of ZnSO4 taken in ml Burette Reading Volume of EDTA run

1 10
2 10
3 10
CALCULATIONS:
V1 = Volume of ZnSO4 = 10 ml V2 = Volume of EDTA rundown =

M1 = Concentration of ZnSO4 = M2 = Molarity of EDTA = ?

n1 = No. of moles of ZnSO4 =1 n2 = No. of moles of EDTA = 1
STEP 3: Determination of total hardness of water:
20 ml of the water sample is pipetted out into a clean conical flask to this add 3 ml
ammonia buffer solution and 1 or 2 drops of EBT indicator, this produces wine red color.
Titrate with EDTA solution from the burette until the color changes from wine red color to pale
blue.
OBSERVATIONS:
S. No Sample Volume of water Burette Reading Volume of EDTA run

No sample taken in ml Initial Final down in ml
1 1 20
2 2 20
3 3 20
CALCULATIONS:
Volume of water sample taken = 20 ml

Volume of EDTA rundown =
Total hardness in CaCO3mg/lit is given by the formula:
Volume of EDTA X Conc. of EDTA X 100.1 X1000
Total hardness of water = --------------------------------------------------------------- ppm
Volume of water sample titrated
RESULT:
The given water samples contains the following ppm (parts per million) of total hardness.
1. Sample 1 ……… ppm
3. Sample 3………. ppm
SIGNIFICANCE
Hardness of water has a permissible limit for use in laundering purpose and industrial
applications, so this experiment assumes importance in the analysis of the water samples from
time to time, so that the water has the desired quality parameters. If not, proper rectifications
can be made to change the quality of water, based on the requirements. This data is relevant for
knowing the quality of water for other purposes in industrial equipment such as boilers, house
old equipment, heaters, water pipes etc.
STUDENT REPORT: Based on the Hardness of water (ppm), would you say your water is soft,
moderately hard, hard or very hard? Give a very brief explanation while addressing the
following questions.
Explain the deviations of your water sample with other water samples
1. What is hard water?

2. Which causes hardness to water?
3. How is water classified based on the degree of hardness?
4. List the types of hardness present in water
5. State the salts responsible for temporary and permanent hardness of water
6. What is meant by softening of water?
7. What is EDTA?
8. Why is disodium salt of EDTA preferred to EDTA for estimation of hardness?
9. What is EBT ?
10. What is a buffer solution? Give an example.
11. Why is ammonium hydroxide-ammonium chloride buffer added during the
determination of hardness of water?
12. Mention the disadvantages of hard water for industrial purpose.
13. List the methods of determining hardness of water.
14. What is the significance of this experiment?

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1:– Preparation of 0.01M zinc sulphate solution:
OBSERVATIONS:
1 W1
2 W2
CALCULATIONS:

STEP-2: Standardization of EDTA solution:
OBSERVATIONS:
S. No Volume of ZnSO4 taken in ml Burette Reading Volume of EDTA run

1 10
2 10
3 10
CALCULATIONS:
STEP 3: Determination of total hardness of water:

OBSERVATIONS:
S. No Sample Volume of water Burette Reading Volume of EDTA run

No sample taken in ml Initial Final down in ml
1 1 20
2 2 20
3 3 20
CALCULATIONS:
RESULT:
The given water samples contains the following ppm (parts per million) of total hardness.
3. Sample 3………. ppm
STUDENT REPORT:


DETERMINATION OF PERCENTAGE OF IRON IN CEMENT SAMPLE BY

COLORIMETRY
OBJECTIVES:
 Determination of amount of iron in the given test sample

 Computation of percentage of iron
 Comparison of the result with true value
THEORY/PRINCIPLE:
Colorimetric method is an instrumental method by which concentration of any test

solution (colored solutions) [what if not colored?] can be determined by measuring its
absorbance at a specific wavelength [why specific wavelength?]. [How concentration and
absorbance are related to each other?]. For illustration, a series of solutions of varying
concentration of KMnO4 may be prepared and the relation between concentration and intensity
of color can be established (Fig.1).
Fig.1 Relation between concentration and color intensity

This relation has been explained by Beer-Lamberts law. The law states the concentration
of a chemical is directly proportional to the absorbance of a solution. The relation may be used
to determine the concentration of a chemical species in a solution using a colorimeter.
Equation for Beer's Law
Beer's Law may be written simply as:
A = εbc
Where A is absorbance (no units)
ε is the molar absorptivity with units of L mol-1 cm-1 (formerly called the extinction coefficient)
b is the path length of the sample, usually expressed in cm
c is the concentration of the compound in solution, expressed in mol/lit
Reference: Principles of Instrumental Analysis, Skoog, West and Holler
[Do Beer’s valid for all conditions? What are its limitations?]
Test your understanding:
A sample is known to have a maximum absorbance value at 490 nm. Its molar absorptivity
is 8400 M-1cm-1. The width of the cuvette is 1 cm. A spectrophotometer finds A = 0.70. What is the
concentration of the sample?
[Try to study the effect of path length (b) on the absorbance measurements]
Fig.2 Schematic of digital colorimeter
In the present experiment, concentration of iron in a given test sample of cement is to be

determined using colorimeter. Beer’s law is valid only for very dilute solutions. When a highly
concentrated solution is used for the study, depending on the nature of the test sample, either
association or dissociation of the chemical takes places results in the deviations in absorbance
measurements. Hence always very dilute solutions are preferred (ppm range) for colorimetric
determinations. As we have to determine the concentration of iron and as it is a colorless
solution, in carrying out colorimetric experiment we are in need of a chromogen (color
generating reagent). It was found in literature (Reference: Text Book of quantitative analysis,
Vogel 5th Edition, pp 690) potassium thiocyanate {KSCN} forms an instantaneous, stable, clear
red colored compound. Strong acids {HCl or HNO3 of concentration 0.05-0.5M} should be
present to suppress the hydrolysis of iron. [Why not sulphuric acid?]
Fe+3 + n SCN- [Fe(SCN)n]3-n
PROCEDURE:
STEP-1: Preparation of 0.01M stock solutions of ferric iron salt
0.5g of AR grade ferric ammonium sulphate is weighed accurately and into a clean
100ml volumetric flask. The amount is dissolved completely in a small amount of distilled
water and 2ml of conc. nitric acid to prevent hydrolysis then it is made up to 100ml.
(Molecular weight of the salt, ferric ammonium sulphate = 482.18)
Weight of the salt x 1000

Concentration of ferric iron solution, C = --------------------------------------------------------------
Molecular weight of the salt x 100

STEP 2: Construction of a standard curve of Beer’s law

The above solution is further diluted to low concentration by pipetting out 5.5ml ferric
iron solution 100ml volumetric flask and made up to the mark with distilled water.
The concentration of this stock solution M = 5.5 X C/100 =
Five cleaned 25ml volumetric flasks are labeled as 1,2,3 and 4 . The diluted ferric iron
solution of 2.5ml, 5ml, 7.5ml and 10ml aliquots are transferred into these labeled volumetric
flasks respectively. 0.5ml of Nitric acid and 4ml of potassium thiocyanate (KSCN) solution are
added to aliquots in each of these labeled flasks. Red colour is developed in each of these flasks.
They are then made up to the mark. Using the formula M1V1 =M2V2, the concentration of ferric
iron in each of these labeled flasks is calculated and tabulated (M is the concentration of the
second stock solution of ferric iron salt prepared as above).
S. No Sample No. Volume of Fe(III) taken in ml Concentration (calculated)

1 1 2.5+0.5ml HNO3+4ml KSCN 2.5xM = M1 x 25 M1 =
2 2 5.0+0.5ml HNO3+4ml KSCN 5xM = M2 x 25 M2 =
4 4 10.0+0.5ml HNO3+4ml KSCN 10xM = M4 x 25 ,
M4 =
The colorimeter is switched on 15 minutes before the start of the experiment. The
appropriate filter 490nm is adjusted by turning the knob smoothly. A clean blank cuvette is
filled with distilled water up to two thirds level and smoothly inserted into the cuvette holder of
the colorimeter. The digital reading in the panel is adjusted to zero by adjusting the proper
knob and the cuvette is removed. Then the contents of the 25ml. volumetric flask no.1 are
transferred slowly into another clean cuvette and the same is inserted smoothly into the holder.
The reading in the digital panel (optical density, OD) is noted after attaining stability. The same
operation is repeated with solutions in the remaining volumetric flasks 2,3,4 and 5 and
correspondent readings on the digital panel (OD) are recorded in table below.
S. No Concentration of ferric iron solution OD(Optical

( Molar) Density)
1. 0 0
2. M1
3. M2<
4 M3
5 M4
6 Unknown solution

A graph is drawn to the concentration on X-axis and OD on Y-axis to obtain a straight

line passing through the origin, which is the calibration curve of Beer’s law.
STEP-3: Preparation of cement sample and development of color

About 1 g of given sample is weighted accurately and transferred in to a clean 250ml
conical flask. About 40ml of 2N HCl is added to the conical flask and the mixture is boiled for ten
minutes thereby iron oxide present in cement dissolves. Then the solution is carefully cooled to
room temperature, filter through a filter paper and then filtrate is made to up to the mark.
STEP-4 : Determination of ferric iron in the given test sample
About 10ml of above cement solution is
transferred into a 100ml volumetric flask and 5
ml of KSCN solution and 30ml of 4M HNO3 is
added and made up to the mark with deionized
water shaken well for uniform concentration. The
absorbance of the solution is measured in a
colorimeter; the amount of iron present is read
directly from the standard calibration curve
.
The reading of OD is noted. This obtained OD is then matched in the calibrated graph and the
concentration of unknown solution of ferric iron is deduced from the graph. From calculations,
the amount of ferric iron is determined in the unknown sample
From the plot concentration of iron in the test sample (cement) can be determined.
Concentration of sample of given ferric iron solution = M
(From calibration curve)
Amount of ferric iron present in the given 100 ml of solution = Conc. of Iron (III) x 55.86 x100
1000
, = grams
,
Interpretation of results
From the standard table, iron (iron oxide) in cement sample must be in the range 0.5-6.
Iron in cement sample provides

 Iron oxide imparts color to cement.

 It acts as a flux.
 At a very high temperature, it imparts into the chemical reaction with calcium and
aluminum to form tricalcium alumino-ferrite.
 Tricalcium alumino-ferrite imparts hardness and strength to cement.
In the light of the above facts, the present experiment gains importance.
S. No % of Iron in Cement Grade

1 4.94 53
2 3.56 43
3 3.4 33
4. 13.1 High alumina cement
The role of iron oxides (FeO, Fe2O3) is decisive in the development of the melt phase of
the clinker and in reducing the temperature of clinker-forming reactions. The CaO-Al2O3- Fe2O3
system includes many compounds affecting composition and development of Portland clinker.
From the viewpoint of clinker chemistry only the crystal compound series likely to develop
between the incongruous dicalcium ferrite (C2F) and different calcium aluminates, primarily
C2Al, is of interest. Among these crystal compounds the brownmillerite (C4AF) holds a notable
place. In the development of the cement quality, ferric compounds are only of significance by
facilitating calcination and reducing the burning temperature. This feature of ferric compounds
gets an increasing actuality by improving the energy balance of clinker combustion.
CONCLUSION:
From the standards it is noticed that, the presence of 0.5-6% of iron oxide in cement is
significant for hardness and its strength. In the present experiment, the results showed that the
test sample has 4% (for example) of iron oxide in it. As this value is in the range given by
standards, it can be concluded that the test sample is of good quality.
STUDENT REPORT:
Compare and explain the deviations of your result with standard values and other samples
given among your batch
1. Relation between concentration and absorbance of a solution

2. Beer’s law and it’s mathematical expression

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Preparation of 0.01M stock solutions of ferric iron salt
STEP 2: Construction of a standard curve of Beer’s law

S. No Sample No. Volume of Fe(III) taken in ml Concentration (calculated)

2 2 5.0+0.5ml HNO3+4ml KSCN 5xM = M2 x 25 M2 =
4 4 10.0+0.5ml HNO3+4ml KSCN 10xM = M4 x 25
,
M4 =
S. No Concentration of ferric iron solution OD(Optical

( Molar) Density)
1. 0 0
2. M1
3. M2<
4 M3
5 M4
6 Unknown solution
STEP-3: Preparation of cement sample and development of color

STEP-4 : Determination of ferric iron in the given test sample

.
CALCULATIONS:
Amount of ferric iron present in the given 100 ml of solution = Con. of Iron (III) x 55.86 x100
1000
, = grams
,
STUDENT REPORT:

pH Metric Titrations
OBJECTIVES
 Determination of concentration of a strong acid using a strong base.

 Comparison of the result obtained with true value.
INTRODUCTION
The concept of pH was given by Sorensen in 1909. It is a scale to measure the acidity or
alkalinity of an aqueous solution. It is defined as the as the negative logarithm (to base 10) of
the hydrogen ion concentration at low concentrations.
i.e., pH = -log [H+]
According to Arrhenius theory, H+ causes acidic nature and OH- causes alkalinity. Pure
water in solution state has a tendency to dissociate into H+ and OH- ions, equal in their number,
thus making water neutral. The ionic product of water at 22 oC has been found to be 10-14,
[H+][OH-] = 10-14
Since, each water molecule dissociated to give hydrogen and hydroxyl ions, each of their
concentration in pure neutral water shall be 10-7.
[H+] = [OH-] = 10-7
Thus for all neutral solutions, their hydrogen (or hydroxyl) ion concentration shall be 10 -7
and the corresponding pH value calculated is 7. For acid solutions, the concentration of hydrogen
ions shall be greater than 10-7 and hence their corresponding pH value shall be less than 7.
Similarly for alkaline solutions, the hydrogen concentration shall be less than 10 -7 and hence their
corresponding pH value shall be greater than 7 up to 14.
Thus in pH scale from 0 to 14, 0 to 7 indicates acidity, 7 indicates neutrality and 7

to 14 indicates alkalinity of an aqueous solution. The pH values of strong acids lie in 0 to
1 region while that of strong bases lie in 13 to 14 region.
How to measure pH?
There are several methods with indicator solutions and indicator papers for the instant
determination of pH. Even though quick, they are approximate. The best and widely used
accurate method for the determination of pH is the measurement of EMF produced by H+
ions around an electrode in the instrument pH meter, it is a suitably modified
potentiometer calibrated in terms of pH.
Here the basic principle is that when two electrodes are kept in two solutions having
different hydrogen ion concentration and the electrodes are connected to a potentiometer and
the solutions via salt bridge, a small potential difference (EMF) can be observed. If the standard
EMF produced by hydrogen ion species of a known concentration is known, the EMF can be
measured by comparison and calibration. The pH and EMF are related by the equation,

pH = (EMF/0.00019837) T
Where ‘T’ is the absolute temperature.
Hence, pH value of the solution increases with the increase in temperature
How to measure the EMF produced by Hydrogen ion species?
The measurements of pH are carried out with a glass electrode.
A glass electrode consists of a thin glass membrane that is responsive to changes in H +
activity. The glass used for construction of the glass electrode is a special glass of approximate
composition of SiO2 (72%), Na2O (22%) and CaO (6%). These satisfactorily work over the pH
range 0-10. If Na2O is replaced by Li2O, glass electrode can measure the pH values from 0 to 14.
If the glass electrode is coupled with another reference electrode such as calomel or
silver/sliver chloride electrode as a combined electrode, the hydrogen ion concentration and
the pH of an unknown solution can be directly measured as EMF of the cell constituted by the
two electrodes.
Contact between the test solution and reference electrode is usually achieved by means
of a liquid junction, which forms part of the reference electrode. The pH meter is a high
impedance electrometer, calibrated in terms of pH.
The glass electrode as a half-cell contains a very thin glass membrane with constant
hydrogen ion activity on one side (0.1M HCl) and the variable hydrogen ion activity on the
other side (of the unknown solution).
The glass electrode is applicable for use in all solutions including those containing
oxidizing and reducing agents. The solutions are not contaminated and the sensitivity is up to
0.01%. However, since glass membrane is attacked by strong alkalis like NaOH or KOH, it may
not function well beyond pH 10 and loses its sensitivity in such a case.
Glass electrode pH Combination electrode

How does pH meter look like?

The pH meter is basically a high impedance meter amplifier that accurately measure the minute
electrode voltages and displays the resistants’ directly in pH units. The block diagram the pH
meter is as follows.
Calibration of the instrument (why the instrument has to be calibrated?*)
 Changing Characteristics – Over time, aging and coating of pH electrodes can cause
changes in their characteristics, and even the most stable electrodes cannot be produced
with exactly the same characteristics. Calibration helps to match the current
characteristics of the pH meter with the pH sensor in use, compensating for any
difference between a pH electrode’s behavior in theory and reality.
 Higher Accuracy – A minimum of three standards are required for a calibration curve,
and a pH meter cannot be calibrated without a standardized buffer. If pH meter
calibration has not been performed properly, the resulting measurements are likely to
be inaccurate.
 Reduced Drift – Measurement drift is a common issue with pH meters, as with any
other instruments using electrodes. While drift from calibrated settings can’t be
eliminated or prevented, regular equipment calibration helps you maintain accuracy in
measurement results.
 Sample Differences – Multiple samples of the same substance can have different
characteristics, and calibrating pH meters against standardized buffers helps to prevent
membrane-related issues such as differences in ionic strength.

Instrument calibration for pH meters is generally conducted in two ways:

1. Two-Point Calibration – In this method, a microprocessor-based pH meter calculates the
real slope and offset error for the pH electrode. Based on this information, the meter’s mV/pH-
equation is then adjusted to match the characteristics of the pH electrode in use.
The two calibration points bracket the range of values to be measured, so this method is
also known as bracketing calibration. Readings that go past the calibrated range may be
displayed with slight deviations from the true value, since they are extrapolated by the pH
meter assuming linearity.
2. Multi-Point Calibration – With some pH meters, calibration can be performed for more than
two pH values on both sides of the zero point, which in this case is pH 7.00.
Calibration at three or more pH values increases the measurement range of the device without
recalibration being required.
This is generally done by measuring different buffer solutions with standardized,

well-defined values, and then adjusting the pH meter based on any deviations from the
buffer’s known pH value.
Calibration of the instrument:
The instrument is calibrated by using two point calibration method. Two buffers of pH = 4.01
and 9.14 (at 30°C) are used for calibrating the instrument.
Model Graphs:
Normal graph First derivative graph


pH METRIC TITRATION OF STRONG ACID (HCl) AND STRONG BASE (NaOH)
Aim: Determination of concentration of a strong acid solution, hydrochloric acid with a strong
base, sodium hydroxide solution, by a pH metric titration method.
APPARATUS & CHEMICALS REQUIRED: pH meter with electrode, burette (50 ml), volumetric
flask (100 ml), conical flask (100 ml), pipette (10 ml/25 ml), beakers (100 ml), stirrer/glass
rod, hydrochloric acid solution, sodium hydroxide solution, oxalic acid AR solid.
PRINCIPLE:
The neutralization reaction between electrolytic solutions of HCl and NaOH is
H+ + Cl- + Na+ +OH- Na+ + Cl- + H2O
A measured volume of HCl solution is taken in a 100 ml beaker in which the combined
electrode is immersed without touching the bottom and NaOH solution is added from the
burette, when the above reaction occurs, forming feebly ionized water molecules by the
combination of H+ and OH- ions.
With the progress of the titration, as the NaOH solution is gradually added, highly mobile
H+ ions disappear and are replaced by less mobile Na+ ions causing a decrease in the potential
of the solution. This trend of decrease continues till the end point is reached, when all the H +
ions present in solution due to HCl are neutralized by combination with OH- ions and disappear,
due to addition of NaOH. Beyond end point, further addition of NaOH solution results in gradual
change in potential due to unreacted OH- ions and Na+ ions. At the point of neutralization, the
pH value of the solution is constant. A plot of pH on Y-axis measured at each addition versus
volume of NaOH solution added, on X-axis gives a smooth curve and the sudden inflexion (jump
in pH) indicates the end point. The corresponding value of NaOH added with respect to the
inflexion gives the titer value.
The following series of steps are involved in the experiment.
STEP–1: Preparation of Standard Oxalic acid (0.25M) solution:
Around 3.15g of oxalic acid (H2C2O4. 2H2O) is weighed accurately and transferred into a
100ml volumetric flask using a funnel. This is dissolved in a minimum amount of distilled water
and finally made up to the mark.
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:
W1 = Weight of weighing bottle with oxalic acid = g
W2 = Weight of weighing bottle after transferring the oxalic acid = g

Amount of the oxalic acid transferred = W1–W2 = g

W1 - W2
GMW of Oxalic acid
x 1000
100
Gram molecular weight (GMW) of oxalic acid = 126g
STEP–2: Standardization of Sodium Hydroxide solution supplied:

The stoichiometric equation of the neutralization reaction between sodium hydroxide
and oxalic acid is
H2C2O4 + 2NaOH Na2C2O4 + 2H2O
According to the above equation, two moles of sodium hydroxide react with one mole of oxalic
acid.
10mL of standard oxalic acid solution is pipetted out and transferred carefully into a
250ml conical flask. To this 10ml of distilled water and 2 drops of phenolphthalein indicator is
added. The contents of the conical flask are then titrated with sodium hydroxide solution from
the burette until the color changes from colorless to pink. The volume of NaOH rundown is
recorded and the procedure is repeated until we get the concurrent readings.
S. No Volume of oxalic acid taken in ml Burette reading Volume of NaOH

1
2
3
CALCULATIONS:
STEP–3: pH metric titration of hydrochloric acid solution with standardized sodium

hydroxide solution.
pH metric titrations are usually carried out by taking a test sample solution in a beaker,
in which the glass electrode is immersed without touching the bottom. The titrant is added

from the burette, with continuous stirring and the stable value of pH is measured after each
addition of sodium hydroxide.
The pH meter should be switched on 15 minutes before the start of the experiment for a
warm up. The pH meter is calibrated by immersing the electrode in a buffer solution of known
pH value (usually 4.0/9.0) or it can be calculated by using proper electronic probe of a definite
known pH value.
10 ml of HCl pipetted out into a 100 ml beaker, to this add 40 ml of distilled water. The
contents are then titrated with NaOH by measuring the changes in pH using a pH meter. Two
titrations are performed namely, pilot titration and accurate titration.
In pilot titration, the NaOH is added 1mL at a time by simultaneous measurement of pH

at each time of addition of NaOH. The sudden change in pH from acidic range to basic range is
noted and the corresponding volumes are recorded.
In the accurate titration, the titrimetric procedure is repeated as above, 0.1 ml of NaOH is
added from the volumes where a change in pH value is noted. At the equivalence point, the rate
of change of pH is high and next 0.1 ml of NaOH added will give the end – point. The average
value of the end point is calculated by plotting a graph between the volume of NaOH taken on X
– axis and the corresponding pH values on Y – axis. For more accurate results, a first derivative
graph is plotted between change in volume of NaOH on X – axis and corresponding change in
pH values on Y – axis.
OBSERVATIONS:
Volume of HCl solution taken = 10 ml

Temperature of the solution = oC
Pilot titration
S. No Volume of NaOH added, ml pH measured
1
2
3
4
5
6
7
8
9

Accurate titration
S. No Volume of NaOH pH value Change in Change in pH ∆pH/∆V

added in (V ml) volume (∆V) value (∆pH)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
CALCULATIONS:
V1 = Volume of HCl taken = 10 ml V2 = Volume of NaOH required =
M1 = Molarity of HCl solution = ? M2 = Molarity of NaOH =
n1 = No of moles of HCl =1 n2 = No. of moles of NaOH = 1
SIGNIFICANCE:
pH metric titration is very valuable at low titrant concentrations of the range of
0.0001 M, at which the normal titrimetric methods fail. This method can be used with much
diluted solutions or with colored or turbid solutions, in which end point cannot be seen with
naked eye.

Further, choice of an indicator for titrations weak acids, weak bases and sometimes
both, is difficult to be carried out and pH metric titrations are accurate alternative for such
experiments.
However, in pH metry, no observation of end point is necessary and one single

experiment is sufficient as there is no visual location of the end point, as it is located graphically
by extrapolation. Any errors creeping in the operation shall stand minimized or averaged out.
APPLICTIONS:
1. Agriculture
2. Brewing
3. Corrosion prevention
4. Dyeing
5. Jam and Jelly manufacturing
6. Printing
7. Pharmaceutical industry
References:
i. Vogel’s text book of quantitative analysis, 5th Edition, Pearson Education, Singapore.
ii. Text book of quantitative analysis, I.M. Kolthoff, 3rd Edition.
iii. Standard methods of chemical analysis, I M Kolthoff and Belcher, Van Nostrand
Company, USA
iv. Text book of Quantitative chemical analysis, D C Harris, W. H. Freeman and Company,
New York, USA.
Engineering Chemistry, Jain and Jain, 16th edition, Dhanpat Rai Publications.
STUDENT REPORT: Compare the result with amount Cao in various grades of cement and
answer the following questions
1. What is pH?
2. What is the effect of temperature on pH?
,
<
,
3. What is the pH of pure water at 25 °C?
4. Does the addition of the salt having a common ion onto weak acid change the pH of the
solution?
5. What is the pH scale range?
6. How the end point of the titration is obtained in pH metry?
7. How do you measure the pH of a solution?
8. What is the composition of the glass membrane in glass electrode?
9. What is the primary standard used in this experiment?
10. What is the pH of 0.1M HCl and 0.1M H2SO4

AIM:
PRINICIPLE:
PROCEDURE:
STEP–1: Preparation of Standard Oxalic acid (0.25M) solution:
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

STEP–2: Standardization of Sodium Hydroxide solution supplied:

1
2
3
CALCULATIONS:
STEP–3: pH metric titration of hydrochloric acid solution with standardized sodium

hydroxide solution.

OBSERVATIONS:
Pilot titration
S. No Volume of NaOH added, ml pH measured
1
2
3
4
5
6
7
8
9
Accurate titration
S. No Volume of NaOH pH value Change in Change in pH ∆pH/∆V

added in (V ml) volume (∆V) value (∆pH)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
CALCULATIONS:
STUDENT REPORT:

CONDUCTOMETRIC TITRATIONS
OBJECTIVES:
 Determination of concentration of a strong acid using a strong base
 Comparison of the result obtained using true value.
INTRODUCTION
In this titration electrolytic conductivity of the reaction mixture is continuously monitored

as one reactant is added. The end point in these titrations is determined by means of a conductance
measurement. They are based on the principle that the conductance of an electrolyte solution
depends on the number of ions, their charge and mobilities. As a reaction proceeds during a
titration, number of ions or concentration of ions vary. Also, the ions of one kind are replaced by
ions of other kind, differing in the mobilities. As a result, the conductance of the solution changes
with every addition of the titrant. At the equivalence point, a sharp change in the conductance is
observed. Thus, if the conductance of the solution measured during the course of titration is plotted
against the volume of the titrant added, the end point can be conveniently obtained by the
extrapolation of straight lines obtained at the point of their intersection.
The method can be used for titrating colored solutions or homogeneous suspensions, which
cannot be used with normal indicators.
Condcutometric titration works on the principle of Ohm's law.
Acid-base titrations and redox titrations are often performed with conductometer, in which
located with help of indicator. However, electrical conductance measurements used to locate the
end point.
In the titration of HCl with NaOH as the titration progresses, the protons are neutralized
to form water for each amount of NaOH added equivalent amount of hydrogen ions is removed.
Effectively, the faster moving H+ ion is replaced by the slower moving Na+ ion, and the
conductivity of the titrated solution as well as the measured conductance of the cell will fall. This
continues until the equivalence point is reached, at which we have a solution of sodium chloride,
NaCl. If more base is added an increase in conductivity or conductance is observed, since more ions
Na+ and OH- are being added and the neutralization reaction no longer removes an appreciable
number any of them. Consequently, in the titration of a strong acid with a strong base, the
conductance has a minimum at the equivalence point. Conductometric titration curve is a plot of the
measured conductance or conductivity values against the number of ml of NaOH solution added.
THEORY/ PRINCIPLE:
Conductance (C) is the reciprocal of the electric resistance (R): C =1/ R
Conductance unit is Ohm-1 (also called Siemens, S). Conductance of aqueous electrolyte
solutions is, as rule in the range of µS (micro Siemen) to mS (milli Siemen)

In order to do conductance measurements, two metal electrodes (Pt) should be immersed in

the solution and connected to an alternating current (AC) voltage source (Fig. 1).
Under the effect of the potential difference between electrodes, each ion in solution moves to
the electrode of opposite charge. According to Ohm’s law, the electric current in this circuit
(including the solution) is: (2)
L depends on both solution properties (i.e. conductivity, k) and geometrical parameter of the
cell (i.e. electrode area, A, and distance between electrodes, l, Fig.1) according to the following
equation:
C= k (A/l)
Conductivity measurements of various samples

Sample Type Conductivity Range At 25 OC
High Pressure Boiler Water <0.1 µs/Cm To 0.2 µs/Cm
Demineralized Water 1 µs/Cm To 80 µs/Cm
Drinking Water 100 µs/Cm To 1 Ms/Cm
Waste Water 85µs/Cm To 9ms/Cm
Surface Water 100µs/Cm To 10ms/Cm
Industrial Process Water 8 Ms/Cm To 103ms/Cm
Concentrated Acids And Dyes 85ms/Cm To >1000ms/Cm

Cell calibration
250 ml standard 0.1000 M KCl solution should be prepared and used to adjust the
measuring instrument according to the KCl solution conductivity at the working temperature.
Temperature oC 18 20 25
1M KCl 98.201 102.024 111.733
0.1 M KCl 11.1919 11.6676 12.8862
Conductivity of KCl solutions(in mS cm- ) at various temperatures
1

STRONG ACID WITH A STRONG BASE

AIM: Determination of concentration of hydrochloric acid sodium hydroxide solution by a conductometric
titration method.
APPARATUS & CHEMICALS REQUIRED: Conductivity meter (with cell connected to the apparatus via jack
pins provided), burette (50 ml), volumetric flask (100 ml), conical flask (100 ml), pipette (10 ml, 25 ml),
beakers (100 ml), stirrer / glass rod, hydrochloric acid solution, sodium hydroxide solution.
PRINCIPLE:
The neutralization reaction between electrolytic solutions of HCl and NaOH is
H+ + Cl- + Na+ + OH- Na+ + Cl- + H2O
HCl titration against NaOH
HCl is a strong acid which dissociates completely in solution:
HCl → H+ + Cl-
Neutralization occurs when NaOH is added:
(H+;Cl- ) + (Na+;OH-) ⎯⎯ → ←⎯ ⎯ H2O + Cl- + Na
Titration of HCl by NaOH leads therefore to a

gradual replacement of the fast H+ ions by slower Na+
ions. Accordingly, the conductivity decreases until
the end point is reached. Further, the excess of NaOH
brings about a gradual increase of conductivity. The
equivalence volume lies at the intersection of the two
linear branches of the titration curve. Points in the
region of the end point slightly deviates from the
linear trend and should be disregarded.
<
PROCEDURE:
STEP-1: Preparation of standard oxalic acid (0.25M) solution (Primary standard):
About 3.15g of AR grade oxalic acid solid sample is weighed accurately in a clean, dry
weighing bottle and transferred into a 100 ml volumetric flask through a glass funnel. The
substance is dissolved completely in a minimum amount of distilled water and the solution is
made up to the mark. The solution is made homogeneous by thorough shaking in the stoppered
volumetric flask. The particulars of the weights used are tabulated and the concentration of
oxalic acid is calculated using the given formula.

OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:
W1 - W2
GMW of Oxalic acid
x 1000
100
STEP-2: Standardization of sodium hydroxide solution supplied
H2C2O4 + 2NaOH Na2C2O4 + 2H2O

According to the above equation, two moles of sodium hydroxide react with one mole of oxalic
acid.
10mL of standard oxalic acid solution is pipetted out and transferred carefully into a
250mL conical flask. To this 10mL of distilled water and 2 drops of phenolphthalein indicator is
added. The contents of the conical flask are then titrated with sodium hydroxide solution from
the burette until the color changes from colorless to pink. The volume of NaOH rundown is
recorded and the procedure is repeated until concurrent readings are obtained.
OBSERVATIONS:
1
2
3
CALCULATIONS:

STEP-3: Conductometric titration of hydrochloric acid solution with standardized sodium

hydroxide solution.
Conductometric titrations are usually carried out by taking a solution to be titrated in a
beaker kept at constant temperature (Why).
The titrant (NaOH)is added from the burette, with continuous stirring and the stable value
of conductance is measured after each addition.
The conductivity bridge instrument should be switched on 15 minutes before the start of the
experiment for a warm up. The temperature shall be adjusted to room temperature and reading
knob for conductance measurement shall be adjusted to a proper value. Adjust CAL knob till the
display reads 1000.
The burette is filled with standardized sodium hydroxide solution. The given HCl solution is
made up to the mark with distilled water (in the 100 ml volumetric flask). 25 ml of sample solution
and 25 ml of distilled water taken in a 100 ml beaker. The platinum electrode should be completely
immersed in the HCl solution. After attaining stability in reading, small volumes of standardized
sodium hydroxide solution from the burette are added into the beaker containing HCl slowly with
stirring. After every addition of NaOH, the conductance displayed in the meter should be noted.
There will be a gradual fall in the conductance and soon after neutralization is complete, there will
be a raise in the value. All the readings are to be tabulated.
OBSERVATIONS:
S. No Volume of NaOH Conductance measured, mho

added, ml
Conductance (C)
1
2
3
4
5
6
7
8
CALCULATIONS:
V1 = Volume of HCl taken = 25 ml V2 = Volume of NaOH required =
M1 = Molarity of HCl solution =? M2 = Molarity of NaOH =

n1 = No of moles of HCl =1 n2 = No. of moles of NaOH =1
Concentration of the supplied strong acid solution = M

The conductance measurements were tabulated. A plot of volume of NaOH versus corrected
conductance is plotted. The intersection point of the two straight lines gives the end point for
the titration.
STUDENT REPORT:
The result obtained is compared with the standard/true value. And deviations from the true
value are explained.

AIM:
PRINICIPLE:
PROCEDURE:
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

OBSERVATIONS:
1
2
3
CALCULATIONS:
STEP-3: Conductometric titration of hydrochloric acid solution with standardized sodium

hydroxide solution.

Volume of HCl solution taken = 25 ml.


added, ml
Conductance (C)
1
2
3
4
5
6
7
8
9
10
11
12
CALCULATIONS:

STUDENT REPORT:

WEAK ACID WITH A STRONG BASE

Acetic acid (a weak acid) has low conductivity, as represented by A. As NaOH is added, the
poorly conducting acid is converted into highly
ionized salt CH3COONa And consequently, the
conductivity goes up along AB. When the acid
is neutralized, further addition of the alkali
causes a sharp rise in conductance along BC
(due to addition of more conducting OH- ions).
The intersection of AB and BC, therefore,
represents the equivalence point
STEP-1 and STEP- 2 are similar to the previous experiment

STEP-3: Conductometric titration of weak acid (acetic acid) solution with standardized
sodium hydroxide solution
The burette is filled with standardized sodium hydroxide solution. The given CH3COOH
solution is made up to the mark with distilled water (in the 100 ml volumetric flask). 25 ml of
sample solution and 25 ml of distilled water taken in a 100 ml beaker. The platinum electrode
should be completely immersed in the CH3COOH solution. After attaining stability in reading,
small volumes of standardized sodium hydroxide solution from the burette are added into the
beaker containing CH3COOH slowly with stirring. After every addition of NaOH, the
conductance displayed in the meter should be noted. There will be a gradual fall in the
conductance and soon after neutralization is complete, there will be a raise in the value. All the
readings are to be tabulated.
OBSERVATIONS:
S. No Volume of NaOH Conductance measured, S/cm

added, ml
Conductance (C)
1
2
3
4
5
6

7
8
CALCULATIONS:
V1 = Volume of CH3COOH taken = 25 ml V2 = Volume of NaOH required =
M1 = Molarity of CH3COOH solution = ? M2 = Molarity of NaOH =
n1 = No of moles of CH3COOH = 1 n2 = No. of moles of NaOH =1
The conductance measurements were tabulated. A plot of volume of NaOH versus corrected
conductance is plotted. The intersection point of the two straight lines gives the end point for
the titration.
CONCLUSION: The result obtained is compared with the standard/ true value. And deviations
from the true value are recorded.
STUDENT REPORT: Compare and explain the deviations of your result with standard values
and other samples given among your batch answer the below questions.
1. Differentiate between classical method of titration and instrumental method.
2. Narrate the applications of this experiment.
3. What happens if DC source is used for the instrument?
4. Discuss the principle behind working of conductometer.
5. Explain the effect of temperature on conductance.
6. Give the advantage of condcutometric titration.
7. Study the effect of dilution on conductance measurement
8. Write various applications of conductometry.
9. As an engineer why this experiment is significant.
10. Can you calculate conductance of acid at a given volume say 1.26 ml?
11. Illustrate the following plot in your own words

AIM:
PRINICIPLE:
PROCEDURE:
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

OBSERVATIONS:
1
2
3
CALCULATIONS:
STEP-3: Conductometric titration of weak acid (acetic acid) solution with standardized
sodium hydroxide solution

OBSERVATIONS:

added, ml
Conductance (C)
1
2
3
4
5
6
7
8
9
10
11
12
CALCULATIONS:

STUDENT REPORT

POTENTIOMETRY
OBJECTIVES:
• How the potential changes with relative concentration of oxidized/reduced from
• Perform a redox titration of ammonium iron (II) sulphate using potassium dichromate as
oxidizing agent
• Determine the equivalence point of the redox titration by plotting titration curve using
potential change values and amount of oxidizing agent added during titration
• Estimate the strength of iron (II) ions in the given solution
• Advantages of potentiometry in redox titrations
THEORY
Potentiometric titration is based on the oxidation-reduction reaction between the titrant
and the titrate. Here the end pint is detected using a potentiometer from the Nernst equation.
During the titration, the solution potential changes due to the change in the concentration of
oxidized/reduced form. At one stage, where either of the form is absent i.e. at the end point,
there is a sharp change in potential.
Potential is measured by using an indicator electrode and a reference electrode. The

indicator electrode forms an electrochemical half-cell with the interested ions in the test
solution. The reference electrode forms the other half cell, holding a consistent electrical
potential. The overall electric potential is calculated as Ecell = Eind -Eref + Esol and Esol is the
potential drop over the test solution between the two electrodes. E cell is recorded at intervals
as the titrant is added. A graph of potential against volume added can be drawn and the end
point of the reaction is half way between the jumps in voltage. Equivalence point is located
through the graph as the point where the inflexion is maximum.
Ecell depends on the concentration of the interested ions with which the indicator electrode is
in contact. For example, the electrode reaction may be
Mn+ + ne- M
As the concentration of Mn+ changes, the Ecell value changes correspondingly. Thus the
potentiometric titration involves measurement of Ecell with the gradual incremental addition
of titrant.
Types of potentiometric titrations:
1. Acid-base titration (total alkalinity and total acidity)

2. Redox titration (HI/HY and cerate)
3. Precipitation titration (halides)
4. Complexometric titration (EDTA).
The reference electrode: An electrode dipped in a solution containing an ion with respect to
which the electrode is reversible is called the reference electrode. Most commonly, the
reference electrode is the silver/silver chloride electrode. The potential is based on the
following equilibrium:
AgCl(s) + e- Ag(s) + Cl-(aq)
The half cell is: Ag│AgCl(Saturated)│KCl(xM)║
The indicator electrode: The glass electrode is hydrogen ion sensitive electrode and hence is
used as the indicator electrode in potentiometric titrations involving acidimetry - alkalimetry.
The points to be considered while carrying out a potentiometric titration are
1. Stir well after every addition of titrant.

2. Allow some time after every addition of titrant so that the electrode may attain
equilibrium.
3. EMF measured shall be constant within 1 mV fluctuation is enough. When the drift in
EMF is within this, further volume of titrant may be added.
4. The region near the end point is important in locating the exact equivalence point
accurately. With the addition of the titrant, as the change in EMF becomes greater
and greater, the volume increment of the titrant should be small, say it shall be
reduced to 0.2 to even 0.1 ml. This increment should be maintained both below and
above the end point.
5. To prevent unnecessary dilution of the solution, the titrant must be 10 times
concentrated.

POTENTIOMTRIC TITRATION OF FERROUS IRON [Fe (II)] WITH POTASSIUM

DICHROMATE
AIM: Determination of ferrous iron concentration with standard potassium dichromate
APPARATUS & CHEMICALS REQUIRED: Potentiometric titration setup with combined

electrode , magnetic stirrer with paddle, beakers, wash bottle with distilled water, weighing
bottle, watch glass, funnel, pipette, volumetric flasks, conical flask, ferrous ammonium sulphate,
potassium dichromate AR solid, sulphuric acid.
PRINCIPLE:
Potassium dichromate is an oxidizing agent and in acid medium; it follows the half
reaction to give Cr (III) as the reduction product.
K2Cr2O7 + 6FeSO4 + 7H2SO4 K2SO4 + 3Fe2 (SO4)3 + Cr2 (SO4)3 + 7H2O
Fe2+ + Cr6+ Fe3+ + Cr3+
PROCEDURE:
STEP-1: Preparation of standard potassium dichromate solution (Primary standard)
About 0.4910g of AR grade potassium dichromate solid sample is weighed accurately in
a clean, dry weighing bottle and transferred into a 100 ml volumetric flask through a glass
funnel. The substance is dissolved completely in a minimum amount of distilled water and the
solution is made up to the mark. The solution is made homogeneous by thorough shaking in the
stoppered volumetric flask. The particulars of the weights used are tabulated and the
concentration of potassium dichromate is calculated using the given formula.
OBSERVATIONS:
1 W1
2 W2
CALCULATIONS:
W1 = Weight of weighing bottle potassium dichromate = g
W2 = Weight of weighing bottle after transferring potassium dichromate = g
Amount of the potassium dichromate transferred (W1–W2) = g
(W1–W2) x 1000
Concentration of potassium dichromate solution = -----------------------------------
Mol. Wt. of K2Cr2O7 x 100
= M
Molecular weight of potassium dichromate = 294. 185

STEP-2: Determination of ferrous ammonium sulphate with standard potassium

dichromate solution by a potentiometric titration
The given ferrous ammonium sulphate sample solution is made up to the mark in 100 ml
volumetric flask with distilled water. The potentiometer knobs are adjusted to read mV and
the room temperature, the potentiometer digital reading is standardized to1.0183V. (The
EMF of a Weston cadmium cell is 1.0183V and is constant over a wide range of time.)
The burette is filled with standard potassium dichromate solution. 10 ml of the ferrous
ammonium sulphate solution is mixed 10 ml of 4N sulphuric acid and 30 ml of distilled water
and taken into a 100 ml beaker in which the electrodes are immersed. The solution is stirred
well to give a constant reading in the potentiometer, which is noted as zero reading. Small
incremental volumes of standard potassium dichromate solution are added into the beaker
containing ferrous ammonium sulphate slowly with vigorous stirring. The correspondent
reading in the digital panel is noted against the volume added in the table.
There will be a gradual raise in the potential and soon after the oxidation of ferrous iron
present in the solution of the beaker is complete, there will be a steep upward jump in the
potential value. The addition of potassium dichromate from burette is continued until the
equivalence point has been passed by 0.5 –1.0 ml. All the readings are tabulated.
Volume of the sample of ferrous ammonium sulphate taken = 10 ml

Temperature = oC
Pilot titration
S. No Volume of K2Cr2O7 added, ml Potential measured, mV
1
2
3
4
5
6
7
8
9
10

Accurate titration
S. No Volume of K2Cr2O7 added, ml Potential measured, mV ΔE ΔE/ΔV
1
2
3
4
5
6
7
8
9
11
12
13
14
15
16
17
A graph is plotted to the volume of potassium dichromate added on X-axis and

corresponding potential in mV measured on Y-axis. The steep upward jump in potential in the
curve causing a change of 200 – 300mV in the EMF is the point of neutralization and the
corresponding volume of potassium dichromate gives the volume required to oxidize the 10
ml of ferrous ammonium sulphate taken. The concentration of ferrous ammonium sulphate is
calculated as below.
CALCULATIONS:
M1= Concentration of ferrous iron solution = ?

V1 = Volume of ferrous iron solution pipetted out = 10 ml
n1 =No. of moles of ferrous Iron = 6
M2 =Concentration of potassium dichromate solution =
V2 = Volume of dichromate solution rundown =
n2 =No. of moles of dichromate = 1

Concentration of ferrous iron present in given 100 ml of solution (M1) =
Amount of ferrous iron [Iron (II)] present in given 100ml solution =
Atomic weight of iron = 55.86
RESULT: The amount of ferrous iron [Fe (II)] present in a given sample 100ml = g
SIGNIFICANCE: Potentiometric titration is very valuable at low titrant concentrations of the

range of 0.0001 M, at which the normal titrimetric methods fail. This method can be used with
much diluted solutions or with colored or turbid solutions, in which end point cannot be
seen with naked eye. This method can be used in reactions where there is no suitable
indicator and has many applications, i.e. it can be used for acid- base, redox, precipitation, or
complex titrations. There is no need to use any indicator here as such the cumbersome
process of selection of an indicator altogether is eliminated. Further, choice of an indicator for
titrations weak acids, weak bases and sometimes both, is difficult to be carried out and
potentiometric titrations are accurate alternative for such experiments. Since the end point is
located graphically, any errors creeping in the operation shall stand minimized. No
observation of end point is necessary and one single experiment is sufficient as there is no
visual location of the end point, as it is located graphically by extrapolation.
Model graph

and other samples given among your batch and below questions.
1. The indicator electrode

2. The reference electrode
3. Applications of potentiometry
4. Advantages potentiometry
5. Which is used to measure the potential?
6. Why the potentiometer knobs are adjusted to read mV and the room temperature
7. Why 4N sulphuric acid is added
8. What is potential, oxidation potential and reduction potential?

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Preparation of standard potassium dichromate solution (Primary standard)
OBSERVATIONS:
1 W1
2 W2
CALCULATIONS:

STEP-2: Determination of ferrous ammonium sulphate with standard potassium

dichromate solution by a potentiometric titration
Volume of the sample of ferrous ammonium sulphate taken = 10 ml

Temperature = oC
Pilot titration
S. No Volume of K2Cr2O7 added, ml Potential measured, mV
1
2
3
4
5
6
7
8
9
10

Accurate titration
S. No Volume of K2Cr2O7 added, ml Potential measured, mV ΔE ΔE/ΔV
1
2
3
4
5
6
7
8
9
11
12
13
14
15
16
17
CALCULATIONS:

RESULT: The amount of ferrous iron [Fe (II)] present in a given sample 100ml = g
STUDENT REPORT

DETERMINATION OF ACID NUMBER AND SAPONIFICATION NUMBER OF A

TEST SAMPLE OF LUBRICATING OIL
INTRODUCTION
Lubricating oils has to possess the following desirable properties.
 Available in suitable viscosities
 Inertness (resistance to deterioration of the lubricants)
 Corrosion protection (resistance to deterioration of sliding surfaces)
 Low cost
In all working machines, the surfaces of moving or sliding or rolling parts rub against each
other. Due to mutual rubbing of one part against another, a resistance is offered to their
movement. This resistance is known as friction.
Friction causes a lot of wear and tear of surfaces of moving parts; and a large amount of
energy is dissipated in the form of heat, thereby causing a loss in efficiency of machine and also,
moving parts get heated up, damaged or sometimes results in seizure.
Lubricant is a substances used to reduce the frictional force between moving or sliding
surfaces and the process of reducing the frictional resistance between two moving by the
introduction of lubricant is known as Lubrication.
Lubrication is simply the use of a material to improve the smoothness.
Lubricants are usually liquids (Lubricating oils) or semi solids (Greases)
Oils are esters of higher fatty acids. They may be saturated or unsaturated
The lubricating oils used for commercial purposes are tested for the following properties and
their quality is assessed by measuring them.
 Acid Number
 Saponification number
 Viscosity
 Cloud point and pour point
 Flash and fire point
 Oiliness
 Emulsification
 Volatility
 Decomposition stability
 Aniline point
 Specific gravity
 Ash content
The acid number is used as a guide to determine the quality and age of the lubricant and the
saponification number helps us to identify whether the lubricant under test contains vegetable
or animal oil.
ACID NUMNER
Determination of acidic constituents is more common and it is referred to as “Acid Number”.
Acid Number is defined as “the number of milligrams of KOH required to neutralize the free
acids in 1g of oil”.
Generally free acids are not present in the lubricants, unless refined in a faulty manner.
Usually lubricating oils are blended with vegetable or animal oils. These oils when exposed to
high temperatures or moisture conditions or under service conditions, easily oxidize,
consequently leading to formation of oxidized products, besides gum and sludge formation.
Acidic characters are caused by numerous chemical additives such as organic and
inorganic acids, esters, phenolic compounds, lactones, resins, salts of heavy metals, salts of
ammonia and other weak bases, acid salts of poly basic acids and additives such as inhibitors
and detergents.
The rate of change of acid number is more important. The rapid change is due to
excessive degradation at high temperatures, moisture conditions or under service conditions.
These oils – fats rancidify or oxidize, where the triglycerides are converted into fatty acids and
alcohols causing a change (increase) in the acid number.
Lubricating oil should possess acid number less than 0.1. For example compressor
and turbine oils usually run at 0.01 – 0.25 mg of KOH per gram of sample, gearbox and lube
oil at 0.1 – 10 mg of KOH per gram of sample and lubricant additives at 20 – 200 mg of KOH
per gram.
SIGNIFICANCE:
Fresh and used petroleum products contain acidic constituents as additives or as
degradation products formed during service conditions (viz. oxidation products). The relative
amounts of these materials are determined by simple acid – base titration.
 Acid number is used as a guide in the quality control of the lubricating oil formulations.
 This acid number is a measure of the amount of acidic substance presents in the oil–
under the test conditions.
 It is also sometimes used as a measure of lubricant degradation in service and also used
as an indicative to the age of the oil.

SAPONIFICATION NUMBER
It is defined as the number of milligrams of KOH required to saponify the fatty
material present in one gram of oil. Saponification means to hydrolyze a fat with an alkali to
form an alcohol and a salt of fatty acid.
Usually mineral oils do not saponify at all, but vegetable and animal oils do. This method
helps us to ascertain whether the oil under test is animal or vegetable oil or mineral oil or
a compounded oil containing mineral and vegetable oil.
SIGNIFICANCE AND USE (SAPONIFICATION NUMBER)

 Saponification value gives an estimation of non-fatty impurities present in an oil or fat
i.e. the extent of adulteration.
 Saponification value is used to distinguish between vegetable and animal oil, fatty and
mineral oils.
 Saponification value is used to identify given fatty oil, (Every fatty oil has its own
characteristic value).
 This is also used in setting the product specifications for lubricants and additives.

DETERMINATION OF ACID NUMBER OF AN OIL SAMPLE
AIM: To determine the acid number of given oil sample
APPARATUS REQUIRED: Conical flask, burette, water bath.
REAGENTS REQUIRED:
1) 0.1M Potassium hydroxide solution (KOH)

2) Oil sample
3) Ethyl alcohol
4) Phenolphthalein indicator
PROCEDURE:
STEP-1: Determination of acid value
A clean and dry 250 ml conical flask is taken and weighed accurately. 5 g of lubricating
oil is added and is again weighed. The difference in weights gives the weight of the oil sample
taken. 10 ml of ethyl alcohol (why ethanol) and 2-3 drops of phenolphthalein indicator is
added and titrated with 0.1M KOH until colorless solution turns to pale pink. The procedure is
repeated until concurrent readings are obtained.
Ethanol is a neutral solvent. The neutral solvents help you find the exact acidity from free
fatty acids present in a fat sample. If it is acidic it may consume more potassium hydroxide and
less if it is basic, leading to wrong estimation of fee fatty acid analysis.
Solution in the burette : 0.1M KOH

Solution in the conical flask : Oil sample under test + 10ml of Ethyl Alcohol + 2-3
drops of Phenolphthalein
Indicator used : Phenolphthalein
Color change at endpoint : Colorless to pink
Burette Readings Volume of KOH solution

S. No. Weight of oil sample taken in g
1
2
3
CALCULATIONS:

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Determination of acid value
Burette Readings Volume of KOH solution

S. No. Weight of oil sample taken in g
1 10
2 10
3 10
CALCULATIONS:
=
DETERMINATION OF SAPONIFICATION NUMBER OF AN OIL SAMPLE

AIM: To determine the saponification value of oil
CHEMICALS REQUIRED:
1. 0.5M Alcoholic potassium hydroxide solution

2. 0.5M hydrochloric acid solution
3. Phenolphthalein indicator
Saponification is a process that involves conversion of fat or oil into soap and alcohol by the
action of heat in the presence of aqueous alkali
Chemical reaction
PROCEDURE:
STEP-1: Determination of saponification number

A clean and dry 250 ml conical flask is taken and weighed accurately. 5 ml of lubricating
oil is added and is again weighed. The difference in weights gives the weight of the oil sample
taken. 25 ml of 0.5M alcoholic KOH is added and the contents in the flask are refluxed for 30
minutes. Now, to this, 2–3 drops of phenolphthalein indicator is added and is titrated with 0.5M
HCl solution until pale pink colored solution changes to colorless. The volume of HCl run down
is recorded.
A blank titration is performed by taking 0.5M KOH solution in a 250 ml conical flask. 2-3
drops of phenolphthalein indicator is added and then titrated with 0.5M HCl from the burette
until the pale pink colored solution changes to colorless.
OBSERVATIONS
Burette Readings Volume of HCl run down

S. No. Weight of oil sample taken, gm
Initial Final in ml
1
2
3
Solution in the burette : 0.5M HCl

Solution in the conical flask : Oil sample under test + 2 -3 drops of Phenolphthalein
Indicator used : Phenolphthalein

Color change at endpoint : Colorless to pink
CALCULATIONS:
Weight of the empty conical flask (W1 gm) =
Weight of the conical flask with oil (W2 gm) =
Weight of the oil taken (W1-W2 gm) =
Volume of 0.5 M HCl solution used by the blank (a ml) = 25 ml
Volume of 0.5 M HCl solution used by the oil (b ml) =
Saponification value of oil sample = X 3
=
RESULT: The Saponification value of the given oil sample is __________
References:
1. ASTM D974-14 - Standard test methods for determination of Acid or Base Number by
Color – Indicator titration.
2. ASTM D94-02 – Standard test methods for the Saponification Number of Petroleum
Products.
3. Engineering Chemistry, O . G. Palanna, 2nd edition, Mc Graw Hill Education series.
Some domestic oils with their saponification number chart
S. No Name of the oil Saponification number (Using KOH)
1 Almond Oil 190 – 200
2 Bees wax 60 –102
3 Castor oil 176–187
4 Cocoa Butter 192–200
5 Coconut oil 248–265
6 Corn oil 187–195
7 Cotton Seed Oil 189 –207
8 Olive oil 184 –196
9 Palm Oil 190 –209
10 Ground nut oil 187–196
11 Rice Bran Oil 187–190
12 Soya Bean Oil 187–195
13 Sunflower oil 189 –195
Source: http://www.certified-lye.com/lye-soap.html

and other samples given among your batch and answer the following questions
1. What is lubrication?
2. What is a lubricant?
3. What is oil?
4. Define acid number.
5. Why ethanol is used as a solvent in the determination of free fatty acids (acid
number)?
6. How one can analyze the quality of the oil using acid number?
7. What is saponification number?
8. What is the indicator used in the determination of saponification value?
9. What is the significance of saponification number?
10. Is saponification number same for all oils/fats?

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Determination of saponification number
OBSERVATIONS
Burette Readings Volume of HCl run down

S. No. Weight of oil sample taken, mg
Initial Final in ml
1 10.0
2 10.0
3 10.0
CALCULATIONS:

Saponification value of oil sample = X3
=
RESULT: The Saponification value of the given oil sample is __________
STUDENT REPORT:

PREPARATION OF THIOKOL RUBBER
OBJECTIVES: By doing this lab the student will able to

 Demonstrate the synthesis of a polysulfide rubber
 Calculate the weight %-yield
 Determine the density of product,
 Determine the melting point of product
 Determine the solubility of product in various solvents,
 Write the repeat unit of the product,
 Describe the end product uses of this polymer
THEORY: Thiokol rubber (poly sulphide rubber) is an elastomer which is obtained by co-
polymerization of 1,2-dichloroethane and sodium tetra sulphide. This rubber cannot undergo
vulcanization and it cannot form a hard rubber. It possesses extremely good resistance to
mineral oils, fuels, oxygen, solvents, ozone, and sunlight and possesses low abrasion resistance
PROPERTIES: The properties of the polymers depend on the length of the aliphatic groups and
the number of sulphur atoms present in it. The polymer behaves like elastomer when four
sulphur atoms, or greater, are present per monomer; lower amounts of sulfur give a
hard, brittle resin. Some of the important properties are:
(i) Thiokol is resistant to the action of oxygen and ozone.

(ii) It is also resistant to the action of petrol lubricants and organic solvents.
(iii) Thiokols outstanding resistance to swelling by organic solvents but benzene and its
derivatives cause some swelling.
(iv) Thiokol films are impermeable to gases to a large extent.
(v) But Thiokol has poor heat resistance and low tensile strength. The odour of thiokol
is very bad. It tends to lose its shape under continuous pressure.
USES
(i) Thiokol mixed with oxidizing agents is used as a solid fuel in rocket engine.
(ii) It is used to engine gaskets and other such products that come into contact with oil.
(iii) Thiokol’s are used for hoses and tank lining for the handling and storage of oils and
solvents.

Aim: To prepare the sample of thiokol rubber by co-polymerization.

Apparatus required: 100 ml Breaker, 100 ml Measuring cylinder, glass rod.
Reagents required: 1,2-Dichloro ethane (ethylene dichloride), Sodium hydroxide, Powdered
sulphur.
Procedure: Dissolve 2g of NaOH in 50-60 ml of warm water taken in a 100 ml beaker. Boil the
solution and add 4g of sulfur powder in lots with constant stirring till the yellow solution turns
deep red color. Cool it to 60-70 oC and add 10 ml of 1,2-dichloroethane with stirring. Stir the
solution for another 20 min till the rubber polymer gets separated out as a lump. Eliminate the
liquid from the beaker to obtain thiokol rubber. Wash it water under the tap and dry the
sample.
Record the physical properties of the product
Find the dry mass of the product and determine the %-yield
Labeled 5 test tubes: acetone, conc. nitric acid, conc. sulfuric acid, 6M sodium hydroxide, and
methyl alcohol. Place 1 mL of the appropriate solvent into each test tube. Add a small amount of
your polymer product. Shake gently to mix. Record your observations
RESULT: The yield of thiokol rubber obtained is ……………………gm.
Turn in the remainder of the sample to your instructor along with your results and the answers
to the questions.
STUDENT REPORT:
1. Will this material bounce? Do its elastic properties resemble like rubber band?
2. Does the polymer have any objectionable features?
3. There are two types of Thiokol produced. Identify and describe these two types Which type
did you produced?
4. What is the repeated unit of your polymer product?
5. What can be said about the solubility of this polymer?
6. Based on your observations (and research), what end product applications would this
material fit?

7. What is copolymerization?
8. What is vulcanization?
9. Why thiokol rubber does not undergo vulcanization?
10. Give the properties of thiokol rubber?
11. What is Thiokol rubber also called as?
12. Give the reaction for synthesis of thiokol rubber?
13. Industrial and domestic applications of Thiokol rubber
References:
1. Budavari, Susan, Ed. The Merck Index, Twelfth Edition; Merck Research
Laboratories:Whitehouse Station, 1996; p. 1593.
2. Shakhashiri, B.Z. Chemical Demonstrations, Volume 1; The University of Wisconsin
Press:Madison, 1983; pp. 245-246

AIM:
PRINICIPLE:
PROCEDURE:
Chemical reaction:
Synthesis of Thiokol rubber
Procedure:
RESULT: The yield of thiokol rubber obtained is ……………………gm.
STUDENT REPORT:
Labeled 5 test tubes: acetone, conc. nitric acid, conc. sulfuric acid, 6M sodium hydroxide, and
methyl alcohol. Place 1 mL of the appropriate solvent into each test tube. Add a small amount of
your polymer product. Shake gently to mix. Record your observations do the above tests write
your observations in student report along with the answers to the questions.


DETERMINATION OF VISCOSITY OF POLYMER SOLUTION USING SURVISMETER
OBJECTIVES:
 To measure viscosity and surface tension of a polymer solution.
AIM: Determination of viscosity of a polymer solution using Survismeter.
APPARATUS AND CHEMICALS REQUIRED: Man Singh Survismeter, polymer

solution, stop watch
INTRODUCTION
Currently a survismeter was fabricated based on 2-in-1 technique for surface
tension and viscosity data measurement. As the innovations keep going on for
betterment in experimental techniques for reducing the consumptions of the time,
efforts and materials used in. Survismeter resolve hurdles in obtaining such data for
biological solutions (very expensive and get spoiled on exposure to atmosphere) for the
study of the atherosclerosis with minimum operational steps.
MATERIAL AND METHODS
The triple distilled water was used to determine the survismeter constant at
desired temperatures. The methanol, ethanol, glycerol, ethyl acetate and n-hexane each
of analytical reagent (AR, Merck, India) grade were distilled and used for the
measurements. The tetrahydrofuran (THF), dimethylformamide (DMF),
dimethylsulfoxide (DMSO) and acetronitrile (AR, Merck, India) are distilled in the lab; for
purity, their solution were prepared w/w, in ultra-pure water. The deionized water was
triply distilled in KMnO4 and KOH (AR, Merck, India) for removing dissolved CO2 and
boiled off for further removal of the dissolved gases, its conductivity was maintained to be
1 ×10-6 V-1 cm-1.
Handling and operation
The survismeters were washed very cautiously with freshly prepared chromic acid
followed with ordinary and distilled water, the final was made with aqueous acetone. It
was dried in oven for 24 h at 120 oC. The reference liquid and solutions were
separately filled in the bulb number 8 of both the survismeters with utmost care; sucking
of the liquids from bulb number 8 to the bulbs 7, 6 and 5 for flow times and bulbs number
7 and 9 for drop numbers were made very cautiously. The attention was paid to avoid the
formation of the air bubble in the liquid at any step during sucking operation as it disrupts
the smooth flow. The sucking was made with 100 × 10-3 dm3 capacity syringe connecting
the needle of the syringe and the respective upper end of the survismeter limb.

Handling
Usually, survismeter are calibrated with any standard solution, however ultra-pure
water is preferred, and their calibration constants are known as survismeter constants
and are found in the range of 0.1 m2 s-2. Unit numbers 4 and 2 are calibrated separately
for viscosity and surface tension measurements, respectively.
Measurement of Viscosity
About 15 × 10-3 dm3 of solution of known viscosity value is taken in the 8th bulb
through 3rd limb keeping the other ends of the limbs open for pressure control. The
survismeter was mounted on the stainless steel stand and kept in thermostat at desired a
temperature with F0.018C control, read with Beckman thermometer. The solution was
sucked upward from bulb number 8 through syringe. With needle syringe, one end of
Teflon/PVC tube is attached and another end is attached to a movable stopper with hole.
The stopper is fixed in the socket of the 4th limb and, pulling out the plunger, sucks up
the solution to bulb number 5; once filled up, the stopper is removed. During sucking of
the solution, the socket of limb 3 is kept open, while that of the 2nd and 1st are blocked
with stoppers; for down flow of solution, the syringe and stopper of limb number 1 are
taken back. The flow time between upper and lower marks of bulb number 6 is counted. The
flow times were recorded for four to five times to ensure the reproducibility in values;
similarly, the time data are collected for solutions.
After taking the sample in the reservoir bulb, close the pressure limb and the surface
tension limb with the operational stoppers. Place the glass adaptor of the syringe pump over
the viscosity limb and close it air tightly. Now pull the plunger of the syringe pump slowly and
you will see the sample getting into the control pressure unit. Continue pulling the plunger and
you will observe that the sample starts to fill into the viscosity unit without going to the surface
tension limb. Pulling the plunger slowly helps in maintaining homogeneous pressure inside the
Survismeter unit and maintains uniform pressure distribution among the constituents of the
liquid sample. The viscosity limb contains two bulbs: the lower bulb is the functional bulb and
the upper one is the buffer bulb. Fill the viscosity limb until the buffer bulb is half filled. The role
of the buffer bulb is to give the user an extra time to start the analysis. This also gives
the constituents of the sample to achieve proper orientation, since extra pressure used to lift
the sample in the viscosity limb increased the overall kinetic energy of the system. This matters
a lot when the sample is protein or surfactant solution and this buffer zone helps the
constituents to attain the same energy state with ordered orientation as they were, before the
start of the analysis. After the attainment of equilibrium, open the glass adaptor of the syringe
from the viscosity limb. There will be no formation of viscous flow seen in the control pressure
unit till now. To start the viscous flow formation, open the operational stopper from the
pressure limb. The viscous flow formation is continuous because the flow of the sample is not
stopped in the midway and the sample solution continuously flows due to gravity. When the
sample solution cross the upper mark located between the functional bulb and the
buffer bulb of the viscosity limb, start the digital timer and stop the timer once the sample
crosses the lower mark located below the functional bulb and record the viscous flow time
taken between the two marks. Repeat the experiment again without taking out the sample from
the reservoir bulb to find out the repeatability associated with the experiment. For viscosity
calculation, in addition to the viscous flow time recorded for the sample solution, the viscous
flow time record between the two marks of the viscosity limb for a reference liquid is also
required at the experimental temperature. The solvent in which the sample solution is
prepared is generally selected as the reference liquid. For the viscosity limb, at a given
temperature, the viscous flow time for a particular reference liquid will always be constant and
hence with every sample there is no need to find the viscous flow time for the reference liquid,
as it can the taken from previous experiment at that temperature. For example, suppose the
experimental temperature is 25 degree Celsius and the sample is 0.1 % weight by weight
aqueous solution of any water soluble protein. The reference liquid will be water. The viscous
flow time for water can be taken from any previous experiments where the viscous flow time
was recorded for water at 25 degree Celsius. Now, to calculate the viscosity of the sample, the
viscous flow time of the sample and the reference liquid are now used in the formula as:

Fig. 1. The schematic diagram of survismeter

type I
,
Test your understanding
1. Define viscosity. Give its units.

2. Give the significance of viscosity in engineering
3. Write the effect of temperature on viscosity
4. What is the importance of a survismeter?
5. Can you compare your result with standard values? Prepare a chart of standard viscosity
values of different polymer solutions.

AIM:
PRINICIPLE:
PROCEDURE: Determination of viscosity of a polymer solution by using survismeter
FORMULA:
CALCULATIONS:

STUDENT REPORT: Answer the question given in test your understanding

ADSORPTION
OBJECTIVES:
 To demonstrate the adsorption phenomena.
 To show students how to determine the adsorption parameters.
THEORY
Adsorption is a process that occurs when a gas or liquid solute accumulates on the
surface of a solid or a liquid (adsorbent), forming a molecular or atomic film (adsorbate). It is
different from absorption, in which a substance diffuses into a liquid or solid to form a solution
APPLICATIONS
Its first application was probably the use of bone ashes to remove colour from syrups or alcohol.
Today, adsorbent materials are widely used at water-treatment (softening of hard water)
plants to remove especially organic impurities and chlorine as purification treatment.
In glass masks: All gas masks are devices containing suitable adsorbent so that the poisonous
gases present in the atmosphere are preferentially adsorbed and the air for breathing is
purified.
In catalysis: The gaseous reactants are adsorbed on the surface of the solid catalyst. As a result,
the concentration of the reactants increases on the surface and hence the rate of reaction
increases.
In removing moisture from air: In the storage of delicate instruments
which may be harmed by contact with the moist air are kept out of contact with moisture using
silica gel.
There are two types of adsorptions
Physisorption or physical adsorption is a type of adsorption in which the adsorbate adheres
to the surface only through Van der Waals (weak intermolecular) interactions.
Chemisorption is a type of adsorption whereby a molecule adheres to a surface through the
formation of a chemical bond, as opposed to the Van der Waals forces which cause
physisorption.
Adsorption is usually described through adsorption isotherms, that is, functions which
connect the amount of adsorbate on the adsorbent, with its pressure (if gas) or concentration
(if liquid).
Several models describing process of adsorption, namely
Freundlich isotherm, (an isotherm for liquids adsorbed on solids, single layer)
Langmuir isotherm, (an isotherm for gases adsorbed on solids, single layer)
BET isotherm, (adsorption of vapors on porous solids at high vapor pressures a multi-layer
adsorption)
ADSORPTION OF ACETIC ACID ON CHARCOAL

AIM: To study the adsorption of acetic and determine the adsorption isotherm of acetic acid by
charcoal.
CHEMICALS: Activated charcoal, glacial acetic acid, 0.1M NaOH and phenolphthalein indicator
APPARATUS: 5-6 stoppered reagent bottle, thermostat (or a large trough), burette, conical
flask, filter paper and pippete and measuring flasks.
PRINCIPLE:
1. The Freundlich isotherm may be written as;
x/m = k Ce a
(OR)
ln(x/m) = lnk + alnCe
Therefore ln(x/m) Vs lnCe is a straight line
2. Langmuir isotherm may be written as
x/m = k1k2/(1+k1 Ce).
Ce/(x/m) = 1/(k1k2) + Ce/k2
Where x is the mass of the solute adsorbed on mass ‘m’ of the adsorbent and Ce is the
equilibrium concentration of the adsorbate in the solution.
Hence, a plot of Ce/(x/m) Vs Ce will be a straight line from which the constants k1 and k2 can be
calculated.
PROCEDURE:
0.05M Oxalic acid primary solution is prepared by dissolving 0.630g of Oxalic acid solid
in 100 ml distilled water.
OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:
W1 - W2
GMW of Oxalic acid
x 1000
100


Take 10 ml of oxalic acid solution into a conical flask, add 20 ml of distilled water and a
drop of phenolphthalein indicator then titrate against sodium hydroxide solution taken in a
burette until color of the solution changes from colorless to pale pink. Repeat the titration for
OBSERVATIONS:
S. No Volume of oxalic acid taken in Burette reading Volume of NaOH

ml Initial Final run down in ml
1
2
3
CALCULATIONS:
Concentration of the sodium hydroxide solution = M
STEP-3:
(i) Weigh out accurately about 2g finely ground activated charcoal in each of the thoroughly
cleaned and dried bottles, numbered as 1 to 6.
(ii) Prepare 250 ml approximately 0.5M acetic acid solution by taking 7.8 ml of glacial acetic and
diluting it to 250 ml in a volumetric flask.
(iii) By means of burettes, add 50, 40, 30, 20, 10 and 5ml of the acid solution and 0, 10, 20, 30,
40 and 45 ml of distilled water in bottle Nos. 1, 2, 3, 4, 5 and 6 respectively. Shake the bottles
vigorously and leave them in a thermostat at the desired temperature for about one hour.
(v) Filter the solutions of each of the bottles through different small dry filter papers, and
collect the filtrates in properly labeled flasks. Reject first 5-10 ml (why) of the filtrate in each
case.

(vi) Take an aliquot of each filtrate (5 ml from the first and second, 10 ml from third and fourth,
and 20 ml from fifth and sixth bottles), and titrate with standardized NaOH solution. Calculate
the equilibrium concentration (Ce) of the acid in each bottle.
(vii) Tabulate your observations and results as in previous experiment.
OBSERVATIONS:
S. No Volume of filtrate taken in ml Burette reading Volume of NaOH

1 5 ml
2 5 ml
3 10 ml
4 10 ml
5 20 ml
6 20 ml
CALCULATIONS:
The equilibrium concentration (Ce) and amount of acetic acid adsorbed (x) of the acid in each
bottle is given by the formula
V1 = Volume of acetic acid taken = V2 = Volume of NaOH rundown =

M1 = Molarity of acetic acid = ? M2 = Molarity of NaOH =
(After adsorption)
n1 = No. of moles of acetic acid = 1 n2 = No. of moles of NaOH = 1
Where M1 is referred as equilibrium concentration (Ce)
Bottle Vol. Vol. of Eq. Amount Weight of log log

No. of distilled Con. of acetic the Ce
acetic water (Ce) acid adsorbent
acid ml molar adsorbed (m) in g
sol. (x) in mg
1 50 0
2 40 10

3 30 20
4 20 30
5 10 40
6 6 05
Initial concentration of acetic acid (C0) = 0.5M
The weight of acetic acid adsorbed (x) per unit mass of charcoal can be computed as
x = (C0-Ce) MV.
Where, C0= initial concentration in mol/lt. of acetic acid before adsorption

Ce = equilibrium concentration in mol/lt. of acetic acid after adsorption
M = molecular weight of acetic acid
V = volume in liters of solution.
Ce and x are calculated for each sample and are tabulated.
m = weight of the adsorbent (2 g)
GRAPHS: Plot two graphs
1. A graph may be plotted against log and logCe to test the Freundlich adsorption
isotherm and logk values are calculated from the straight-line plot as slope = a, and
intercept = lnk.
2. A graph may be plotted between and Ce. A straight line indicates the validity of
Langmuir adsorption isotherm. k1 and k2 are obtained from the graphs as;
Slope = 1/k1 and intercept = 1/(k1k2).
The Freundlich adsorption isotherm is,

ln(x/m) = lnk + lnCe.
From the graph of ln(x/m) Vs lnCe
Slope, a =
Intercept, k =
The Langmuir adsorption isotherm is,
Ce/(x/m) = 1/(k1k2) + Ce/k2
From the graph of Ce/(x/m) Vs Ce,
Slope, k1 =
Y-intercept, k2 =

RESULT: The adsorption of acetic acid on activated charcoal is studied and the constants of the
equations of Langmuir and Freundlich isotherms are estimated and are:
Freundlich isotherm:
a = -------
k = -------
Langmuir isotherm:
k1 = -------
k2 = -------
Reference:
1. Experiments in physical chemistry by Ghosh, Bharati Bhawan
2. Practical Engineering Chemistry by K. Mukkanti, etal, B.S. Publications,Hyderabad.
3. Instrumental methods of chemical analysis, Chatwal, Anand, Himalaya Publications.
4. Inorganic quantitative analysis, Vogel
STUDENT REPORT:
1. Comment on the result (which isotherm is suitable for the above experiment)
2. Applications of adsorption
3. During the filtration first few ml of filtrate were rejected why?
4. What is % acetic acid adsorbed by the charcoal in each case

AIM:
PRINICIPLE:
PROCEDURE:

OBSERVATIONS:

1 W1
2 W2
CALCULATIONS:

OBSERVATIONS:
S. No Volume of oxalic acid taken in Burette reading Volume of NaOH

ml Initial Final run down in ml
1
2
3
CALCULATIONS:
Concentration of the sodium hydroxide solution = M
STEP-3:

OBSERVATIONS:
S. No Volume of filtrate taken in ml Burette reading Volume of NaOH

1 5 ml
2 5 ml
3 10 ml
4 10 ml
5 20 ml
6 20 ml
CALCULATIONS:
Bottle Vol. Vol. of Eq. Amount Weight of log log

No. of distilled Con. of acetic the Ce
acetic water (Ce) acid adsorbent
acid ml molar adsorbed (m) in g
sol. (x) in mg
1 50 0
2 40 10
3 30 20
4 20 30
5 10 40
6 6 05

GRAPHS: Plot two graphs
RESULT: The adsorption of acetic acid on activated charcoal is studied and the constants of the
equations of Langmuir and Freundlich isotherms are estimated and are:
Freundlich isotherm:
a = -------
k = -------
Langmuir isotherm:
k1 = -------
k2 = -------
STUDENT REPORT:

Nanomaterials
Definition: The nanochemistry is explained as the study of the synthesis of materials and
properties of materials in the range of nanoscale.
Therefore, 1nm = 10-7 cm (Or) 1nm = 10-9 m
Note: Surface of a material increases with decrease in the particle size
Classification of nanomaterials:
The types of nanomaterials are explained in the below figure:
1. One dimensional nanomaterial: This type of material has one dimension arrangement of
atoms in the nanoscale range. The examples for one dimension nanomaterial are surface
coatings and thin films.
2. Two-dimensional nanomaterial: This type of material has two dimension arrangements

of atoms in the nanoscale range. The examples for two dimension nanomaterial are
biopolymers, nanotubes, and nanowires.
3. Three-dimensional nanomaterial: This type of material has three dimension

arrangements of atoms in the nanoscale range. The examples for three dimension
nanomaterial are fullerenes.
The significance of nanoscale:
It is observed that the properties are distinct on the nanoscale from those at the larger scale.
The properties like quantum, mechanical and thermodynamical become vital at the nano level
and these are not seen at the macroscopic level. The nanoscience is based on the fact that along
with the physical dimensions of the materials the properties of the materials also change. The
transformation in the properties of the materials in these confined spaces is because of the

changes in the electronic structure of the materials. The properties of the materials are distinct
at the nano level due to the following two reasons:
 Increased surface area
 Quantum confinement effect
Properties of nanomaterials:
The properties of the nanomaterials depend on the crystal structure and size and few
properties of the nanomaterials are explained below:
1. Physical properties: In the nanoscale range, surface area to volume enhances. This
enhancement transforms the surface pressure and results in a change in the interatomic
spacing. This feature is explained in the below figure:
2. Mechanical properties: The nanomaterials have the application on both the low
temperatures and high temperatures. So, the mechanical properties of the
nanomaterials are studied at low temperatures and also at the high temperatures.
3. Magnetic properties: The magnetic behavior of the nanomaterials is size dependent. In

the tiny ferromagnetic particles, the magnetic properties are distinct from that of the
very large material. In the range of nanoscale, magnetic material has a single magnetic
domain. As an outcome, the remanent magnetization and coercive field exhibit a strong
dependence on the size of a particle.
4. Optical properties: If the particles of a semiconductor are made tiny then the effects of
quantum come into play which limits the energies at which the electrons and holes can
exist in the particles.
5. Thermal properties: The nanocrystalline materials are expected to have a low

conductivity of thermal when compared with the conventional materials.
6. Surface area: Nanomaterials have large surface area and the nanocrystal’s surface area
is inversely proportional to the crystal’s size.
7. Catalytic activity: Nanomaterials can be availed as effective catalysts in many reactions.
8. Electrical properties: Nanomaterials exhibit electrical properties in between

semiconductors and metals depending on the chirality of the molecules and diameter of
the molecules.
9. Semiconductors: Most of the nanomaterials play the role of a semiconductor and these
nanowires which have the feature of being a semiconductor are used in making distinct
components.
10. Superconductors: Few nanomaterials behave as the superconductors.

Applications of nanomaterials:
The nanomaterials have its applications in distinct fields and few of them are as follows:
 Material technology
 Information technology
 Biomedicals
 Energy storage
 The carbon nanotubes and nanowires are utilized in making many components
Synthesis of nanomaterials:
The processes used for the synthesis of nanomaterials are explained in the below figure:
Few methods of a top-down process are explained below:
 Ball milling
 Plasma arching
 Laser sputtering
 Vapour destination
Few methods of a bottom-up process are explained below:
 Sol-gel
 Colloidal
 Electrodeposition
 Solution phase reductions

PREPARATION OF ZINC FERRITE/MAGNESIUM FERRITE NANO PARTICLES

AIM: To synthesize zinc/magnesium ferrite nano particles by using sol-gel method.
MATERIALS: Magnesium nitrate [Mg(NO3)2. 6H2O], Zn(NO3)2. 6H2O Ferric nitrate

[Fe(NO3)3. 9H2O], PVA(Polyvinyl alcohol), PEG(poly ethylene glycol) and Citric
acid [C6H8O7]
PRINCIPLE: Zn(NO3)2 . 6H2O + 2 Fe(NO3)2. 9 H2O → ZnFeO4 + Volatiles (H2O + CO2 + NO2)
PROCEDURE:
STEP-1: Calculation of the molecular weight of the required product
Ex: ZnFe2O4 (Zinc ferrite)
Zn → 65.380 x 1 ( No. of atoms in the formula) = 65.38

Fe → 55.840 x 2 = 111.68
O → 15.999 x 4 = 63.996
241.056
STEP-2: Calculation of the amount of required metal nitrate of the respective metal
ferrite for the desired quantity of metal ferrite
Where 10 is the desired quantity of metal ferrite
Example: Amount of zinc nitrate required for the preparation 10 g of ZnFe2O4 (Zinc ferrite)
[Zinc nitrate hexahydrate (Zn(NO3)2.6H2O)= 297.4815]
= 8.1046 grams
STEP-3: Combustion
Dissolve metal nitrates individually in slightly excess volume of solvent than their
respective amounts and stir these solutions for 30 minutes for the complete dissolution then
add PVA (poly vinyl alcohol) equal amount to metal nitrate, and heat the mixture to 50 oC until

it dissolves then mix the solutions and continue the heating at 65 oC for 15-30 minutes and 135
oC for further 45 minutes.
STUDENT REPORT: Write the report along with answers to the following
1. What is nano material

2. How the nano material are classified
3. Mention any two properties of nano materials
4. Mention any two applications of nano materials
5. Mention any two properties of metal ferrite nanomaterials
6. Mention any two applications of metal ferrite nano materials
7. How can you ascertain that the formed product is a nano material
8. Compare the obtained % of yield with others, write the deviation if any
Literature survey
Collect literature on zinc ferrite nano particles and write repot on the
synthesis(preparation), properties and applications of zinc ferrite nano particles

AIM:
PRINICIPLE:
PROCEDURE:
STEP-1: Calculation of the molecular weight of the required product
STEP-2: Calculation of the amount of required metal nitrate of the respective metal
ferrite for the desired quantity of metal ferrite
STEP-3: Combustion

STUDENT REPORT

Project Based Learning

At the end of the engineering chemistry lab every student has to perform one
project based lab, taking a real-world problem and highlight the interdisciplinary nature
of chemistry with little relevance to our everyday life, by using the learning experiences,
principles, techniques and safety precautions which have been understood and carried
out during his/her course work.
The goals of the project based lab were threefold:

(1) To increase students’ interest in science early in their academic careers, particularly
engineering students
(2) To raise students’ awareness in finding applications for what they have learned to
apply in various situations.
(3) To engender a more sophisticated view of science among engineering students.
To achieve these goals, five modules have been developed covering all the topics of
Engineering Chemistry course to influence students early in their careers in implementing this
project based approach. Every group (max 6 students) has to select one project from each
module. Each module consists of a set of projects exploring the same concepts of various
aspects of laboratory.
Module1 1. Does tooth paste protect your teeth?

2. What is the mass of CaCO3 in Egg Shells?
3. Tap into quality of water
4. Water is Life
Module2 1.Facts and Fallacies of Milk
2. Study the concentration of sulphuric acid in various lead acid batteries used in
automobiles and the effect of concentration on voltage.
3. Metal corrosion as a natural clock
4. What are the concentrations of phosphate ions in soft drinks?
Module 3 1. How much NaHCO3 is in one effervescent tablet?
2. Determination of concentration of acids present (if any) in soft drinks- an
Investigation
3. How polymers are essential for products like diapers (literature survey)
4. Collect literature on polymers(any one) and write repot on the
synthesis(preparation), properties and its applications
Module 4 1. Vinegar and its significance in our kitchen
2. Removal of dyes from waste water using adsorbent- a case study
3. Have you checked Ca/Mg ratio in your soil samples?
4. Adsorption of Ca2+ and Mg2+ from waste water(domestic/industrial) over corn
cobs
Module 5 1. Study on the extent of adulteration of domestic oils with reference to
saponification value

2. Explore the content of ferric iron in cement

3. Explore the content of calcium oxide in cement
4. Do you know the parameters of cooking oil?
5. Collect literature on zinc ferrite nano particles and write repot on the
Module 1
1. Does tooth paste protect your teeth?
Carry out experiments to compare at least three different brands of toothpaste. You may use
chicken eggshells to substitute for human teeth.
Concept: Volumetric analysis- Acid-base Titration
2. What is the mass of CaCO3 in Egg Shells?
Determine the percentage by mass of calcium carbonate in hen eggshells
3. Tap into quality of water
Analyse the water samples in different areas in Vizianagram to assess the quality of water
especially Hardness of water samples. Your task is to plan to collect water samples and
estimate the above contents by applying good methods.
Concept: Volumetric analysis- Complexometric titration.
4. Water is Life
Analyze the water samples in different areas in Vizianagram to assess the quality of water
especially DO, COD, alkalinity, acidity and CO2. Your task is to plan to collect water samples
and estimate the above contents by applying good methods.
Module 2
1. Facts and Fallacies of Milk
Assess the contents of the calcium and magnesium in milk.
Concept: Volumetric analysis- Complexometric titration.
2. Study the concentration of sulphuric acid in various lead acid batteries used in
automobiles and the effect of concentration on voltage.
Concept: Volumetric analysis- Redox titration
3. Metal corrosion as a natural clock
Check the quality of material in terms of corrosion. Analyze the % of ferric iron in material
Concept: Volumetric analysis- Redox titration.
4. What are the concentrations of phosphate ions in soft drinks?
Use pH meter or acid-base indicators
Module 3
1. How much NaHCO3 is in one effervescent tablet?
Carry out an investigation to determine the percent by mass of sodium bicarbonate in
Effervescent tablets.

2. Determination of concentration of acids present (if any) in soft drinks- an

Investigation
Use pH meter or acid-base indicators
3. How polymers are essential for products like diapers
Collect the literature about the polymer which are used in the diapers preparation and write
comprehensive report on its preparation, properties and applications
Concept: synthesis of polymers
4. Collect literature on polymers(any one) and write repot on the synthesis
(preparation), properties and its applications
Literature survey
Concept: synthesis of polymers
Module 4
1. Vinegar and its significance in our kitchen
As a engineer you suggest proper method and assess the amount of vinegar
Concept: Adsorption-adsorption of acetic acid on charcoal
2. Removal of dyes from waste water using adsorbent- a case study
Concept: Adsorption of dyes by using charcoal form waste water
3. Have you checked Ca/Mg ratio in your soil samples?
Analyse the soil samples in different agricultural fields in and around areas to assess the
quality of soil especially Ca/Mg ratio. Collect soil samples and estimate the above
parameters by applying good methods.
Concept: Volumetric analysis- Complexometric titration
4. Adsorption of Ca2+ and Mg2+ from waste water(domestic/industrial) over corn cobs
Concept: Volumetric analysis- complexometric Titration
Module 5
1. Study on the extent of adulteration of domestic oils with reference to saponification
value
Analyze the saponification value of various domestic oils and compare with their standard
values
Concept: Saponification value
2. Explore the content of ferric iron in cement
Assess the percentage of ferric iron in various grads of cements
Concept: Volumetric analysis- Spectrophotometry
3. Explore the content of calcium oxide in cement
Assess the percentage of calcium oxide in various grads of cements
Concept: Volumetric analysis- Complexometric titration
4. Do you know the parameters of cooking oil?
Assess the quality of oil samples in terms of saponification and acid value. So collect
different oil samples suggest proper method and assess the above parameters.
Concept: acid value end saponification number

5. Collect literature on zinc ferrite nano particles and write repot on the
Note: Apart from the above mentioned concept for each PBL the following concepts are also
explored.
 pH Meter
 Conductivity Meter
 Potentiometer

2020 21 Ec Lab Manual Student Version

Uploaded by

Copyright:

Available Formats

2020 21 Ec Lab Manual Student Version

Uploaded by

Document Information

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

2020 21 Ec Lab Manual Student Version

Uploaded by

Copyright:

Available Formats

ENGINEERING CHEMISTRY LABORATORY

MANUAL (A2 Regulation)

Maharaja Vijayaram Gajapathi Raj College of Engineering (Autonomous)

S. No Experiment Date Signature Grade

M V G R College of Engineering (Autonomous), Vizianagaram. Page 1

S. No. CONTENTS Page. No.

M V G R College of Engineering (Autonomous), Vizianagaram. Page 2

INTRODUCTION TO CHEMISTRY LAB

Quantitative chemical analysis is further divided into two types:

error. Volumetric analysis, which involves the accurate measurements of volume of

ESSENTIAL CONDITIONS FOR ACCURATE TITRIMETRY

TERMS USED IN VOLUMETRIC ANALYSIS

M V G R College of Engineering (Autonomous), Vizianagaram. Page 4

M V G R College of Engineering (Autonomous), Vizianagaram. Page 5

k. MEASURING CYLIDER OR JAR: This is a graduated cylindrical glass vessel to draw

M V G R College of Engineering (Autonomous), Vizianagaram. Page 6

STANDARD SOLUTION: A solution of known strength is called as standard solution. It is

PRIMARY STANDARD SUBSTANCE: A Primary Standard Substance should satisfy the

In practice an ideal primary standard is difficult to be obtained and a compromise in the

PRIMARY STANDARD SUBSTANCES COMMONLY EMPLOYED:

M V G R College of Engineering (Autonomous), Vizianagaram. Page 7

In precipitation titrations: Sodium chloride, Potassium chloride, etc.

In oxidation-reduction titrations: Potassium dichromate, sodium oxalate, arsenium oxide etc.

In Complexometric titrations: Zinc sulphate solution

SECONDARY STANDARD SUBSTANCES: Those substances which do not loose water of

CLASSIFICATION OF REACTIONS IN VOLUMETRIC ANALYSIS:

1. Neutralization reactions (acidimetry and alkalimetry): These reactions are based on

Concentration of a standard solution is generally expressed in following chemical units.

NORMALITY: The normality of a solution is defined as the number of gram – equivalents of

M V G R College of Engineering (Autonomous), Vizianagaram. Page 8

Where w is the number of grams of solute and W is no of grams of solvent.

1. When student entering into in a laboratory you must always:

M V G R College of Engineering (Autonomous), Vizianagaram. Page 9

M V G R College of Engineering (Autonomous), Vizianagaram. Page 10

M V G R College of Engineering (Autonomous), Vizianagaram. Page 11

INSTRUCTIONS TO THE STUDENTS

M V G R College of Engineering (Autonomous), Vizianagaram. Page 12

INSTRUCTIONS TO WRITE LAB RECORD

10. An experiment is deemed to be complete when it is satisfactorily performed and the

M V G R College of Engineering (Autonomous), Vizianagaram. Page 13

UNDERTAKING BY THE STUDENT

I …………………………………………………………. here by undertake to state that, I have

M V G R College of Engineering (Autonomous), Vizianagaram. Page 14

 Determination of strength of HCl

STEP-1: Preparation of 0.05 M sodium carbonate solution

S. No Contents in the pan grams milligrams Total weight(g)

M V G R College of Engineering (Autonomous), Vizianagaram. Page 15

STEP-2: Determination of the concentration of the given hydrochloric acid solution

S. No Volume of sodium carbonate Burette reading Volume of HCl run down in ml

V1 = Volume of HCl consumed =

Concentration of the supplied HCl solution = M

The determination of hydrochloric acid or principle of acidimetry or alkalimetry

M V G R College of Engineering (Autonomous), Vizianagaram. Page 16

Note: Lab concentration of HCl in a fresh bottle is 11.3 molar

Lab concentration of HCl = 10 x Specific gravity x % purity of HCl/GMW of HCl

STUDENT REPORT : Write the report by answering the below questions

1. Why HCl is titrated with standard sodium carbonate

M V G R College of Engineering (Autonomous), Vizianagaram. Page 17

EXPERIMENT NO. 1 Date:

Name of the experiment